9600 Operator Manual Rev.D

®
AUTOPORE V SERIES
MERCURY INTRUSION POROSIMETER
OPERATOR MANUAL
962-42800-01
Nov 2017
(Rev D)
TRADEMARKS
Alconox is a registered trademark of the Alconox Company.
AutoPore is a registered trademark of Micromeritics Instrument Corporation.
Micromeritics is a registered trademark of Micromeritics Instrument Corporation.
Microsoft, Windows, and Windows 7 are registered trademarks of Microsoft Corporation.
Python is a registered trademark of Python Software Foundation.
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This application may contain a binary form of the Info-ZIP tool to create .zip files. That source code is provided under
the following license:
This software is provided "as is," without warranty of any kind, express or implied. In no event shall Info-ZIP or its
contributors be held liable for any direct, indirect, incidental, special or consequential damages arising out of the
use of or inability to use this software.
Permission is granted to anyone to use this software for any purpose, including commercial applications, and to
alter it and redistribute it freely, subject to the following restrictions:
1. Redistributions of source code must retain the above copyright notice, definition, disclaimer, and this list of
conditions.
2. Redistributions in binary form must reproduce the above copyright notice, definition, disclaimer, and this list
of conditions in documentation and/or other materials provided with the distribution.
3. Altered versions — including, but not limited to, ports to new operating systems, existing ports with new
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must not be misrepresented as being the original source. Such altered versions also must not be mis-
represented as being Info-ZIP releases — including, but not limited to, labeling of the altered versions with
the names "Info-ZIP" (or any variation thereof, including, but not limited to, different capitalizations), "Pocket
UnZip," "WiZ" or "MacZip" without the explicit permission of Info-ZIP. Such altered versions are further pro-
hibited from misrepresentative use of the Zip-Bugs or Info-ZIP e-mail addresses or of the Info-ZIP URL(s).
4. Info-ZIP retains the right to use the names "Info-ZIP," "Zip," "UnZip," "WiZ," "Pocket UnZip," "Pocket Zip," and
"MacZip" for its own source and binary releases
Copyright
The software described in this manual is furnished under a license agreement and may be used or
copied only in accordance with the terms of the agreement.
______________________________________________________________________________
Copyright © 2014 - 2017. Micromeritics Instrument Corporation. All rights reserved.

Warranty
WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each instrument it
manufactures to be free from defects in material and workmanship impairing its usefulness under normal use and service
conditions except as noted herein.
Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of any instrument or
defective parts when returned prepaid to us and which our examination discloses to have been defective. The purchaser is
responsible for all transportation charges involving the shipment of materials for warranty repairs. Failure of any instrument
or product due to operator error, improper installation, unauthorized repair or alteration, failure of utilities, or environmental
contamination will not constitute a warranty claim. The materials of construction used in MICROMERITICS instruments and
other products were chosen after extensive testing and experience for their reliability and durability. However, these
materials cannot be totally guaranteed against wear and/or decomposition by chemical action (corrosion) as a result of
normal use.
Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date of shipment.
No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and authorization to
return the instrument or product. All repairs or replacements are made subject to factory inspection of returned parts.
MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are made by
persons other than its own authorized service personnel unless such work is authorized in writing by MICROMERITICS.
The obligations of this warranty will be limited under the following conditions:
1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under their respective
brand names or trade names. We, therefore, make no express or implied warranty as to such products. We shall use
our best efforts to obtain from the manufacturer, in accordance with his customary practice, the repair or replacement
of such of his products that may prove defective in workmanship or materials. Service charges made by such man-
ufacturer are the responsibility of the ultimate purchaser. This states our entire liability in respect to such products,
except as an authorized person of MICROMERITICS may otherwise agree to in writing.
2. If an instrument or product is found defective during the warranty period, replacement parts may, at the discretion of
MICROMERITICS, be sent to be installed by the purchaser, e.g., printed circuit boards, check valves, seals, etc.
3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and stems,
seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects. Such items which
perform satisfactorily during the first 45 days after the date of shipment are assumed to be free of manufacturing
defects.
Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against
MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manufactures a
special product to the purchaser’s specifications.
MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products
other than the liability stated above. This warranty is in lieu of all other warranties, express or implied, including but not
limited to, the implied warranties of merchantability or fitness for use.
AutoPore V Series Operator Manual

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962-42800-01 (Rev D) — Nov 2017
Contact Us
CONTACT US
Micromeritics Instrument Corporation
4356 Communications Drive
Norcross, GA / USA / 30093-2901
Phone: 1-770-662-3636
Fax: 1-770-662-3696
www.Micromeritics.com
---------------
U.S. Inquiries
U.S. Sales Phone: 1-770-662-3636
[email protected]
---------------
Quotes, Orders, and Customer Satisfaction

Customer Service Phone: 1-770-662-3636
[email protected]
---------------
U.S. Instrument Service Department

U.S. Service Department Phone: 1-770-662-3666
[email protected]
---------------
Micromeritics Scientific Services

Customer Support Portal
http://techsupport.micromeritics.com/portal

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About this Manual
ABOUT THIS MANUAL

Log in to your customer portal to access the following:
l Calculations
l Error Messages
l AutoPore V Series Operator Manual in PDF format
l MicroActive Report Tutorials
Parts and accessories can be found online at www.Micromeritics.com.
The following icons may be found in this manual:
NOTE - Notes contain important information applicable to the topic.
CAUTION - Cautions contain information to help prevent actions that may damage the
analyzer or components.
WARNING - Warnings contain information to help prevent actions that may cause per-
sonal injury.

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Table of Contents
Warranty i
Contact Us ii
About this Manual iii
1 Analyzer Components 1-1

Front Panel 1-1
Rear Panel 1-2
Operational Safety Features 1-3
The Basic Workflow 1-4
Specifications for AutoPore V 1-5
2 About the Software 2-1

Software Setup 2-1
Software Updates 2-2
Uninstall the Software 2-2
Menu Structure 2-2
Common Fields and Buttons 2-3
File Status, Description, Extension, and Location 2-6
Keyboard Shortcuts 2-8
Option Presentation 2-9
Libraries 2 - 11
Methods 2 - 12
Configure the Analyzer 2 - 13
Atmospheric Pressure 2 - 13
Measured Temperature Warning 2 - 14
Specify Unit Selections 2 - 14
Unit Configuration 2 - 15
Instrument Status 2 - 16
Show Instrument Schematic 2 - 16
Show Status 2 - 19

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Show Dashboard 2 - 19
Show Instrument Log 2 - 21
Export Files 2 - 22
List Files 2 - 22
3 About Sample Files 3-1

Sample Files 3-1
Open a Sample File 3-4
Sample Averaging 3-5
Baseline Error Correction Methods 3-5
Create Blank Correction File 3-6
Formula Correction 3-7
Combine a Penetrometer Calibration and Blank Correction File 3-7
Manually Enter Data 3-8
4 About Parameter Files 4-1

Analysis Conditions 4-2
Material Properties 4-8
Penetrometer Properties 4 - 10
Report Options 4 - 11
5 Perform an Analysis 5-1

Select a Penetrometer 5-1
Prepare the Sample 5-5
Clean the Penetrometer 5-5
Load the Sample 5-6
Seal the Penetrometer 5-7
Weigh the Assembled Penetrometer with Sample 5-9
Install the Penetrometer 5 - 10
Perform a Low Pressure Analysis 5 - 11
Evacuate Low Pressure 5 - 13
Generate Low Pressure 5 - 14
Monitor a Low Pressure Analysis 5 - 15

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Perform a High Pressure Analysis 5 - 16
Generate High Pressure 5 - 18
Monitor a High Pressure Analysis 5 - 19
High Pressure Differential Analysis 5 - 20
Reference Material Analysis 5 - 21
High Pressure Reference Material Analysis 5 - 21
Low Pressure Reference Material Analysis 5 - 22
Leapfrogging - Suggested Sequence for Maximum Throughput 5 - 23
6 About Reports 6-1

SPC Report 6-1
Regression Report 6-2
Control Chart Report 6-4
PSD History Report 6-7
Interactive Reports 6-9
MicroActive Reports 6 - 10
Report Features and Shortcuts 6 - 11
Report Header Shortcuts 6 - 12
Report Toolbar 6 - 13
Tabular Report Features and Shortcuts 6 - 14
Graph Features and Shortcuts 6 - 15
Graph and Sample Overlays 6 - 21
Generate Pore Size Distribution Graph Overlays 6 - 21
Import ASCII Pore Distribution Data 6 - 23
Overlay Multiple Mercury Porosimetry Graph Options 6 - 24
Overlay Multiple Sample Files 6 - 25
Report Examples 6 - 26
7 Selected Reports 7-1

Advanced Report Options 7-1
Graph Report Options 7-2
Cavity to Throat Size Ratio Report Options 7-5
Fractal Dimension Report Options 7-6

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Material Compressibility Report Options 7-7
Mayer-Stowe Report Options 7-8
Options Report 7-9
Pore Structure Options 7 - 10
Reverberi Report Options 7 - 11
Sample Log Report 7 - 12
Summary Report 7 - 12
Tabular Report Options 7 - 16
8 Diagnostics 8-1
Start Diagnostic Test 8-1
Schedule Diagnostic Tests 8-2
Diagnostic Test Report 8-3
Save Files for Problem Diagnosis 8-4
9 Calibration 9-1
Calibrate the Low Pressure Servo 9-1
Calibrate Signals 9-2
Calibrate the Penetrometer 9-4
Load Calibration from File 9-5
Save Calibration to File 9-5
10 Hardware Components and Accessory Installation 10-1

Install a Penetrometer in a High Pressure Chamber 10-1
Install a Penetrometer in a Low Pressure Port 10-3
Remove a Penetrometer from a High Pressure Chamber 10-5
Remove a Penetrometer from a Low Pressure Port 10-6
11 Maintenance and Troubleshooting 11 - 1

System Components 11 - 4
Low Pressure System Components 11 - 4
High Pressure System Components 11 - 7
Change the Fuses 11 - 9

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Drain the Low Pressure System 11 - 10
Drain Spilled Mercury Dish 11 - 11
Enable Manual Control 11 - 12
Preventive Maintenance 11 - 16
Maintain Mercury Level 11 - 17
Maintain High Pressure Fluid Level 11 - 18
Seal the High Pressure Chamber 11 - 19
Grease Low Pressure Ports 11 - 20
Handling Mercury Overfill 11 - 21
Replace Chamber Cup Seals 11 - 21
Replace the Vent Valve O-ring 11 - 22
Change High Pressure Fluid and Clean High Pressure Chamber 11 - 23
Maintain Hydraulic Pump Fluid Level 11 - 23
Vacuum Pump 11 - 25
Replace Vacuum Pump Exhaust Filter 11 - 25
Replace the Mercury Vapor Filter 11 - 26
Change or Add Vacuum Pump Oil 11 - 27
Check Valves for Leaks 11 - 29
Clean Valves 11 - 29
Clean the Analyzer 11 - 31
Remove Moisture from the Analyzer 11 - 31
Replace the Banana Plug 11 - 32
High Pressure Chamber 11 - 32
Low Pressure Capacitance Detector 11 - 32
Penetrometer Nut 11 - 34
Remove the Penetrometer Nut 11 - 34
Tighten the Penetrometer Nut 11 - 35
Power Analyzer On and Off 11 - 36
Recover from a Power Failure 11 - 36
A Blank and Sample Compression Corrections A-1

Baseline Errors A-1
Approaches for Error Compensation A-2

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B Choose Proper Pump-Down Rates for Unfamiliar Sample Materials B-1
C Proper Handling of Mercury C-1

Proper Use of Mercury as a Tool in Pore Structure Analyses C-3
D Theory D-1
E Use of the Maximum Intrusion Volume Option E-1
F Worksheets F-1
Analysis Conditions Worksheet F-2
Penetrometer Properties Worksheet F-3
Pressure Table and Tabular Data Worksheet F-4
Report Options Worksheet F-5
Sample Data Worksheet F-6
Volumetric Reference Capsule Worksheet F-7
Density of Mercury Table F-8
G Exported Data Example G-1
H Compute Volumetric Compressibility of a Sample Material H-1
I Advanced Reports - Python Module I-1

Advanced Report Options I-2
Scripts I-3
Summary Report I-5
Tabular Report I-6
Graphic Report I-7
Acquire Basic Information for Mercury Porosimetry I-8
Mic Module Python Calls I - 11
Tables I - 11
Summary Reports I - 12
Graphic Reports I - 13
Get Intrusion-Extrusion Data I - 15

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Get Mercury Properties I - 16
Get Properties of Sample Material I - 17
Index Index - 1

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1 Analyzer Components
1 ANALYZER COMPONENTS
FRONT PANEL
Front Panel Components

Component Description
High Pressure Ports Pressurized. Illuminates when the high pressure system is
[LED light] pressurized, when the computer system is not connected, or when the
computer is connected but the application is not running.
Low Pressure Ports Pressurized. Illuminates when the low pressure system is
[LED light] pressurized, when the computer system is not connected, or when the
computer is connected but the application is not running.
Hg Up. Illuminates when the amount of mercury in the low pressure

system is sufficient to fill the penetrometers.
Hg Drained. Illuminates when mercury has been drained from the low
pressure system.
Power [LED light] Illuminates when power is supplied to the analyzer.

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REAR PANEL
Rear Panel Components

Aux RS232 Port Used by service personnel.
Ethernet Port Port for an Ethernet cable allowing communication between the ana-
lyzer and the computer.
Exhaust Port Provides ventilation for the analyzer. This exhaust can be vented to the
outside using flexible tubing similar to the type used on a home clothes
dryer, and a vent system which pulls air from the exhaust port.
Gas Inlet Port Used for connecting an external gas supply to the analyzer when gen-
erating pressures in the low pressure system.
Power cord connector For setting the power voltage and connecting the analyzer to the
power supply.
Power Switch Powers the analyzer on and off. It also provides electrical overload pro-
tection.
Reset buttons 10 Amp. Resets the internal vacuum pump.
25 Amp. Resets the internal vacuum pump in a high pressure

analyzer.

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Operational Safety Features
OPERATIONAL SAFETY FEATURES

The AutoPore V comes with multiple safety features:
l Mercury Drip Trays

Safe collection of mercury for disposal in the case of compromised penetrometer seals or
operator error resulting in broken penetrometers
l Mercury Temperature Sensor
Automatic measurement of mercury temperature allows automatic calculation of mercury density
used for penetrometer calibrations. The ability to set a temperature limit in manual mode allows
the display of a warning message if the temperature is exceeded.
l Improved Mercury Funnel Design
Attached screw cap and funnel-shaped opening eliminates mercury contamination and possible
drip spillage associated with separate detached filling funnel. Attached screw cap prevents loose
cap and possible vapor release.
l Triple Fail Safe-One Penetrometer Safety Caps
In case of operator error, this device prevents penetrometer or rod being released from port
unintentionally
l Triple Fail Safe-Two Interlock on Locking Cap
Verifies that capacitance detector is installed on low pressure port, automatically suspends run if
cap is not in place. This prevents the penetrometer from being accidentally released while under
pressure. If error is corrected, suspend run can be resumed.
l Triple Fail Safe-Three System Pressure Vent on manifold
Works in concert with cap interlock to automatically vent system pressure if above ambient
pressure and error condition is detected.
l Mercury Vapor Detection Device
Hand held device to check localized mercury vapor levels that exceed defined safety limits.
Portable device allows point checks at the analyzer or any location within lab exposed to mercury.
l Mercury Vapor Capture Filter
Affixed to vacuum pump, this filter prevents release of mercury vapors. This is a superior solution
to cold trap dewars, particularly if the cryogen level is insufficiently maintained.
l Software Control for Fine Powder Samples
Prevents fine powder from accidental aspiration into low pressure ports during analysis.

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THE BASIC WORKFLOW

Before a sample can be analyzed, it must be:
1. Weighed and the mass recorded, and

2. A sample file must be created that describes the sample and gives the analysis conditions and
other parameters for the analysis. This file also includes a pressure table, which lists the pres-
sure points at which data are collected during the analysis.
To begin the analysis, a sample is placed in a penetrometer then the penetrometer is installed into a
low pressure port. The low pressure analysis consists of two phases:
1. The first phase is the evacuation of gases from the penetrometer. The penetrometer is then
filled automatically with mercury.
2. The second phase is the collection of data at pressures up to and including the last low
pressure point specified in the pressure table.
When the low pressure analysis is complete, remove the penetrometer from the low pressure port
and weigh it, then install it in a high pressure port. The mass of the penetrometer with sample and
mercury can be entered in the sample file or in the window for starting the high pressure analysis.
Pore volume data are calculated by determining the volume of mercury remaining in the
penetrometer stem. As pressure increases, mercury moves into the sample’s pores, vacating the
stem (this is called intrusion). Intrusion of different size pores occurs at different pressures. (The
greater the pressure, the smaller the pore diameter into which the mercury can be forced.) Because
mercury has a high surface tension and is nonwetting to most materials, its angle of contact and
radius of curvature can be used to calculate the pore diameter into which it intrudes at a given
pressure.
The volume of mercury in the penetrometer stem is measured by determining the penetrometer
electrical capacitance. Capacitance is the amount of electrical charge stored per volt of electricity
applied. The penetrometer capacitance varies with the length and diameter of the penetrometer
stem that is filled with mercury.
When the penetrometer is initially filled with mercury, the mercury extends the entire length of the
penetrometer. As increasing pressure causes the mercury to intrude into the sample’s pores, the
volume of mercury in the penetrometer stem decreases by an amount equal to the volume of the
pores filled. This decrease in the length of the penetrometer stem that is filled with mercury causes a
reduction in the penetrometer capacitance. The analysis application converts measurements of the
penetrometer capacitance into data points showing the volume of mercury intruding into the
sample’s pores.
Theory on page D - 1 provides a thorough discussion of the theory of porosimetry.

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Specifications for AutoPore V
SPECIFICATIONS FOR AUTOPORE V

Characteristic Specification
Electrical
Frequency 50 to 60 Hz
Power 500 VA maximum
Voltage 100/120/220/240 VAC ±10%
Gas
Nitrogen or other clean, dry gas at 50 psig (345 kPa)
High Pressure Model 9600 and 9605
Measurement From atmospheric pressure to 33,000 psia (228 MPa)
Pore Diameter Range 6 to 0.005 µm
Resolution 0.165 psi (1400 Pa) from 3300 psia (21 MPa) to 33,000 psia
Servo Control Precision 0.5% of target, min 5 psia, no overshoot
Transducer Accuracy ±0.1% of full scale (transducer manufacturer's specifications)
Transducer Hysteresis .05% of full scale
High Pressure Model 9610 and 9620
Measurement From atmospheric pressure to 60,000 psia (414 MPa)
Resolution 0.3 psia from atmospheric pressure to 60,000 psia
Servo Control Precision 0.5% of target, min 5 psia, no overshoot
Transducer Accuracy ± 0.1% of full scale (transducer manufacturer's specifications)
Transducer Hysteresis .05% of full scale
Intrusion
Accuracy ±0.1% of maximum penetrometer stem volume
Resolution Better than 0.1 μL
Low Pressure
Measurement 0.2 to 50 psia (345 kPa)
Resolution 0.00025 psi

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Characteristic Specification
Servo Control Precision 1% of target, min. .05 psia, no overshoot
Transducer Accuracy ±0.1% of full scale (transducer manufacturer’s specifications)
Penetrometers
Sample Size Maximum: a cylinder 2.54 cm diameter × 2.54 cm long (1 in.
diameter × 1 in. long)
Stem Intrusion Volumes 0.38, 1.1, 1.7, 3.1, and 3.9 cc
Physical
Height 143 cm (56.25 in.)
Width 54.3 cm (21.38 in.)
Depth 78 cm (30.75 in.)
Weight (9600 and 9610) 227 kg (500 lb)
Weight (9605 and 9620) 250 kg (550 lb)
Computer Requirements
l Operating System. Windows 7 Professional or higher operating system is recommended for

the best user experience.
l Desktop Installation Required. The application should not be installed on a network drive
with shared access. Multiple users cannot operate the application at the same time.
l 10 Base T or 100 Base T Ethernet Port. If the computer is to be connected to a network, two
Ethernet ports are required. If more than one Ethernet based unit is connected to the same com-
puter, an Ethernet switch will also be required.
l Read / Write Permissions. All users of the application will need Read/Write permission to all
directories and subdirectories where the application is installed.
l Drives. CD-ROM drive and thumb drive.
In keeping with a policy of ongoing product improvement, specifications are subject to change
without notice.

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2 About the Software
2 ABOUT THE SOFTWARE

The analyzer allows other computer programs to run while an automatic operation is in progress.
The Help menu provides access to the online operator manual.
Report options can be specified when creating the sample file. When running an analysis, data
gathered during the analysis process are compiled into the predefined reports. Reports can also be
defined and generated after an analysis has been run. Each selected report is displayed on its own
tab and reflects data collected during the analysis.
The MicroActive feature offers a Windows interface with an easy way to collect, organize, archive,
reduce raw data, and store sample files for later use. Scalable and editable graphs, and copy and
paste graphics, are easily generated. Customized reports can be generated to screen, paper, or
exported for use in other programs.
In addition to customizable standard reports, user defined calculations and reports can be created
through the Advanced reports feature (using Python).
Data can be manipulated and displayed interactively using MicroActive reports.
SOFTWARE SETUP
If the computer is to be connected to a network, a second Ethernet port on the computer

must be used for that purpose.
The Setup program is located on the installation media and is used to reinstall the software and
make analyzer changes — such as adding or removing a unit, etc.
If the IP address needs to be changed on the computer connected to the analyzer, refer
to the computer's operating system manual or the internet for instructions. The
IP address for the computer and the IP address specified in the setup program must
match. The default IP address is 192.168.77.100.

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SOFTWARE UPDATES
Log in to your customer portal to access and download the latest analyzer software version.
When performing a software update, existing data files are not overwritten. There are three types of
subsequent installation:
l a later version than the current installation

l the same version as the current installation
l an earlier version than the current installation
Insert the setup media into the media drive. The setup program starts automatically. If the program
does not start automatically, navigate to the installation media drive, locate and double click the
setup.exe file.
UNINSTALL THE SOFTWARE

When the software is uninstalled, only the files required to run the application are removed.
Parameter files, sample files, reports, calibration files, and data files are not removed.
To uninstall the software, double click the uninstall.EXE file located in the software installation
directory, then follow the screen prompts.
MENU STRUCTURE
All program functions use standard Windows menu functionality. The title bar contains a Unit
Number. If multiple units (analyzers) are installed, ensure the appropriate unit is selected before
continuing.
Main Menu Bar Options

Option Description
File Use to manage files used by the application — such as sample files, ana-
lysis conditions files, report options files, etc.
Unit [n] Use to perform analyses, calibrations, and other analyzer operations. Unit
[n] displays on the menu bar for each analyzer attached to the computer.
Reports Use to run reports and view the results.
Options Use to edit the default method, specify system configuration, specify units,
and change presentation options.
Window Use to manage open windows and display a list of open windows. A check-
mark appears to the left of the active window.
Help Provides access to the online operator manual, the Micromeritics web
page, the analyzer web page, and information about the analyzer.

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Common Fields and Buttons
COMMON FIELDS AND BUTTONS

The fields and buttons in the following table are located in multiple windows throughout the analyzer
application and have the same description or function. Fields and button descriptions not listed in this
table are found in tables in their respective sections.
Common Fields and Buttons Table

Field or Button Description
Add Add an item to the list.
Add Log Entry Use to enter information to appear in the sample log report that cannot
be recorded automatically through the application. Click the button
again to enter multiple log entries.
Append Use to insert one row at the end of a table.
Autoscale When enabled on report parameters windows, allows the x- and y-
axes to be scaled automatically. Autoscale means that the x- and y-
ranges will be set so that all the data is shown. If Autoscale is not selec-
ted, the entered range is used.
Axis Range On report parameters windows, the From / To fields are enabled when
Autoscale options are not selected. Enter the starting and ending val-
ues for the x- and/or y-axes.
Bar Code Enter bar code reader information if a bar code reader is connected to
the computer’s USB port. If a bar code reader is not used, this alpha-
numeric field can be used to enter additional information about the
sample, such as a sample lot number, sample ID, etc.
Browse Searches for a file.
Cancel Discards any changes or cancels the current process.
Clear Use to clear the table entries and display only one default value.
Close Closes the active window.
Close All Closes all active windows. If changes were made and not yet saved, a
prompt displays for each changed file providing the option to save the
file.
Comments Enter comments about the sample or analysis. Comments display in
the report header.
Copies Select the number of copies to print. This field is only enabled when
Print is selected.
Delete When working with pressure tables and pressures, Delete removes
the selected information.
Destination Select the report destination.

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Common Fields and Buttons Table (continued)

Edit When working with report parameters, highlight the item in the Selec-
ted Reports list box and click Edit to modify the report details.
Exit Exits the application. If a file is open with unsaved changes, a prompt
displays providing the option to save the changes and exit or to exit the
application without saving the changes.
Export Exports data in a sample file as a .REP, .TXT or .XLS file. When saved
to a file, the data can be imported into other applications.
File Select the destination directory. Enter a new file name in the File name
field, or accept the default. Select to save the file as a report system
(.REP), a spreadsheet (.XLS), a portable document format (.PDF), or
an ASCII text (.TXT) file format.
File name Select a file name from the list shown or enter a file name. If the
required file type is not shown, select the type of file on the left.
From / To When working with report parameters windows, enter the From and
To range for x- and/or y-axes.
Insert Use to insert one row above the selected row in the table.
List Creates a list of sample or other type files. The list will contain file
name, date / time the file was created or last edited, file identification
and file status.
Name column A list of files in the selected directory or library.
Next Click to move to the next window or next step.
OK Saves and closes the active window.
Open Opens the selected file. Alternatively, double click the file name in the
Name column to open the file.
Prev Click to move to the previous window.
Preview Previews predefined reports. Click the tabs at the top of the window to
preview each selected report. When an analysis has not been run on a
sample, this button is disabled.
Print Sends the report to the selected destination (screen, printer or file).
Remove Remove the selected file or files from the list.
Replace Click to select another file where the values will replace the current
file’s values.
Replace All Click to select another .SMP file where the values will replace all val-
ues for the active sample file. The original file will remain unchanged.

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Common Fields and Buttons
Common Fields and Buttons Table (continued)

Report Click to display a window to specify report output options.
Save Saves changes to the active window.
Save As Saves a file in the active window under a different file name.
Start Starts the report, test, analysis, or operation.
Start Date Displays a calendar to select the start date for the report.
View Operation. Use to display the data from the current analysis.
Instrument Log. Use to display recent analyses, calibrations, errors

or messages.
Instrument Schematic. Use to display a schematic of the analyzer

system.

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FILE STATUS, DESCRIPTION, EXTENSION, AND LOCATION

In the File Selector window, the Mic Description column and the Mic Status column display file
description and file status. The File Selector incorporates standard Windows features for resizing
windows, reordering and repositioning columns, and right clicking an entry to display a menu of
standard Windows functions.
File Status and Description Table

File Status Description
Analyzing Sample files that are currently being used for analysis.
HP Complete l A high pressure analysis has been performed using this sample
file.
l A low pressure analysis must be performed on a sample before
a high pressure analysis can be performed; files with the status
HP Complete have finished one low pressure analysis and at
least one high pressure analysis.
l Multiple high pressure analyses can be performed on a sample,
so files with the status HP Complete may have finished more
than one high pressure analysis.
LP Complete A low pressure analysis has been performed using this sample file.
(Only one low pressure analysis may be performed on each file.)
No Analysis Sample files which have not been used to perform an analysis.
File Type, Extension, and Location Table

File Type File Name Default Location
Extension
Analysis Conditions .ANC Param Directory
Material Properties .MTP Param Directory
Methods .MTH Param Directory
Penetrometer .PEN Param Directory
Report Options .RPO Param Directory
Sample File .SMP Data Directory

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File Status, Description, Extension, and Location
File types available when printing or exporting reports:

Portable document .PDF
format
Report .REP
Spreadsheet .XLS
Unicode .TXT

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KEYBOARD SHORTCUTS
Shortcut keys can be used to activate some menu commands. Shortcut keys or key combinations
(when applicable) are listed to the right of the menu item.
Certain menus or functions can also be accessed using the Alt key plus the underlined letter in the
menu command. For example, to access the File menu, press Alt + F, then press the underlined
letter on the submenu. For example, Alt + F opens the File menu, then press O to access the File
Selector for opening files.
If the underscore does not display beneath the letter on the menu or window, press the
Alt key on the keyboard.
Keyboard Shortcut Table

Alt +[Unit n] Opens the Unit [n] menu.
Alt + F Opens the File menu.
Alt + F4 Exits the program. If files are open with unsaved changes, a prompt to save
changes displays.
Alt + H Opens the Help menu.
Alt + I Opens the Options menu.
Alt + R Opens the Reports menu.
Alt + W Opens the Window menu.
Shift + F9 Opens the shortcut menu of (1) selected component on analyzer schematic
when manual control is enabled or (2) onscreen reports.
Ctrl + N Opens a new sample file.
Ctrl + O Opens the File Selector.
Ctrl + P Opens the File Selector to start a report from a selected .SMP file.
Ctrl + S Saves the open file.
F1 Opens the online help operator manual.
F2 Displays the File Selector window.
F3 When in the File Selector window, opens the file search box.
F4 When in the File Selector window, opens the address bar.

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Option Presentation
Keyboard Shortcut Table (continued)

F6 Cascades open windows.
F7 Tiles open windows.
F8 Opens the File Selector to start a report from a selected .SMP file.
F9 Closes all open reports.
OPTION PRESENTATION
Options > Option Presentation
Use to change the way sample files and parameter files display: Advanced, Basic, or Restricted.
Each display option shows sample information and options differently.
Option Presentation Display Table

Presentation Display Description
Advanced Displays all parts of sample information and parameter files. Navigate
to parameter windows by selecting the tabs across the top of the win-
dow.
Basic Displays sample information in a single window. This display option is
used after the parameter files have been created. The previously
entered or default parameter files are then accessible using drop-
down lists.
Restricted Displays the sample file in a single window similar to the Basic display
option with certain functions disabled. A password is set when the
Restricted option is selected. That same password must be entered to
change to the Basic or Advanced display option. This display type is
typically used in laboratories where analysis conditions must remain
constant — such as the pharmaceutical industry. The Advanced option
is not available at the bottom of the window when using the Restricted
display option.
Show Splash Screen Enables (or disables) the splash screen upon application startup.
Specify or change the default option presentation by selecting Options > Option
Presentation, or select Basic or Advanced from the drop-down list at the bottom of the
window.

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The following examples show the same sample file in Advanced and Basic display. Basic and
Restricted displays will look the same.
A sample file must be created for each analysis. The file can be created prior to or at the
time of analysis. The sample file identifies the sample, guides the analysis, and specifies
report options.

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Libraries
LIBRARIES
Options > Manage Libraries
This feature is available only for Windows 7 and higher operating systems.
The library provides an easy way to locate and open specific analyzer files. Libraries are located
within the File Selector window and can be viewed only within the application.
The library gathers sample and parameter files that are stored in multiple locations — such as folders
on a C: drive, a network location, a connected external hard drive, or a connected USB flash drive —
providing access to all files. Even though libraries do not store actual sample and parameter files,
folders can be added or removed within each library.
One library can include up to 50 folders. Other items such as saved searches and search connectors
cannot be included.
When removing a folder from a library, the folder and its contents are not deleted from the original file
storage location. However, when deleting files or folders from within a library, they are deleted from
their original file storage location.

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METHODS
File > New Method
Options > Default Method
File > Open > [.MTH File]
See also:
Sample Files on page 3 - 1
A Method determines the default sample identification format and sequence number. A Method is a
template of specifications that go into a newly created sample file. It allows for the definition of
complete sets of parameters for each type of sample commonly analyzed, so that only a single
selection is required for each new sample file created.
The Method drop-down list displays only those methods applicable to the open sample file type.

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Configure the Analyzer
CONFIGURE THE ANALYZER

ATMOSPHERIC PRESSURE
Options > Atmospheric Pressure
For accurate analysis, the application must adjust pressure measurements to account for variations
in local atmospheric pressure (barometric pressure).
Enter the current atmospheric pressure or accept the system default of 14.7 psia (0.1014 MPa).
When the port is open, it is recommended to enter the value on the low pressure display. It is
recommended to enter the current atmospheric pressure daily (or more frequently if atmospheric
pressure rises or falls rapidly during the day).
Select Determine high pressure transducer offset to enable the system to determine automatically
the high pressure transducer offset.
If the atmospheric pressure is above the entered value and the Determine high pressure transducer
offset option is selected, a warning will display.

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MEASURED TEMPERATURE WARNING

Options > Warnings
Enable this option to have the analyzer automatically display a warning if the measured temperature
rises above the entered temperature.
SPECIFY UNIT SELECTIONS

Options > Units
Use to specify how data should appear on the application windows and reports. This menu option is
not available if using Restricted option presentation.

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Unit Configuration
UNIT CONFIGURATION
Unit [n] > Unit Configuration
Use to display hardware / software configurations.
Unit Configuration Fields and Buttons Table

Calibration group box Displays the dates of the last high and low pressure servo calibrations
and signals.
Configuration group box Displays the IP address used by the analysis program, serial number,
and type of analyzer.
Change IP [button]. Displays the Unit IP Setup window. The IP

address and subnet mask assigned during installation display. Do not
edit these fields unless instructed by a Micromeritics service
representative.
Board ID [button]. Displays information from the electronic circuit

boards in the analyzer. These parameters cannot be edited.
Software Versions Displays the software versions of the controller start up code, analysis
group box program, and type of analyzer.

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INSTRUMENT STATUS
SHOW INSTRUMENT SCHEMATIC
Unit [n] > Show Instrument Schematic
To operate the valves and elevator from the schematic, manual control must be enabled (Unit [n] >
Enable Manual Control).
Analyzer Schematic Icon Table

Icon or Symbol Description
Open Valve. Green indicates an open valve.
Closed Valve. Yellow indicates a closed valve.
Servo Valve. Closed.
Servo Valve. Open.

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Show Instrument Schematic
Low Pressure Schematic Icons

Mercury Degasser. Displays the mercury level.
Drained Partially Filled Filled Overfilled. This alarm

displays
with a red background.
This is an alarm state.
Mercury Trap. Displays the state of the mercury trap.
Empty Contains more than 6 mm of mercury.

Mercury Reservoir. Displays the level of mercury in the reservoir.
If the mercury level is low, see Maintain Mer- Level is OK.

cury Level on page 11 - 17.
Hg Reservoir Vacuum Switch
When illuminated, indicates that mercury reser-
voir has been evacuated.

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High Pressure Schematic

Hydraulic Pump
When the pump is operating, the target pressure
displays below the icon. A green icon indicates the
pump is ON. A yellow icon indicates the pump is
OFF. To set the target pressure when the icon is
yellow, either double-click the pump icon or right
click the icon and select Set.
Intensifier. Displays the state of the intensifier limit switches.
Midway Top Bottom
Instrument Schematic Shortcut Menus
Each manually controlled schematic component has a shortcut menu displaying the operations
available for that particular component. To access the shortcut menu, hover the mouse pointer over
the component and right click.
Schematic Shortcuts Table

Schematic Shortcut Available Options:
Icon
Valve options Automatic. Automatically operates the servo valve during dosing or
evacuation. Enter the target pressure.
Close. Closes the selected valve.
Disable. Select to disable the servo pump. To enable the pump, right
click the servo pump icon and select Set to verify or set a target
temperature. When the pump is enabled, the target temperature
displays below the servo pump icon.
Open. Opens the selected valve.
Pulse. Use to quickly turn the valve on and off allowing the operation
to proceed in small increments.
Set. Use to set the servo pump target pressure.

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Show Status
SHOW STATUS
Unit [n] > Show Status
If multiple units are attached to the computer, select Show Status on each Unit [n] menu. The status
for all units display.
SHOW DASHBOARD
Unit [n] > Show Dashboard
The dashboard displays the following:
l Number of days until low pressure system service is due

l Days until high pressure system service is due
l Days until Hg filter replacement is due
l Low pressure manifold outgas rate
l Hg temperature (°C) mean ±2σ, min/max
l High pressure cycles completed
l Low pressure analyses completed / started
l High pressure analyses completed / started
Data for the dashboard comes from the logged diagnostic data. The dashboard is automatically kept
current as the relevant diagnostic data items are updated. The gauges will be updated even if the
dashboard window is not open.
Red numbers on the dashboard require attention. To reset the dashboard numbers,
right click on the dashboard setting, then click Reset.

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Dashboard Gauges and Descriptions Table

Days until high pres- The number of days until service is required on the high pressure sys-
sure system service is tem. When the displayed value is 30 or less, the value is displayed in
due red. Red negative numbers display if maintenance is past due.
Days until Hg filter The number of days until the mercury filter replacement is due. When
replacement is due the displayed value is 30 or less, the value is displayed in red. Red neg-
ative numbers display if maintenance is past due.
Days until low pressure The number of days until service is required on the low pressure sys-
system service is due tem. When the displayed value is 30 or less, the value is displayed in
red. Red negative numbers display if maintenance is past due.
Hg temperature Displays the statistics of the manifold temperature reading. The mean,
the value at two standard deviations, the minimum, and the maximum
display.
High pressure analyses Displays N/M where N is the number of high pressure analyses that
completed / started have finished data collection and M is the number of analyses that
have been started. Analyses canceled or terminated by errors before
the termination stage starts are not counted as completed.
High pressure cycles Indicates the number of completed high pressure cycles. Cycles can-
completed celed or terminated by errors before the termination stage starts are
not counted as completed.
Low pressure analyses Displays N/M where N is the number of low pressure analyses that
completed / started have finished data collection and M is the number of analyses that
have been started. Analyses canceled or terminated by errors before
the termination stage starts are not counted as completed.
Low pressure manifold Provides the qualitative indication of the outgas rate in the dosing
outgas rate manifold. LED images constitute a bidirectional bar graph of the
outgas rate.
l Three green LEDs are lit if outgas rate is below 30% of outgas rate
limit.
l At 30%, the left LED turns off.
l At 60%, the center LED turns off.
l At 90%, three green LED lights turn off and the center yellow LED is
turned on.
l At 110% and above, only the red LED is lit and attention is required.

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Show Instrument Log
SHOW INSTRUMENT LOG

Unit [n] > Show Instrument Log
Use to display a log of recent analyses, calibrations, errors, or messages. The log displays:
l 7 days of analysis data

l 30 days of messages
l 30 days of calibration data
Instrument Log Fields and Buttons Table

Add Log Entry To manually enter information into the log file, enter the text into the
text field to the left of the Add Log Entry button, then click Add Log
Entry.
Analysis /
Calibration /
Select the logs to display.
Message /
Conductivity
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 3.

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EXPORT FILES
File > Export
See also:
Exported Data Example on page G - 1
Provides the option to print the contents of one or more sample files to either the screen, a printer, or
to a file. Intrusion data can be exported as a .PDF, .REP, .TXT, or .XLS file format. The type of data
to include or exclude can be selected during the export process. When exported to a file, the data
can be imported into other software that read .TXT or .XLS file formats.
LIST FILES
File > List
Provides the option to create a list of sample file information —such as file name, date, time the file
was created or last edited, file identification, and file status.

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3 About Sample Files
3 ABOUT SAMPLE FILES

Sample files include the information required by the analyzer to perform analyses and collect data. A
sample file identifies the sample, guides the analysis, and specifies report options and may be
displayed in either Advanced, Basic, or Restricted presentation display mode. After data has been
collected, the file will be shown in MicroActive mode.
A sample file consists of parameter sets; however, parameter sets can also stand alone. A sample
file may be created either prior to or at the time of analysis.
Parameter files allow for repeated use of parameter sets. For example, if the same analysis
conditions exist for multiple analyses, an Analysis Conditions file containing the recurring conditions
can be created. When the sample file is created, the Analysis Conditions file can be selected for the
analysis conditions. Once it becomes part of the new sample file, the new file can be edited as
needed without affecting the original Analysis Conditions file.
The analysis software contains a default method. A method is a template for sample files that
contains the parameters to be used for an analysis. When a new sample file is created, all the
parameters are filled with the values in the default method.
Specify or change the default option presentation by selecting Options > Option
Presentation, or select Basic or Advanced from the drop-down list at the bottom of the
window.
SAMPLE FILES
Options > Option Presentation > [Advanced / Basic / Restricted]
File > New Sample
File > Open > [.SMP File]
Each analysis must be linked with a sample file before the analysis can proceed.
Specify or change the default display option by selecting Options > Option Presentation or select
Basic / Advanced from the drop-down list at the bottom of the window.
The values for individual parameters in a file must be initially entered in Advanced mode and the file
saved. Sample files can then be created in Advanced, Basic, or Restricted mode by selecting
predefined Methods or Analysis Conditions and Report Options.
The values specified in the parameter portions of the default sample file are saved as the defaults for
new sample files. To navigate from one set of parameters to another, select the parameter tab
across the top of the window.

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Sample File Fields and Buttons Table

Assembly mass This field is entered after the low pressure analysis is completed.
[text box] Sample + penetrometer + mercury mass after the low pressure ana-
lysis.
Bar Code Enter bar code reader information if a bar code reader is connected to
the computer’s USB port. If a bar code reader is not used, this
alphanumeric field can be used to enter additional information about
the sample, such as a sample lot number, sample ID, etc. To rename
the field label, go to Options > Default Method and deselect the
Omit option.
Comments [text box] Enter comments about the sample or analysis. Comments display in
the report header.
Material [drop-down box] Select the material to be analyzed from the drop-down list. See Mater-
ial Properties on page 4 - 8.
Method [drop-down box] Select a method from the drop-down list. See Methods on page 2 -
12.
Operator [text box] Enter operator identification information. This field label may have
been renamed or may not display if modified in Options > Default
Methods.
Penetrometer Select a penetrometer file from the drop-down list, or click Edit to
[drop-down box] modify or create a new Penetrometer file. See Penetrometer Prop-
erties on page 4 - 10.
Sample [text box] Enter a sample description.
Submitter [text box] Enter submitter identification information. This text box may have been
renamed or may not display if modified in Options > Default Meth-
ods.

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Sample Files
Sample File Fields and Buttons Table (continued)

Type of Data [group box] Automatically collected. Select if the type of data will be
automatically collected by the system while an analysis is running.
Manually entered. Use to enter data manually that was collected

from another source. If Manually entered is selected, the Intrusion
Report becomes available in the Basic/Advanced drop-down list for
pasting or importing data into the file.
See Manually Enter Data on page 3 - 8.

User Parameters These fields are primarily used for the SPC (Statistical Process
[group box] Control) reporting to specify sample characteristics or its
manufacturing process but may be used for other data by entering
specific analysis conditions or sample criteria.
The entered parameters display on the Summary Report. Some fields

may not display (or may have a different field label) if modified in the
method from which the sample file was created, either through
Options > Default Method or File > Open > Method.
tons on page 2 - 3.

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OPEN A SAMPLE FILE

File > Open > [.SMP File]
When working with an existing sample file, consider making a copy of the sample file to
maintain the original configuration options.
File Type File Status Displays

Analyzing
Entered Tabbed file editor
Mercury Porosimetry No analysis
HP Complete
MicroActive report window
LP Complete

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Sample Averaging
SAMPLE AVERAGING
File > Average
A sample file can be created in which the collected data are the average of up to four similar
analyses. All information in the new sample file will be the same as in the first selected file except for
the information entered in the Sample Averaging window. The collected data in the file will be the
average of the data in the selected files.
Sample averaging can be used for sample files and blank correction files.
BASELINE ERROR CORRECTION METHODS

The penetrometer parts, the mercury, and the sample are all affected differently by the pressures
exerted on them during analysis. Each material compresses to a different degree and at a different
rate. Also, the increasing pressure within the high pressure port can cause the temperature of one or
more of these materials to rise.
As a result, analysis data may show intrusion where none actually exists. For example, if the sample
compresses sharply at a given pressure (compared to the compression of the mercury at that
pressure), mercury moves from the penetrometer stem into the sample bulb to fill the space vacated
by the shrinking sample. This reduction in the amount of mercury in the stem is interpreted by the
software as intrusion.
These baseline errors can be reduced or eliminated through one of two correction methods:
l formula correction, and

l blank correction
The correction method is selected in the Penetrometer Properties file and displays in the Sample file.

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CREATE BLANK CORRECTION FILE

File > Open > [enter new .SMP file name]
A sample file must be created even if there is no sample or if the sample is non-porous.
A blank correction file contains analysis data using one of the following:
l Mercury only (a blank run)

l A nonporous sample of the same mass and material as the samples to be analyzed
To be used as a correction file, the blank run should use the same analysis conditions
and penetrometer properties as the sample analysis. Therefore, a separate blank cor-
rection file should be created for each type of sample and set of analysis conditions to be
used.
No matter which type of blank correction run is used, the procedure is the same (follow the
instructions for creating a sample file (even if there’s no sample), then run the analysis. (When the
blank file’s sample file is created, select None for correction method.)
1. Create the sample file. Enter zero for the sample mass.
2. Perform the low and high pressure analysis. See Perform a Low Pressure Analysis on
page 5 - 11 and Perform a High Pressure Analysis on page 5 - 16.
An alternative method for creating the blank correction file is to perform a High Pressure
Differential analysis which analyzes the blank and sample simultaneously. See Perform
a High Pressure Analysis on page 5 - 16.

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Formula Correction
FORMULA CORRECTION
A formula for correction is available for each type of penetrometer. The formula is a part of the
application software, therefore when the Formula option in the Penetrometer Properties file is
selected, the formula is applied.
The recommended method of correction is by blank correction file. The formula is provided for use
when comparison with historical data is required.
COMBINE A PENETROMETER CALIBRATION AND BLANK CORRECTION FILE

1. Calibrate the penetrometer. See Calibrate the Penetrometer on page 9 - 4. Enter the ana-
lysis conditions and pressure table to be used when samples are analyzed with this blank cor-
rection file.
2. After the low pressure run, do not empty the penetrometer. Weigh it and record the assembly
mass. Use a syringe to withdraw a small amount of mercury from the tip of the capillary so that
the mercury column recedes approximately 1/8 in. to 1/4 in. into the stem. This enables meas-
urement of any rise or fall of mercury in the stem during high pressure analysis and prevents
spilling of mercury into the high pressure chamber. Then install the penetrometer in a high
pressure port.
3. Create blank correction files by completing the high pressure run. See Create Blank Cor-
rection File on the previous page.
4. Create a new Penetrometer Properties file for this penetrometer. See Penetrometer Prop-
erties on page 4 - 10. From the file selection list, choose the default file for this type of pen-
etrometer. Change the identifier to include the penetrometer serial number. Enter the
calibrated volume and save the file. The Penetrometer Properties file now includes the cal-
ibrated penetrometer volume. A blank correction file has also been created for this pen-
etrometer.

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MANUALLY ENTER DATA

This process allows the manual entry of pressure data from a sample file with a Complete status.
There are two methods for manually entering data into a sample file:
l Copy and paste onto the graph area of the interactive window
l Import data into the interactive window
COPY AND PASTE MANUALLY ENTERED DATA

1. Open a sample file with a Complete status. The file will open to the interactive reports window.
2. Right click in the graph area of the interactive reports window, then select Copy data.
3. Open another sample file using Advanced option presentation.

4. On the Sample Description tab, select Manually entered in the Type of Data group box.
5. Click the Advanced down arrow at the bottom of the window, then select Intrusion .

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Manually Enter Data
6. Ensure that all parameter fields are set appropriately, then click the Paste button.

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IMPORT MANUALLY ENTERED DATA

When importing isotherm data from an external ASCII text file using the Import button on the
interactive window, the ASCII text file must use the following rules:
ASCII text file format rules
Data must be in two columns and separated by a comma or white-space. Acceptable column
headings are:
l Pressure (psi)
l Pressure (MPa) l Intrusion (cm3)
l Pressure (kPa) l Intrusion (cm3)
l Pressure (Pa) l Intrusion (ml)
l Pressure (bar) l Intrusion (mm3)
l Pressure (mbar) l Intrusion (mm3)
l Pressure (Atm)
Sample Mercury Porosimetry ASCII Text File
Cumulative Intrusion for Cycle 1

Pressure (MPa) Cumulative Intrusion (cm³/g)
0.138151 0.0
0.155414 0.00637965
0.310025 0.0327685
0.458529 0.0377315
0.816881 0.0411021
1.46145 0.0427142
2.60941 0.0444728
4.00728 0.0460848
5.35594 0.0474771
7.24049 0.0495286
9.63008 0.0519466
13.7208 0.0561233
24.4012 0.0808897
46.6833 0.800216
83.4181 1.15068
159.718 1.1586
286.294 1.16834
412.525 1.17574

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Manually Enter Data
To import the ASCII text file
1. Open a new sample file in Advanced option presentation.

2. On the Sample Description tab, select Manually entered.
3. Click the Advanced down arrow at the bottom of the window, then select Intrusion..
4. Ensure that all parameter fields are set appropriately, then click Import.
5. Open the .TXT file. The data from the original sample file is imported and displayed. If an error
message appears instead, verify that the .TXT file format is correct.

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4 About Parameter Files
4 ABOUT PARAMETER FILES

Parameter files allow for repeated use of parameter sets. For example, if the same analysis
conditions exist for multiple analyses, an Analysis Conditions file containing the recurring conditions
can be created. When the sample file is created, the Analysis Conditions file can be selected for the
analysis conditions. Once it becomes part of the new sample file, the new file can be edited as
needed without affecting the original Analysis Conditions file.
Methods include both analysis conditions and report options, offering the most convenient way to
repeat most analyses.
Predefined parameter files are included with the program and can be edited as needed or new
parameter files can be created.
The following file types can exist as part of the sample file as well as individual parameter files:
File Type File Extension

Analysis Conditions .ANC
Material Properties .MTP
Method .MTH
Penetrometer Properties .PEN
Report Options .RPO

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ANALYSIS CONDITIONS
File > Open > [.ANC File]
(or click the Analysis Conditions tab when in Advanced option presentation)
Analysis conditions specify the parameters used to guide an analysis.
Analysis Conditions Fields and Buttons Table

Button Use to Specify...
Autocalculate Reverberi Select to have the application automatically use the Reverberi
pressures [selection] pressures. Selecting this option disables the pressures table. Click
Options to enter additional Reverberi options.
Enter target pressures Select to manually enter pressures into the table.
[selection]
High Pressure Equilibrate by. Select the option for equilibration based on elapsed
[group box] Time (in seconds) or decrease in Rate of intrusion (or extrusion) in

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Analysis Conditions
Analysis Conditions Fields and Buttons Table (continued)

mL/g per second.
Scan by:
l Pressure. The analyzer goes through a sequence of segments,
with each segment starting at the end of the previous one. Each
segment ends at the specified pressure. The pressure is pro-
grammed to increase or decrease at a rate to give a constant time
per decade of pressure. Along the way, the analyzer takes intrusion
points at the specified number of points per decade, ending at the
specified ending pressure. Also, any points in the pressure table, as
well as points separated by the maximum intrusion volume, are col-
lected.
l Intrusion. The analyzer goes through a sequence of segments,

with each segment starting at the end of the previous one. Each
segment ends at the specified pressure The pressure rate is the
maximum achievable safe rate (up to 0.5 min/decade) and is pro-
grammed to increase or decrease at a rate to give a constant intru-
sion / extrusion rate. The analyzer takes intrusion points at the
specified number of points per decade, ending at the specified end-
ing pressure. Also collected are points in the pressure table, as well
as points separated by the maximum intrusion volume.
If both high pressure ports are in use, they may have different
intrusion rates. In this case, the left port (port 1) determines when
data are collected. The right port collects data at the same times as
the left. This allows a differential analysis to be performed in this
mode.
l Hold at maximum pressure. Enter additional amount of time to
remain at the maximum pressure in a pressure table intrusion seg-
ment before beginning extrusion.
Low Pressure Evacuation . Select if the sample is a Formed solid, Powder, or

[group box] Other. If Other is selected, the remaining fields are enabled. This
window is also available from Unit [n] > Evacuate Low Pressure.

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l Initially evacuate at. Enter the initial maximum evacuation rate.

l Switch to medium at. Enter the method and pressure the system
must reach before medium evacuation begins.
o Use pressure transducer
o User vacuum gauge
o Skip medium evacuation
l Switch to fast at. Enter the pressure the system must reach
before fast evacuation begins.
l Evacuation target. Enter the evacuation pressure.
l Continue evacuating for. Enter the evacuation duration.
Filling pressure. The penetrometer is filled with mercury at this
pressure. It is recommended to set the filling pressure slightly lower
than the first low pressure point on the pressure table.
A filling pressure of at least 0.5 psia is recommended.

Because mercury generates pressure and because fill
pressures less than 0.5 psia can fail to fill the corner radii
and gaps between the glass and sample in the pen-
etrometer, using a lower pressures may reduce the accur-
acy of data.

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962-42800-01 (Rev D) — Nov 2017
Analysis Conditions

If the filling pressure is higher than any point in the table,

an error message occurs. Delete the pressures lower
than the filling pressure or change the filling pressure.
Equilibrate by. Select the option for equilibration based on elapsed

Time (in seconds) or decrease in Rate of intrusion (or extrusion) in
mL/g per second.
Mercury [button] Enter the mercury properties. Mercury properties may change with
variations in temperature.
Advancing contact angle. Enter the advancing (intrusion) contact

angle.
Receding contact angle. Enter the receding (extrusion) contact

angle.
Surface tension. Enter the surface tension of mercury.
Density.
l Enter. Select to manually enter a density.

l Calculate from the measured temperature. Select to use the
entries in the table.
l Linear compressibility. Enter the linear compressibility coef-
ficient.
l Quadratic compressibility. Enter the quadratic compressibility

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962-42800-01 (Rev D) — Nov 2017

coefficient.
Table Options Last Low Pressure. Select the row to indicate the last low pressure.
Starting Pressure. This column is not editable. The data are taken
from the Ending Pressure of the preceding row and the Filling
Pressure for the first row.
Pressure Increment. Enter the pressure increment for this segment

if a sequence of linearly spaced pressures is preferred. Either the
Pressure Increment or Points Per Decade can be specified. If one is
entered, the other is automatically set to zero and displayed as blank.
By default, both columns are blank (zero) when a new row is inserted
or appended. If both columns are blank, only the Ending Pressure will
be used.
Points per Decade. Enter the number of points per decade for this
segment if a sequence of logarithmically spaced pressures is
preferred. Either the Pressure Increment or Points Per Decade (but
not both) can be specified. If one is entered, the other is automatically
set to zero and displayed as blank. By default, both columns are blank
(zero) when a new row is inserted or appended.
Ending Pressure. Enter the ending pressure for this segment.
Maximum Intrusion. The analyzer automatically takes additional

readings between points on the pressure table when this volume of
additional intrusion is detected. Enter the intrusion volume per gram of
sample that must be reached in order for additional data pair readings
to be recorded. Use 0 to prevent readings between pressure points.
See Use of the Maximum Intrusion Volume Option on page E -
1. The Maximum Intrusion entry is set to the same value as the
preceding row by default when a new row is inserted or appended.
Scan Rate. If scanning by pressure, enter the minutes per decade for
this segment. If scanning by intrusion, enter the intrusion rate for this
segment. The Scan Rate column is set to blank (zero) and disabled for
all rows up to and including the Last Low Pressure. If Scan By
Pressure or Intrusion is selected, the column title will display the
appropriate units (min/decade) or (mL/g-sec) and each high pressure
row must contain a value. The value for the previous row is set by
default when a new row is inserted or appended, or the default value
(5 min/decade or 0.001 mL/g-sec) for the first high pressure row.

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962-42800-01 (Rev D) — Nov 2017
Analysis Conditions

Insert Range. Click to display the Enter Pressure Range window for
entering parameters for the system to autofill the table with starting
pressure, ending pressure, and the number of points to insert within
the specified range.
tons on page 2 - 3.

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MATERIAL PROPERTIES
File > Open > [.MTP File]
Material properties specify the properties of the material to be used in an analysis. This information is
only required if it is to be used in a report. See Report Options on page 4 - 11.
Material Properties Fields and Buttons Table

BET Surface Area Enter the BET surface area.
[text box]
Linear compressibility Enter the linear compressibility coefficient.
[text box]
Quadratic com- Enter the quadratic compressibility coefficient.
pressibility [text box]
Use entered con- Select if using the entered conductivity formation factor for per-
ductivity formation meability calculations and enter the factor in the text box.
factor... [check box]
Use entered density Select if using the entered density and enter the bulk and /or true
[check box] density in the appropriate text boxes. The entered values are used in
the intrusion summary results, Mayer-Store report, and the pore
structure report. The Mayer-Stowe particle size calculation has
meaning mostly in the range of interstitial filling. For larger pressures
after which the interstitial space is filled, the particle size calculation
has less meaning.

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962-42800-01 (Rev D) — Nov 2017
Material Properties
Material Properties Fields and Buttons Table (continued)

Use entered threshold Select if using the entered threshold pressure and enter the threshold
pressure [check box] pressure in the text box.
tons on page 2 - 3.

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962-42800-01 (Rev D) — Nov 2017
PENETROMETER PROPERTIES
File > Open > [.PEN File]
Penetrometer properties specify the properties of the penetrometer to be used in an analysis.
Penetrometer Properties Fields and Buttons Table

Maximum head pres- Enter the maximum head pressure. See Select a Penetrometer on
sure [text box] page 5 - 1.
Constant [text box] Enter the penetrometer constant provided with the penetrometer.
Verify the field contents if the Replace option has been used.
Correction Method Blank. If using the blank correction method, click Browse to select a
[selection] sample file. See Create Blank Correction File on page 3 - 6.
Formula. See Formula Correction on page 3 - 7.
None.
Mass [text box] Mass of the empty, assembled penetrometer (excluding the spacer).
Penetrometer Enter identifying information for this file.
[drop-down box]
Stem volume [text box] Enter the penetrometer stem volume provided with the penetrometer.
Volume [text box] Enter the volume of the penetrometer. This is required to calculate
density or when using the blank correction formula. See Calibrate the
Penetrometer on page 9 - 4.
tons on page 2 - 3.

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Report Options
REPORT OPTIONS
File > Open > [.RPO File]
(or click the Report Options tab when in Advanced format)
Use to specify report options for data collected from an analysis or manually entered data. Report
Options files also help in customizing report details such as axis scale, axis range, and column
headings. These files may contain tabular reports, plots, or both, as well as user-defined report
tables.
Customized report options files can be created then loaded into a sample file, allowing quick and
easy generation of reports.
Report Options files may be defined to include overlay options. This system allows the overlay of up
to 25 plots of different samples onto a plot of the same type or overlay one plot type onto a different
plot type from the same analysis. See Overlay Multiple Mercury Porosimetry Graph Options
on page 6 - 24.
Report Options Fields and Buttons Table

Edit [button] Edit graph options.
Plot Points. Select to plot points on the graph.
Plot Curve. Select to plot curves on the graph.
Show Histogram. Select to show the graph as a histogram. When

selected, the Plot Points and Plot Curve selections are disabled.

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962-42800-01 (Rev D) — Nov 2017
Report Options Fields and Buttons Table (continued)

Header Options [button]
Show report title. Enter a report title to appear on the report header.
Show bitmap. Displays the selected graphic on the report header.
Height / Width. Enter the height and width of the selected graphic.
These values determine the graphic appearance on the generated
report.

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962-42800-01 (Rev D) — Nov 2017
Report Options

Intrusion Data Options This button is also located on Intrusion reports.
[button]
Adjust intrusion for compressibility:
l Use coefficients from compressibility report. Select to have

the application use the coefficients from the Material Com-
pressibility report rather than from the Material Properties.
l Use material properties. Select to have the application use the
parameters from Material Properties rather than from the Material
Compressibility report.
Report negative intrusion. Select to report small incorrect polarities
(negative intrusions or positive extrusions) which may indicate the
presence of noise, improper blank correction, or analyzer malfunction.
Select Data Included in Intrusion Reports. Enter range of

pressure. This range applies to the first twelve reports on the options
list. When these selections are changed in the intrustion report, the
lower right graph x-axis and the intrusion data in the graph will change
accordingly. The two blue range bars can then be used to select the
required range of data.
l Pressure. The default behavior of the application is to select data

using pressure as this is the quantity which is varied during mercury
porosimetry analysis. The maximal range of data (all data) is selec-
ted by default. It is advisable to use this default setting unless there
is a specific goal is required.

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962-42800-01 (Rev D) — Nov 2017

l Pore size. Uses the Washburn equation to translate the user

entered pore size range to a corresponding pressure range used for
data selection.
l Particle size.This option is less commonly used. In the Material
Properties window, select the checkbox Use entered density and
complete the Bulk density and effective Particle density fields. See
Material Properties on page 4 - 8. The effective Particle density
and Bulk density quantities are necessary to compute the interstitial
porosity of the powder used in the Mayer-Stowe calculation.
Smooth differentials. Select to apply smoothing to any differentials
reported in tables or graphs.
Overlays [button] Select the files to overlay.
Reference [button] Select a sample file to compare analysis results with the current
sample.
Selected Reports Select the report names to include in the report.

[check box]

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962-42800-01 (Rev D) — Nov 2017
Report Options

Specification [button] Selects the sample files to be used for the boundaries of the coarse
and fine specifications. This helps in determining if the results of the
current sample are within the specified boundaries.
tons on page 2 - 3.

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962-42800-01 (Rev D) — Nov 2017
5 Perform an Analysis
5 PERFORM AN ANALYSIS
A low pressure analysis must be performed on a sample before a high pressure analysis can be
performed.
SELECT A PENETROMETER
Selecting the most appropriate penetrometer with which to test a particular material depends on
sample form or shape, sample porosity, and the quantity of sample.
Penetrometers are available with three sample volumes, with five intrusion capacities, and in
configurations for either solid pieces or powders. Refer to the Penetrometer Selection Guide in this
section.
Ensure the sample nearly matches the size of the sample bulb and that the capillary volume is large
enough to satisfy intrusion.
Penetrometer Selection Guide

Maximum
Bulb Sample Maximum Total Head Physical Dimensions Part
Type Measurable Stem Pressure Number
Volume
Volume Volume (psia) (kPa) I (mm) H (mm) D (mm)
(cc) (cc) (cc)
3 Solid 0.387 0.412 4.68 32.3 227 242 1.473 950-61713-00

3 Solid 1.116 1.190 4.68 32.3 227 242 2.502 950-61715-00
3 Powder 0.387 0.412 4.68 32.3 227 242 1.473 950-61714-00
3 Powder 1.116 1.190 4.68 32.3 227 242 2.502 950-61716-00
5 Solid 0.366 0.392 4.45 30.7 215 230 1.473 950-61707-00
5 Solid 1.057 1.131 4.45 30.7 215 230 2.502 950-61709-00
5 Solid 1.716 1.836 4.45 30.7 215 230 3.188 950-61711-00

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962-42800-01 (Rev D) — Nov 2017
Penetrometer Selection Guide (continued)

Maximum
Bulb Sample Maximum Total Head Physical Dimensions Part
Type Measurable Stem Pressure Number
Volume
Volume Volume (psia) (kPa) I (mm) H (mm) D (mm)
(cc) (cc) (cc)
5 Powder 0.366 0.392 4.45 30.7 215 230 1.473 950-61708-00

5 Powder 1.057 1.131 4.45 30.7 215 230 2.502 950-61710-00
5 Powder 1.716 1.836 4.45 30.7 215 230 3.188 950-61712-00
15 Solid 0.366 0.392 4.45 30.7 215 230 1.473 950-61701-00
15 Solid 1.057 1.131 4.45 30.7 215 230 2.502 950-61703-00
15 Solid 1.716 1.836 4.45 30.7 215 230 3.188 950-61705-00
15* Solid 3.007 (3.263) 4.45 30.7 215 230 4.813 950-61724-00
15* Solid 3.857 (4.185) 4.45 30.7 215 230 4.813 950-61725-00
15 Powder 0.366 0.392 4.45 30.7 215 230 1.473 950-61702-00
15 Powder 1.057 1.131 4.45 30.7 215 230 2.502 950-61704-00
15 Powder 1.716 1.836 4.45 30.7 215 230 3.188 950-61706-00
* The first 3 mm of stem on these penetrometers have an inside diameter (D) of 1.5 mm. In
computing maximum measurable (intrusion) volume, the value of I should be reduced by 3 mm.
l Maximum measurable volume = [(3.14)(D2)(I)/4] × [0.001

cm3/mm3]
l Total Stem (Capillary) volume = [(3.14)(D2)(H)/4] × [0.001
cm3/mm3]
l Maximum Head Pressure (psia) = [H] × [0.01934 psia/mmHg]
l Maximum Head Pressure (MPa) = [H] × [0.000133 MPa/mmHg]
A powder penetrometer should be used when the sample consists of small grains or particles.
Chunks of material or formed objects (maximum size is 25 mm OD × 25 mm long) should only be
installed in a “solid” penetrometer.

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962-42800-01 (Rev D) — Nov 2017
Select a Penetrometer
Best results, generally, are obtained when the bulb of the selected penetrometer is nearly filled by
the minimum amount of sample that is representative. Next, the estimated pore volume of the
sample should not exceed 90% nor be less than 25% of the total stem volume (see column 4 of the
Penetrometer Selection Guide). Once materials of similar characteristics have been tested, it will
usually be possible to select the optimum penetrometer almost without fail.
As an example, suppose the sample consists of a single sintered pellet of nickel (density 8.9 g/cc)
weighing 29 g and having an estimated pore volume of 20% of the true sample volume to analyze.
The following characteristics are calculated:
Volume of sample = mass/density = (29g)/(8.9g/cc) = 3.26 cc
Approximate pore volume = fractional pore volume × sample volume =

0.20 (3.26 cc) = 0.652 cc
Approximate total volume = volume of pores + volume of sample

(3.26 + 0.652) cc = 3.91 cc
Hence, the penetrometer listed sixth in the Penetrometer Selection Guide as solid, 5 cc sample
volume, 1.131 cc total stem volume would be the appropriate choice unless the pellet shape dictates
use of a larger one. The percent of maximum measurable intrusion volume required by this sample is
(0.652 cc/1.131 cc) × 100% = 58%, which falls below the suggested 90% maximum.
The penetrometer for powdered or granular materials is chosen similarly, but remember that the
spaces among the material grains are likely to constitute a void of about 40%. As another example,
assume that 15 g of a granular material (density 3.5 g/cc) had been determined the minimum
quantity for representation. Assume the powder has low porosity: 3%.
Volume of sample = mass/density = (15 g)/(3.5 g/cc) = 4.29 cc
Approximate pore volume of material = fractional porosity x sample volume =

0.03 (4.29 cc) = 0.13 cc
Approximate volume of interstice = (4.29 cc + 0.13 cc) (40/60) = 2.95 cc
Total volume of powdered sample = 4.29 cc + 0.13 cc + 2.95 cc = 7.37 cc
Three powder penetrometers listed in the Penetrometer Selection Guide will contain 7.37 cc of
sample. Considering the sample size, the one having a total stem volume of 0.392 cc is most
appropriate. The sample requires approximately 33% [0.13/0.39] of the stem capacity of the
penetrometer. Optimum performance would be achieved if, instead of merely using the minimum 15
g of sample, the penetrometer were filled to capacity, which is approximately 30.5 g [15 × 15/7.37].
The penetration volume would then be about 0.26 cc [0.13 × 15/7.37] or nearly 66% [0.26/0.39] of
the total stem volume.

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962-42800-01 (Rev D) — Nov 2017
The previous calculations assume that all interstitial volume will be filled with mercury at
the filling pressure. A minimum fill pressure of 0.5 psia will fill cavities of approximately
500 mm diameter, whereas a filling pressure of 1.5 psia will fill cavities as small as 120
mm diameter. If some interstitial volume remains unfilled at this point, allowance for this
additional volume must be made in choosing the appropriate stem volume.
The percentage of the maximum intrusion (stem) volume utilized in each station is displayed on the
Status Display as a guide for the operator. A % STEM reading of less than 25% or more than 90%
suggests the need for a procedural change. The first instance suggests a larger quantity of sample
might give better resolution and the second indicates that the capillary is on the verge of being
depleted.

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962-42800-01 (Rev D) — Nov 2017
Prepare the Sample
PREPARE THE SAMPLE

To achieve gains in productivity and reduction in analyzer maintenance, as well as improved data
quality, dry the sample material in a shallow pan at 150 ºC or higher for one hour. A vacuum oven
may be used, although it is not necessary to do so. Use of a vacuum oven is particularly beneficial if
the oven is backfilled with dry nitrogen prior to opening. Once the sample is dried, minimize any re-
exposure to the atmosphere.
The drying of samples prior to analysis is important, especially for sample types such as fluid
cracking catalysts, porous silicas, porous aluminas, and zeolites, which are almost impossible to
evacuate without fluidization unless first dried.
The preparation process consists of:
1. Clean the Penetrometer below

2. Load the Sample on the next page
3. Seal the Penetrometer on page 5 - 7
4. Weigh the Assembled Penetrometer with Sample on page 5 - 9
5. Install the Penetrometer on page 5 - 10
CLEAN THE PENETROMETER

Clean, dry penetrometers are essential for accurate, reproducible results.
It is recommended that rubber gloves be worn when handling penetrometers.
Never use an ultrasonic bath to clean penetrometers. Ultrasonic cleaning systems will
damage the metal plating and remove the serial number information.
1. Dissolve Alconox® (or other suitable detergent) in water. Ensure the detergent is completely
dissolved before placing the penetrometer into the solution.
2. Place the mercury waste container in a shallow pan of water in case of spills.
3. Hold the penetrometer upright over a mercury waste container to allow any accumulated mer-
cury to drain out.
4. Remove the cap from the penetrometer If the cap is difficult to remove, see Penetrometer
Nut on page 11 - 34.
5. Turn the penetrometer over and pour remaining sample into the waste container.
6. Immerse the penetrometer in the detergent solution. Clean the outside of the penetrometer
stem and the bulb with a brush. Then clean the inside of the stem with one of the smaller
brushes.

5-5
962-42800-01 (Rev D) — Nov 2017
7. Rinse the penetrometer with warm water. Hold the penetrometer upright and enure that water
runs from the bulb through the stem freely.
8. Rinse the penetrometer with IPA.
9. Immerse the stainless steel cap and nylon closure components in the detergent solution.
Clean with appropriate brushes and rinse in warm water.
10. If there is any mercury in the bottom of the detergent solution, dispose of the solution properly.
11. Use dry nitrogen to dry the penetrometer, cap, and closure components.
LOAD THE SAMPLE
To avoid transferring skin oils, it is recommended to wear latex gloves when handling
penetrometers. Skin oils may affect results.
1. Enter the sample file name (or identifier) on the Sample Data Worksheet on page F - 6.
2. Weigh the sample using an analytical balance. Record the mass on the data sheet as Sample
mass.
3. Hold the penetrometer with the stem down and carefully pour the sample into the bulb.
When pouring powders into the bulb, place a finger over the stem opening in the center of the
bulb so that powder does not enter the stem. A small funnel is useful for loading powders.
Large granules or chunks may be loaded with forceps.

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962-42800-01 (Rev D) — Nov 2017
Seal the Penetrometer
SEAL THE PENETROMETER
It is important that penetrometers are clean and dry. See Clean the Penetrometer on page 5 - 5.
1. A vacuum-tight seal is required. Therefore, vacuum grease (Apiezon H) must be used to fill
the inevitable roughness of the ground glass lip and polished surface of the cap. To apply
grease:
Follow these instructions carefully. Too much grease exposes the sample to an
unwanted coating and is likely to cause slippage and misalignment of the mating
surfaces. Too little grease results in an imperfect seal.
a. Use a fingertip to apply a light coating of grease to the lip of the bulb.
b. Smooth the grease evenly around the lip of the bulb.
c. Remove all excess grease from both the inside and outside of the bulb.
2. Hold the penetrometer upright. Place a cap over the greased bulb and turn the cap one half
turn to seat.

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962-42800-01 (Rev D) — Nov 2017
3. Place the penetrometer tool over the nut.
4. Place the wrench peg into a hole in the penetrometer nut. Use the penetrometer tool to
stabilize the cap while tightening the nut counter-clockwise.

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962-42800-01 (Rev D) — Nov 2017
Weigh the Assembled Penetrometer with Sample
5. Weigh the penetrometer before installing it in the low pressure port. See Weigh the
Assembled Penetrometer with Sample below.
WEIGH THE ASSEMBLED PENETROMETER WITH SAMPLE
1. Weigh the assembled penetrometer with sample using an analytical balance. Do not include
the spacer when weighing.
2. Record the mass on the Sample Data Worksheet as Sample + Penetrometer mass.
3. Subtract Sample mass from Sample + Penetrometer mass. Record on the Sample Data
Worksheet as Penetrometer mass.
The mass of the penetrometer must be determined by this method in order to account
for the mass of the sealing grease, which varies with each application.

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962-42800-01 (Rev D) — Nov 2017
INSTALL THE PENETROMETER
l Install a Penetrometer in a High Pressure Chamber on page 10-1

l Install a Penetrometer in a Low Pressure Port on page 10-3
l Remove a Penetrometer from a High Pressure Chamber on page 10-5
l Remove a Penetrometer from a Low Pressure Port on page 10-6

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962-42800-01 (Rev D) — Nov 2017
Perform a Low Pressure Analysis
PERFORM A LOW PRESSURE ANALYSIS

Unit [n] > Low Pressure Analysis
l Select the sample files for analysis for each port

l Edit the penetrometer properties
l Edit analysis conditions
l Monitor analysis as data are collected
Prior to starting an analysis, verify that the tank pressure for the gas regulator is at least
200 psig. Pressures less than 200 psig may cause inaccurate data or termination of ana-
lysis.
1. Select Operation from the View drop down to enter or edit analysis information.
2. Install a Penetrometer in a Low Pressure Port. Install a steel rod with cap detector in any low
pressure port that does not contain a penetrometer. See Install a Penetrometer in a Low
Pressure Port on page 10-3.
3. For a selected port, click Browse and select a sample file or click New to create a sample file.
If needed, change the Penetrometer mass and/or Sample mass field for the sample material
being analyzed.
4. Click Start to start the analysis. A window displays data as they are collected. A short delay is
encountered before the port status at the bottom of the window changes from the Idle state.
See Monitor a Low Pressure Analysis on page 5 - 15.

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962-42800-01 (Rev D) — Nov 2017
l When the Start button is clicked, if any low pressure station does not show a cap
detector reading that indicates the station has a penetrometer or rod and its cap
detector in place, a warning message will be displayed and the analysis will not start.
l When the next scheduled pressure is above atmospheric pressure and a cap
detector and rod or pen is not in place, the same warning will be displayed and the
analysis will be suspended until the operator has corrected the problem and
resumed.
l If a cap detector is removed when the pressure is above atmospheric pressure, the
low pressure system will be vented to atmosphere and the analysis canceled, with an
explanatory error message.
5. When the analysis is complete, remove the penetrometer and store (or dispose of) the sample
material as applicable. See Remove a Penetrometer from a Low Pressure Port on
page 10-6.
Low Pressure Analysis Fields and Buttons Table
Penetrometer mass This information is pulled from the selected sample file. Modify the pen-
etrometer mass in this field as needed.
Sample mass This information is pulled from the selected sample file. Modify the
sample mass in this field as needed.
tons on page 2 - 3.

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962-42800-01 (Rev D) — Nov 2017
Evacuate Low Pressure
EVACUATE LOW PRESSURE

See Low Pressure in Analysis Conditions on page 4 - 2
Unit [n] > Evacuate Low Pressure

Select the type of sample when performing a low pressure evacuation. This window is also available
using the Evacuation button on the Analysis Conditions tab.
Select if the sample is a Formed solid, Powder, or Other. If Other is selected, the remaining fields are
enabled.
Evacuate Low Pressure Fields and Buttons Table

Initially evacuate at Enter the initial maximum evacuation rate.
Switch to medium at Enter the method and pressure the system must reach before medium
evacuation begins.
l Use pressure transducer

l User vacuum gauge
l Skip medium evacuation .
Switch to fast at Enter the pressure the system must reach before fast evacuation

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962-42800-01 (Rev D) — Nov 2017
Evacuate Low Pressure Fields and Buttons Table (continued)

begins.
Evacuation target Enter the evacuation pressure.
Continue evacuating Enter the evacuation duration.
for
GENERATE LOW PRESSURE

Unit [n] > Generate Low Pressure
Pressure can be generated in the low pressure system when a low pressure analysis is not already
in progress.
Threaded penetrometer closures are required for pressures above 30 psia or

0.2068 MPa.

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962-42800-01 (Rev D) — Nov 2017
Monitor a Low Pressure Analysis
MONITOR A LOW PRESSURE ANALYSIS

This live graph displays data as they are collected. It also shows intrusion as a function of pressure.
The status section below the graph displays the following for each port:
l Sample file name

l Intrusion volume
l Percent of the penetrometer stem that is filled with mercury
When monitoring a low pressure analysis, the analyzer schematic can be displayed to
show the state of the low pressure system components. See Show Instrument
Schematic on page 2 - 16.
Low Pressure Analysis Fields and Buttons Table

Pressure Displays the current pressure in the low pressure system. The reading
shown is from either the vacuum gauge or the 50 psia transducer,
depending upon which is currently in range.
Resume Restarts the suspended analysis.
Skip Moves to the next step. Select the ports to skip.
Status Displays current low pressure status.
Suspend Suspends an analysis in progress.
tons on page 2 - 3.

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962-42800-01 (Rev D) — Nov 2017
PERFORM A HIGH PRESSURE ANALYSIS

The analyzer is designed to perform two high pressure analyses simultaneously. To run only one
analysis, the other chambers must be closed tightly and have sufficient high pressure fluid to be
drawn into the vent valve.
Unit [n] > High Pressure Analysis

Low and high pressure analyses can be performed simultaneously.
l Select the sample files for analysis for each port

l Edit the penetrometer properties
l Edit analysis conditions
l Monitor analysis as data are collected
Each sample’s high pressure analysis should be performed on the same analyzer as the
low pressure analysis. The analyzer checks to see that the same analyzer is used before
it begins the high pressure analysis; if it is not, the analyzer displays a warning message.
The analysis can be continued or canceled.
1. Select the sample file with a status of Low Pressure Complete or High Pressure Complete.
If a selected sample file to be analyzed on a 9605 analyzer contains pressures exceeding
33,000 psia, the following message displays:
l Click Yes to proceed with the analysis; only pressures less than
33,000 psia will be used.
l Click No to cancel the analysis.

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Perform a High Pressure Analysis
2. Install a Penetrometer in a High Pressure Port. See Install a Penetrometer in a High Pres-
sure Chamber on page 10-1.
3. Click Start to start the analysis immediately. A live graph of the analysis displays as data are
being collected. See Monitor a High Pressure Analysis on page 5 - 19.
4. Remove the penetrometer after the analysis. See Remove a Penetrometer from a High
Pressure Chamber on page 10-5.
If it was not requested that the transducer offset be determined (Options >
Atmospheric Pressure), and if the current high pressure reading differs significantly
from the atmospheric pressure, a prompt displays requesting verification that the system
is at atmosphere.
For maintenance purposes, it is possible to perform a high pressure analysis with no

penetrometer. Open the High Pressure Analysis window and enter the name of a file
with a No Analysis status. Continue the analysis after a warning message displays.
High Pressure Analysis Fields and Buttons Table

Analysis type Regular. Performs a differential analysis with the blank penetrometer
in port 1.
Differential, blank in port 1. Performs a differential analysis with the

blank penetrometer in port 1.
Differential, blank in port 2. Performs a differential analysis with the

blank penetrometer in port 2.
See High Pressure Differential Analysis on page 5 - 20

Assembly mass Sample + penetrometer + mercury mass.
Atmospheric pressure Enter the atmospheric pressure if it differs from the default entry. The
default entry is pulled from the information entered in Options
> Atmospheric Pressure.
Determine transducer Select to allow the system to determine the transducer offset. The
offset default entry is pulled from the information entered in Options
> Atmospheric Pressure.
tons on page 2 - 3.

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GENERATE HIGH PRESSURE

Unit [n] > Generate High Pressure
Pressure can be generated in the high pressure system when a high pressure analysis is not already
in progress.

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Monitor a High Pressure Analysis
MONITOR A HIGH PRESSURE ANALYSIS

This live graph displays data as they are collected. It also shows an intrusion as a function of
pressure. The status section below the graph displays the following for each port:
l Sample file name

l Intrusion volume
l Percent of the penetrometer stem that is filled with mercury
When monitoring a high pressure analysis, the analyzer schematic can be displayed to
show the state of the high pressure system components.
High Pressure Analysis Fields and Buttons Table

Pressure Displays the current pressure in the high pressure system.
Skip Moves to the next step. Select the ports to skip.
Resume Restarts the suspended analysis.
Status Displays the high pressure's current status.
Suspend Suspends an analysis in progress.
tons on page 2 - 3.

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HIGH PRESSURE DIFFERENTIAL ANALYSIS

If using a blank correction file as the correction method, the correction file must exist before the
sample data file can be completed (since a blank correction file must be selected when the sample
file is created).
If a blank analysis has not been performed in advance, run a differential analysis of the sample and
the corresponding blank simultaneously. The application associates the sample file with the blank
correction file after the analysis is completed.
An advantage of using differential analysis is that both the sample and blank penetrometers are
subjected to nearly identical conditions (time, temperature, and pressure). Properly used, the
differential analysis option provides the most accurate low porosity sample data possible.
1. Create a sample file. Also create a sample file for the blank penetrometer using Nonefor the
correction method. See Sample Files on page 3 - 1.
2. Run the low pressure analysis on both files. See Perform a Low Pressure Analysis on
page 5 - 11.
3. To start the high pressure analysis, select either the Differential, Blank in port 1 or Differential,
Blank in port 2. Perform a high pressure analysis. See Perform a High Pressure Analysis
on page 5 - 16.

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Reference Material Analysis
REFERENCE MATERIAL ANALYSIS

HIGH PRESSURE REFERENCE MATERIAL ANALYSIS
Unit [n] > High Pressure Reference Analysis
A reference material analysis is used to verify the analyzer is operating properly and producing
optimum results. These methods provide specifications for critical report quantities and reporting of
whether quantities are in or out of specification.
When running a reference material analysis, use the appropriate reference material provided in the
accessories kit to perform this analysis. The results should match those shown on the label of the
reference material bottle, within the tolerance level.
High Pressure Reference Material Analysis Fields and Buttons Table

Assembly mass This information is pulled from the selected sample file.
Sample + penetrometer + mercury mass.
tons on page 2 - 3.

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LOW PRESSURE REFERENCE MATERIAL ANALYSIS

Unit [n] > Low Pressure Reference Analysis
A reference material analysis is used to verify the analyzer is operating properly and producing
optimum results. These methods provide specifications for critical report quantities and reporting of
whether quantities are in or out of specification.
When running a reference material analysis, use the appropriate reference material provided in the
accessories kit to perform this analysis. The results should match those shown on the label of the
reference material bottle, within the tolerance level.
Low Pressure Material Reference Material Analysis Fields and Buttons Table
Penetrometer Penetrometer description from the selected sample file.
Penetrometer mass Penetrometer mass from the selected sample file.
Sample mass Sample mass from the selected sample file.
tons on page 2 - 3.

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Leapfrogging - Suggested Sequence for Maximum
Throughput
LEAPFROGGING - SUGGESTED SEQUENCE FOR MAXIMUM THROUGHPUT

Leapfrogging is a procedure for running low and high pressure systems simultaneously to maximize
throughput. This process describes leapfrogging a group of eight samples. It is possible to leapfrog
groups of samples continuously.
If samples require longer vacuum preparation or heated evacuation, increase the

throughput by preparing samples in a vacuum oven.
1. Prepare and weigh eight samples. Load eight penetrometers with samples then weigh them.
Complete the Sample Data Worksheet on page F - 6 and install samples 1 through 4 in
the low pressure ports.
2. Create sample files for at least the first four samples.
3. Go to Unit [n] > Low pressure analysis to start the low pressure analysis.
4. When the run is complete, remove samples 1 through 4 from the low pressure ports and
weigh them. Install samples 5 through 8 in the low pressure ports.
5. Start another low pressure run.
6. Place samples 1 and 2 in the high pressure chambers.
7. Go to Unit [n] > High pressure analysis to start the high pressure analysis.
While waiting for analysis to complete, samples files can be created and other samples
can be prepared for analysis.
8. When the high pressure run is complete, remove samples 1 and 2 from the high pressure
chambers and replace with samples 3 and 4.
9. Start another high pressure run.
10. Automatic reports specified in each sample file will print when that sample’s high pressure run
ends.
11. When the second low pressure run and the second high pressure run end, remove samples 3
and 4 from the high pressure chambers. Remove samples 5 through 8 from the low pressure
ports and weigh them.
12. Install samples 5 and 6 in the high pressure chambers. Start another high pressure run.
13. When the third high pressure run is finished, install samples 7 and 8 in the high pressure cham-
ber and start another high pressure run.

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6 About Reports
6 ABOUT REPORTS
Reports > Open Report > [.REP file]
Opens a saved report.
Reports > Close Reports

Closed all open reports. This option is unavailable if reports are being generated.
Reports > Start Report

Generates a report an a sample analysis.
Reports can be generated for data collected on a sample that has completed analysis, collected on a
sample currently being analyzed, or manually entered.
SPC REPORT
Reports > SPC Report Options
Use to generate reports with various SPC (Statistical Process Control) options. All selected
variables must be computed for each sample file used in an SPC report; therefore, it is more efficient
to select only the necessary variables.

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6 About Reports
REGRESSION REPORT
Reports > Regression Report
Use to generate a Statistical Process Control (SPC) Regression report to determine the
interdependency between two variables. Up to three dependent variables (y-axis) may be plotted
against a single independent variable (x-axis). The degree of correlation between the variables is
also reported.
Regression Report Fields and Buttons Table

Autoscale [check box] When enabled, allows the x- and y-axes to be scaled automatically.
Axis Range [text box] Enter the beginning and ending values for the x- and y-axis ranges.
These fields are disabled if Autoscale is selected.
Label data [check box] Use to label the points on the plot to correspond with the values in the
sample files.
Recalculate archived Use to have archived SPC values recalculated ensuring any changes
SPC results [check box] made to the SPC Report Options are included in the new report. This
option lengthens the time required to generate the report.
If this recalculation option is enabled and sample files from

an earlier application version are selected, it is recom-
mended that copies of the archived sample files be used
rather than the original. Selecting this option will make
some archived sample files unreadable by the original
application. If an earlier application version will not be
reused, this warning message can be safely disregarded.
When this option is selected, this message will display:

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Regression Report
Regression Report Fields and Buttons Table (continued)

Saving the recalculated SPC data may render some files
unreadable by the original application. Saving the SPC
data speeds up future SPC reports.
If Do not show me this message again is selected, the mes-

sage cannot be redisplayed without Micromeritics assist-
ance.
The first time this option is used, the time it takes to generate the report
is lengthened. The second time the report is generated, if using the
same sample files used in the initial calculation, it is recommended that
this option not be selected since the data was recalculated previously.
If a sample file is added or removed from the report after the initial
recalculation, this option should be selected again to ensure the data
from the newly added or removed sample file is recalculated.
Samples [button] Select additional sample files to add to the report.
Save as Default [button] Click to save selected report options as default report settings.
Show graphic Use to show a graphic on the report header.
[check box]
report.
Show report title Select and enter a report title to appear on the report header.
[check box]
Tabular report Generates a tabular report of the included samples. A tabular report
[check box] contains the numeric values contributed by each sample.
X- and Y-Axis Variable Use to designate the x- and y-axes variables. The variables in the
[drop-down box] drop-down lists are those selected in the Reports > SPC Report
Options window. Use these options to plot the regression of up to
three y-axis variables against the x-axis variable.
tons on page 2 - 3.

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6 About Reports
CONTROL CHART REPORT

Reports > Control Chart
Generates a Statistical Process Control (SPC) control chart report which plots the changes in a
statistic.
Control Chart Fields and Buttons Table

Graph [n] [button] Defines the y-axis of each graph.
Statistic. Displays the SPC variables selected on the Reports >

SPC Report Options window. The selected variable will be plotted
for each selected sample. This selection also becomes the y-axis label.
Autoscale. Allows the y-axis to be scaled automatically. To specify a

range, deselect this option and enter a range in the From and To fields.
Center Line. Displays placement options for the center line in the
graph. Select Entered to specify placement of the line or Mean to place
the center line at the calculated mean value for the selected samples.
Limit Lines group box. Displays limiting lines options. Lines can be
placed at some multiple of the standard deviation or at specified
positions (Entered). When Entered is selected, enter the High limit and
Low limit fields with appropriate values.

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Control Chart Report
Control Chart Fields and Buttons Table (continued)

Recalculate archived Use to have archived SPC values recalculated ensuring any changes
SPC results [check box] made to the SPC Report Options are included in the new report. This
option lengthens the time required to generate the report.
If this recalculation option is enabled and sample files from

an earlier application version are selected, it is recom-
mended that copies of the archived sample files be used
rather than the original. Selecting this option will make
some archived sample files unreadable by the original
application. If an earlier application version will not be
reused, this warning message can be safely disregarded.
When this option is selected, this message will display:
Saving the recalculated SPC data may render some files

unreadable by the original application. Saving the SPC
data speeds up future SPC reports.
If Do not show me this message again is selected, the mes-

sage cannot be redisplayed without Micromeritics assist-
ance.
The first time this option is used, the time it takes to generate the report
is lengthened. The second time the report is generated, if using the
same sample files used in the initial calculation, it is recommended that
this option not be selected since the data was recalculated previously.
If a sample file is added or removed from the report after the initial
recalculation, this option should be selected again to ensure the data
from the newly added or removed sample file is recalculated.
Report [button] Generates the report.
Show graphic Use to show a graphic on the report header.
[check box]
report.
[check box]
Tabular report Generates a tabular report of the included samples. A tabular report
[check box] contains the numeric values contributed by each sample.

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6 About Reports
Control Chart Fields and Buttons Table (continued)

X Axis Order by Select the order in which x-axis statistics are placed. Sort by:
[group box]
Time. Time the files were analyzed.
File name. Alphanumeric order.
Date. Date the files were analyzed.
Minutes. Minutes elapsed from the first file placed on the list, which is
the earliest-analyzed file.
Days. Number of days elapsed from the first file placed on the list,
which is the earliest-analyzed file.
tons on page 2 - 3.

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PSD History Report
PSD HISTORY REPORT

Reports > PSD History
The PSD History Report generates a sequence of full pore size distribution graphs.
PSD History Report Fields and Buttons Table

Report [button] Generates the report.
Save as Default [button] Click to save selected report options as default report settings.
Show [selection] Select one of the following options:
First Intrusion. Select to show the first intrusion segment.
First Extrusion. Select to show the first extrusion segment.

Show bitmap Use to show a graphic on the report header.
[check box]
report.
[check box]

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6 About Reports
PSD History Report Fields and Buttons Table (continued)

X-axis Order By Select one of the following:
[selection]
Time. Time the files were analyzed.
File name. Alphanumeric order.

X Axis variable Select one of the following to display on the graph:
[selection]
Pressure.
Pore size.
Y Axis variable Select one of the following to display on the graph:
[selection]
Diff. volume.
Diff. % volume.
Diff. area.
tons on page 2 - 3.

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Interactive Reports
INTERACTIVE REPORTS
When opening a sample file that contains data from a complete or in-progress analysis, the
interactive reporting feature is enabled.
1. When opening a sample file that contains analysis data, a window with the following inform-
ation will display:
l an intrusion linear plot and log plot of the data collected during analysis
l a summary of the analysis giving a single total intrusion volume and other important quant-
ities
2. Modify the intrusion graph to show all or first intrusion and/or extrusion segments by selecting
an option from the Intrusion or Extrusion drop-down lists.
3. Add an overlay to the intrusion graph by selecting an option from the Overlay drop-down list.
4. To view the reports selected for generation during or after analysis, click Preview.
5. From the drop-down list at the bottom of the window:
l change the option presentation of the sample information window to either Basic or
Advanced to modify certain file parameters, or
l select another plot from the list and edit the data contained in the plot.
6. When ranges are edited, the changes are reflected immediately in the plots and the summary
data displayed in the window. Some editing options are:
l Drag the blue bars to increase or decrease the range of data included in the plot.
l Right click to display a popup menu to include reports; enable or select overlays; edit
curves, axes, legends, titles; and copy and paste the data in a graph or in tabular format
7. Click Save.

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6 About Reports
MICROACTIVE REPORTS
MicroActive reports are generated automatically after an analysis is performed. This feature
provides a quick and easy way to investigate and manipulate analysis data using a variety of
reporting methods.
When a sample file with a status of Complete, Analyzing or Entered is opened, a linear plot and log
plot of the data collected during analysis are displayed as well as a summary of the analysis giving
the total pore volume. Numerous reports are accessible from a drop-down menu.
When a report is opened, plots and summary data are displayed, and in some reports certain
parameters (for example, permeability constant and pore shape exponent) are also displayed. Plots
may be edited by selecting the data points or data point range to be included in the plots and
modifying the parameters. When a report is edited, the results are immediately reflected in the plots
and summary data.
Log in to your customer portal to access MicroActive Report Tutorials.

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Report Features and Shortcuts
REPORT FEATURES AND SHORTCUTS

Reports can be customized and manipulated using the toolbar, shortcut menus, the zoom feature, or
axis cross-hairs.
l After analysis, reports can be viewed, printed, and/or copied and pasted into other documents.
l The report zoom feature provides the viewing of fine graph details and the ability to shift the axes.
l All reports contain a header displaying file statistics.
If configured, the report header can also contain a graphic and/or a title.
l Tabular and graphical reports contain sample and analyzer statistics such as analysis date / time,
analysis conditions, etc.
l The headers contain notes of sample file changes occurring after analysis.
l Summary report headers contain the same information as tabular and graphical reports with the
exception of notes.

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6 About Reports
REPORT HEADER SHORTCUTS

Display header shortcuts by right clicking in the report header.
If configured, the report header can also contain a graphic and a title.
l Tabular and graphical reports contain sample and analyzer statistics — such as analysis date,
analysis time, analysis conditions, etc.
l The headers contain notes of sample file changes occurring after analysis.
l Summary report headers contain the same information in tabular and graphical reports with the
exception of notes.
Report header Shortcut Field and Button Table
Copy header as text Use to copy the report header as text. Text is copied to the clipboard
and then can be pasted into other documents.
Edit Use to edit the report title and/or graphic in the report header.

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Report Toolbar
REPORT TOOLBAR
The Report window has a toolbar on the right portion of the window and selectable tabs at the top of
the report header. To view a specific report, either select the tab or the report in the Reports list box,
then click Show.
Report Toolbar Fields and Buttons Table

Default Style [button] Specify default report parameters for fonts and curve properties.
Delete [button] Deletes the selected report in the Reports list box. Deleted reports will
have to be regenerated if deleted in error.
Hide [button] Hides (or temporarily removes) the selected report from the tabbed
view. The report name remains in the Reports list box.
Print [button] Displays the Print window for report output.
Reports [group box] Contains a list of all generated reports. The same reports display as
tabs at the top of the report header unless the report has been hidden
using the Hide button.
Show [button] Displays the selected or hidden report in the Reports list box.
tons on page 2 - 3.

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6 About Reports
TABULAR REPORT FEATURES AND SHORTCUTS

Display tabular report shortcuts by right clicking in the body of the tabular report. Column shortcuts
require right clicking on the column to be modified.
Tabular Reports Shortcut Options and Descriptions Table

Align column Select to change the column alignment to either left, right, or centered.
Copy table as text Use to copy the report contents to the clipboard as tab-delimited text. It
can then be pasted into another document.
Edit title Use to edit the report title and/or title font attributes. Click Font to
modify font attributes.
Move column Right click the column to be moved. Select Move column on the short-
cut menu and select Left or Right for the move.
Rename column Right click the column to be renamed. Select Rename column on the
shortcut menu and enter the new column name.
Resize column Right click the column to be resized. Select Resize column on the short-
cut menu and enter the new column width in inches.
Show column Displays a list of all columns. Click a column to add a checkmark to
show the column or remove the checkmark to hide the column.
Table data font Right click in the report data. Select Table data font on the shortcut
menu.
Table header font Right click in the report data. Select Table header font on the shortcut
menu.
tons on page 2 - 3.

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Graph Features and Shortcuts
GRAPH FEATURES AND SHORTCUTS

Display graph report shortcuts by right clicking in the body of the graph area.
Graph Shortcuts Options and Description Table

Autoscale all axes Returns the report to full view after using the zoom feature.
Display imported data Displays imported data.
Edit axis Use to edit the selected axis properties.
Autoscale minimum / maximum. To manually specify minimum

/ maximum autoscale, deselect the option and enter the new
amount in the text box.
Grid lines. Use to change how to display major / minor grid lines.
Invert scale. Use to invert the scale.

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6 About Reports
Graph Shortcuts Options and Description Table (continued)

Linear / Logarithmic. Select the option to scale the graph as
linear or logarithmic.
Scale font. Use to modify the font for the scale label. Deselect
Use default font to enable font options.
Title. Use to edit the selected axis label.
Title font. Use to modify the font for the selected axis label.
Deselect Use default font . Select new font attributes for report
data. Enable Use default font to reset default fonts.

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Edit curve Use to edit selected curve properties.
Color. Click to change the curve color.
l Curve [group box]. Use to change the interpolation, point style

and pen style for the selected curve. These options are disabled
if Use default fill style is selected in the Histogram group box.
l Histogram [group box]. Enabled only if Histogram is selected
in the Style drop-down list. Use to specify the type of fill, fill color
and label position for the selected curve.
Label. Select where the graph point labels will display (left, right,
center, etc.) on the SPC report.
Style. Use to select another style for the collected data curve.
Title. Use to change the title of the selected curve.
Use default thickness. Uses the default curve thickness.

Deselect to enter a new thickness number in the Thickness text
box.
Edit imported data Used with pore distribution data reports only. Use to select
ASCII text files for import onto the active graph.

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6 About Reports

Edit legend Use to change the legend location and font.
Edit title Use to change the graph title and font.

Enable Overlays If overlays have been selected, this option displays (or hides) the
overlays.
Include report When selected, places a checkmark to the left of the report in the
Select Reports list box on the Report Options tab.
Paste Data Used with pore distribution data reports only. Use to paste ASCII
text data from the clipboard onto the active graph.
Reset axis limits to initial Removes the cross-hair and returns the graph back to the initial
setting setting.
Select overlays... Displays the option to select files to overlay onto the active graph.
To view the overlays, click Enable Overlays on the shortcut menu.
Show curve Displays a list of all curves. Select the curve(s) to display.
tons on page 2 - 3.

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Axis Cross-Hair
Left click on the graph to view the cross-hair coordinates.

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6 About Reports
Graph Grid Lines
Options > Graph Grid Lines
Use to select how grid lines appear on reports. This menu option is not available if using Restricted
option presentation.
Graph Grid Lines Fields and Buttons Table

Grid Line Styles Select if the major and/or minor grid lines should appear as solid or dot-
[selection] ted lines.
X-Axis / Y-Axis Select major and/or minor lines to display in reports for the logarithmic
[selection] and linear scales. Deselect this option to remove the grid lines.
tons on page 2 - 3.
Zoom Feature
Use the zoom feature to examine graph details. Click, hold, and drag the left mouse button on the
graphical area to be enlarged. A box will display in the area to be enlarged. To return to normal view,
right click in the graph and select Autoscale.

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Graph and Sample Overlays
GRAPH AND SAMPLE OVERLAYS

Use the graph overlay functions to compare multiple graph options. Graphical lines are differentiated
by the use of varying colored symbols outlined on a legend. Overlays may be generated in two ways:
l Multiple Graph Overlays. Overlay two different types of graphs from one sample.
l Multiple Sample Overlays. Overlay graphs of the same type with that of the current plot.
This feature is available only when using Advanced option presentation. Go to Options
> Option Presentation > Advanced.
GENERATE PORE SIZE DISTRIBUTION GRAPH OVERLAYS

The following reports in the mercury porosimetry application can produce graphical results for a
sample material's pore size distribution:
Physical Adsorption Mercury Porosimetry
l BJH Adsorption / Desorption l Cumulative

l Dollimore-Heal Adsorption / Desorption l Differential
l Horvath-Kawazoe l Incremental Intrusion graphs
l DFT Pore Size
Two methods can be used to import and overlay report data into another interactive graph using
shortcut menu options:
l Import ASCII text data. Data can be imported from an ASCII text file into the interactive graph.
The ASCII text file must follow certain rules.
l Copy / paste. Data can be copied and pasted from one sample file (source) and pasting into
another sample file (target).
Pore size distribution report overlays menu selections are:
l Copy data. Used to copy data sets.

l Paste data. Used to paste data sets.
l Edit Imported Data. Used to edit data sets.
l Display Imported Data. Used to hide or show the imported data.

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6 About Reports
IMPORT ASCII TEXT DATA

ASCII text file format rules
l The header must consist of one line to include title, two unit specifications, and distribution type:
o Accepted pore dimension units are: A, nm, um

o Accepted pore volume units are: cm3/g, cm3/g, ml/g
o Accepted distribution types are: cumulative, incremental
Two examples of a header format:
My Title (A, cm3/g, incremental)

My Title (A, cm3/g, cumulative)
l The data must be in two columns and should be separated by a comma or white-space.
l The data lines must be ordered so that pore dimensions are monotonically increasing or decreas-
ing.
Sample ASCII Text File
silica alumina bjh (A, cm3/g, cumulative)
456.657 0.0133559
444.847 0.0546427
429.168 0.0869924
425.419 0.119721
419.629 0.132681
360.634 0.156611
340.859 0.197672
326.601 0.233092
Window appearance will vary depending on the selected report. This function can be performed on
samples files with a Completed status or during an analysis.
1. Create the ASCII text file using the proper format as indicated above.
2. In the analyzer application, go to File > Open. Select a sample file to overlay graphs on to.
Click Open (or double-click the file name).
3. Right click in the graph area and select Edit imported data.
4. In the Select Imported Overlays window, if the ASCII text file does not display, click Import to
locate the file. Select the ASCII text file in the Select Imported Overlays window, then click
OK. If an error message will display instead, verify that the .TXT file format is in the correct
format.
5. To include the overlay data in a printed report, see Print Pore Size Distribution Overlay
Data in Reports on the facing page.

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Import ASCII Pore Distribution Data
OVERLAY PORE SIZE DISTRIBUTION DATA USING COPY/PASTE

1. Open a source sample file and a target sample file; both should have a Complete status. The
report will open to the interactive reports window.
2. In the source sample file, right click on the graph and select Show Curve. Deselect any dif-
ferential curve data to hide them in the graph.
3. Right click in the graph area again and select Copy Data.
4. Change to the target sample file, right click the graph, and select Paste data. The graph now
displays overlayed data from the source sample file.
Typically, one new graph will appear showing both the cumulative and differential curves. To
show or hide individual curves, right click the graph and select (or deselect) Display imported
data.
5. Ensure that all parameter fields are set appropriately, then click the Paste button.
6. To include the overlay data in a printed report, see Print Pore Size Distribution Overlay
Data in Reports below.
Print Pore Size Distribution Overlay Data in Reports
1. Open the sample file containing the overlay data and select Advanced from the drop-down list
at the bottom of the window.
2. Click the Report Options tab.
3. In the Selected Reports list box, select the cumulative, differential, or incremental intrusion
graph to show the imported distribution data, then click Edit (or double-click the selected
report).
4. In the Overlay drop-down box, select Imported.
5. Click OK to close the window.
6. Click Preview on the Report Options tab. Click Print in the reports toolbar section to display
print options.
IMPORT ASCII PORE DISTRIBUTION DATA
IMPORT AN ASCII TEXT FILE USING GRAPH SHORTCUTS

1. Create an ASCII text file. See Manually Enter Data on page 3 - 8.
2. Open a report with a Complete status.
3. Select a pore-size distribution report from the drop-down list at the bottom of the window.
4. Right click on the graph and select Edit imported data on the shortcut menu.
If the ASCII text file does not display on the Selected Imported Overlays window, click Import.
Locate and select the file, then click Open. Header information from the ASCII text file will
appear in the Select Imported Overlays window. Select the entry, then click OK. If an error
message appears, verify that the .TXT file format is correct.

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6 About Reports
5. To hide or show imported data, right click in the graph area and use the Display imported data
option on the shortcut menu.
COPY / PASTE AN ASCII TEXT FILE USING GRAPH SHORTCUTS

1. Create an ASCII text file. See Manually Enter Data on page 3 - 8.
2. Copy the ASCII text data to the clipboard.
3. Open a report with a Complete status.
4. Select a pore-size distribution report from the drop-down list at the bottom of the window.
5. Right click on the graph and select Paste data on the shortcut menu.
COPY / PASTE GRAPH DATA FROM ANOTHER GRAPH

1. Open a source pore distribution data report with a Complete status.
2. Right click on the graph and select Copy Data on the shortcut menu.
3. Open the target pore distribution data report.
4. Right click on the graph and select Paste Data on the shortcut menu.
OVERLAY MULTIPLE MERCURY POROSIMETRY GRAPH OPTIONS

1. Go to File > Open.
2. Select the .SMP file, then click Open.
3. Select Advanced from the drop-down list at the bottom of the window.
5. In the Reports list box, highlight a plot report, then click Edit.

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962-42800-01 (Rev D) — Nov 2017
Overlay Multiple Sample Files
6. On the Plot Options window, select Options to include in the overlay. If the x- and/or y-axes are
to be autoscaled, select Autoscale; otherwise, enter the From and To points for the axes.
7. In the Y-Axis group box, select Variable and/or Overlay options.
8. Click OK to return to the Report Options tab.
9. Click Save, Save As, or Preview.
OVERLAY MULTIPLE SAMPLE FILES

This feature is applicable to overlaying samples from samples files with an LP Complete, HP
Complete or Entered status.
1. Go to File > Open.

2. Select the .SMP file, then click Open. Select Advanced from the drop-down list at the bottom
of the window to display the Report Options tab.
4. In the Reports list box, highlight a plot report, then click Overlays.
5. On the Plot Overlay Sample Selection window, move files from the Available Files box to the
Selected Files box.
6. Click Save, Save As, or Preview.

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6 About Reports
REPORT EXAMPLES
REVERBERI REPORT PLOT

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Report Examples
SILICA ALUMINA REFERENCE MATERIAL REPORT

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6 About Reports
GARNET TABULAR REPORT

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Report Examples
CONTROLLED PORE GLASS PLOT

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7 Selected Reports
7 SELECTED REPORTS
To edit reports, open the Sample Information file. Select the Report Options tab, then
highlight the report name in the Selected Reports list box. Click Edit.
ADVANCED REPORT OPTIONS
The Selected Reports list box may display a User-Defined option rather than an
Advanced option. These options are the same.
Up to five Advanced reports, each with up to 10 summary reports, 10 tabular reports, and 10
graphical reports can be created. To use this feature, a file containing a Python script that imports a
"mic" Python module must be created. See Mic Module Python Calls on page I - 11 for an
example of Python script and functions for the "mic" Python module.
1. Create the Python script and save it in the Scripts directory.

2. Open a sample file with a Completed status.
3. Select Advanced in the drop-down list at the bottom of the window to return to the tabbed
view.
4. On the Report Options tab, select Advanced in the Selected Reports list box, then click Edit.
5. On the Advanced Report Options window, click Add in the Available Scripts group box to loc-
ate and select the Python script. Repeat for each script to be added.
6. In the Selected Reports group box, click the drop-down arrows to select up to five Python
scripts previously added in the Available Scripts box.
7. Click Pressures to add pressure points to the report. Click OK to return to the Report Options
tab.
8. Select the Overlay samples checkbox to enable the overlay sample feature.

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7 Selected Reports
9. On the Report Options tab, click Preview. The Python Reports will be included on the tabs
across the top portion of the Reports window.
Advanced Report Options Fields and Buttons Table

Add [button] Click to add additional Python reports.
Available Scripts Lists the available reports and provides the option to add, replace, edit
[group box] or remove reports.
Overlay samples (if Use to overlay samples as defined by the function.
shown) [check box]
Advanced Report 1 Use the drop-down lists to select currently-defined functions used to
through 5 define the report calculations and output.
[drop-down box]
tons on page 2 - 3.
GRAPH REPORT OPTIONS

l Cumulative Area vs Size Plot Options
l Cumulative Volume vs Pressure Plot Options
l Cumulative Volume vs Size Plot Options
l Difference from Reference % Volume Plot Options
l Differential Intrusion Plot Options
l Differential Volume vs Size Plot Options
l Incremental Volume vs Pressure Plot Options
l Incremental Volume vs Size Plot Options
l Log Differential Intrusion Plot Options
l Out of Specification % Volume Plot Options

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Graph Report Options
Graph Report Options Fields and Buttons Table

Autoscale [check box] When enabled on the report parameters windows, allows the x- and
y- axes to be scaled automatically. Autoscale means that the x- and
y- ranges will be set so that all the data is shown. If Autoscale is not
selected, the entered range is used.
Options [check box] Plot Points. Select to plot the points on the graph.
Plot Curve. Interpolated from data points.
Show As Histogram. When selected, Plot Points and Plot Curve

options are disabled.
Overlays [button] Select sample files that contain data to be overlayed onto the selected
plot.
Reference [button] Select a sample file to compare analysis results of the current sample.
Specification [button] Specify sample files to use for the boundaries of the coarse and fine
specifications.
X-Axis [group box] Select options for the x-axis.
Variable.
Scale.
Y-Axis [group box] Select options for the y-axis.
Variable. Select the y-axis variable from the drop-down list.
Overlay. [Optional]. Select an option to overlay.

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7 Selected Reports
Graph Report Options Fields and Buttons Table (continued)

Intrusion / Extrusion. Select the data points to plot.
l None. No intrusion (or extrusion) data points

l First. Points from the first intrusion (or extrusion) cycle
l All. Include all intrusion (or extrusion) data points
tons on page 2 - 3.

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Cavity to Throat Size Ratio Report Options
CAVITY TO THROAT SIZE RATIO REPORT OPTIONS
Select to show the cavity to throat size ratio plot ratio table.
Cavity to Throat Size Ratio Fields and Buttons Table

Cavity to throat size Displays the ratio plot.
ratio plot [check box]
Cavity to throat size Displays the ratio table
ratio table [check box]
Pressures [button] Enter the minimum and maximum calculation pressure range.
tons on page 2 - 3.

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7 Selected Reports
FRACTAL DIMENSION REPORT OPTIONS

The fractal dimensions can be shown as a graph, table, or both. The graph and table reports contain
the fractal dimension and the RMS error to give an indication of the quality of the fit.
Fractal Dimension Report Fields and Buttons Table

Backbone region Enter the pressure at which the calculations are to be performed.
[text box]
Percolation region Enter the pressure at which the calculations are to be performed.
[text box]
Pressures [button] Select to enter minimum and maximum pressures.
Select Reports Show Log(V) vs Log (P-Pt) graph. Select to generate an additional
[check box] graph to help select linear range for calculations.
Backbone region.
Percolation region.
tons on page 2 - 3.

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Material Compressibility Report Options
MATERIAL COMPRESSIBILITY REPORT OPTIONS

The compressibility calculations can be shown as a graph, table, or both. The graph and table
reports contain the linear and quadratic c compressibility values and the RMS error to give an
indication of the quality of the fit. The linear and quadratic compressibility coefficients from this report
can be copied into a Material Properties parameter file for use in future sample analyses with the
same material.'
Material Compressibility Fields and Buttons Table

Pressures [button] Enter the Calculation pressure range.
Range [text box] P1. Enter the beginning pressure.
P2. Enter the ending pressure.

Select Reports Material compressibility correction plot. Displays the results in
[group box] graph format. The graph plots pressure on a log scale on the x-axis
and the volume compressed readings as points on the y-axis, with the
theoretical curve based on the calculated values overlaid.
Tabular report. Displays the results in table format. The table

displays pressure, volume compressed, predicted volume
compressed, and error.
tons on page 2 - 3.

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7 Selected Reports
MAYER-STOWE REPORT OPTIONS
Mayer-Stowe Options Fields and Buttons Table

Cumulative volume vs particle size plot Select to show the ratio plot.
[check box]
Pressures [button] Select to enter the minimum and maximum cal-
culation pressure range.
Tabular report [check box] Select to show the ratio table
tons on page 2 - 3.

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Options Report
OPTIONS REPORT
The Options report for mercury porosimetry analyses lists the conditions used to perform the
analysis— such as:
l Analysis conditions
l Mercury properties
l Evacuation options
l Penetrometer properties
l High pressure options
l Reverberi options
l Low pressure options
l Sample information
l Material properties
Options reports cannot be edited.

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7 Selected Reports
PORE STRUCTURE OPTIONS
Pore Structure Options Fields and Buttons Table

Permeability constant Viewed on Report Summary
[text box]
Pore shape exponent Viewed on Report Summary
[text box]
Pressures [button] Select to enter minimum and maximum pressures
Select Reports [group box] Select the report type.
Surface Area [group box] Select the type of Surface Area to reference.
tons on page 2 - 3.

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Reverberi Report Options
REVERBERI REPORT OPTIONS
Reverberi Fields and Buttons Table

Cavity diameter Select Show all to display all diameters or enter a specific range to dis-
[check box] play.
Show 2D graph of Displays a 2D graph with this description.
cumulative distribution
... [check box]
Show 2D graph of dV/d- Displays a 2D graph with this description.
log (throat diameter) ...
[check box]
Show 3D graph of dV/d- Displays a 3D graph with this description.
log (throat diameter) ...
[check box]
Show table [check box] Displays a table in the report.
Throat diameter Select Autoscale to autoscale the throat diameter or enter a specific
[check box] range to display.
tons on page 2 - 3.

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7 Selected Reports
SAMPLE LOG REPORT

This report provides information on:
l Manual control operations performed during analysis

l Information entered using Add Log Entry on the sample file editor
l Warnings and/or errors which occurred during analysis
SUMMARY REPORT
The Summary Report provides a condensed listing of selected data results.
Summary Report Fields and Buttons Table

Intrusion Summary Select the intrusion options to include in the report. If Bulk Density is
[group box] selected, enter the pressure for the measurement. If the entered pres-
sure is below the filling pressure, the filling pressure will be used in the
report.
Physical Properties Select the physical properties to display on the report.
Summary [button]

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962-42800-01 (Rev D) — Nov 2017
Summary Report
Summary Report Fields and Buttons Table (continued)

Pore Structure Select the pore structure to be included in the report.
Summary [button]
Show Graph [check box] Displays the report in graph format. Click Options to select how the
graph should display.
See Report Options on page 4 - 11 for a description of fields and

buttons on this window.

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7 Selected Reports

Show Peak Table Displays the peak table in the report. Click Options to select how the
[check box] graph should display.
Auto. Select to have the system automatically identify peaks based on

the entered minimum valley depth to separation peaks. Enter the
minimum settings.
Manual. Select to manually enter the minimum and maximum

diameter or volume for each peak in the table.
Show Percent Intrusion Click Options to enter the percentile intrusion for the report. Use the
[table] drop-down fields to specify the data to appear in the specified columns
for report generation.

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962-42800-01 (Rev D) — Nov 2017
Summary Report

Show Pore Size Table Select to show pore size in the report. Click Options to select points to
[check box] display. Use the drop-down fields to specify the data to appear in the
specified columns for report generation.
Show Pressure Table Select to display pressure points in the report. Click Options to select
[check box] points to display. Use the drop-down fields to specify the data to
appear in the specified columns for report generation.
Total intrusion volume Enables the Pass/Fail button.

[check box]
Upper / Lower. Specify upper and lower limits for the selected
parameter. A range can be left open by not selecting the limit. In the
text box to the right of Upper / Lower, enter operator instructions to be
displayed if a failure is encountered.
tons on page 2 - 3.

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7 Selected Reports
TABULAR REPORT OPTIONS

Tabular reports display the numerical values for the data points. Up to six columns of data can be
selected to display on the report.
In the Tabular Data Definition group box, indicate select either Collected data or Tabular data set for
this report.
Tabular Report Options Fields and Buttons Table

Column [n] Use the drop-down fields to specify the data to appear in the specified
[drop-down box] columns for report generation.
Tabular Data Definition Collected data. Select to use data points collected during analysis.
[group box] Data are collected at equilibration points on or about the pressure
points specified in the pressure table used for each analysis.
Tabular data set. Select to have a table of specific pressure points or

pore sizes included in tabular reports. Allows for the comparison of
data from various runs, because it interpolates values from each
sample run at the points specified in the table. When this option is
selected, the Table button is enabled.

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962-42800-01 (Rev D) — Nov 2017
Tabular Report Options
Tabular Report Options Fields and Buttons Table (continued)

l Data Type. Select either Pressure Pointsor Pore sizes as the data
type.
l Click Insert to insert a data point immediately before the selected
point. To complete the table quickly, enter the highest value in the
set, then click Insert to enter points below that value.
tons on page 2 - 3.

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8 Diagnostics
8 DIAGNOSTICS
Unit [n] > Diagnostics
Use to display diagnostic readings, start and schedule diagnostic tests, and open saved diagnostic
reports. Each test generates a file to the default directory name and path of ...\...\Service\userdiag
unless another directory name was specified. These reports can be sent to a Micromeritics service
representative for examination.
START DIAGNOSTIC TEST

Unit [n] > Diagnostics > Start Diagnostic Test
Provides a method to start a diagnostic test immediately. Upon completion of the diagnostic test, the
file is saved as a .REP file which can be retrieved by going to Reports > Open Report and
selecting the report file.
Start Diagnostic Test Fields and Buttons Table

Comments [text box] Displays comments from the selected diagnostic test.
Estimated time (min.) Approximate time for test completion.
File [group box] Shows a status bar of steps complete once the test begins.
Next [button] Starts the next test.
Operator [text box] Enter information to identify the person running the service test.
Repeat [button] Repeats the selected diagnostic test.
Report after test Automatically generates reports to the selected destination when the
[check box] test is complete.
Sequence Sequence number assigned to the test.
Start [button] Starts the diagnostic test.

8-1
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8 Diagnostics
Start Diagnostic Test Fields and Buttons Table (continued)

Test [drop-down box] Select the diagnostic test to be performed.
tons on page 2 - 3.
SCHEDULE DIAGNOSTIC TESTS

Unit [n] > Diagnostics > Schedule Diagnostic Tests
Allows the specification of one-time or periodic running of a sequence of diagnostic tests. A separate
list of tests is saved for each of the possible test frequencies. Tests are categorized and flagged as
requiring intervention or not. If tests requiring intervention are scheduled, the operator has the option
of omitting the tests if the operator does not respond within a specified time after an initial prompt is
displayed and before the test is started. Events are logged in the analyzer log for all starting, ending,
and omitted tests.
Schedule Diagnostics Test Frequency Fields and Buttons Table

Available Tests Select one or more tests to run unattended.
[drop-down box]
Insert [button] Inserts the selected test in the Available Tests drop-down list.
Skip these tests if the Check this option if any test requiring operator intervention should be
operator does not omitted if the operator does not respond within the specified time.
respond within [n]
minutes [check box]

8-2
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Diagnostic Test Report
Schedule Diagnostics Test Frequency Fields and Buttons Table (continued)

Start test sequence if Enter a from and to time for an unattended test to begin if the instru-
instrument is idle any ment is idle at any time during the entered time frame.
time between 00:00:00
and 00:00:00 [text box]
Test Frequency [selec- Select how often the test is to run unattended.
tion]
Test Sequence Provides the test file identification and estimated run time. A
[group box] checkmark in the Intervention Required column indicates that operator
intervention is required.
To remove a test from the sequence, select the test, then click Delete.
To add a test to the test sequence, highlight a row in the Test

Sequence box, select a test from the Available Tests list, then click
Insert.
tons on page 2 - 3.
DIAGNOSTIC TEST REPORT

Unit [n] > Diagnostics > Diagnostic Test Report
Displays previously run diagnostic service tests. Separate directories store tests run once, daily,
weekly, and monthly. Diagnostic test report files have a .SVT file extension and are stored in the
...\Service directory.

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8 Diagnostics
SAVE FILES FOR PROBLEM DIAGNOSIS

Unit [n] > Diagnostics > Save Files for Problem Diagnosis
Use to compress pertinent diagnostic information into a single zip file. This file can be sent to a
Micromeritics Service Representative for problem resolution.
1. Complete the form. A default file named Diagnostics-[date].zip is created unless another file
name is specified.
2. When the file is saved, log in to the customer portal.
3. Click the Requests tab.
4. Click New Request, then complete all fields.
5. To attach the zipped file, click the Attach File(s) link, then select the Diagnostics-[date].zip file.
6. Click Add Request to submit the problem request.
7. Return to the portal to track the progress of the problem solution.
Save Files for Problem Diagnostic Fields and Buttons Table

Comment [text box] Enter information that would be helpful to the Micromeritics rep-
resentative. If the computer is not connected to the internet, complete
this field. If the computer is connected to the internet, this information
can be completed on the Micromeritics Customer Support portal.

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Save Files for Problem Diagnosis
Save Files for Problem Diagnostic Fields and Buttons Table (continued)
Include Files Add. Click to select additional files to send with this problem diagnosis.
Delete. Select the file in the Include Files box, then click Delete to
remove the file from the list.
Clear. Click to clear all files from the Include Files box.
Save As [button] Click to specify the name and location of the compressed file. Make a
note of the file name and location. This file will need to be sent to your
Micromeritics representative for problem resolution.
Micromeritics rep- Enter the name of your Micromeritics representative. This information
resentative [text box] will remain on the window each time files for problem diagnosis need
to be submitted (can be modified as necessary).
User Information Enter information for the person to be contacted by a Micromeritics rep-
[text box] resentative. This information will remain on the window each time files
for problem diagnosis need to be submitted (can be modified as neces-
sary).
tons on page 2 - 3.

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9 Calibration
9 CALIBRATION
Unit [n] > Calibration
A calibration file was created specifically for the analyzer and included with the accessories. It is not
necessary to recalibrate the system unless it seems out of calibration.
Disabled calibration menu options can be accessed only with the assistance of an authorized
Micromeritics service representative. Calibrations can be saved to a file and reloaded later.
To review calibration details of the analyzer, go to Unit [n] > Unit Configuration.
Generally it will not be necessary to change the data in the calibration file. However, if a condition
occurs during the operational verification that requires changes to the calibration data, changes
should be saved in a file. Calibration data files are retained in the analyzer history file and can be
reloaded in the event that calibration data becomes corrupt.
CALIBRATE THE LOW PRESSURE SERVO

Unit [n] > Calibration > Low Pressure Servo
Ensure the pressure transducer was calibrated by a service technician before starting
this process.
This procedure will calibrate the servo valve to the pressure transducer.

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9 Calibration
CALIBRATE SIGNALS
Unit [n] > Calibration > Signals
During calibration, the capacitance detectors, vacuum gauge, reference gauge, transducer, etc. are
read. Analysis cannot be started while the calibration window is open.
To manually enter calibration data, click the button containing the value to be changed and enter the
data on the popup window.
Calibration Signals Fields and Buttons Table

Low Pressure Reading. Displays the current values from each capacitance detector.
Low Cal. Displays the capacitance of the reference device with the
lower value.
Hi Cal. Displays the capacitance of the reference device with the

higher value.
Calibrated. The date the capacitance detector was last calibrated.
Raw Count. The digital value produced by the analyzer for each
capacitance detector.
Vac µmHg.
l Reading. The current value from the vacuum gauge.

l Low Cal. The pressure value read on a reference vacuum gauge
after vacuum is achieved.
l High Cal. The pressure value read on a reference vacuum gauge
when higher pressure is applied.

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Calibrate Signals
Calibration Signals Fields and Buttons Table (continued)

l Calibrated. The date the vacuum gauge was last calibrated.

l Raw Count. The digital value produced by the analyzer for the
vacuum gauge.
50 PSIA
l Reading. The current value from the 50 psia transducer.

l Low Cal. The pressure value read on a reference transducer after
vacuum is achieved.
l High Cal. The pressure value read on a reference transducer
when higher pressure is applied.
l Calibrated. The date the 50 psia transducer was last calibrated.
l Raw Count. The digital value produced by the analyzer for the 50
psia transducer .
High Pressure Reading. Displays the current values for the left and right capacitance
detectors.
Low Cal. Displays the left and right capacitance detectors of the
reference device with the lower value.
Hi Cal. Displays the capacitance of the left and right capacitance

detectors with the higher value.
Calibrated. The date the left and right capacitance detectors were last
calibrated.
Raw Count. The digital value produced by the analyzer for left and
right capacitance detectors.
Temperature Reading. The transducer's current temperature.
Temp Cal. The calibration setting for the transducer. Click to reset the
temperature.
Calibrated. The date the transducer was last calibrated.
Raw Count. The digital value produced by the analyzer for the
transducers.
tons on page 2 - 3.

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9 Calibration
CALIBRATE THE PENETROMETER

Unit [n] > Calibrate Penetrometer
Up to 4 penetrometers can be calibrated simultaneously.
To have the application determine sample density or if blank correction by formula will be used, the
calibrated empty volume of each penetrometer must be entered in the Penetrometer Properties file.
The file can then be selected and used for analyses.
1. For each penetrometer to be calibrated, click the drop-down arrow to the right of the Pen-
etrometer field and select a Penetrometer Properties file. If this is a new penetrometer, a new
Penetrometer Properties file must be created for each new penetrometer, then select the Pen-
etrometer Properties file from the drop-down list. A new Penetrometer Properties file can be
added by clicking Browse from the drop-down list and entering the new file name. See Pen-
etrometer Properties on page 4 - 10.
2. Verify that the Empty mass field contains the correct information for each file selected. If neces-
sary, modify the field. The Fill button is disabled unless at least one port has a penetrometer
selected, and until each port with a penetrometer has an Empty Mass value greater than (not
equal to) 1.0000.
3. In the Mercury Density group box, select either Enter density to manually enter the mercury
density in the text box or select Calculate from the measured temperature to use the tem-
perature and density entered in the table.
To modify the table parameters, click in the appropriate cell and enter the new parameter.
4. Prepare and load the penetrometers as for a low pressure analysis (see Perform a Low
Pressure Analysis on page 5 - 11). Click Fill and wait for the operation to complete, then
weigh the penetrometers and enter the Full Mass for each. The Measurements Completed
field will update to include the measurement just finished. The Full Mass fields will be initialized

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962-42800-01 (Rev D) — Nov 2017
Load Calibration from File
to 1.0000. The Repeat and Accept buttons will be disabled until all selected ports have a Full
Mass greater than their Empty Mass. When a valid Full Mass is entered, the penetrometer
volume for this measurement is calculated and the Mean Volume and standard deviation for
all measurements are updated.
5. Repeat these steps as many times as needed (three times are recommended). The system
will automatically calculate the Mean Volume and report it. Click Accept when finished. The
Mean Volumes will be stored in the selected Penetrometer Properties files.
LOAD CALIBRATION FROM FILE

Unit [n] > Calibration > Load from File [button]
Use to load a previously saved calibration file.
It is recommended that the current calibration settings be saved using Unit [n] > Calibration >
Save to File prior to loading another calibration file. When loading a previously saved calibration file,
a backup of the current file is created and saved as [SN]last.cal. The backup file is overwritten each
time a new one is created.
Changing the calibration may affect the analyzer’s performance.
SAVE CALIBRATION TO FILE

Unit [n] > Calibration > Save to File [button]
Use to save the current calibration settings to a backup file which can later be reloaded using Unit
[n] > Calibration > Load from File menu option.
The default file naming convention for calibration files can be used or the file name can be changed.
The default file name of 0217-2013-04-25.CAL is interpreted as:
0217 is the analyzer serial number

2013-04-25 is the date the calibration file was saved
.CAL is the file name extension

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10 Hardware Components and Accessory Installation
10 HARDWARE COMPONENTS AND ACCESSORY

INSTALLATION
INSTALL A PENETROMETER IN A HIGH PRESSURE CHAMBER
Before opening the high pressure chamber, check the status display to ensure the sys-
tem is not pressurized.
1. Turn the vent valve slowly counter-clockwise to release excess pressure.

2. Unscrew the chamber plug assembly by turning the arms counter-clockwise. Lift the chamber
plug assembly as far as it will go. The chamber assembly contains a latching device which
automatically locks into place when the assembly is in the topmost position.
3. Gently lower the penetrometer assembly, bulb down, into the chamber until it rests firmly on
the banana plug.
4. Verify that the oil in the high pressure chamber just covers the ledge inside the chamber. Add
more oil, if needed. See Seal the High Pressure Chamber on page 11 - 19 and Maintain
High Pressure Fluid Level on page 11 - 18.
5. Pull the latch release down to unlock the chamber plug assembly.Gently lower the assembly
while ensuring that the penetrometer is inserted into the assembly hole.After making sure the
penetrometer goes into the hole, lower the assembly the rest of the way and screw the cham-
ber plug in.

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962-42800-01 (Rev D) — Nov 2017
6. After the chamber plug is screwed, check the fluid level in the plastic cup above the vent valve.
to ensure all the air bubbles are out of the chamber, and sealing the vent valve. See Seal the
High Pressure Chamber on page 11 - 19.

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Install a Penetrometer in a Low Pressure Port
INSTALL A PENETROMETER IN A LOW PRESSURE PORT

If fewer than four samples are to be analyzed, a steel rod with a receptacle for the cap detector must
be installed in each unused low pressure port. The cap detector must see that a rod is installed.
If a penetrometer or blank rod is not installed in each port, vacuum conditions cannot be
achieved and an analysis cannot be performed.
1. Remove the capacitance detector from the low pressure port by turning it counter-clockwise
and pulling forward. Place it on top of the analyzer or stand it on the surface next to the high
pressure chamber.
2. Turn the plastic cap counter-clockwise to remove.

3. Turn the retaining knob counter-clockwise until it turns with little resistance.
Do not remove the knob; internal components may become misaligned.

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962-42800-01 (Rev D) — Nov 2017
4. If the low pressure port contains a blank rod, remove it. If it contains a penetrometer, see
Remove a Penetrometer from a Low Pressure Port on page 10-6.
5. If using a 3 cc penetrometer, install the spacer over the penetrometer stem. Insert the pen-
etrometer stem into the port and push it in as far as it will go. The spacer is required for the 3 cc
penetrometer only.
6. Tighten the retaining knob by turning it clockwise until the penetrometer is firmly seated. Do
not tighten with excessive force.
7. Place the plastic cover over the penetrometer assembly and turn clockwise to tighten.
8. Install the capacitance detector over the penetrometer and turn clockwise to tighten.

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Remove a Penetrometer from a High Pressure Chamber
REMOVE A PENETROMETER FROM A HIGH PRESSURE CHAMBER
When analysis is finished, ensure the high pressure system indicator PRESSURIZED is
not lit.
1. Loosen the vent valve counter-clockwise approximately 1/8 turn to make the plug removal
easier.
2. Unscrew the chamber plug by turning the arms counter-clockwise. Lift the plug assembly as
far as it will go. Fluid begins to drain from the vent valve. Pause a few seconds to allow fluid to
drain back into the chamber.
3. Remove the penetrometer assembly. Hold it over the chamber for a few moments to allow the
high pressure fluid to drain.
4. Clean the penetrometer. See Clean the Penetrometer on page 5 - 5.

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REMOVE A PENETROMETER FROM A LOW PRESSURE PORT

1. Ensure the low pressure ports have returned to near atmospheric pressure and the Hg
Drained indicator on the front analyzer panel is illuminated.
Removing penetrometers when the Hg Drained indicator is not illuminated may allow
mercury to spill from the port. See Drain the Low Pressure System on page 11 - 10.
2. Hold the retaining knob to prevent rotation, then turn the capacitance detector counter-clock-
wise to loosen and remove it.
3. Turn the plastic cap counter-clockwise and remove.

4. Turn the retaining knob counter-clockwise, then carefully withdraw the penetrometer
assembly. Do not pull on the penetrometer cap.
As the penetrometer is withdrawn, tilt the bulb end down and the stem end up, so
mercury does not spill from the open stem end.
5. Remove the penetrometer spacer if used.

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Remove a Penetrometer from a Low Pressure Port
If the assembly is not to be placed immediately in the high pressure chamber, store it
with the stem upward so that none of the mercury will be spilled. The rack for full
penetrometers (part number 962-25827-00) can be used for this purpose.
6. Weigh the penetrometer assembly (remove the spacer first) if density calculations are to be
made or blank correction by formula is used. Record this mass on the Sample Data Work-
sheet.
Do not wait an extended period of time before performing the high pressure run.
Mercury remaining in contact with the sample for long periods of time after the low
pressure analysis may oxidize and reduce the reproducibility of results.

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11 Maintenance and Troubleshooting
11 MAINTENANCE AND TROUBLESHOOTING

The analyzer has been designed to provide efficient and continuous service; however, certain
maintenance procedures should be followed to obtain the best results over the longest period of
time. When unexpected results occur, some common operational problems not indicated on the
window and their respective causes and solutions are provided:
Log in to your customer portal to access error messages. Parts and accessories can be found online
at www.Micromeritics.com.
Status display is too large for computer monitor.
Cause: Monitor resolution is set below 800 × 600.

Action: Refer to the computer operating system manual to reset the monitor resolution
at or above 800 × 600.
Difficulty attaining adequate vacuum conditions during low pressure analyses.
Cause A: Vacuum pump oil is low.

Action A: Add vacuum pump oil.
Cause B: Vacuum hose not properly connected.
Action B: Ensure the connection to the vacuum pump is good and that external clamps
are tight.
Cause C: Sample contains excess moisture adsorbed from atmosphere.
Action C: Prepare samples (prior to loading penetrometer) by heat and/or vacuum to
remove moisture.
Never heat a sample that has contacted mercury.
Cause D: Proper sealing not achieved on penetrometers

Action D: 1. Use blank rods to test the ports to eliminate the possibility of having a leaking
penetrometer cap / bulb seal.
2. Lightly grease the rods with a high grade vacuum grease, then insert the
rods in the low pressure ports.
3. Tighten the retaining knobs on the low pressure ports. If vacuum conditions
are satisfactory, check the penetrometer for scratches or chips in the bulb.
Cause E: Scratches or other imperfections in either the lip of the penetrometer bulb or the
penetrometer cap.

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962-42800-01 (Rev D) — Nov 2017
Action E: 1. Polish the lip of the bulb and the cap using 600 grit emery paper or crocus
cloth.
2. Place the paper or cloth on a flat surface, grit-side up.
3. Clean all grease from the surface to be polished with solvent.
4. Lightly press the surface down on the grit and rub in a circular motion. A
minute of this polishing action is usually sufficient, but it must be continued
until the surface is free from flaws. Examination of the surface under low
magnification (approximately 20X) helps determine when the surface is free
from flaws.
5. Clean the ground surface before regreasing.
Cause F: Leaking valves.
Action F: Check the valves for leaks. See Check Valves for Leaks on page 11 - 29.
Cause G: Moisture has accumulated in the system.
Action G: Remove the accumulated moisture. See Remove Moisture from the Ana-
lyzer on page 11 - 31.
The low pressure analysis is complete and the system has returned to near atmosphere,
but the mercury drained indicator is not illuminated.
Cause A: Indicator is not working properly.

Action A: Verify the state of the mercury degasser by looking at the status display win-
dow. If the status display does not agree with the indicator, the indicator may not
be working properly. Contact your Micromeritics service representative.
If the status display window shows that the mercury has overfilled (the alarm
state), see Handling Mercury Overfill on page 11 - 21. If the status display
shows that the mercury degasser is either filled or partially filled, see Drain the
Low Pressure System on page 11 - 10.
Cause B: Mercury is not drained. Status display shows either filled or partially filled.
Action B: See Drain the Low Pressure System on page 11 - 10.
Mercury warning buzzer sounds in pulses. (Mercury overfill).
Cause: Mercury detected by overflow sensor in low pressure port system.

Action: See Handling Mercury Overfill on page 11 - 21.
Mercury warning buzzer sounds with continuous tone.

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962-42800-01 (Rev D) — Nov 2017
Cause: Mercury has been improperly drawn into the mercury trap.
Action: Drain excess mercury into the reservoir. See Handling Mercury Overfill on
page 11 - 21. Remove the plug extending down from the mercury trap. The
plug is reached through the front door. Facing the analyzer, the plug is in the
upper back right corner. See Drain Spilled Mercury Dish on page 11 - 11.
Position a container beneath the trap before removing the plug.
The high pressure system failed to attain the specified pressure.
Cause: Low fluid level in the hydraulic pump.

Action: Add fluid to the hydraulic pump. See Maintain Hydraulic Pump Fluid Level
on page 11 - 23.
High pressure system failed to retain a reasonably constant pressure.
Cause: Leakage around the high pressure chamber cap.

Action: Replace the cup seals and backup rings on the high pressure chamber cap.
See Replace Chamber Cup Seals on page 11 - 21.
Cannot attain low pressure data points above atmospheric pressure.
Cause: Gas supply pressure too low.

Action: Verify gas supply regulator is set to 40 to 45 psig (276 to 310 kPa) and that there
is sufficient gas in the supply bottle.

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962-42800-01 (Rev D) — Nov 2017
SYSTEM COMPONENTS
LOW PRESSURE SYSTEM COMPONENTS
Low Pressure System Valves

Item # Component Description
1 Servo isolation Ensures no leaking occurs through the servo. It is open when the
valve servo is in use and closed when the servo is off.
2 Fast evacuation Used at the end of the evacuation routine to achieve the best
valve vacuum. When this valve is open, the sample stations are directly
connected to the vacuum system.
3 Vacuum valve The vacuum valve is opened to evacuate the back of the servo
valve during the ramping part of the evacuation sequence. This
allows the servo valve to control the evacuation rate.
When the pressure is low enough, the evacuation through the

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962-42800-01 (Rev D) — Nov 2017
Low Pressure System Components
Low Pressure System Valves (continued)

reservoir proceeds. This is accomplished by alternately opening
Valve 8 (to allow gas from the sample to move to the reservoir)
and Valve 3 (to evacuate the reservoir for the next step).
4 Gas inlet valve Allows pressurization at the back of the servo valve. The servo can
then be used to dose pressures from 0.2 psia to 50 psia onto the
low pressure stations. Dry nitrogen or argon is the preferred gas.
Do not use air unless it is dried to remove water vapor.
5 Mercury fill valve Mercury flows into the degasser then into the low pressure sta-
tions and is controlled by the fill valve. The drain valve allows mer-
cury to flow back into the reservoir.
6 Drain valves See Mercury fill valve [5].
7 Mercury reservoir Connects the vacuum line to the mercury reservoir.
evacuation valve
8 Evacuation Reser- See Vacuum valve [3].
voir valve
Low pressure ports A sample encased in a penetrometer is first evacuated, filled with
mercury, then pressurized to between 15 and 50 psia.
Penetrometer stems inserted into a station are sealed for vacuum

and against mercury leakage by compression of a soft, gum
rubber cylinder near the tip. The rubber is compressed by turning
the large knob or pressure collar that protrudes from the front. The
inner rim of this knob serves also as the mounting mechanism for a
capacitance transducer after the knob has been tightened.
Mercury storage reservoir Holds 7 to 10 pounds of mercury and is located behind the front
panel. The level of mercury is visible through a small window in the
front panel. Before beginning a low pressure analysis, the applic-
ation verifies that the level of mercury in the reservoir is adequate.
Mercury degasser Removes trapped gases as mercury passes to low pressure

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962-42800-01 (Rev D) — Nov 2017
Low Pressure System Valves (continued)

stations then into the penetrometer.
HG Up indicator. Illuminates when mercury level fills the

penetrometers. The sensor completes an electric circuit and flow
is stopped by closure of the mercury fill solenoid valve.
Drained indicator. Illuminates when the mercury drain valve is

closed and the level of mercury in the degasser is below the level
in the low pressure stations.
Alarm buzzer. If the level of mercury rises above the normal filling
level, the sensor causes both the mercury fill valve and the
mercury drain valve to close and a buzzer alarm sounds. See
Handling Mercury Overfill on page 11 - 21.
Mercury trap Serves as a large volume reservoir for mercury in the event that
operator error or a malfunction allows mercury to travel toward the
vacuum system. If not stopped, mercury can severely damage the
analyzer. Should this occur, a high-pitched, continuous alarm
sounds if more than 6 mm (0.25 in.) of mercury accumulates in the
trap. The fault must be corrected and the mercury removed before
proceeding.

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962-42800-01 (Rev D) — Nov 2017
High Pressure System Components
HIGH PRESSURE SYSTEM COMPONENTS
High Pressure System Components

High pressure chamber The two high-pressure chambers are closed by the chamber plug
assemblies. These are sealed into the chambers with large threads
and tightened by turning two short handles. The closure components
are counter-sprung so that they are readily raised and lowered. On top
of each closure is a manual valve for venting or purging air that may be
trapped when a high pressure chamber is closed.

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962-42800-01 (Rev D) — Nov 2017
High Pressure System Components (continued)

Hydraulic pump The basic high-pressure generating unit is a hydraulic pump. The
pump has a hydraulic fluid reservoir and a pressure gauge. The relief
valve limits the maximum pressure to 2800 psia. The pump and drive
motor rotation are reversible to allow the pressure adjustment.
Pump speed and direction are controlled by the application which

prevents overshooting of the target pressure while minimizing time
required to attain a target pressure.
Pressure intensifier The required psia is generated by a double- action, dual piston intens-
ifier connected to the hydraulic pump. Two limit switches are located
near the upper and lower limits of piston travel. The first of these
switches alerts the operating program; the second interrupts the
power to the motor.
Transducer High pressure measurements are made with one pressure transducer.
The signal from this transducer is processed by electronic circuitry to
yield two pressure output signals.

11 - 8
962-42800-01 (Rev D) — Nov 2017
Change the Fuses
CHANGE THE FUSES

Fuse the input power line according to local safety practices. The input power connector can be used
with either a single-fuse arrangement or a double-fuse arrangement.
The power cord should be disconnected from the analyzer before removing the cover
from the power input connector. Failure to disconnect the power cord could result in elec-
trical shock.
l If the single-fuse arrangement is needed, position the fuse block so that the side with the single-
fuse slot and the jumper bar is away from the cover.
l If the double-fuse arrangement is needed, position the fuse block so that the side with the double-
fuse slots is away from the cover.
1. Reposition the fuse block, if necessary:
a. Remove the fuse block retaining screw.
b. Lift the fuse block from the cover.
c. Rotate the fuse block.
d. Mount the fuse block to the cover.
e. Replace the retaining screw.
2. Insert appropriate fuse for the input power source. Refer to the chart below for the appropriate
fuse rating.
The fuse used in the analyzer must be identical in type and rating to that specified. Use
of other fuses could result in electrical shock and/or damage to the unit.
Power Source Fuse

100-120 VAC 3AG 6.25 Amp Slow-Blow
200-240 VAC 5 x 20 mm 5.0 Amp Slow-Blow
3. Insert fuse block and cover assembly into input power connector and snap it into place. After
the fuse block and cover assembly are in place, the position of the indicator pin shows the
input power selected.

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962-42800-01 (Rev D) — Nov 2017
4. Connect the power cord to the analyzer and plug into an appropriate power source.
DRAIN THE LOW PRESSURE SYSTEM

Unit [n] > Generate Low Pressure
1. Specify a pressure of 10 psia. After the system reaches 10 psia and returns to Idle status,
open the reservoir evacuation valve (#7) for 20 seconds.
The Hg reservoir evacuated indicator should be displayed on the analyzer schematic. If it is not
shown, do not proceed to the next step. Instead, verify that the mercury reservoir fill cap is
properly sealed on top of the mercury filling funnel (see Maintain Mercury Level on page 11
- 17). If the Hg reservoir evacuated indicator still is not displayed, contact a Micromeritics
Service Representative.
2. Open the mercury drain valve until the mercury drains.
3. Close the mercury drain valve.
4. Close the mercury reservoir evacuation valve.
5. To return the system to atmosphere, go to Unit [n] > Generate Low Pressure and enter a
pressure of 15 psia.
If the system still indicates that the mercury is not drained (the status display, the mer-
cury drained indicator or both), see Handling Mercury Overfill on page 11 - 21.

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962-42800-01 (Rev D) — Nov 2017
Drain Spilled Mercury Dish
DRAIN SPILLED MERCURY DISH

A dish for collecting mercury is located just behind the high pressure chambers. Pour approximately
1.0 to 2.0 cc of oil into the dish to prevent the mercury from vaporizing.
If mercury accumulates in the dish, remove it by removing the cover and extracting the mercury with
the syringe accessory.
Approximately 3 mm (1/8 in.) of oil should remain in the container to prevent the escape
of mercury vapors.

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962-42800-01 (Rev D) — Nov 2017
ENABLE MANUAL CONTROL

Unit [n] > Enable Manual Control
Use to enable the manual control of certain system valves and elevator components on the analyzer
schematic. When this option is enabled, a checkmark appears to the left of Unit [n] > Enable
Manual Control.
If the analyzer schematic is not immediately visible, go to Unit [n] > Show Instrument Schematic.
Schematic Components Table

Schematic Description
Components
1 Servo isolation valve
2 Fast evacuation valve
3 Vacuum valve
4 Gas inlet valve
5 Mercury fill
6 Mercury drain

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962-42800-01 (Rev D) — Nov 2017
Enable Manual Control
Schematic Components Table (continued)

Schematic Description
Components
7 Mercury reservoir evacuation
8 Evacuation reservoir
9 Vent valve
A Hg Reservoir Indicator
B Mercury reservoir
C Mercury degasser
D Mercury temperature sensor
E Mercury trap
F Intensifier
G Hydraulic pump
Pressure l Displays the current pressure in the system.
l The pressure is shown in the units selected in Options > Units.
l The reading shown is from either the vacuum gauge or the 50 psia trans-
ducer, depending upon which is currently in range.
Status Provides the sample file name and sequence number, the intrusion volume,
and the percent of the penetrometer stem already used.
Analyzer Schematic Icon Table

Icon or Symbol Description
Open Valve. Green indicates an open valve.
Closed Valve. Yellow indicates a closed valve.
Servo Valve. Closed.
Servo Valve. Open.

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962-42800-01 (Rev D) — Nov 2017
Low Pressure Schematic Icons

Mercury Degasser. Displays the mercury level.
Drained Partially Filled Filled Overfilled. This alarm

displays
with a red background.
Mercury Trap. Displays the state of the mercury trap.
Empty Contains more than 6 mm of mercury.

Mercury Reservoir. Displays the level of mercury in the reservoir.
If the mercury level is low, see Maintain Mer- Level is OK.

cury Level on page 11 - 17.
Hg Reservoir Vacuum Switch
When illuminated, indicates that mercury reser-
voir has been evacuated.

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962-42800-01 (Rev D) — Nov 2017
Enable Manual Control
High Pressure Schematic

Hydraulic Pump
When the pump is operating, the target pressure
displays below the icon. A green icon indicates the
pump is ON. A yellow icon indicates the pump is
OFF. To set the target pressure when the icon is
yellow, either double-click the pump icon or right
click the icon and select Set.
Intensifier. Displays the state of the intensifier limit switches.
Midway Top Bottom

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962-42800-01 (Rev D) — Nov 2017
PREVENTIVE MAINTENANCE
Perform the following preventive maintenance procedures to keep the analyzer operating at peak
performance. Micromeritics also recommends that preventive maintenance procedures and
calibration be performed by a Micromeritics Service Representative every 12 months.
Maintenance Required Frequency

Banana plug Check every 600 samples or 3 months. Replace as needed.
Chamber plug seals Replace every 600 samples or 3 months.
High pressure chambers Check and clean every 600 samples or 3 months.
High pressure fluid Check every 600 samples or 3 months.
High pressure fluid level Check prior to performing a high pressure analysis. Fill as
needed.
Hydraulic pump fluid Check every 6 months. Fill as needed. Change annually.
Low pressure ports Grease every 600 samples or 3 months.
Mercury dish Check daily for spills. Service as needed.
Mercury level Service daily.
Mercury vapor filter Replace annually.
Moisture in system Remove as needed.
Vacuum pump exhaust filter Replace every 600 samples or 3 months.
Vacuum pump fluid Change every 1200 samples or 3 months.
Vacuum pump fluid level Check monthly. Fill as needed. Refer to the vacuum pump
user manual for instructions.
Valves Check for leaks and clean as needed.

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962-42800-01 (Rev D) — Nov 2017
Maintain Mercury Level
MAINTAIN MERCURY LEVEL

Each analysis may extract from 3 to 15 mL of mercury from the reservoir depending on the
penetrometer and sample size used. When running a low pressure analysis, a pop-up message
displays on the Low Pressure Analysis window when the level of mercury drops below the minimum
level. The mercury level should be within 0.5 to 1.0 in. (1 to 3 cm) below the top of the mercury
viewing window. It must never reach above the viewing window. To avoid delays, check the mercury
level, adding mercury when necessary, at the beginning of each day.
Ensure the use of triple distilled mercury that is at least 99.999% pure.
The analyzer requires approximately 5 lbs of mercury (minimum) to begin analyses. Do not use more
than 10 lbs.
A spilled-mercury container, located in the center of the analyzer work surface behind the high
pressure chambers, is provided so that any accidentally spilled mercury can be immediately brushed
into it. Pour approximately 1.0 to 2.0 cc of oil into the container to prevent the mercury from
vaporizing.
1. Remove the mercury reservoir cap.

2. Slowly pour the mercury into the reservoir to within 0.5 to 1.0 in. (1 to 3 cm) from the top of the
viewing window.
3. Replace the reservoir cap.

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962-42800-01 (Rev D) — Nov 2017
Overfilling may interfere with the vacuum system. Reservoir cap should be finger tight
only.
Ensure that the mercury filling funnel is tightly secured. If it is necessary to tighten the fun-
nel, use an appropriate tool. If the funnel is not tightened, there could be a gas leak and
the vacuum will not pull properly.
MAINTAIN HIGH PRESSURE FLUID LEVEL

The high pressure fluid level in the high pressure chamber should be checked when preparing for a
high pressure analysis. The fluid level should be up to the ledge when a penetrometer is installed.
Add high pressure fluid as needed.

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962-42800-01 (Rev D) — Nov 2017
Seal the High Pressure Chamber
SEAL THE HIGH PRESSURE CHAMBER
High pressure fluid leaking past the chamber seal indicates one of three problems:
l Too much fluid. Remove fluid, clean the seal and try again.
l Damaged seal. Replace the seal, then try again.
l Fluid in the threads. Clean and reseal.
The chamber plug seals the high pressure chamber. Proper sealing does not require the use of
excessive force. The outside diameter of the elastic seal on the plug is slightly larger than the inner
diameter of the pressure chamber. Lowering the chamber plug into the pressure chamber presses
the seal against the chamber wall, sealing the chamber. Then, as pressure increases during an
analysis, the outer lip of the seal is forced more tightly against the chamber wall, preventing leakage.
1. Push the plug into the chamber until it contacts the chamber shoulder. Several threads of the
plug will remain exposed.
2. Ensure the vent valve is partially open (unscrewed). Slowly turn the plug clockwise into the
chamber to force air from the chamber. Continue turning until high pressure fluid (or air
bubbles and fluid) appears in the transparent cup on top of the vent valve.
Tightening the plug too quickly may cause unwanted intrusion caused by pressure cre-
ated when the chamber is closed.
3. The cup should not be completely full. If the cup is too full, slowly open the chamber and
recheck the fluid level. Fluid may need to be removed. See Maintain High Pressure Fluid
Level on the previous page for instructions on how to remove excessive fluid. Repeat the
previous steps to release trapped air.

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962-42800-01 (Rev D) — Nov 2017
l Large air bubbles may be caught in the chamber. Slowly loosen and tighten the plug
approximately 1/2 turn several times. This should cause any air bubbles to rise through the
transparent cup to the surface. Any remaining tiny bubbles will not affect the analysis.
l If no fluid is visible in the cup when the plug is fully tightened, open the chamber and
recheck the fluid level. It is likely that fluid may need to be added. Repeat the previous
steps to release trapped air.
Small amounts of high pressure fluid can be added to or removed from the cup on top of
the vent valve without opening the chamber. To do so, remove the cap and use appro-
priate tools, such as a syringe.
GREASE LOW PRESSURE PORTS

The screw threads visible behind each low pressure port retaining knob should be greased monthly.
1. Remove the capacitance detectors by turning counter-clockwise.

2. Remove the plastic caps.
3. Unscrew the retaining knobs until the threads disengage.
4. Lubricate the retaining knob threads and mating surfaces with a medium consistency grease
such as white lithium grease.
5. Screw the retaining knobs back into the low pressure ports.
6. Replace the plastic caps and capacitance detectors.

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962-42800-01 (Rev D) — Nov 2017
Handling Mercury Overfill
HANDLING MERCURY OVERFILL

1. On the Manual Control window, open the reservoir evacuation valve. Evacuate for twenty
seconds.
The Hg reservoir evacuated indicator should be displayed on the analyzer schematic. If it is not
shown, do not proceed to the next step. Instead, verify that the mercury reservoir fill cap is
properly sealed on top of the mercury filling funnel (see Maintain Mercury Level on page 11
- 17). If the Hg reservoir evacuated indicator still is not displayed, contact a Micromeritics
Service Representative.
2. Open the gas inlet valve. Close the gas inlet valve when at least 15 psia or atmosphere is
attained.
3. Open the mercury drain valve.
4. Open the front panel of the analyzer and locate the Override switch on the small control
panel.
5. Press the switch. This allows mercury to drain back into the reservoir.
6. Release the switch as soon as the pulsed buzzing stops. Close the mercury drain valve.
7. Close the reservoir evacuation valve. If the pulsing tone remains, call the Micromeritics Ser-
vice Department. The analyzer may be powered off.
REPLACE CHAMBER CUP SEALS

The chamber plug is sealed into the high pressure chamber by means of a cup seal and a backup
ring. There is also an O-ring in the vent valve. See Replace the Vent Valve O-ring on the next
page.These rings should be checked monthly and replaced when the backup ring extrudes, small
slivers come from the cup seal or backup ring, or pinched areas appear on the cup seal. The rings
may also need replacing when oil appears around the top of the chamber or when it is difficult to
maintain pressure in the high pressure chamber
1. Remove the chamber cup seal and backup ring without scratching the surrounding surfaces.

11 - 21
962-42800-01 (Rev D) — Nov 2017
2. Replace the backup ring on the lower portion of the chamber plug with the backup ring upper-
most and with the groove of the cup seal downward.
3. Replace the O-ring in the vent valve.
REPLACE THE VENT VALVE O-RING
1. Remove the vent valve from the top of the high pressure chamber by turning the vent valve
counter-clockwise.
2. Gently remove the O-ring on the vent valve and replace with a new one.

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962-42800-01 (Rev D) — Nov 2017
Change High Pressure Fluid and Clean High Pressure
Chamber
CHANGE HIGH PRESSURE FLUID AND CLEAN HIGH PRESSURE

CHAMBER
The high pressure fluid should be changed after every 600 samples or 3 months to ensure accurate
results. It should also be changed if mercury is spilled into a high pressure chamber. Small drops of
mercury in the bottom of the chamber can cause erroneous results.
1. Remove the high pressure fluid from the high pressure chambers using the syringe provided.
2. Clean the high pressure chambers using a clean cloth dampened with IPA.
3. When the chambers are completely dry, add new high pressure fluid.
MAINTAIN HYDRAULIC PUMP FLUID LEVEL
When changing the hydraulic pump fluid, use only Mobil-1 50W-50 Synthetic Motor Oil
(Micromeritics part number 004-16011-00).
The hydraulic pump fluid container is located in the lower left corner inside the analyzer's front door.
Check the fluid level when the intensifier on the schematic is in the down position. Add fluid as
necessary to keep the fluid level near the top of the container.

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962-42800-01 (Rev D) — Nov 2017
Filling the fluid container when the intensifier is in the up position can cause the fluid to
overflow the when intensifier is lowered.
To add fluid to the container, remove the cap to the fluid container and add fluid as necessary.
Replace the cap when done.

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962-42800-01 (Rev D) — Nov 2017
Vacuum Pump
VACUUM PUMP
REPLACE VACUUM PUMP EXHAUST FILTER
The exhaust filter is attached to the mercury vapor filter on the vacuum pump.
1. Loosen the wing nut that secures the clamp between the exhaust filter and the mercury vapor
filter by turning the nut counterclockwise. Open the clamp and remove it, the centering ring,
and the exhaust filter.
2. Inspect the centering ring for wear and replace if necessary.
3. Align the centering ring between the replacement exhaust filter and the mercury vapor filter.
4. Open the clamp and place it around the lip of the exhaust filter, mercury vapor filter, and cen-
tering ring.
5. Close the clamp and secure it by turning the wing nut clockwise. Tight the wing nut finger tight.

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REPLACE THE MERCURY VAPOR FILTER
Mercury vapor filters are used on vacuum pumps to minimize the release of mercury
vapors.
The mercury vapor filter should be replaced annually when preventive maintenance is
performed. When the mercury exhaust filter is replaced, go to Unit [n] > Show Dash-
board. Right click the Days until Hg filter replacement is due box and click Reset. The
counter resets to 365 days until the next filter change is due. Service Mode and pass-
word are required to make this change.
1. Loosen the wing nut that secures the clamp between the exhaust port and the mercury vapor
filter by turning the nut counter-clockwise.
2. Open the clamp and remove it.
a. Remove the protective cover if this is an initial installation.
b. If this is not an initial installation, remove and inspect the centering ring for wear and
replace if necessary.
3. Align the centering ring between the mercury vapor filter and the exhaust port.
4. Open the clamp and place it around the lip of the exhaust port, mercury vapor filter, and cen-
tering ring.
5. Close the clamp and secure it by turning the wing nut clockwise. Tighten the wing nut finger
tight.

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962-42800-01 (Rev D) — Nov 2017
Change or Add Vacuum Pump Oil
CHANGE OR ADD VACUUM PUMP OIL
Drain the oil while the pump is warm and disconnected from the power source.
The pump must be removed from the analyzer to change the oil. Use oil supplied by Micromeritics or
refer to the vacuum pump manual for other acceptable oils.
1. Unplug the vacuum pump from the power source.

2. Remove the exhaust filter by loosening the wing nut on the clamp between the vacuum pump
exhaust filter and the mercury vapor filter.
3. Remove the centering ring and place to the side.
4. Remove the vacuum hose from the vacuum pump by loosening the wing nut on the clamp
between the vacuum pump and the vacuum hose.
5. Remove the centering ring and place to the side.
6. Remove the pump from inside the analyzer.
7. Remove the vacuum pump from inside the analyzer .
8. at the top of the oil vapor trap. Swing the clamp open and remove the trap from the hose.
9. Grasp the handle on top of the vacuum pump and place the pump on a work surface.
10. Place a waste container under the drain spout.
11. Remove the drain plug and drain the oil into the waste container.
12. Replace the drain plug.
13. Remove the drain plug from the oil-fill port on top of the pump.

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962-42800-01 (Rev D) — Nov 2017
14. Slowly add oil to the port until the level is midway between the indicator lines in the oil-level win-
dow when the pump is running.
Do not allow oil to rise above the midway position when the pump is running. Doing so
may cause oil to splash into the oil filter causing contamination.
15. Check the washer or O-ring used at the oil-filling port and replace if necessary.
16. Insert the oil-fill plug and turn clockwise to tighten.
17. Return the vacuum pump to the original position inside the analyzer.
18. Reconnect the vacuum pump hose.
19. Reconnect the exhaust filter to the top of the mercury vapor filter.
20. Reconnect the power cord to the power source.
21. Turn the vacuum pump on and recheck the oil level.
22. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture from the
fresh fluid and to produce efficient vacuum operations.

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Check Valves for Leaks
CHECK VALVES FOR LEAKS

Valve leakage due to sample particles or oxidized mercury deposits on valve seats can cause
difficulty in attaining adequate vacuum conditions. To test for leakage:
1. Open valves 1, 2, 3, and 8.

2. If the pressure does not reach 100 µm in less than five minutes, the system has a leak. If this
occurs, clean the valves. See Clean Valves below.
CLEAN VALVES
Ensure all mercury is below drain valves. Evacuate the reservoir and open the drain and
fill valves with the low pressure manifold at atmospheric pressure. Failure to do so could
result in a mercury spill.
Power off the analyzer before removing the rear panel. Failure to do so could result in
personal injury.
1. Disconnect the power cord.

2. Remove the upper rear panel by removing the retaining screws.

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962-42800-01 (Rev D) — Nov 2017
3. Remove the 11/16 in. nut retaining the valve actuating coil from the mercury fill [5] and drain [6]
valves. Pull the coils off.
Valve Locations
Valve Location Description
1 Servo isolation valve
2 Fast evacuation valve
3 Vacuum valve
4 Gas inlet valve
5 Mercury fill valve
6 Mercury drain valve
7 Mercury reservoir evacuation valve
8 Evacuation reservoir valve
9 Vent valve. If a cap detector is removed when the pressure is above atmo-
spheric pressure, the low pressure system will be vented to atmosphere
with this valve.

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962-42800-01 (Rev D) — Nov 2017
Clean the Analyzer
4. Place a container below the valves to capture any retained mercury.

5. Remove the plunger housing from each using the special spanner wrench from the accessory
kit.
6. Clean the plunger and housing with IPA and expose the valve seat. Use a pipe cleaner to
clean the valve seat. Ensure that no lint remains on the sealing surface.
7. Re-assemble the valves.
8. The slow / medium, medium, and fast evacuation valves, and the gas inlet solenoid valve are
much less likely to collect debris. They can be cleaned (as outlined above) if cleaning the mer-
cury valves did not solve the vacuum difficulty.
CLEAN THE ANALYZER

The exterior casing of the analyzer may be cleaned using a clean cloth dampened with isopropyl
alcohol (IPA), a mild detergent, or a 3% hydrogen peroxide solution. Do not use any type of abrasive
cleaner.
Do not allow liquid to penetrate the casing of the analyzer. Doing so could result in
damage to the unit.
REMOVE MOISTURE FROM THE ANALYZER

A difficult-to-detect vacuum problem arises if moisture is allowed to collect in the system. A probable
accumulation point is the restricting frits that control flow rates. The best way to remove moisture is to
evacuate the analyzer at full rate for several days. If the indicated vacuum continues to decrease
slowly over this period, accumulated moisture is the probable cause of the vacuum difficulty.
To prevent the accumulation of moisture in the future, do not evacuate samples which hold
excessive water vapor. This is best done by precleaning samples in a drying oven.

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962-42800-01 (Rev D) — Nov 2017
REPLACE THE BANANA PLUG

HIGH PRESSURE CHAMBER
1. Remove the fluid from the high pressure chamber using the syringe provided.
2. Remove any mercury droplets found in the high pressure chamber. Clean the high pressure
chamber using a clean dry cloth.
3. Locate the feedthru assembly in the bottom of the high pressure chamber. Remove the
banana plug from the feedthru assembly using the banana plug tool provided.
4. Insert a new banana plug into the banana plug tool, ensuring the flat sides of the hex fit down
into the slot.
5. Screw the banana plug into the feedthru assembly. Do not cross-thread or overtighten the
banana plug.
6. Refill the high pressure chamber with clean high pressure fluid.
LOW PRESSURE CAPACITANCE DETECTOR

1. Remove the low pressure capacitance detector from the low pressure station.
2. Remove the banana plug from the low pressure capacitance detector using the banana plug
tool provided.
3. Insert a new banana plug into the banana plug tool, making sure the flat sides of the hex fit
down into the slot.

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962-42800-01 (Rev D) — Nov 2017
Low Pressure Capacitance Detector
4. Screw the banana plug into the low pressure capacitance detector.

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PENETROMETER NUT
REMOVE THE PENETROMETER NUT

If the penetrometer nut cannot be easily opened by hand, it may have become sealed too tightly
during analysis. Use the penetrometer wrench to remove it.
2. Place the wrench peg into a hole in the penetrometer nut. Use the penetrometer tool to sta-
bilize the cap while tightening the nut counter-clockwise.
3. Position the wrench so the peg on the wrench fits into the notch on the nut.

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962-42800-01 (Rev D) — Nov 2017
Tighten the Penetrometer Nut
4. While holding the penetrometer tool, turn the wrench clockwise to loosen and remove the nut.
TIGHTEN THE PENETROMETER NUT

1. Apply grease to the penetrometer bulb and remove any excess grease.
2. Hold the penetrometer upright (sample bulb opening facing upward) and place a seal on the
bulb opening.
3. Turn the seal one half turn to smooth the grease and seat the seal.
Take care not to move the seal after seating onto the penetrometer bulb. The grease
may extrude too much and cause an air leak.

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962-42800-01 (Rev D) — Nov 2017
4. Place the wrench peg into a hole in the penetrometer nut. Use the penetrometer tool to sta-
bilize the cap while tightening the nut counter-clockwise.
POWER ANALYZER ON AND OFF
DO NOT connect or disconnect cables when the analyzer is powered ON.
Power ON the equipment in the following order:
The vacuum line from the low pressure system and the vacuum pump filter must be
installed before applying power to the vacuum pump. Refer to your vacuum pump
manual.
1. Analyzer
2. Computer, monitor, and printer
Power OFF the equipment in the following order:
1. Exit the analysis program. Failure to do so could result in loss of data.

2. Computer, monitor, and printer
3. Analyzer
RECOVER FROM A POWER FAILURE

The analyzer saves entered and collected data in case of power failure. File parameters and any
other data entered will still be present when power is restored. If an analysis was in progress when
the power failure occurred, it will be canceled when the analyzer restarts. Any data collected during
the analysis will still be present, but the analysis should be restarted in order to produce complete
results.

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A Blank and Sample Compression Corrections
A BLANK AND SAMPLE COMPRESSION CORRECTIONS

Baseline errors in AutoPore V data are errors that occur even when no sample is placed in the
sample bulb and when a zero intrusion or extrusion volume of mercury would be expected as the
pressure is increased to its maximum pressure and then decreased again. The material which
follows relates the causes of these errors and discusses ways to minimize and compensate for them
when maximum accuracy is required.
BASELINE ERRORS
When the AutoPore applies pressure to the mercury, penetrometer, and surrounding high pressure
oil, compression occurs.
Compressibility effects account for a substantial portion of the baseline errors. The penetrometer
bulb and capillary are made of glass which decreases in linear dimensions by about 0.8% and in
volume by 2.3% at 60,000 psia. If the mercury were incompressible, a typical penetrometer having a
400 microliter capillary and a 5 milliliter bulb would experience a rise of mercury in the capillary of
about 124 microliters or 31% of the capillary. Fortunately, mercury compresses also, but slightly
more than glass such that the capillary actually falls some as the pressure is increased. The
compressibility amounts to about 150 microliters in this example leaving a net fall of 26 microliters or
about 6% of the capillary. The oil which surrounds the penetrometer and transmits the pressure to
the mercury compresses at more than 10 times the rate of the mercury and occupies only 3/4 the
original volume at 60,000 psia. Some of the oil is in the electric field of the capacitor, especially
around the sample bulb and its connection to the exterior. The dielectric constant of the oil increases
with its density. This contributes an increasing capacitance which cancels some of the decrease due
to the net fall of mercury with compression.
Other effects caused by compression arise from the plastic insulators which are used on the
penetrometer bulb base to prevent an electrical short circuit. Not only does the plastic compress
almost as much as the oil, but it lags behind and only slowly assumes its final density. This is
especially pronounced upon release of pressure where the plastic may continue to increase in
dimensions for almost an hour. It also tends to increase the dielectric constant and capacitance with
increasing pressure. The pressure vessel expands as the internal pressure is increased and, like the
plastic, requires considerable time to stabilize. The resulting changes in spacing from the sample
bulb to the walls and bottom causes a decrease in capacitance. Micromeritics has minimized this
effect by making the initial spacings as large as is practical.

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962-42800-01 (Rev D) — Nov 2017
Another effect, and the one most difficult to predict, arises from the similarity of the penetrometer to a
thermometer. This would not be troublesome if its temperature could be maintained constant, but
compression of the surrounding oil causes a temperature rise of nearly 50 ºC in the oil and a smaller
change in the glass and mercury. How quickly this heat is transferred to the mercury depends upon
how rapidly the pressure is being increased, the relative amounts of oil and mercury present, and
how recently the vessel has been previously cycled and the metal and oil warmed relative to the
penetrometer. Release of the pressure causes the inverse effect, chilling the oil and setting up a
reversal of the heat flow. The thermal gradient across the glass of the penetrometer may be
considerable such that little benefit may be derived from precisely equalizing the temperature
coefficients of the mercury and glass. As might be expected this problem is worst when the sample
bulb is large and the capillary volume small. Choosing the right penetrometer helps minimize this
effect. Make sure the sample nearly matches the size of the sample bulb and that the capillary
volume is large enough to satisfy intrusion.
APPROACHES FOR ERROR COMPENSATION

Situations arise where the typical errors of about 1.0% of capillary volume are significant or where
the errors exceed this level due to unfavorable sample characteristics. Most commonly, this happens
when one of the following is encountered: 1) The amount of sample available is so limited that the
intrusion volume is only a small fraction of the smallest diameter capillary; 2) adequate sample is
available but the porosity is so low that a limited amount of the smallest capillary is used even though
the largest sample bulb is filled; 3) the sample is of small or moderate porosity and its compressibility
or thermal properties differ considerably from those of mercury; 4) accuracy and reproducibility
specifications have been imposed at levels tighter than the typically expected levels for mercury
porosimetry. In such cases “blank corrections” may be used to advantage.
Micromeritics’ AutoPore provides four different ways to apply blank corrections. The first, and
simplest, is by use of stored formulas based upon averages of large numbers of blank runs on
mercury-filled penetrometers under varying rates of pressure build and release. No provisions are
made for entering compressibility data or thermal data since these numbers are seldom known and
the formulas would become very complex. Typical examples of blank runs are shown in Figures 1, 3
and 7. Typical examples of formula blank correction of data are shown in Figures 2 and 6. It is very
important that trial blank runs be made when applying these formulas to ensure that a reasonable
degree of correction is actually attained under the running conditions being used.
The second technique is apt to be much more useful. It permits the user to run a blank run, store the
results using the exact run conditions and penetrometer type to be used for the real sample, and
subtract this result from other runs. Examples of correction by subtracting a blank run file are shown
in Figures 4 and 8.

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962-42800-01 (Rev D) — Nov 2017
Approaches for Error Compensation
The third technique provides the highest degree of compensation possible and can be attained when
the exact penetrometer to be used later is loaded with a nonporous sample of the same mass and
material as the porous sample to be run later. When analyzed, the non-porous sample will expose all
the aforementioned compressibility effects which can then be subtracted from the porous sample
run. This third technique has the advantage of compensating for differences in compressibility and
thermal effects between mercury and the sample material. Care should be exercised that the interval
between runs, oil temperature, and penetrometer temperature, and any other initial conditions are
made as nearly identical as possible. Figure 9 is a typical baseline run so obtained. Figure 10 is a
subsequent blank run corrected using the Figure 9 data and shows the actual degree of correction
attained.
Besides running blank runs, correction files may be created by manually entering the data. This
fourth technique allows entry of the average of several blank runs, assuring a representative
correction.
Figure 1
A blank run on a 5-mL powder penetrometer with

a 1.1-mL stem volume. The rise in the initial
depressurization data is primarily caused by
thermal effects. As the hydraulic fluid is allowed
to expand, it cools. this in turn cools the mercury
in the penetrometer, causing it to contract and
recede in the stem, giving the appearance of
positive intrusion during depressurization.
Figure 2
The difference between the blank data in Figure

1 and the formula blank correction for a run under
the same conditions. The formula cancels some
of the error, but does an imperfect job in this
case.

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962-42800-01 (Rev D) — Nov 2017
Figure 3
Another blank data set taken under identical

conditions to those for Figure 1. The similarity
between the two blank data sets is an indication
of the excellent repeatability of blank runs.
Figure 4
The difference between the blank data from

Figure 1 and the blank data from Figure 3. This
demonstrates that blank data collection and
subtraction is a powerful method for accurately
removing blank error from sample data.
Figure 5
Uncorrected data from analysis of a sample of

controlled pore glass made of a mixture of three
pore sizes. Note the three distinct regions of
intrusion between 0.03 and 0.01 micrometers on
the pressurization curve, and the corresponding
extrusion regions. The apparent intrusion at sizes
above 10 micrometers is due to interparticle
filling. The apparent intrusion between 0.01 and
0.003 micrometers, and the “loop” in the
extrusion curve from 0.04 to 0.003 micrometers,
are due to a combination of sample compression
and blank error. There is no actual intrusion in
this region.

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962-42800-01 (Rev D) — Nov 2017
Approaches for Error Compensation
Figure 6
The data from Figure 5 with the formula blank

correction applied. Note that the rise at the top
due to blank error has been removed, but the
apparent intrusion due to sample compression
remains. This is because the formula makes no
attempt to account for sample compression.
Figure 7
A blank run with the same type of penetrometer

under the same conditions as the sample in
Figure 5. It is dominated by the initial increase
between pressurization and depressurization,
primarily due to thermal effects.
Figure 8
The sample data from Figure 5 corrected by

subtracting the blank data from Figure 7. Note
that practically all of the blank error and
compression data have been removed, leaving
only the filling curve and the actual intrusion. The
sample compression is effectively canceled
because the compression coefficient of mercury
is close to that of the controlled pore glass used
as sample. Many solid materials have
compression coefficient fairly close to that of
mercury, making this a very effective means of
blank correction in many cases.

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Figure 9
Uncorrected data from an essentially nonporous

sample of the same type of glass shown in Figure
5. The mass of sample used was approximately
equal to the mass of porous sample analyzed, so
that the same volume was occupied. Note the
filling curve and the blank error “loop.” The slight
incline of the intermediate plateau and the angle
of the “loop” are due to compression of the
sample.
Figure 10
The difference between the porous sample data

of Figure 5 and the nonporous sample data of
Figure 9. Some of the filling curve has been
removed, as well as all blank error and sample
compression effect, leaving an accurate picture
of the actual intrusion. This is the preferred
method of blank correction, especially for
materials with compression coefficients
substantially different from that of mercury, and
where maximum accuracy is desired.

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B Choose Proper Pump-Down Rates for Unfamiliar
Sample Materials
B CHOOSE PROPER PUMP-DOWN RATES FOR UNFAMILIAR

SAMPLE MATERIALS
There are a number of characteristics of an unfamiliar sample which can aid you in making a proper
decision as to how aggressively the sample may be pumped down. Some of these characteristics
are listed below. The assumption is always made that the sample material has been first dried in a
shallow pan at 150 ºC or higher for one hour or in a vacuum oven.
Samples, whether in the form of fine powders, granules, or even larger pieces, require extreme
caution if one or more of the following characteristics are noted or known to be the case:
l a fine dust is raised upon stirring or shaking and the sample shows little sign of quickly settling
l the sample is a finely powdered organic material
l the sample is known to be microporous or mesoporous with pores of less than 100 Angstrom
width
l the sample is known or suspected to be a carbon
l the sample is known or suspected to be a zeolite
l the sample is known or suspected to be a fluid cracking catalyst
l the sample has significant fine particle content below 10 mm
l the sample leaves behind a visible deposit of fine particles when transferred from a weighing pan
Such sample materials should be evacuated at initial pump down rates of about 0.5 psia/minute or
more slowly if of marked fineness until a pressure of 0.1 psia is reached. The pulsing of the second
pump down path should be maintained until 100 mmHg is reached before the final shift to the third
and most direct pump down path takes place. The penetrometer must be filled only about 1/3 full so
that there is a margin of clearance between the stem bore and the sample bed.
Sample materials which are coarse, medium, or dense powders, or are composed of obviously non-
shedding chunks, pellets, or extrudates, can be pumped down at rates of 1 to 2 psia per minute until
a pressure of 0.25 psia is reached. The pulsing of the second pump down path should be maintained
until 250 mmHg is reached before the third pump down path takes over.
Sample materials that obviously present little risk such as monolithic chunks or very coarse, dense
granules usually can be pumped down at near maximum rates. For these, specify 5 psia per minute
initial pump down followed by a change to the second path at 0.5 psia and finally a transition to the
direct path at 500 mmHg.
In most cases, you should choose a conservative rate of evacuation to be on the safe side. When
large numbers of samples of a material are to be run, the potential time savings may make it
worthwhile to investigate as to whether faster pump down rates might be possible without risk. To do
so, leave the capacitance transducer off the penetrometer base so that you may observe the sample
during a trial pump down performed at slightly higher than the usual speed. Twenty percent
increases in pump-down rates and pressures of path changeovers are reasonable trial increases.

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B Choose Proper Pump-Down Rates for Unfamiliar
Sample Materials
Monitor closely during all portions of the pump-down sequence, especially as changes from one path
to another occur. Should the sample bed or any particles begin to boil or move, immediately stop the
pump down and return the sample to atmospheric pressure; reduce the pump down rate to a slower
rate and try again. If the pump down was successful, then another twenty percent speed increase
might be attempted. Continue until a suitable rate is found. Note that this procedure is not without
risk and must be done very carefully.
The amount of time for which to continue the extended pump down after the lowest target on the
third path has been met will depend upon the structure of the sample and what volatile materials may
be present within it. Large chunks of porous materials such as sandstone or green ceramics or
concrete may present a considerable diffusion barrier for gases and vapors traveling to their surface
and may require extended exposure times to vacuum to sufficiently clear the internal pores of this
obstructive matter which would prevent fully measuring the true porosity. Experience and prior
knowledge of the sample can be used for guidance.
Additionally, a manual mode test can be done in which you pump the sample down to the target
pressure, and then close it off from further vacuum and monitor the rate and ultimate value of the
pressure rebound that results from the tardy release of gas or vapor. The amount of time before the
rebound ceases or remains within tolerable limits will serve to guide you in choosing an extended
evacuation time for future automatic runs of the sample material.

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C Proper Handling of Mercury
C PROPER HANDLING OF MERCURY

Because of its low melting point (-38.87 ºC), mercury (Hg) is slightly volatile at ordinary room
temperatures and its vapor may pose a health hazard if allowed to accumulate in the work space.
Although mercury can enter the body through the skin, lungs or digestive system, breathing air laden
with high concentrations of mercury vapor is the most common cause of mercury poisoning. Chronic
poisoning caused by long-term exposure to low levels of mercury is occasionally found among those
working with mercury. Mining, chemical, electrical, dentistry materials, pharmaceutical, explosive,
porcelain, photography, printing, battery, paint, engraving, jewelry, cosmetics and color are some of
the industries that use mercury in their manufacturing or processing.
Governmental agencies, i.e., National Institute for Occupational Safety and Health (NIOSH),
Environmental Protection Agency (EPA), etc., and some industries have set criteria and
recommended standards to protect the health and safety of workers exposed to mercury. A
Threshold Limit Value (TLV) of 0.05 mgHg/cubic meter of air, recommended by the American
Conference of Governmental Industrial Hygienists, was among the first hygienic guides for
controlling exposure of mercury in the U.S. Values well below this level can easily be met through
proper ventilation, prompt and thorough cleanup of spills, good personal hygiene and safe storage
when working with mercury.
Health hazards from mercury can be prevented by limiting the average concentration of mercury to
values below the TLV in an 8-hour workday. This is achieved through proper ventilation in the work
area where mercury is handled; for example, a local exhaust ventilation system can be designed and
maintained to prevent the accumulation or recirculation of mercury vapor, dust and fume; all handling
of mercury can be confined to a hood, etc. Appropriate protective respiratory devices can be used
when mercury exposure continues to exceed the recommended standard. To ensure TLV levels are
met, governmental agencies suggest environmental levels of inorganic mercury be monitored every
six months: breathing-zone samples are collected to permit calculation of a time-weighted average
exposure for every operator. When any time-weighted average exposure is at or above the TLV,
immediate steps are required to reduce exposure below the standard.
Maintaining low temperature where mercury is used will help limit mercury concentration. Vapor
pressure of mercury goes up exponentially with temperature, for example, 20 ºC: P = 1.20 × 10-3
mmHg. As temperature increases from 20 to 40 ºC, the partial pressure of mercury vapor increases
fivefold.
Proper clean-up of mercury spills and disposal of mercury-contaminated articles will limit exposure.
In a poorly ventilated, closed area, where mercury spills have not been properly and thoroughly
cleaned, mercury concentration in air can become significantly elevated above the TLV of 0.05 mg
per cubic meter of air. The following figure shows that the equilibrium concentration of mercury at a
room temperature of 25 ºC reaches a level of 20 mg per cubic meter of air. This is 400 times the TLV,
resulting in a dangerous work environment. Surveys in labs where mercury is routinely used reveal
the presence of mercury in porous surfaces, in pools under cabinets or floors, and inside drawers
and lab equipment. This accumulation can be attributed to the lack of an effective clean-up
procedure for both large and small spills.

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C Proper Handling of Mercury
Mercury spills should be cleaned immediately and thoroughly by mechanical, chemical or other
appropriate means. Micromeritics uses and recommends that you use plastic or rubber gloves and a
small vacuum pump equipped with a mercury vapor absorbing filter on the exhaust and a vacuum
probe with a mercury trap on the inlet for efficient pick-up of small mercury particles in cleaning
mercury spills. Afterwards, the spill area should be swabbed with a mercury decontaminants1 ) and
allowed to dry.
The health status of those working with mercury should be monitored regularly, with emphasis
placed on good personal hygiene to prevent contamination of hands, mouth, clothing or food. Hand
washing facilities, including hot and cold running water, soap, hand cream, and towels should be
made available adjacent to mercury work areas. Clothing contaminated with mercury should be
stored in vapor-proof containers pending removal for laundering.
1 ) Mercury decontaminants may be purchased from Fisher Scientific (800/766-7000) or Lab Safety
Supply (800/356-0783). They also may be available from your local laboratory supplier.

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Proper Use of Mercury as a Tool in Pore Structure Ana-
lyses
Open containers for storage of mercury in the work area should be covered with an aqueous or an oil
layer and kept at ambient temperatures to prevent vaporization. Because of permeability of
polyethylene or plastic bottles to mercury vapor, thick glass bottles, stainless steel or cast iron
containers are recommended for storing mercury. To avoid dangerous chemical reactions, mercury
should not be stored with acetylene, fulminic acid, ammonia and oxalic acid.
PROPER USE OF MERCURY AS A TOOL IN PORE STRUCTURE

ANALYSES
Micromeritics’ Mercury Intrusion Porosimeters obtain accurate and reproducible pore structure
analyses using mercury. Mercury is ideal as an intrusion liquid in the porosimetry method because it
does not wet nor react with most materials. By measuring the amount of mercury intruded into the
pores of a powdered or solid sample, the porosimeters give valuable data from which pore size,
volume and distribution, as well as apparent densities, pore surface area and particle size can be
determined.
All of Micromeritics’ porosimetry instruments are designed with safety in mind. They come equipped
with built-in spill and vapor safeguards that minimize operator exposure to mercury. They also are
designed so that you may connect them to a ventilation system that pulls ambient air over the
counter, through the instrument and out a duct at the rear. A built-in tray work area allows the
operator to easily wipe exposed mercury to a dish where it is covered with oil. Our product literature
on porosimetry supplies detailed site recommendations to assure safe operation.
Mercury vapor levels well below the accepted safe level can easily be achieved through regular
monitoring, diligent handling and proper clean-up practices.

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D Theory
D THEORY
Mercury porosimetry is based on the capillary law governing liquid penetration into small pores. This
law, in the case of a non-wetting liquid like mercury and cylindrical pores, is expressed by the
Washburn equation
where D is pore diameter, P the applied pressure, γ the surface tension, and ϕ the contact angle, all
in consistent units. The volume of mercury V penetrating the pores is measured directly as a function
of applied pressure. This P-V information serves as a unique characterization of pore structure.
Pores are rarely cylindrical, hence the above equation constitutes a special model. Such a model
may not best represent pores in actual materials, but its use is generally accepted as the practical
means for treating what, otherwise, would be a most complex problem.
The surface tension of mercury varies with purity; its usually accepted value and the value
recommended here is 485 dynes/cm. The contact angle between mercury and the solid containing
the pores varies somewhat with solid composition. A value of 130 degrees is recommended in the
absence of specific information to the contrary.
Mercury extruding from pores upon reduction of pressure is in general accord with the above
equation, but indicated pore diameters are always offset toward larger diameters. This results from
equivalent volumes of mercury extruding at pressures lower than those at which the pores were
intruded. It is also commonly observed that actual pores always trap mercury. The first phenomena
is usually attributed to receding contact angles being less than advancing ones. The second is likely
due to pore irregularities giving rise to enlarged chambers and “inkwell” structures. These
phenomena give rise to hysteresis phenomena, i.e., distinct intrusion and extrusion P-V curves.
Log in to your customer portal to access the Calculations document for a discussion on Pore Surface
Area Computation.

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E Use of the Maximum Intrusion Volume Option
E USE OF THE MAXIMUM INTRUSION VOLUME OPTION

Using the maximum intrusion volume option allows routine analyses with fewer points in a pressure
table while maintaining good resolution. However, use of the maximum intrusion volume requires
some knowledge of the total pore volume of the sample to be analyzed. You should use about 2% of
the sample’s total pore volume as the maximum intrusion volume. This would give about fifty points
for the intrusion pore spectrum and should be adequate to completely characterize most samples.
The AutoPore IV will automatically add a pore spectrum point any time it sees an increment of
intrusion equal to the maximum intrusion volume specified.
Care should be taken not to use too small a maximum intrusion volume. Use of a value less than
0.4% of the total intrusion volume will cause too many points to be taken at lower pressures. The
total of 1000 data points will be exhausted and the analysis will terminate prematurely.
Use of too small a maximum intrusion volume can also cause points to be taken too close together on
the pressure axis. If this causes pressures to be taken within the target pressure tolerance of each
other, an apparent pressure decrease may be reported during the intrusion sequence. A reported
pressure drop greater than 10 psi or 0.5% of the target pressure will be interpreted as the end of the
intrusion segment. Reported summary data (such as total intrusion volume) will be reported at this
point, rather than at the maximum pressure as intended. Data for graphs other than cumulative
intrusion volume will also be terminated at this point.

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F Worksheets
F WORKSHEETS
Worksheets in this section may be copied as needed.
See also:
l Analysis Conditions Worksheet on the next page

l Penetrometer Properties Worksheet on page F - 3
l Pressure Table and Tabular Data Worksheet on page F - 4
l Report Options Worksheet on page F - 5
l Sample Data Worksheet on page F - 6
l Volumetric Reference Capsule Worksheet on page F - 7

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F Worksheets
ANALYSIS CONDITIONS WORKSHEET

File Name: __________________________________________________________
Analysis conditions identifier

Low pressure equilibration
¨ Time ¨ Rate
Max. intrusion volume
Evacuation Initially evacuate at
Switch to medium at
Switch to fast at
Evacuation target
Continue evacuating for
High pressure equilibration ¨ Time ¨ Rate
¨ Pressure-controlled scan
¨ Intrusion-controlled scan
Max. intrusion volume
Mercury Properties
Advancing contact angle
Receding contact angle
Hg surface tension
Hg density

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Penetrometer Properties Worksheet
PENETROMETER PROPERTIES WORKSHEET

File Name: __________________________________________________________
Penetrometer Number (etched on pen-

etrometer)
Mass. Weigh the loaded penetrometer.
Subtract the mass of the sample. Enter
the difference.
Volume
Constant
Stem Volume
Max. head pressure
If Blank, give file name:
Correction method
¨ Blank ¨ Formula ¨ None

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F Worksheets
PRESSURE TABLE AND TABULAR DATA WORKSHEET

l For pressure table, enter:
Filling pressure: ________________________________________________
Last low pressure point index: ____________________________________
l For tabular data, select:

¨ Pressure
¨ Pore size
¨ Percent intrusion
Entry Entry Entry Entry

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Report Options Worksheet
REPORT OPTIONS WORKSHEET

File name
Calculation range
¨ Pressure ¨ Pore size

Reports
Overlays
Sample 1 Sample 5
Sample 2 Sample 6
Sample 3 Sample 7
Sample 4 Sample 8

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F Worksheets
SAMPLE DATA WORKSHEET

______ Basic presentation sample file
______ Advanced presentation sample file
Port 1 Port 2 Port 3 Port 4

Sample file name or identifier (optional)
Penetrometer number (optional - etched

on penetrometer)
Sample mass(g). Enter this value on the
Sample Description tab.
Sample + penetrometer mass. Load the
penetrometer with sample and weigh.
Penetrometer mass. Subtract the sample
mass from the Sample + penetrometer mass
and enter the difference.
l If using Basic presentation, enter this

value on the Sample Information window.
l If using Advanced presentation, enter this
value on the Penetrometer Properties win-
dow.
High pressure port number (optional).

Enter the number of the high pressure port
where the sample is loaded.
Assembly mass. The mass of the sample
+ penetrometer + mercury. (Weigh the pen-
etrometer after the low pressure analysis.)
Enter this value on the Start High Pressure
Analysis window.

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Volumetric Reference Capsule Worksheet
VOLUMETRIC REFERENCE CAPSULE

WORKSHEET
Calculate the volumetric reference capsule volume three times, then record the average of these
calculations. When creating the penetrometer properties file, enter the average volume.
Penetrometer Number Date:

By:
First Calibration of Reference Capsule Volume:
1. Mass of capsule filled with mercury g

2. Mass of sealed, empty capsule g
3. Mass of mercury (line 1 minus line 2) g
Room Temp = _____________ °C Density of mercury * = g/ml

4. Volume of capsule (line 3 ÷ density of mercury) ml
Second Calibration of Reference Capsule Volume:


Third Calibration of Reference Capsule Volume:


Average Reference Capsule Volume: ml
* See Density of Mercury Table on the next page for values.

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F Worksheets
DENSITY OF MERCURY TABLE

Density of Mercury Table
°C g/ml °C g/ml °C g/ml °C g/ml
18.0 13.5512 23.2 13.5384 25.2 13.5335 27.2 13.5286
19.0 13.5487 23.4 13.5379 25.4 13.5330 27.4 13.5281
20.0 13.5462 23.6 13.5374 25.6 13.5325 27.6 13.5276
21.0 13.5438 23.8 13.5369 25.8 13.5320 27.8 13.5271
22.0 13.5413 24.0 13.5364 26.0 13.5315 28.0 13.5266
22.2 13.5408 24.2 13.5359 26.2 13.5310 29.0 13.5242
22.4 13.5403 24.4 13.5354 26.4 13.5305 30.0 13.5217
22.6 13.5399 24.6 13.5350 26.6 13.5301 31.0 13.5193
22.8 13.5394 24.8 13.5345 26.8 13.5296 32.0 13.5168
23.0 13.5389 25.0 13.5340 27.0 13.5291 33.0 13.5144

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G Exported Data Example
G EXPORTED DATA EXAMPLE

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H Compute Volumetric Compressibility of a Sample Mater-
ial
H COMPUTE VOLUMETRIC COMPRESSIBILITY OF A SAMPLE

MATERIAL
Ideally, you should choose a sample material that is completely non-porous; if this is not the case,
then you should choose the pressure range over which the compressibility test is conducted such
that no pore filling occurs within it. Closed pores may not always cause volume changes during
testing but they may alter the results due to stress concentrations around them or because of their
effects upon measured density. Closed pores may also abruptly fail and even become open during
testing and cause invalid compressibility results to be reported. In some cases, such as the testing of
plastic foams at low pressures, the presence of closed pores may be acceptable and expected.
The sample mass and sample density must be known and available to a resolution and accuracy at
least three significant digits (preferably better) to permit accurate computation of the initial volume of
the sample material. Alternatively, an accurate geometric volume of a material such as one
containing closed pores (such as plastic foam) may be supplied. Before data reduction can be
performed, you must have available a “blank run” file consisting (at least ideally) of a run made with
the same penetrometer and accessory hardware that is to be used in the compressibility test and
(again ideally) on the same instrument ports as will be used in the compressibility run. The pressure
range of the blank run must, at a minimum, fully encompass the planned range to be used in the
compressibility measurement and have a minimum of seven uniformly spaced (linear basis) data
points inside the planned computation range and with the beginning and ending data points within
5% (pressure) of the planned computation range end points. It is also permissible for the “blank run”
to consist of a manually entered data file.
The first and second order isostatic pressure coefficients of volumetric compressibility for mercury
over the pressure range from zero psia to 60,000 psia must be known and available. All standard
input information such as sample material identity, equilibration times, evacuation information,
penetrometer constants, etc. that would be required for standard runs is required for a
compressibility run. Note that sample volume, bulk volume / density, and skeletal volume / density as
measured during the mercury porosimetry run are, in general, far too imprecise to yield good results
if used in the compressibility computations. For this reason, you must enter very accurate material
density and sample mass values to be used in computing an accurate initial sample volume or,
alternatively, directly enter a measured initial sample material volume.
The pressure table entered must contain at least seven pressure points uniformly spaced (on a linear
basis), with these points coinciding as closely as possible to those in the blank run which is to be used
along with the data in the final computation. As indicated above, the pressure values of the end
points achieved during the run must be within 5%

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I Advanced Reports - Python Module
I ADVANCED REPORTS - PYTHON MODULE
See also:
Mic Module Python Calls on page I - 11
The mic Python module is automatically imported when running a user supplied script. The module
provides access to intrusion / extrusion data and provides support for summary, tabular, and
graphical reports.
l Summary reports. Consist of summary sections, each containing a two-column table of label
and value pairs. Summary reports are created with the mic.summary call.
l Tabular reports. Consist of one or more tables each containing one or more labeled columns of
data. Tabular reports are created with the mic.table call.
l Graphical reports. Consist of a single graph with one or more curves on one or two y-axes.
Graphical reports are created with the mic.graph call.
Calls for accessing the sample file data can be found in the Mic Module Python Calls section of this
appendix. More advanced example python scripts are included in the analyzer software. Application
specific discussions can be found on http://www.micro-report.com
The examples in this topic are also included as a part of the Micromeritics installation pro-
cess and are located in the Scripts sub-directory.

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ADVANCED REPORT OPTIONS
The Selected Reports list box may display a User-Defined option rather than an
Advanced option. These options are the same.
Up to five Advanced reports, each with up to 10 summary reports, 10 tabular reports, and 10
graphical reports can be created. To use this feature, a file containing a Python script that imports a
"mic" Python module must be created. See Mic Module Python Calls on page I - 11 for an
example of Python script and functions for the "mic" Python module.
1. Create the Python script and save it in the Scripts directory.

2. Open a sample file with a Completed status.
3. Select Advanced in the drop-down list at the bottom of the window to return to the tabbed
view.
4. On the Report Options tab, select Advanced in the Selected Reports list box, then click Edit.
5. On the Advanced Report Options window, click Add in the Available Scripts group box to loc-
ate and select the Python script. Repeat for each script to be added.
6. In the Selected Reports group box, click the drop-down arrows to select up to five Python
scripts previously added in the Available Scripts box.
7. Click Pressures to add pressure points to the report. Click OK to return to the Report Options
tab.
8. Select the Overlay samples checkbox to enable the overlay sample feature.
9. On the Report Options tab, click Preview. The Python Reports will be included on the tabs
across the top portion of the Reports window.

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Scripts
Advanced Report Options Fields and Buttons Table

Add [button] Click to add additional Python reports.
Available Scripts Lists the available reports and provides the option to add, replace, edit
[group box] or remove reports.
Overlay samples (if Use to overlay samples as defined by the function.
shown) [check box]
Advanced Report 1 Use the drop-down lists to select currently-defined functions used to
through 5 define the report calculations and output.
[drop-down box]
tons on page 2 - 3.
SCRIPTS
RUN A SCRIPT
1. Open a sample file with a Complete file status.
2. Select Advanced in the drop-down list at the bottom of the window.
3. Select the Report Options tab.
4. Highlight Advanced in the Reports list box, then click Edit.
5. On the Advanced Report Options window, click Add. Locate and select one or more python
scripts then click Select. The selected scripts become a part of the drop-down list in the Avail-
able Scripts section of the Advanced Report Options window.
6. In the Selected Reports section, select up to five Advanced reports in the drop-down lists. Use
the Pressures button to include or exclude available pressures in the report.
7. Click OK.
8. Click Preview on the Report Options tab to view all reports selected in the previous window.

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EDIT A SCRIPT
When a script is added, the code is stored within the application. If the script changes out-
side of the application, the script file will have to be re-added to the Advanced Report
Options window for the changes to take affect.

Add Adds one or more scripts to the Available Scripts box. The added
scripts then become available as options in the Selected Reports
section.
Edit Edits the script stored within the application but does not affect the
original .py text file.
Remove Removes the script from the Available Scripts box but does not affect
original .py text file
Replace Replaces the contents of the selected script however, the script name
remains the same.
REMOVE A SCRIPT
Select the script in the Available Scripts box then click Remove. The script is removed from the
application however, the original .py text file is not affected.

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Summary Report
SUMMARY REPORT
This script produces a summary report with two summaries:
import mic
mic.summary( "My Summaries" )
mic.summary.add( "Summary A",

["label 1:", "label 2:", "label 3:"],
["val1", "val2", "val3"] )
mic.summary.add( "Summary B",

["label 4:", "label 5:", "label 6:"],
["val4", "val5", "val6"] )
The result is:

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TABULAR REPORT
If more than one column is required, the call mic.table is employed. This script produces a tabular
report consisting of two tables. NOTE: This script uses the Python package "numpy" and c-style
formatting of the numerical values.
import mic
import numpy as np
mic.table("My Tables")
mic.table.addtable( "My set A" )

mic.table.addcolumn( "x", ["1.0", "2.0", "3.0"] )
mic.table.addcolumn( "y", ["0.5", "1.0", "1.5"] )
x1 = 0.2
x2 = 0.5
x3 = 3.14159/2
mic.table.addtable( "My set B" )
mic.table.addcolumn( "x", ["%8.3f" % x1,
"%8.3f" % x2,
"%8.3f" % x3 ] )
mic.table.addcolumn( "sin(x)", ["%8.3f" % np.sin(x1),

"%8.3f" % np.sin(x2),
"%8.3f" % np.sin(x3)] )
mic.table.addcolumn( "cos(x)", ["%8.3f" % np.cos(x1),

"%8.3f" % np.cos(x2),
"%8.3f" % np.cos(x3)] )
The result is:

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Graphic Report
GRAPHIC REPORT
This script is an example of the mic module producing a graph with two curves:
import mic
import numpy as np
mic.graph( 'My Graph', 'x', 'f(x)' )
myx = np.array( [0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0 ] )
mic.graph.add( 'x^2', myx, myx*myx, marker='o' )
mic.graph.add( 'sin(x)', myx, np.sin(myx), marker='^' )
The results are:

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ACQUIRE BASIC INFORMATION FOR MERCURY POROSIMETRY

This script produces a graph of the intrusion and extrusion data, and a graph of the corresponding
distribution of pores. It applies the mic module python calls mic.intrusion and mic.extrusion.
import mic
xdat1, ydat1 = mic.intrusion('pressure', 1)

xdat2, ydat2 = mic.extrusion('pressure', 1)
mic.graph( 'Cumulative Intrusion vs. Pressure',
'Pressure (psi)', 'Cumulative Intrusion (mL/g)', xlinear = False )
mic.graph.add( 'Intrusion: Cycle 1', xdat1, ydat1 )
mic.graph.add( 'Extrusion: Cycle 1', xdat2, ydat2 )
xdat3, ydat3 = mic.intrusion('diameter', 1)

xdat4, ydat4 = mic.extrusion('diameter', 1)
mic.graph( 'Cumulative Intrusion vs. Diameter',
'Diameter (Angstroms)', 'Intrusion Volume (mL/g)', xlinear = False)
mic.graph.add( 'Intrusion: Cycle 1', xdat3, ydat3 )
mic.graph.add( 'Extrusion: Cycle 1', xdat4, ydat4 )
The results are:
The following script applies the generic mic module python calls mic.sample_information and
mic.report and also applies the AutoPore application specific calls mic.material_properties, and
mic.mercury_properties. Three summaries are produced:
l Sample Information
l Material Mercury Properties
l Intrusion Summary Results

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Acquire Basic Information for Mercury Porosimetry
import mic
mic.summary( "Summaries" )
mic.summary.add( "Sample Information:",

[ "Description:",
"Sample mass (g):",
"Assembly mass (g):",
"Penetrometer mass (g):"],
[ mic.sample_information("sample description"),
"%8.3f" % mic.sample_information("sample mass"),
"%8.3f" % mic.sample_information("assembly mass"),
"%8.3f" % mic.sample_information("penetrometer mass") ] )
mic.summary.add( "Material & Mercury Properties",

[ "Material name:",
"BET surface area (m^2/g):",
"Mercury Density (g/ml):",
"Mercury Surface Tension (dynes/cm):",
"Advancing Contact Angle (degrees):",
"Receding Contact Angle (degrees):" ],
[ mic.material_properties("material name"),
"%8.3f" % mic.material_properties("bet surface area"),
"%8.3f" % mic.mercury_properties("density"),
"%8.3f" % mic.mercury_properties("surface tension"),
"%8.3f" % mic.mercury_properties("advancing contact angle"),
"%8.3f" % mic.mercury_properties("receding contact angle") ] )
mic.summary.add( "Intrusion Summary Results",

[ "Total intrusion volume (mL/g):",
"Pore area (m^2/g):",
"Bulk density (g/mL):",
"Apparent density (g/mL):",
"Median diameter by volume (Angstroms):",
"Median diameter by area (Angstroms):",
"4 V/A average diameter (Angstroms):",
"Porosity (%):",
"Tortuosity:",
"Tortuosity factor:",
"Permeability (mdarcy):",
"Permeability constant:",
"Break-through pressure ratio:",
"linear compressibility coefficient (1/psi):",
"quadratic compressibility coefficient (1/psi^2):" ],
[ "%8.3f" % mic.report("hgsum", "total intrusion volume"),
"%8.3f" % mic.report("hgsum", "pore area"),
"%8.3f" % mic.report("hgsum", "bulk density"),

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"%8.3f" % mic.report("hgsum", "apparent density"),

"%8.3f" % mic.report("hgsum", "median diameter by volume"),
"%8.3f" % mic.report("hgsum", "median diameter by area"),
"%8.3f" % mic.report("hgsum", "4 V/A average diameter"),
"%8.3f" % mic.report("hgsum", "porosity"),
"%8.3f" % mic.report("hgsum", "tortuosity"),
"%8.3f" % mic.report("hgsum", "tortuosity factor"),
"%8.3f" % mic.report("hgsum", "permeability"),
"%8.3f" % mic.report("hgsum", "permeability constant"),
"%8.3f" % mic.report("hgsum", "break-through pressure ratio"),
"%8.3f" % mic.report("hgsum", "linear compressibility coefficient"),
"%8.3f" % mic.report("hgsum", "quadratic compressibility coefficient")])
The results are:

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Mic Module Python Calls
MIC MODULE PYTHON CALLS

TABLES
Available Mic Python calls for tables:
l Create a new tabular report

l Add a column
l Add a table
ADD A TABLE
This script adds a table to the last created tabular report:
mic.table.addtable( name )
Keyword arguments:
name --- the table name
ADD A COLUMN
This script adds a column to the last created table:
mic.table.addcolumn( header, values )
Keyword arguments:
header --- column header; must be a string (or convertible)

values --- column values; must be a list of strings (or convertible)
CREATE A NEW TABULAR REPORT

mic.table( title='User Table' )
Keyword arguments:
title --- the tabular report title (default = 'User Table')

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SUMMARY REPORTS
Available Mic Python calls for summary reports:
l Add a summary section to the last created summary report

l Create a new summary report
ADD A SUMMARY SECTION

This script adds a summary section to the last created summary report:
mic.summary.add( name, labels, values )
Keyword arguments:
name --- summary section name

labels --- column of labels; must be a list of strings
(or convertible) and the same length as values
values --- column of values; must be a list of strings
(or convertible) and the same length as labels
CREATE A NEW SUMMARY REPORT

mic.summary( title='User Summary' )
Keyword arguments:
title --- the summary title

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Graphic Reports
GRAPHIC REPORTS
Available Mic Python calls for graphic reports:
l Add a curve
l Add a curve using the second Y-axis
l Create a new graphic report
ADD A CURVE
This script adds a curve to the last created graphical report:
mic.graph.add( name, x, y, yyaxis=False, color=None, linestyle='-', mark-

er='a', graphtype='both' )
Keyword arguments:
name --- the curve name

x --- list of x values; must be a list of floats
(or convertible) and the same length as y
y --- list of y values; must be a list of floats
(or convertible) and the same length as x
yyaxis --- place this curve on the yy-axis if True
otherwise place on the y-axis (default = False)
color --- RGB color as an HTML hex string (e.g., '#4169e1')
or a three-element list or tuple (e.g., [65,105,225]);
if None, color is automatically selected (default = None)
linestyle --- line style; (default = '-')
'-' : solid
'--' : dash
'.' : dot
'-.' : dash dot
'-..' : dash dot dot
marker --- marker shape; (default = 'a')
'+' : plus
'o' or '0' : circle
'x' : cross
'^' : up triangle
'v' : down triangle
's' : square
'd' : diamond
'8' : hourglass
'~' : horizontal hourglass
'' or None : no marker
'a' : automatically selected

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graphtype --- graph type; (default = 'both')

'curve' or 'c' : curve
'points' or 'p' : points
'both' or 'b' : curve-and-points
'hist' or 'h' : histogram
ADD A CURVE USING THE SECOND Y-AXIS

This script adds a curve to the last created graphical report using the second y-axis:
mic.graph.addyy( name, xx, yy )
Add a curve to the last created graphical report using the second
y-axis. The arguments to this call are the same as to mic.graph.add
with the argument
CREATE A NEW GRAPHICAL REPORT

mic.graph( title='User Graph', xlabel='X axis', ylabel='Y axis', yylabel='YY
axis', xlinear=True, ylinear=True, yylinear=True )
Keyword arguments:
title ---
the graphical report title (default = 'User Graph')
xlabel ---
x-axis label (default = 'X axis')
ylabel ---
y-axis label (default = 'Y axis')
yylabel ---
yy-axis label (default = 'YY axis')
xlinear ---
x-axis linear scale; if false, use log scale
(default = True)
ylinear --- y-axis linear scale; if false, use log scale
(default = True)
yylinear --- yy-axis linear scale; if false, use log scale
(default = True)

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Get Intrusion-Extrusion Data
GET INTRUSION-EXTRUSION DATA

mic.intrusion( xaxis = 'pressure', cycle = 1 ) :
Keyword arguments:
xaxis --- Specifies what the defendant variable will be

'pressure' in units of psi (default)
diameter' in units of Angstrom
cycle --- Specifies the cycle number

(default = 1)
Usage:
p, v = mic.intrusion()
p, v = mic.intrusion('pressure', 2)
d, v = mic.intrusion('diameter')
p --- array of pressures (psi)

d --- array of diameters (Angstrom)
v --- array of intrusion volumes (ml/g)
mic.extrusion( xaxis = 'pressure', cycle = 1 ) :
Keyword arguments:
xaxis --- Specifies what the defendant variable will be

pressure' in units of psi (default)
'diameter' in units of Angstrom
cycle --- Specifies the cycle number

(default = 1)
Usage:
p, v = mic.intrusion()
p, v = mic.intrusion('pressure', 2)
d, v = mic.intrusion('diameter')
p --- array of pressures (psi)
d --- array of diameters (Angstrom)
v --- array of intrusion volumes (ml/g)

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GET MERCURY PROPERTIES

mic.mercury_properties( property='' , sample_number = 0 ) :
Keyword arguments:
property --- the property value to return.

If '' or None, then return all the properties
strings available for the sample material.
Default value is None.
sample_number --- Identifier for the sample material to retrieve

0 : current sample file (default)
1 through 8 : corresponding overlay sample file
Usage:
property_list = mic.mercury_properties()
mercury_density = mic.mercury_properties( 'density')
In the above first usage case, the list of all available mercury
property keywords is returned.

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Get Properties of Sample Material
GET PROPERTIES OF SAMPLE MATERIAL

mic.material_properties( property='' , sample_number = 0 ) :
Keyword arguments:
property --- the property value to return.

If '' or None, then return all the properties
strings available for the sample material.
Default value is None
sample_number --- Identifier for the sample material to retrieve

0 : current sample file (default)
1 through 8 : corresponding overlay sample file
Usage:
property_list = mic.material_properties()
material_name = mic.material_properties( 'material name')
In the above first usage case, the list of all available material
property keywords is returned.

I - 17
962-42800-01 (Rev D) — Nov 2017
Index
INDEX chamber
replace plug seals 11 - 21
clean
exterior 11 - 31
A components
analyzer 1 - 1
about this manual iii contact us ii
advanced presentation option control chart report 6 - 4
sample files 3 - 1
advanced report options 7 - 1, I - 2
analysis D
low pressure 5 - 11
low pressure reference 5 - 22 dashboard
perform 5 - 1 show 2 - 19
analysis conditions data
create parameter file 4 - 2 manually enter 3 - 8
worksheet F - 2 diagnostics
analyzer available options 8 - 1
components 11 - 4 save files for problem diagnosis 8 - 4
high pressure 11 - 7 schedule 8 - 2, 8 - 2
low pressure 11 - 4 start test 8 - 1
configure 2 - 13 test report 8 - 3
show status 2 - 19
software 2 - 1
atmospheric pressure 2 - 13 E
axis cross-hair 6 - 19
export files 2 - 22
exported data example G - 1
B
banana plug, replace 11 - 32 F
baseline error correction methods 3 - 5
blank and sample compression corrections A fields and buttons, common 2 - 3
-1 files
blank correction default locations 2 - 6
file creation 3 - 6, 3 - 7 description 2 - 6
export 2 - 22
extensions defined 2 - 6
C list 2 - 22
open a sample file 3 - 4
calibrate status 2 - 6
low pressure servo 9 - 1 formula correction 3 - 7
signals 9 - 2 fractal dimensions 7 - 6
calibration 9 - 1 fuses 11 - 9
load from file 9 - 5
save to file 9 - 5
cavity to throat size ratio 7 - 5

Index - 1
962-42800-01 (Rev D) — Nov 2017
Index
low pressure
G calibrate servo 9 - 1
drain system 11 - 10
graph evacuate 5 - 13
features and shortcuts 6 - 15 generate 5 - 14
generate overlays 6 - 21 grease ports 11 - 20
grid lines 6 - 20 monitor analysis 5 - 15
overlay multiple 6 - 24 perform analysis 5 - 11
report options 7 - 2 reference analysis 5 - 22
H M
hardware maintenance
install components 10-1 and troubleshooting 11 - 1
high pressure banana plug, replace 11 - 32
chamber exterior, clean 11 - 31
remove penetrometer 10-5 grease low pressure ports 11 - 20
seal 11 - 19 vacuum pump
change fluid 11 - 23 exhaust filter 11 - 25
clean chamber 11 - 23 mercury vapor filter 11 - 26
differential analysis 5 - 20 vent valve, replace O-ring 11 - 22
fluid, maintain level 11 - 18 manual control
generate 5 - 18 enable 11 - 12
monitor analysis 5 - 19 manual, about this iii
perform analyses 5 - 16 material
hydraulic pump fluid 11 - 23 compressibility 7 - 7
properties 4 - 8
maximum intrusion volume E - 1
I Mayer-Stowe report 7 - 8
measured temperature warning 2 - 14
install menu structure 2 - 2
hardware components 10-1 mercury C - 1
instrument drain dish 11 - 11
software 2 - 1 handling overfill 11 - 21
status 2 - 16 level 11 - 17
interactive reports 6 - 9 methods, about 2 - 12
MicroActive reports 6 - 10
moisture, remove 11 - 31
L
leapfrogging 5 - 23 O
libraries 2 - 11
list files 2 - 22 option presentation 2 - 9
log advanced 3 - 1
show 2 - 21 sample files 3 - 1
overlays
generate 6 - 21

Index - 2
962-42800-01 (Rev D) — Nov 2017
Index
multiple graph 6 - 21 tables

multiple sample 6 - 25 add I - 11
add column I - 11, I - 11
tabular report I - 6
P
parameter files R
analysis conditions 4 - 2
mercury porosimetry 4 - 1 reference analysis
penetrometer 4 - 10 low pressure 5 - 22
report options 4 - 11 reference material analysis 5 - 21, 5 - 22
penetrometer high pressure 5 - 21
calibrate 9 - 4 regression report 6 - 2
calibration 3 - 7 report examples
clean 5 - 5 controlled pore glass plot 6 - 29
install in high pressure chamber 10-1 garnet tabular report 6 - 28
install in low pressure port 10-3 Reverberi plot 6 - 26
nut 11 - 34 silica alumina reference material plot 6 -
properties 4 - 10 27
properties worksheet F - 3 report options
remove from high pressure chamber 10-5 graphs 7 - 2
remove from low pressure port 10-6 worksheet F - 5
seal 5 - 7 reports
select 5 - 1 about 6 - 1
weigh with sample 5 - 9 advanced report options 7 - 1, I - 2
pore distribution data, import 6 - 23, 6 - 23 advanced, Python module I - 1
pore structure report 7 - 10 axis cross-hair 6 - 19
power analyzer on and off 11 - 36 cavity to throat size ratio 7 - 5
power failure, recover from 11 - 36 control chart 6 - 4
pressure table and tabular data worksheet F - examples 6 - 26
4 features and shortcuts 6 - 11
pump-down rates B - 1 graphs 6 - 15
Python module I - 1 reports 6 - 11
Acquire Basic Information, Mercury I - 8 tabular report 6 - 14
Advanced Reports I - 1 fractal dimension 7 - 6
Create a New Tabular Report I - 11 generate graph overlays 6 - 21
Get Instrusion-Extrusion Data I - 15 graph grid lines 6 - 20
Get Mercury Properties I - 16 header shortcuts 6 - 12
Get Properties of Sample Material I - 17 interactive 6 - 9
Graphic Report I - 7, I - 13 material compressibility 7 - 7
add a curve I - 13, I - 14 Mayer-Stowe 7 - 8
create new I - 14 MicroActive 6 - 10
Mic Module Python Calls I - 11 options report 7 - 9
scripts I - 3 pore structure 7 - 10
Summary Report I - 5, I - 12 PSD history 6 - 7
add a summary section I - 12 regression 6 - 2
create a new I - 12 report options 4 - 11

Index - 3
962-42800-01 (Rev D) — Nov 2017
Index
Reverberi 7 - 11
sample log 7 - 12
T
selected 7 - 1
SPC report options 6 - 1 tabular reports 7 - 16
summary report options 7 - 12 features and shortcuts 6 - 14
tabular 7 - 16 theory D - 1
tabular, Python I - 11 toolbar, report 6 - 13
toolbar 6 - 13 troubleshooting
user-defined 7 - 1, I - 2 and maintenance 11 - 1
zoom feature 6 - 20 manual control, enable 11 - 12
Reverberi 7 - 11 power failure, recover from 11 - 36
preventive maintenance 11 - 16
S
U
safety features 1 - 3
sample 5 - 5 unit configuration, specify gas ports 2 - 15
averaging 3 - 5 unit selections 2 - 14
load and seal 5 - 6 user-defined report options 7 - 1, I - 2
log
report 7 - 12
seal the penetrometer 5 - 7
V
weigh sample 5 - 9
sample data worksheet F - 6 vacuum pump 11 - 25
sample file change oil 11 - 27
defined 3 - 1 exhaust filter 11 - 25
mercury porosimetry 3 - 1 mercury vapor filter 11 - 26
open 3 - 4 valves
schematic check for leak 11 - 29
display 2 - 16 clean 11 - 29
shortcuts 2 - 18 replace vent valve o-ring 11 - 22
shortcuts volumetric capsule worksheet F - 7
application 2 - 8 volumetric compressibility, compute H - 1
report header 6 - 12
schematic 2 - 18
software
W
about 2 - 1
setup 2 - 1 warranty i
uninstall 2 - 2 workflow, basic 1 - 4
updates 2 - 2 worksheets F - 1
SPC report 6 - 1 analysis conditions F - 2
specifications 1 - 5 high pressure volumetric capsule F - 7
status penetrometer properties F - 3
analyzer 2 - 19 pressure table and tabular data F - 4
instrument 2 - 16 report options F - 5
summary report 7 - 12 sample data F - 6
system valves 11 - 12

Index - 4
962-42800-01 (Rev D) — Nov 2017
Index
Z
zoom feature, reports 6 - 20

Index - 5
962-42800-01 (Rev D) — Nov 2017

9600 Operator Manual Rev.D

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Copyright © 2014 - 2017. Micromeritics Instrument Corporation. All rights reserved.

AutoPore V Series Operator Manual

Quotes, Orders, and Customer Satisfaction

U.S. Instrument Service Department

Micromeritics Scientific Services

AutoPore V Series Operator Manual

ABOUT THIS MANUAL

The following icons may be found in this manual:

NOTE - Notes contain important information applicable to the topic.

AutoPore V Series Operator Manual

About this Manual iii

1 Analyzer Components 1-1

2 About the Software 2-1

AutoPore V Series Operator Manual

3 About Sample Files 3-1

4 About Parameter Files 4-1

5 Perform an Analysis 5-1

AutoPore V Series Operator Manual

6 About Reports 6-1

7 Selected Reports 7-1

AutoPore V Series Operator Manual

10 Hardware Components and Accessory Installation 10-1

11 Maintenance and Troubleshooting 11 - 1

AutoPore V Series Operator Manual

A Blank and Sample Compression Corrections A-1

AutoPore V Series Operator Manual

C Proper Handling of Mercury C-1

E Use of the Maximum Intrusion Volume Option E-1

G Exported Data Example G-1

H Compute Volumetric Compressibility of a Sample Material H-1

I Advanced Reports - Python Module I-1

AutoPore V Series Operator Manual

AutoPore V Series Operator Manual

Front Panel Components

Hg Up. Illuminates when the amount of mercury in the low pressure

AutoPore V Series Operator Manual

Rear Panel Components

25 Amp. Resets the internal vacuum pump in a high pressure

AutoPore V Series Operator Manual

OPERATIONAL SAFETY FEATURES

l Mercury Drip Trays

AutoPore V Series Operator Manual

THE BASIC WORKFLOW

1. Weighed and the mass recorded, and

Theory on page D - 1 provides a thorough discussion of the theory of porosimetry.

AutoPore V Series Operator Manual

SPECIFICATIONS FOR AUTOPORE V

AutoPore V Series Operator Manual

l Operating System. Windows 7 Professional or higher operating system is recommended for

AutoPore V Series Operator Manual

2 ABOUT THE SOFTWARE

Data can be manipulated and displayed interactively using MicroActive reports.

If the computer is to be connected to a network, a second Ethernet port on the computer

AutoPore V Series Operator Manual

l a later version than the current installation

UNINSTALL THE SOFTWARE

Main Menu Bar Options

AutoPore V Series Operator Manual

COMMON FIELDS AND BUTTONS