XRF Manual
XRF Manual
XRF Manual
Technical Manual
AA83826 - 00 May 2017 – Preliminary Version
Revision Control
Date Revision Description
2017 May 00 Creation of the manual for instruments with serial number of
>2017
The information in this document is subject to change without notice. We assume no responsibility for any errors
i
ADC Parameters ............................................................................................. 4-24
Chamber Parameters...................................................................................... 4-25
Auto Current Control Parameters ................................................................... 4-26
Logging ........................................................................................................... 4-27
Communication ............................................................................................... 4-28
System Test Settings ...................................................................................... 4-29
Chapter 5 Test and Adjustment Procedures ....................................................... 5-1
Energy Adjustment ....................................................................................................... 5-4
Test Conditions ................................................................................................. 5-4
Test Equipment................................................................................................. 5-4
Procedure ......................................................................................................... 5-4
Power Supply Test and Adjustment ............................................................................. 5-8
System Power Supply (+5, +12, +/-12, +24 V).................................................. 5-8
Interlock Test .................................................................................................... 5-9
Test Equipment................................................................................................. 5-9
Procedure ......................................................................................................... 5-9
MNX high voltage Power Supply Setup ..................................................................... 5-11
Test Equipment............................................................................................... 5-11
Test Conditions ............................................................................................... 5-11
Procedure ....................................................................................................... 5-11
Radiation Survey ........................................................................................................ 5-13
Test Equipment............................................................................................... 5-13
Test Conditions ............................................................................................... 5-13
Safety Precautions .......................................................................................... 5-13
Procedure ....................................................................................................... 5-13
DPP Calibration (DPP Cal) ........................................................................................ 5-16
Test Equipment............................................................................................... 5-16
Test Conditions ............................................................................................... 5-16
Procedure ....................................................................................................... 5-16
Resolution .................................................................................................................. 5-21
Test Equipment............................................................................................... 5-21
Test Conditions ............................................................................................... 5-21
Procedure ....................................................................................................... 5-21
X-ray Tube Conditioning ............................................................................................ 5-23
Test Equipment............................................................................................... 5-23
Test Conditions ............................................................................................... 5-23
Procedure ....................................................................................................... 5-23
Stability ...................................................................................................................... 5-24
Test Equipment............................................................................................... 5-24
Test Conditions ............................................................................................... 5-24
Procedure ....................................................................................................... 5-24
Glossary of Terms........................................................................................... 5-26
Interpreting Test Results ................................................................................. 5-27
ii
Software Hints to Aid Interpretation ................................................................ 5-28
Repeatability .............................................................................................................. 5-30
Test Equipment............................................................................................... 5-30
Test Conditions ............................................................................................... 5-30
Procedure ....................................................................................................... 5-30
Tray Height Adjustment.............................................................................................. 5-32
Test Equipment............................................................................................... 5-32
Test Conditions ............................................................................................... 5-32
Procedure ....................................................................................................... 5-32
Tray Accuracy ............................................................................................................ 5-34
Test Equipment............................................................................................... 5-34
Test Conditions ............................................................................................... 5-34
Procedure ....................................................................................................... 5-34
Live Time Correction .................................................................................................. 5-36
Test Equipment............................................................................................... 5-36
Test Conditions ............................................................................................... 5-36
Procedure ....................................................................................................... 5-36
Test Sample Assembly ................................................................................... 5-37
Stray Lines ................................................................................................................. 5-38
Test Equipment............................................................................................... 5-38
Test Conditions ............................................................................................... 5-38
Procedure ....................................................................................................... 5-38
Minimum Detection Limits .......................................................................................... 5-40
Test Equipment............................................................................................... 5-40
Test Conditions ............................................................................................... 5-40
Procedure ....................................................................................................... 5-40
Chamber Vacuum ...................................................................................................... 5-42
Test Equipment............................................................................................... 5-42
Test Conditions ............................................................................................... 5-42
Procedure ....................................................................................................... 5-42
System Status Voltages ............................................................................................. 5-44
Test Equipment............................................................................................... 5-44
Test Conditions ............................................................................................... 5-44
Procedure ....................................................................................................... 5-44
Helium Flush .............................................................................................................. 5-46
Test Equipment............................................................................................... 5-46
Test Conditions ............................................................................................... 5-46
Procedure ....................................................................................................... 5-46
Alternate Procedure ........................................................................................ 5-47
Beryllium Window Cleaning Procedure ...................................................................... 5-48
Test Conditions ............................................................................................... 5-48
Test Equipment............................................................................................... 5-48
Safety Precautions .......................................................................................... 5-48
iii
Procedure ....................................................................................................... 5-49
QUANT’X Diagnostics ................................................................................................ 5-52
System Noise Spectrum Measurement ...................................................................... 5-54
Test Equipment............................................................................................... 5-54
Test Conditions ............................................................................................... 5-54
Procedure ....................................................................................................... 5-54
Evaluating the Noise Spectrum....................................................................... 5-55
Chapter 6 Periodic Maintenance ......................................................................... 6-1
Procedure .................................................................................................................... 6-4
Procedure .................................................................................................................... 6-7
Procedure .................................................................................................................... 6-9
WinTrace Service Mode ............................................................................................. 6-13
Diagnostic Page ......................................................................................................... 6-14
General Usage Notes ..................................................................................... 6-14
Chapter 7 Component Replacement ................................................................... 7-1
Circuit Boards............................................................................................................... 7-3
Chamber/Spectrometer Control Board ............................................................. 7-3
EDS Board ........................................................................................................ 7-3
DPP, DIMM Memory, and Disk Drive Flash Memory ........................................ 7-4
Power Supplies ............................................................................................................ 7-5
X-ray High Voltage Power Supply..................................................................... 7-5
PS1 +5 V, +12 V, +15 V & -15 V Switching Power Supply ............................... 7-6
PS2 +24V Switching Power Supply .................................................................. 7-7
Sample Chamber Components .................................................................................... 7-8
Filter Wheel Assembly ...................................................................................... 7-8
Sample Tray Drive Assembly............................................................................ 7-8
Sample Spinner Drive Assembly ...................................................................... 7-9
Miscellaneous Items................................................................................................... 7-10
X-ray Tube ...................................................................................................... 7-10
X-ray Tube Cooling Fan .................................................................................. 7-10
Plenum Cooling Fan ....................................................................................... 7-11
Sample Chamber Lid Latch Assembly ............................................................ 7-11
Chapter 8 Optional Equipment ............................................................................ 8-1
Helium Flush ................................................................................................................ 8-3
Specifications.................................................................................................... 8-3
Installation......................................................................................................... 8-4
iv
1
Chapter 1 General Information
General Information
This manual describes the Thermo Scientific™ ARL QUANT’X XRF spectrometer.
The manual is designed to acquaint the technician with the spectrometer, its hardware
and software characteristics, its installation, and the service procedures that can be
performed on site.
This manual is written for technicians who have general experience with electronic
circuits and standard bench spectrometers. No expertise with X-ray or elemental analy-
sis techniques is assumed (the references listed in this section should enable the inter-
ested reader to get acquainted with these topics).
This manual does assume that anyone working with the ARL QUANT’X has become
somewhat familiar with its operation as described in the WinTrace Software user guide.
The following conventions are used in this manual:
• ARL QUANT’X refers to the hardware or complete system.
• WinTrace refers to the Windows software used to run the system.
• SDD means Silicon Drift Detector, and sometimes refers to ARL QUANT’X systems
equipped with the SDD.
Support Solutions
All of our products are carefully engineered to meet your high standards and are cov-
ered by a standard warranty. We want to maintain this high performance level for the life
of your product. We offer versatile Support Solutions designed to maximize the return
on your technology investment, and guarantee that you will always have genuine
Thermo Scientific parts and knowledge to keep your spectrometer optimized, today and
tomorrow. Your ARL QUANT’X warranty may be expanded at any time during the war-
ranty period to include the features listed in our Support Solutions.
Education Services
The following explains the education services available through us.
Product Training
We offer the possibility of a two days on-site product and applications training after the
installation has been completed.
How to Enroll
Class sizes are restricted for maximum efficiency so please enroll at least thirty days
prior to the start date of the course you are attending. When a visa is required to travel
to the training site (USA or Switzerland) pleas enroll at least 90 days prior to the start
date of the course. If you have questions or would like to enroll, please contact us.
Lab Supplies
Preparation and presentation of samples for X-ray analysis is categorized according to
physical form and basic chemical makeup of the sample. There are several methods in
use for sample preparation. The following is a discussion of equipment that may be
necessary and a brief description of its use in XRF analysis.
Sample Cups
Sample cups are available from Thermo Fisher. They have many uses, including analy-
sis of liquids, powders, and small samples that are mounted on the window of the cup.
In almost all cases, use of the sample cup necessitates the use of a window between
the sample cup and the spectrometer. The window can be made of Mylar, polypropyl-
ene, polycarbonate, or Kapton™. These window materials will have different properties
of attenuation, chemical resistance, and various trace impurities.
Presses
Pressing pellets of solid materials (usually powders) is one of the most popular methods
of sample preparation in use for XRF analysis. Usually the sample is placed into a com-
pressible aluminum cup, the cup and sample are placed into a steel die and then
pressed between two tungsten carbide or steel pellets at up to 25 of tons pressure.
When the sample is removed from the die, it is in the form of a briquette that can be
placed directly into the XRF system for analysis without the use of supporting
film/window material.
Fluxers
Fusion is a technique that is used for analysis of powdered solids like cement, ores, and
other geological materials. The advantage of this technique is that the final sample is
usually very close to being an ideal sample: fused disks are usually very homogeneous
and, if not flat or smooth, they can be polished.
Grinders
Any solid samples that are obtained or are to be analyzed as powders may need grind-
ing. In general, the goal is to make the particle size small enough that variations in the
particle size will not cause changes in the measured X-ray intensity.
Polishers
Samples that usually require polishing include alloys and glasses. As with grinding, the
goal of polishing is to remove scratches on the surface of the sample that will change
the measured intensities from that of a perfectly smooth sample.
Standards
Regardless of the application, accurate quantitative analysis requires the use of stand-
ard reference materials similar to the matrix of the sample being analyzed. The use of
fundamental parameters software reduces the need for standards compared to use of
empirical techniques. In preparation for use of an XRF system, appropriate standards
must be obtained.
Product Description
ARL QUANT’X is a compact high-performance Energy Dispersive X-ray Fluorescence
(EDXRF) spectrometer. The spectrometer uses an X-ray tube excitation source and a
solid state detector to provide simultaneous spectroscopic analysis of elements ranging
from fluorine to uranium in atomic number and in concentrations ranging from a few
parts per million to 100 percent. Spectrometer control and data analysis are performed
by a computer that is connected to the system.
For the purpose of introducing the reader to the ARL QUANT’X, this section begins with
a tour of the spectrometer. The name, function, and location of major components are
described. This information provides a basis for understanding the other sections of this
manual. The section concludes with detailed specifications of the unit.
Fig. 2 - 1
The figure above shows the ARL QUANT’X spectrometer. Spectral data transfer and
spectrometer control are established through a dedicated Ethernet cable. The computer
sends commands (X-rays on, vacuum pump on, etc.) to, and receives status from the
embedded microprocessor located in the ARL QUANT’X.
Fig. 2 - 2
The left and right side panels of the spectrometer can be removed by unscrewing
the corresponding two screws situated on the back of the instrument, to provide access
to the detector and detector electronics.
The front panel can be removed once the side panels are removed, by unscrewing
the two screws on each side of the panel to provide access to the internal components
from the front.
When removed, front and side panels give access to a safe zone free of radiation.
The radiation beam is enclosed in the spectrometer chamber and sample chamber lid
keeping the outside area free of radiation (<1µSv/h / <0.1mR/h).
Fig. 2 - 3
The left lid on the top of the spectrometer can be removed to provide access to the
detector and detector electronics.
The spectrometer chamber and the sample chamber lid are made of a
Zinc/Aluminum alloy for radiation safety and are vacuum tight for analysis of low atomic
number elements.
The chamber lid interlocking combines the detection of the sample chamber lid
state (open/closed) and of a solenoid to lock/unlock the chamber lid. The 24V powers
the high voltage power supply for X-ray tube operation can only be delivered when the
operation chamber lid is closed and locked. This is controlled directly by safety relays
and interlocks.
The lid latch assembly contains a solenoid and two switches. The solenoid is ener-
gized to lock the closed chamber lid whenever the X-rays are on. One switch detects if
the solenoid plunger has traveled far enough to lock the lid, the other switch senses if
the chamber lid is closed. Both switches must be activated before X-rays can be gener-
ated.
The "X-rays ON" warning light (X-ray warning light) is located below the sample
chamber lid. This light indicates the status of the X-ray generator. It is activated only
when the X-ray generator is ON. Above the warning light are the Power ON light and
Detector light. The Power On light is on whenever the AC power switch located on the
back of the unit is turned on. The Detector light is normally off, but will flash if the de-
tector is not correctly powered. All the lights are mounted on a computer board called
the display board.
The X-ray high voltage power supply produces the high voltage required for
X-ray tube operation. It operates on +24 VDC and generates up to 50 kV and up to
2 mA with a 50 W power limitation. The power supply is mounted on the right side of the
spectrometer.
The System power supply powers all the DC power supplies used to power the
spectrometer.
The X-ray tube provides the primary X-ray beam used to illuminate the sample. The
X-ray tube is air cooled and may operate at up to 50 W. The target material of the X-ray
tube determines certain characteristics of the tube’s spectral output and is therefore
selected based on the intended application of the spectrometer. For most applications a
rhodium (Rh) target X-ray tube is used. For some specific applications, a silver (Ag)
target X-ray tube is available. The shroud is part of the tube cooling system discussed
below.
The X-ray tube fan is dedicated to tube cooling. The fan and shroud form a cooling
system powered dynamically as a function of the X-ray power necessary for the applica-
tion. The shroud is mechanically coupled to the tube with a heat conductive interface.
The warmed exhaust air is vented internally. The fan is mounted on rubber isolators to
prevent vibration.
Fig. 2 - 4
The ARL QUANT’X DPP Assembly is a self-contained computer for control and
signal processing of the X-ray beam, safety interlocks, sample tray, filter wheel, vacuum
pump, and detectors. Ethernet communication from the computer is evaluated and
distributed to the appropriate components contained in the assembly. The DPP status
display (top view) consists of an internal LED array showing the functional state of the
spectrometer. It is also the connection point for the detector preamplifier signals, control
signals and power supplies.
The detector preamp cable connects the detector assembly to the EDS board.
This cable carries the detector high voltage bias, the detector output signal, and several
DC voltages.
The chamber distribution board (not shown) is a connection point for the motors
and sensors located inside the sample chamber. Two cables connect this board to the
chamber/spectrometer control board via vacuum-tight feed-through fittings in the
chamber wall.
The sample tray drive assembly (optional) drives the sample tray rotation. It
consists of a step motor, drive belt, and optical position sensor. The motor is controlled
by the Chamber/Spectrometer control board located inside the DPP assembly. The
assembly may be easily removed or installed as a single unit.
Fig. 2 - 5
The filter wheel assembly is a nine position turret driven by a step motor. An opti-
cal sensor is used to detect the home position. Each position on the wheel may hold
one transmission filter. The filters are used to modify the characteristics of the primary
X-ray beam emitted from the X-ray tube and are selected based on the elements being
analyzed. The motor is controlled by the chamber control board located in the DPP
assembly. This assembly may be easily removed or installed as a single unit. The mate-
rial of the filters depends on the target material of the X-ray tube selected for specific
applications.
The X-ray tube collimator serves to limit the X-ray beam size. The X-ray tube
beryllium window is located just behind the collimator opening.
CAUTION: The beryllium window is extremely fragile and can be broken by the
lightest touch. Never put anything down the collimator shaft or touch this window in
any way. If the window becomes contaminated, contact us for instructions.
The filter wheel collimator serves to further limit the X-ray beam size. After the
X-ray beam passes through the selected filter, a counterbore above (closer to the sam-
ple) holds the filter wheel collimator. ARL QUANT’X systems using the Varian™ X-ray
tube require an 8.8 mm collimator for operation.
The sample spinner drive assembly (optional, not shown), used together with
the rotating single sample tray or with the 10-position sample tray, rotates the sample
during spectral analysis. Rotation is used on inhomogeneous, rough or odd-shaped
samples because the analysis results change depending on how the sample is placed
in the tray. By rotating during analysis, the variances are averaged out. The drive as-
sembly uses a step motor which is controlled by the chamber control board located in
the DPP assembly. The assembly may be easily removed or installed as a single unit.
The detector collimator limits the detector’s field of view, reducing the incidence of
unwanted X-rays. The detector beryllium window is located just behind the collimator
opening.
CAUTION: The beryllium window is extremely fragile and can be broken by the
lightest touch. Never put anything down the collimator shaft or touch this window in
any way. If the window becomes contaminated, contact us for instructions.
Fig. 2 - 6
The X-ray source key switch breaks the safety interlock circuit thereby preventing
X-ray generation. This is useful for disabling the spectrometer to prevent unauthorized
operation.
The power on/off switch controls all power to the spectrometer.
The spectrometer power input and fuse is the connection point for the primary
power cord. The connection is made via a standard IEC 320 inlet. It is rated for line
voltages of 115 or 230 VAC if the system line voltage selection switches are set ac-
cordingly. It supports European IEC type (single or dual 5 x 20 mm fuses) shocksafe
fusing requirements.
The vacuum pump power input and fuse is the connection point for the second
spectrometer power cord. The vacuum pump power circuit is separate from the spec-
trometer power to reduce the required capacity of an uninterruptible power supply or
power conditioner, if one is used. The connection is made via a standard IEC 320 inlet.
The inlet module has TÜV, NRTL, GS, and CSA safety agency approvals and is rated
for line voltages of 115 or 230 VAC. The shocksafe fuse drawer accepts IEC type fuses.
The AC distribution box assembly (not shown) houses most of the AC wiring in
the spectrometer. It is a closed, grounded metal box. It is the connection point for all
external and internal AC line voltage cables. It also houses a line filter and a solid-state
relay for vacuum pump control.
The Ethernet port is a RJ-45 connector used to connect the spectrometer to the
computer's dedicated Ethernet port.
The vacuum port is the connection port for the vacuum pump hose. It is a 5/8 inch
hose fitting. Vacuum is used to analyze low atomic number elements because their low
energy X-rays would be absorbed by the air in the chamber. Liquid samples may not be
placed under vacuum.
The helium port (optional) is the connection point for the helium gas used to flush
the sample chamber when analyzing low atomic number liquid samples. The input
pressure must be in the range of 15 to 65 psi (1.0 to 4.45 bar). The fitting is a ¼ inch
hose barb.
The vacuum pump power outlet is a standard NEMA 5-15R receptacle. The
vacuum pump power cord is plugged into this outlet. The vacuum pump must be rated
for the AC line voltage connected to the vacuum pump power inlet. The spectrometer
does not convert this voltage. This outlet is a switched outlet under the control of the
analysis software. It is fused as previously described.
The AC line voltage selection switches configure the spectrometer for operation
on 115 or 230 VAC. A panel covers the selection switches and is labeled 115 V and
230 V on opposite sides. Both switches must be set to the appropriate setting before the
power cord is plugged in. Replace the panel cover with the appropriate line voltage
setting visible.
NOTICE: Failure to select the correct AC line voltage switch setting may cause
spectrometer damage.
Specifications
The following table provides the specifications for the ARL QUANT’X system.
Performance
Exitation
X-ray Optics 80º geometry between X-ray tube, sample and detector.
Distance from sample to:
SDD detector: 25.0 mm
X-ray tube target: 54.1 mm
Filter Collimators Small spot analysis with 1 mm, 2.0 mm, 3.5 mm,
8.8 mm
Detector
Type Peltier cooled Silicon Drift Detector (no liquid nitrogen re-
quired), 30 mm² active area, 20 mm² collimated area
Site/Utility Require-
ments
Frequency 50 Hz or 60 Hz
Neutral 0V to ground
Ground <2Ω
Dimensions, Weight
and Noise
Communication Instru-
ment - PC
Software
Important This test procedure must be followed if safety components are re-
placed.
Safety Features
The safety features implemented by the interlock circuit provide protection against the
X-rays being turned on when a potentially unsafe condition exists outside the protected
area.
X-rays are enclosed in the protective chamber with all access controlled to maintain a
level of radiation below 1µSv/hour outside the chamber.
Fig. 3 - 1
Fig. 3 - 2
Interlock Circuit
A specific interlock X-ray Safety system (S502577) is designed to strictly keep the pro-
tective chamber closed during operation.
Interlocks and interlocking devices are connected to the Safety controller to power the
X-ray generator through both safety relays (see Interlock Safety system S502577)
In particular, the interlocks provide the following features:
• All interlocks must be closed for the controller to activate the safety relays and turn
on the X-ray generator. If any of the interlocks is opened, the relays and the X-rays
are turned off immediately by the controller.
• Thus if the circuit is broken at any one of the interlocks, there is no power to the
X-ray tube regardless of the status of the logic circuits monitoring the interlock con-
dition.
• If the interlock circuit is broken, the X-rays do not turn on again until the interlocks
are closed and the operator reinitializes the analysis sequence by switching on the
power on/off switch again.
• The sample chamber lid interlocking device switch uses a Positive-Break design;
the contacts are forced open by a mechanical drive mechanism rather than by a
spring as in a normal switch. It also features a bypass-resistant actuator which re-
quires a unique geometry actuator key to close the contacts.
• The sample chamber lid interlocking device has locking mechanism that locks the
unique geometry actuator key keeping the door closed when X-rays are generated.
• The interlocking device switches and signals behavior is verified by the controller.
• Each of the safety interlock for the X-ray tube and detector presence are magnetic
switches without mechanical interaction. They have double contact open and
closed in order for the controller to verify their normal behavior.
• The circuit is designed with the controller so that failure of any of the electrical
components can only cause the X-rays to turn off, not to turn on.
Command Circuit
The current that powers the high voltage power supply flows through the interlock circuit
relays activated by the safety controller
• The command of switching on the X-ray generator is coming from the Chamber/
Control (CCB) Board when an analysis is requested with Wintrace software.
• Also, the Chamber/ Control (CCB) Board KV PROGRAM line is held at 0 volts
when the control closed lid is open.
• The sample chamber lid has two interlock switches (Lid senses) with separate
circuits and mechanical actuators.
Fig. 3 - 3
• The X-rays ON warning light must be on for the X-rays to turn on.
• The X-ray source key switch must be on for the X-rays to turn on.
• The power on/off switch must be on for the X-rays to turn on.
CCB Interlocks
The overall X-ray system interlock circuit is described in Safety Interlock Circuit. This
discussion focuses on the CCB board circuits only.
The CCB has its own interlock circuit to allow the system to close the interlocking sys-
tem by the software.
There are two microswitches on the sample chamber lid latch assembly. Both switches
are actuated when the lid is closed (the analysis door is closed).
When the Lid is closed, LED 6 is switched on.
On the rear panel of the instrument, a turn key switch is assembled.
This switch allows the user to open or close the interlock of the CCB.
When the interlock is closed (allow the system to command the HVPS), the LED 7 is
switched on.
Fig. 3 - 4
A series of LEDs is included at each step of this sequence for troubleshooting purposes.
The LED names, which are self explanatory, are: LD6 LID CLOSED, LD7 INTERLOCK
IN, LD9 LIGHT ON, and LD8 INTERLOCK OUT. Also, a logic level signal is available to
the DPP at each step of the process so that automatic troubleshooting assistance can
be provided in the form of operator error messages.
The green Power ON light, D2, is on anytime the spectrometer power switch is on.
Power Supplies
The board runs on a single +24 VDC power source supplied via J3 pin 6. Three voltage
regulators, U6-8, are used to generate local supply voltages. U8 is adjusted to +12 V
output by R41. This supply is used to operate the integrated circuits on the board.
Connector J2 is not used in the ARL QUANT’X.
Test Points
Most of the important voltages are present on TP1 for measurement with a voltmeter.
These voltages are also connected to the CCB board via J1 for measurement and dis-
play on the computer monitor. To view these voltages, open the Spectrometer
Manager - System Status tab.
Fig. 3 - 5
Interlock Test
The purpose of this test is to check the operation of the interlock circuit, including opera-
tion of the lid senses and of the interlock device.
Test Equipment
None.
Procedure
To test the interlock:
1. Remove the side panels of the mainframe and the plastic DPP top cover.
2. Turn on the system power.
Fig. 3 - 6
Note LED 'LID CLOSED' should turn on just before LED 'INTERLOCK IN' turns
on.
Radiation Survey
Use this survey to measure the radiation leakage outside the spectrometer at full power
in worst case conditions. This is a safety-related procedure.
This procedure is written for a particular model of survey meter. If your meter is a dif-
ferent model, disregard the particular references and follow your meter manufacturer’s
operating instructions.
Test Equipment
• Dosimeter ring or badge
• Survey meter, monitor 4EC, A039999
• Delrin™ scatter block sample
• 1 inch x1 inch lead sheet
• Radiation Survey Recording Form No. 226
Test Conditions
An X-ray beam collimator must not be installed in the filter wheel holder.
Safety Precautions
This survey may constitute a radiation hazard. Test personnel must wear a dosimeter
during the test.
Procedure
To survey radiation in your ARL QUANT’X system:
1. Fill out the survey form.
2. Verify that the survey meter has been calibrated within the last year.
3. Use the test source supplied with the meter to verify that it is working correctly.
4. Remove the sample tray from the chamber, there will be no sample for the first part
of this test.
5. Ensure that all the QUANT’X enclosure covers are in place.
6. Start Acquisition Manager and choose File > New > Qualitative Tray List.
7. Type anything for a sample name and press the down arrow key.
8. Click inside the Condition cell, choose Edit > Condition Properties.
9. Set up the following conditions.
Condition Setting
Tube Voltage 50 kV
Filter No Filter
Atmosphere Air
Warm up 0 seconds
17. Very, very slowly move the probe around the spectrometer at a distance of 10 cm
from the surface.
The probe must be held parallel to the direction from where X-rays would be leaving
the system.
18. Check all surfaces of the spectrometer.
Pay special attention to the following areas:
• Gap between the chamber lid and baseplate, front and right side
• All frontal surfaces on the chamber end of the spectrometer
• Top of the chamber lid
• Gap around chamber lid while pulling up on the chamber lid
19. If a meter deflection above 1 µSv/h is observed, hold the probe in that location to
verify the measurement.
20. Vary the probe angle slowly to find the maximum reading.
Only stable readings are valid, it is normal for the meter to jump to about 0.01
µSv/h occasionally due to background radiation.
Note Survey meter, Monitor 4EC, A039999 does not request scale correction with
x1 reading.
Note The detection point is 2.5 cm back from the front end (see radiation symbol at
back).
Installation
Installation of the ARL QUANT’X spectrometer is a relatively simple process that con-
sists of hardware setup and performance tests. For maximum efficiency, the steps
should be performed in the order presented. For example, the steps required to cool
and stabilize the X-ray detector are presented early, while the computer may be un-
packed later.
This chapter starts with site preparation requirements and precautions which will help
ensure reliable and stable operation of the ARL QUANT’X spectrometer.
Installation
This section describes the installation of the ARL QUANT’X spectrometer and computer
system, provided that both are supplied by us.
Conditions
The installation site must meet the requirements detailed in the site and safety manual.
Required Equipment
Basic hand tools.
Procedure
To verify or change the AC Mains and Pump fuses regarding voltage
setting:
1. Check the fuses of the MAINS entry and the Vacuum Pump output. If needed, in-
stall correct fuses for the spectrometer and vacuum pump. Refer to the sticker on
the back panel of the instrument in order to find the correct fuse.
2. Turn the spectrometer fuse holder according to the input voltage, either on
110-120V or 220-240V. The corresponding small white triangle must point to the
small white bar.
NOTICE: Make sure the spectrometer power switch is turned off before you con-
nect the power cord.
3. Plug a standard power cord (included) into the power receptacle on the back panel
of the spectrometer and connect it to the distribution unit that is delivered with the
instrument. Make sure that a local plug has been connected to the power supply
cord, then plug it into the power receptacle of the distribution unit and connect it to a
wall socket.
Fig. 4 - 1
4. Set up the computer:
a. Unpack the computer, monitor (for desktop computer) and place them near the
ARL QUANT’X.
b. Verify that the AC line voltage selection on the rear of the computer corre-
sponds to the local line voltage.
c. Plug the computer into the same electrical outlet as the ARL QUANT’X.
d. Connect any remaining computer accessories, such as monitor, mouse or
keyboard.
e. Connect the Ethernet communication cable (provided) between the spectrom-
eter and the computer.
5. The desktop computer should be connected using the Ethernet port labeled
"QUANT’X".
6. Locate and identify the following important accessories.
a. X-ray beam collimator. At least one collimator is provided with the spec-
trometer. The standard 8.8 mm collimator is shown in figure 3.5.
Position the collimator on top of the filter wheel assembly.
b. Copper (Cu) sample.
This metallic disk is used for all performance verification and troubleshooting.
7. Install sample stage or auto-sampler tray.
Note The spectrometer is supplied with one or more sample handler, such as
shown below, depending on options purchased.
Fig. 4 - 2
a. Install the sampler tray in the spectrometer.
The 10-position auto-sampler tray must be used with one of two types of sam-
ple adapters shown below. Locate the sample adapters and insert them into the
tray.
Fig. 4 - 3
b. The single-sample stage is supplied in a plastic bag of accessories.
8. Place the Cu sample in position 1 of the sample tray.
9. Close the sample chamber lid.
10. Turn ON the ARL QUANT’X power switch. Wait 5 minutes for the detector to cool
down and be stable to operate.
Note For safety reasons, the initialization and the following operation are author-
ized only when the lid is closed.
a. Confirm that the power indicator on the front panel comes on.
6. Plug the power jumper cord into the vacuum pump and spectrometer, and then plug
the vacuum power cord into the spectrometer and an AC power source.
Fig. 4 - 4
7. Turn ON the vacuum pump power switch.
The vacuum pump is now ready for operation.
Even though the power switch is on, the pump is controlled by the spectrometer
and will not turn on until instructed by the software.
Connection
This section describes how to establish a live connection between the spectrometer and
the computer to verify that they have been installed, connected and configured correct-
ly.
Conditions
The ARL QUANT’X spectrometer must be powered on and initialized.
Safety Precautions
Routine.
Procedure
To test for a successful live connection.
1. Turn on the computer and log in.
2. Navigate to WinTrace > Spectrometer Manager.
3. Confirm a successful connection as follows:
a. Examine the Windows task bar for one of the following icons.
Icon Meaning
Fig. 4 - 5
If the connection fails, do not continue this procedure. Verify that all installation
steps in this chapter were correctly followed.
4. Click the System Status tab and ensure that all values are within the normal
ranges indicated.
Fig. 4 - 6
5. Click the EDS Status tab and ensure that the Detector State is set to OK.
Fig. 4 - 7
6. Still on the EDS Status tab, check the following parameters:
• % Dead Time: less than 5%
• Detect Rate: less than 200 cps
• Zero Width: less than 100 eV
These boundaries define the normal behavior of a functional system when
"idle" – that is, with X-rays off.
If one or more values fails inspection, wait for another 30 minutes to allow the
detector to cool down further and examine the EDS status again. If still no
success, the spectrometer may require service.
7. Turn the X-Ray Source key switch on the back panel of the spectrometer clockwise
to the Enable position.
Operation
This section describes several simple tests to verify that the spectrometer is fully opera-
tional and ready for analytical work.
Conditions
The ARL QUANT’X spectrometer must be powered and successfully connected.
Required Equipment
Copper (Cu) sample.
Safety Precautions
Routine.
Procedure
To test an ARL QUANT’X system:
1. Verify the Cu sample is in position 1 of the sample tray.
2. Navigate to WinTrace > Acquisition Manager.
3. Choose File >New > Qualitative Tray List.
4. Type X for a sample name and press the "down" arrow key to auto-fill the other
fields.
Your window will now resemble:
Note: If the Start icon is disabled, check the spectrometer connection status. If the
connection fails, you will not be allowed to collect a spectrum. In addition, make sure
that you pressed the down arrow to complete the line.
Fig. 4 - 8
Appearance of a spectrum indicates that the spectrometer is operating and com-
municating properly.
If a spectrum does not appear, then make sure that the installation steps have all
been correctly followed, note any error messages, and contact us.
6. Click Identify Spectrum Peaks to confirm that the peak shown is, in fact, cop-
per (Cu).
7. If the spectrometer is equipped with the vacuum and/or helium options, test them as
follows:
a. Choose Edit > Condition Properties.
Test Procedures
To ensure that the spectrometer is operating correctly after installation, the following
test and adjustment procedures should be carried out in the order listed.
• Interlock Test (see Chapter Theory of Operation - X-ray Safety)
• Energy Adjustment (see Chapter Maintenance)
• Resolution (see Chapter Maintenance)
• Stability (see Chapter Maintenance)
Note You have now completed the basic installation of the ARL QUANT’X. The
remaining procedures in this chapter are for changing and setting parameters.
Computer Configuration
This section describes the procedures required to configure and prepare the computer
system for communication with and control of the ARL QUANT’X spectrometer. This
section is only intended for computer replacement or computers not supplied by us.
Note: A basic familiarity with the computer and the Windows Operating System is
assumed in all of the procedures. Examples are provided for the Windows 7 operat-
ing system. Other Windows OS versions may differ in icon names, location or ap-
pearance. For additional help, contact us or your IT department.
Note: Incorrect configuration of the Network Interface Card will prevent communica-
tion between the computer and the spectrometer.
Fig. 4 - 9
Fig. 4 - 10
System Configuration
This program is used to configure the software for proper operation of the spectrometer,
including hardware options, communication, logging and custom concentration units.
All settings defined by the System Configuration program are stored in an INI file. When
any of the WinTrace programs are started they get their initial settings from this file.
Upon startup, the System Configuration program prompts the user for a password. The
password for service-level access is "service" (without quotes).
The following sections describe the settings available.
Hardware Configuration
This tab describes the hardware options installed in the spectrometer.
Fig. 4 - 11
Item Description
Stage Configuration The type of control desired over certain stage types.
Helium Indicates whether the system will be using the Helium purge
option. If you are using the Helium purge option, observe the
following specifications:
• Input pressure range - 15 to 65 psig (103-448 kPa).
• Consumption (flow rate):
• 2 minute purge - 15 SCFH (425 l/h)
• During analysis - 5 SCFH (142 l/h)
• Fitting - ¼ inch hose barb
Service Mode A special option for use by service personnel and advanced
users. Using this option under normal conditions is not recom-
mended.
Change Password This button lets you change the customer-level password used
to protect the System Configuration settings against unauthor-
ized changes from the default value. If the new password is
forgotten, you must log in as a service engineer to change it
again.
Geometry
This tab describes the X-ray Tube and Detector information relevant to sample analysis,
specifically when using the Fundamental Parameters analysis technique. The figure
below shows the settings for a X-ray tube with Rh anode.
Fig. 4 - 12
Item Description
Tube Anode The atomic number of the X-ray tube target material (anode).
Most systems use Rhodium anodes. Rhodium has atomic
number 45. For Silver anodes, it would be 47.
Electron Incident Angle The angle in degrees of the electron beam to the anode inside
the X-ray tube. The default for all standard systems is 90
degrees.
X-ray Tube Takeoff The angle at which X-rays leave the anode to reach the sam-
Angle ple. The default for all systems is 90 degrees.
X-ray Tube Incident The angle at which X-rays impact the sample. For ARL
Angle QUANT’X systems the angle is 55 degrees.
Be Tube Window The thickness of the Beryllium window on the X-ray tube. For
Thickness most tubes, the window is 2mils or 50 microns thick.
X-ray Detector Takeoff The angle at which X-rays leave the sample en route to the
Angle detector. The default angle for all standard systems is 45
degrees.
Be Detector Window The thickness of the Beryllium window on the detector, typi-
Thickness cally 8 microns.
Filters
This tab describes the X-ray beam filters installed, their location in the filter wheel, and
the associated excitation conditions.
The figure below shows the filters installed for a X-ray tube with Rh anode.
Fig. 4 - 13
The figure below shows the filters installed for a X-ray tube with Ag anode.
Fig. 4 - 14
Item Description
Available Filters The list of filters available for use in the spectrometer. Default proper-
ties for each filter (accessible via the Edit button) are supplied by the
WinTrace installation program.
Active Filters The specific list of filters being used in the spectrometer.
• Pos—The position of the filter in the filter-wheel.
• Def—The selected option button indicates the default filter (con-
dition) to be used for blank method files in Method Explorer or
new Qualitative Tray List in Acquisition Manager.
• Filter—A filter from the Available Filters list.
If the composition or position of the filters in the spectrometer fil-
ter wheel are changed, the Filters configuration tab must be up-
dated to reflect the new hardware configuration.
• To add a filter to the Active list, you must first add this filter to the
Available list. Click the filter in the Available list, highlight the po-
sition in the Active Filters list and click Add.
• To change the position of a filter in Active list, select the filter and
use the up and down arrows to move the filter to its new position.
• To add a filter to the Available list, click New and complete the
filter definition tabs.
• To remove a filter from the Available list, click the filter and click
Delete.
• To change the definition of a filter in the Available list, click the
filter and click Edit.
The figure below shows the filter wheel with its positions. The table shows the configu-
ration for a Rh target X-ray tube and an Ag target X-ray tube.
Fig. 4 - 15
Position Condition Rh X-ray Tube Ag X-ray Tube
Units
This tab describes the units available for calibration and sample analysis.
Fig. 4 - 16
Concentration units are defined on this view. The %, ppm, and wtfrac (weight frac-
tion) units are the default units for the system and cannot be modified or deleted. Addi-
tional units can be added in the rows below.
Name—The name of the concentration units to be defined.
Thermo Scientific ARL Quant'X Technical Manual– Preliminary Version 4-23
Chapter 4 | Installation
Conversion—The conversion factor between the defined units and wtfrac units.
Note At times, user-defined units are not concentration units and/or cannot be con-
verted. In such cases, you may enter a "dummy" value for the conversion factor.
However, in order to obtain accurate analytical results, you must use calibration
standards with values in the same units.
ADC Parameters
This tab contains high-level settings that control the Digital Pulse Processor and deter-
mine both peak position and peak width (resolution).
Fig. 4 - 17
Zero Cutoff (eV)—The energy below which no x-ray events are stored by the Pulse
Processor.
Discriminator (eV)—The approximate zero-width of the detector at a Time Constant
of 50 µs.
Note The Discriminator value is set to 100 eV by default and should not need to
be changed.
Gain DAC—The Fine Gain setting for each Count Rate. These are set by WinTrace
when Energy Adjustment is run. The Reset to Default Values button is used to reset
these values when DPPCal is run, or the values are so badly off that the system is una-
ble to perform an Energy Adjustment.
Time Constant (ns)—The Time Constant (Shaping Time) used for each of the
Count Rates.
Chamber Parameters
This tab contains settings related to chamber control.
Fig. 4 - 18
Vacuum OK (mV)—The Vacuum Sensor reading at which the chamber vacuum is
sufficient for analysis. This should be set in accordance with the Chamber Vacuum test
(see Technical Manual, chapter 5 - Test and Adjustment Procedures).
Note The Vacuum OK value also controls when the system states that venting the
chamber to air is complete. The relationship between the numbers is vent complete
(ARO) is returned when the vacuum sensor reading is less than 0.6 times the Vac-
uum OK level.
Fig. 4 - 19
Target % Dead Time—The % dead time the system will attempt to adjust the Tube
Current to achieve if "Auto" is selected for the current of the condition.
Tube Linearization Coefficient—A detailed description of these parameters is
given on screen. The Tube Calibration program is provided to adjust these automatically
if necessary.
Note These values should not be adjusted unless the analysis results are signifi-
cantly inaccurate. A common cause of this is using standards that require very low
tube current to achieve the Target % Dead Time to calibrate a method used for sam-
ples that require very high tube current to achieve the Target % Dead Time.
Logging
This tab controls logging of informational and error messages encountered during
communication between the hardware and various software modules. Typically, logging
is not enabled; however, logging options may be used to assist with troubleshooting.
Fig. 4 - 20
Note You must close and re-open the WinTrace programs for any changes to take
effect. Due to the possibility of extremely large log files, it is not advised to leave any
of the options that save logs to disk enabled.
Note This log file is overwritten every time Spectrometer Manager is started. As
this log file can become extremely large, these options should only be used for tem-
porarily diagnosing communications.
Note The full information level writes an incredible amount of data to the log file
and can cause the system to run out of hard drive space if left enabled.
Communication
This tab contains the setting used by WinTrace to communicate with the Digital Pulse
Processor.
Fig. 4 - 21
Note Changing any of these values can cause WinTrace to be unable to com-
municate with the spectrometer. These values should only be changed if the appro-
priate changes have been made to the spectrometer as well.
Energy Adjustment
This tab contains the settings used by Acquisition Manager to perform the Energy Ad-
justment.
The figure below shows the settings for an instrument with Rh target X-ray tube.
The figure below shows the settings for an instrument with Ag target X-ray tube.
Fig. 4 - 22
The figure below shows the settings for an instrument with Rh target X-ray tube.
Fig. 4 - 23
The figure below shows the settings for an instrument with Ag target X-ray tube.
Fig. 4 - 24
Resolution Test
This tab contains the settings used by Acquisition Manager to perform the Resolution
Test.
The figure below shows the settings for an instrument with Rh target X-ray tube.
Fig. 4 - 25
The figure below shows the settings for an instrument with Ag target X-ray tube.
Stability Test
This tab contains the settings used by Acquisition Manager to perform the Stability Test.
There are no custom values on this tab.
The figure below shows the settings for an instrument with Rh target and Ag target
X-ray tube.
Fig. 4 - 26
Energy Adjustment
The purpose of the Energy Adjustment is to set the pulse processor gain so that de-
tected X-rays appear at the correct energy. This is a semi-automated process, which
should be performed weekly for optimal quantitative performance.
Note Energy adjustment needs to be run whenever the detector, DPP or X-ray
tube was replaced, as well as after long periods of inactivity. Furthermore, the pro-
cedure has to be run once WinTrace is started for the first time.
Test Conditions
The Digital Pulse Processor (DPP) must be calibrated according to DPP Calibration
(DPP Cal) .
Test Equipment
Copper (Cu) sample.
Procedure
To perform Energy Adjustment:
1. Start Acquisition Manager and choose File > New > Qualitative Tray List.
2. In the System Manager, verify that the analysis parameters are correctly set and
click OK.
- for instruments with Rh target X-ray tube:
3. After a few minutes, a message will appear asking to click on the largest peak in the
spectrum (in yellow in the figure below). You are prompted twice and will move the
Target Peak onto the Kα peak of the test element.
Fig. 5 - 1
4. Upon completion, a Fine Gain Adjustment Report opens on the screen. Verify
whether the parameter values meet the specifications:
Item Values
Final Fine Gain Setting between 25.000 and 30.000
Fig. 5 - 2
The Fine Gain Adjustment Report is saved automatically and can be found in the
C:\QUANT'X\Diagnostics directory.
The Energy Adjustment procedure is now completed.
Test Equipment
Digital voltmeter (DVM).
Test Conditions
None.
Procedure
Each voltage can be adjusted directly on the power supply potentiometer indicated
below:
Fig. 5 - 3
The values must be adjusted at the following tolerances:
Slot N° Adjustment
5 5.1V +/-0.05V (between + and -)
Fig. 5 - 4
1. Measure the voltage on the 24 V switching power supply PS2 as follows.
• Connect the negative lead of the DVM to one of the black wires on the PS2
output terminal strip.
• Connect the positive lead of the DVM to one of the orange wires on the PS2
output terminal strip.
2. The DVM reading should be 24.0 ± 0.2 V.
3. If the DVM voltage reading is outside of the normal range, remove the screw se-
curing the power supply tray and slide the tray forward.
The tray may not be removed, but it will travel far enough to remove the six screws
that secure the RFI shield to the power supply tray.
4. The PS2 power supply has a single adjustment pot (labeled VADJ) near the output
terminal block as shown in the figure above. Adjust the pot for a DVM reading of
24.0 ± 0.2 V.
Interlock Test
The purpose of this test is to check the operation of the interlock circuit, including opera-
tion of the lid senses and of the interlock device.
Test Equipment
None.
Procedure
To test the interlock:
1. Remove the side panels of the mainframe and the plastic DPP top cover.
2. Turn on the system power.
Fig. 5 - 5
3. Close the chamber lid.
4. Verify that LED 'INTERLOCK IN' turns on only when the lid is closed.
5. Open the chamber lid.
LED 'INTERLOCK IN' should turn off.
6. Close the chamber lid.
LED 'INTERLOCK IN' should turn on.
Note LED 'LID CLOSED' should turn on just before LED 'INTERLOCK IN' turns
on.
Test Equipment
• Digital multimeter (DMM)
• Small screwdriver for adjusting circuit board potentiometers
Test Conditions
Fully functional X-ray tube and power supply should be connected. The tube must be
mounted to the shielded sample chamber.
For replacement power supplies, verify the S502713 label on the new supply has been
set to the correct X-ray tube vendor and model X5409 (see figure below). If this label is
incorrect, contact us.
The right side enclosure cover should be removed and interlock switch bypassed.
IMPORTANT Improper adjustment will damage the X-ray tube. For a replace-
ment power supply, verify that potentiometers PH ADJ (Filament Pre-Heat) and FIL I
LIM ADJ (Filament Current Limit) are at the factory settings shown on the S502713
label by using the following procedure.
Fig. 5 - 6
Procedure
To set up the MNX high voltage power supply:
1. With power OFF, remove both of the L-bracket screws.
2. Swing the back of the power supply out to clear the frame, and hold the power
supply in place by temporarily re-fastening the front L-bracket screw.
3. Connect the Digital Multimeter (DMM) lead to the Protective Ground Stud at the
back of the MNX supply.
Note The I/O mating connector (15 SKT DSUB) positions 6, 9, and 14 are filled
with spare unwired terminals, so they can be accessed by the DMM + probe (see
figure below).
Fig. 5 - 7
4. With X-rays OFF, verify the voltage on pin 14 (Filament Preheat) of the I/O con-
nector is equal to the value on the MNX side panel label.
If adjustment is needed, consult a factory service representative.
5. Verify the voltage on pin 9 (Filament Limit) of the I/O connector is equal to the value
on the MNX side panel label.
If adjustment is needed, consult a factory service representative.
6. With the X-rays ON at 4 kV, 2 mA, verify the voltage on pin 6 (Filament Monitor) of
the I/O connector is at least 0.08 VDC less than the Filament Limit value on the la-
bel on the MNX side panel.
If adjustment is needed, consult a factory service representative.
7. Turn X-rays OFF and power OFF.
8. Install the power supply in the chassis using the two L-bracket screws
Note The potentiometers kV ADJ and mA ADJ are not used in this version
(X5409) of the MNX.
Radiation Survey
Use this survey to measure the radiation leakage outside the spectrometer at full power
in worst case conditions. This is a safety-related procedure.
This procedure is written for a particular model of survey meter. If your meter is a dif-
ferent model, disregard the particular references and follow your meter manufacturer’s
operating instructions.
Test Equipment
• Dosimeter ring or badge
• Survey meter, monitor 4EC, A039999
• Delrin™ scatter block sample
• 1 inch x1 inch lead sheet
• Radiation Survey Recording Form No. 226
Test Conditions
An X-ray beam collimator must not be installed in the filter wheel holder.
Safety Precautions
This survey may constitute a radiation hazard. Test personnel must wear a dosimeter
during the test.
Procedure
To survey radiation in your ARL QUANT’X system:
1. Fill out the survey form.
2. Verify that the survey meter has been calibrated within the last year.
3. Use the test source supplied with the meter to verify that it is working correctly.
4. Remove the sample tray from the chamber, there will be no sample for the first part
of this test.
5. Ensure that all the QUANT’X enclosure covers are in place.
6. Start Acquisition Manager and choose File > New > Qualitative Tray List.
7. Type anything for a sample name and press the down arrow key.
8. Click inside the Condition cell, choose Edit > Condition Properties.
9. Set up the following conditions.
Condition Setting
Tube Voltage 50 kV
Filter No Filter
Atmosphere Air
Warm up 0 seconds
Note Survey meter, Monitor 4EC, A039999 does not request scale correction with
x1 reading.
Note The detection point is 2.5 cm back from the front end (see radiation symbol at
back).
Test Equipment
Copper (Cu) sample.
Test Conditions
The ARL QUANT’X spectrometer must be on and initialized. All panels have to be in-
stalled and the X-ray tube activated at 50kV, 1mA for 30 minutes to ensure warmup.
Procedure
Note Prior to starting the DPPCal procedure, make sure that all instances of Win-
Trace software are closed, and confirm that Spectrometer Manager is not running.
Fig. 5 - 8
b. Click the DPP Calibration option. The following dialog opens, allowing to
change the Tube Voltage and Current values:
Good Practice This window remains active throughout the DPPCal pro-
cedure; Move it to the right of the screen so that it remains visible at all times.
c. Click START. You are prompted to place the Test Sample in Position 1.
d. Click OK when ready.
After a few moments the actual DPPCal program starts asking for a password.
Enter “calibrator” without quotes.
3. In the DPPCal program, select the Service Calibration tab.
a. Confirm that the System and Detector are correctly specified. For System,
you should select "Quant'X", for Detector, you should select "Silicon Drift".
b. If changes are needed, make them and click on Write to push the values to
the DPP.
c. Click on Save to Flash to commit the values to the DPP permanently. Fail-
ure to do this step will lose the calibration values if the system is rebooted or
power-cycled.
4. Click the EDS2 Auto Cal tab.
a. You are prompted to adjust the Voltage and Current values of the tube using
the controls on the DPP Calibration window (see step 2 above).
b. Prior to adjusting the values, start Spectrometer Manager with service
mode enabled in System Configuration. On the Diagnostics tab - Excita-
tion, check that 6 is selected. This corresponds to the Medium thick Pd or Ag
filter, depending on the X-ray tube. If needed, select the filter and click on Set.
c. Return to DPP Calibration window and make sure the Tube Voltage is set to
18kV and the Tube Current is set to 0.08mA. If needed, set the conditions
accordingly and click anywhere outside the dialog on the screen. Wait for 30s.
You are prompted that the screen should show approximately one pulse per
screen refresh (see figure below).
d. Click on OK to continue.
e. Wait for Baseline calibration to complete. When completed, a green check
mark is shown next to the button.
a. Use again the controls on the DPP Calibration window (see step 2 above) to
adjust Tube Voltage to 18kV and Tube Current to 0.40mA and wait for 30
seconds. You are prompted that the screen should show approximately five
pulses per screen refresh (see figure below).
Fig. 5 - 9
b. Click on OK to continue.
c. Wait for input RC calibration to complete. When completed, a green check
mark is shown next to the button.
8. Click on Calibrate Discriminators.
a. Use again the controls on the DPP Calibration window (see step 2 above) to
adjust Tube Voltage to 18kV and Tube Current to 0.08mA and wait for 30
seconds. You are prompted that the screen should show approximately one
pulse per screen refresh.
b. Click on OK to continue.
c. Wait for discriminator calibration to complete. When completed, a green check
mark is shown next to the button.
9. Click on CalibDPP Parameters... . The EDS2 Algorithm Calibration window
opens.
10. Enter 1300 in the Discriminator and Discriminator 1 fields of the first column (.1-1
us):
Note You can also save the file clicking on Save. In this case, use the directory
C:\QUANT’X\Diagnostic\DPP\
Resolution
This test verifies the operation of the detector and related circuitry. Often, Manganese
(Mn) is used as the industry standard for resolution specification at 5.89 keV. Copper
(Cu) is more convenient because it is readily available and easier to handle. For con-
venience, we use a Cu sample at 8.04 keV.
Test Equipment
Copper (Cu) sample.
Test Conditions
The Energy Adjustment must have been completed prior to the test.
Procedure
Note These settings remain as the default test configuration until changed.
Test Equipment
Copper (Cu) sample.
Test Conditions
The procedures in MNX high voltage Power Supply Setup must be completed before
running this test.
Procedure
To perform the X-ray tube conditioning:
1. Place the Cu sample in tray Position 1.
2. Start QUANT’X Diagnostics.
3. Select the X-ray Tube Conditioning option and click Next.
4. Select Ramping Speed (fast or slow).
Slow ramping should be used when conditioning a new or replacement X-ray tube.
5. Click Start.
6. The conditioning consists of these two steps:
a. The voltage is ramped from 4 kV up to 50 kV in 1 kV increments at a constant
current of 0.20 mA.
b. The current is ramped from 0.20 mA up to 1.98 mA in 0.01 mA increments at a
constant voltage of 25 kV.
When the system starts operating at voltages that require ramping during
analysis (above 34 kV), pay particular attention to any arcing sounds (which
sound like loud static electricity discharges). Some arcing is normal during the
first several minutes of operation, especially for new tubes at higher voltages
(45–50 kV). However, arcing that persists for more than 5 minutes or occurs
sporadically during the test would be reason for concern, as arcing is often re-
sponsible for X-ray flux instability and other strange phenomena during anal-
yses.
Stability
This important test verifies that the X-ray generation and detection subsystems are
functioning correctly, helps differentiate between problems arising in the two systems
and determine as quickly as possible the hardware component(s) most likely responsi-
ble for the problems. This test should be performed if the system is suspected or known
to be unstable based on the Energy Adjustment report or application results.
Test Equipment
Copper (Cu) sample.
Test Conditions
DPP Calibration (DPP Cal) and "Energy Adjustment" must have been performed.
Procedure
To perform the stability test:
Note These settings remain as the default test configuration until changed.
Note The system should be stable regardless of dead time, as long as the peak
counting statistics are sufficient. Typically, a peak should have at least 500,000 to 1
million counts to qualify.
Note The Stop button is disabled and blinks red when the test collects hardware
status readings. Do not stop the analysis at this time, as it may freeze the system.
Glossary of Terms
The following terms are used in this test.
Term Description
ROI The Region of Interest used to calculate the Peak counts. The
ROI depends on the sample (element) as well as the detector
type used to conduct the test. For example, for a test con-
ducted with a Cu sample on a PCD system, the ROI would be
defined as ± 5 channels or ± 100 eV around the tallest chan-
nel in the very first spectrum analyzed during the test. To
allow for advanced data analysis, the ROI width can be modi-
fied manually prior to the start of the test. For example, it is
possible to use an ROI of ± 4 channels for Cu, if so deemed
necessary.
Peak Counts The sum of all counts that fall inside the ROI as defined
above.
FWHM The Full Width Half Max of the Peak, also called resolution,
calculated as the distance in eV between the left and right
sides of the peak at half of its maximum height.
In the case of peak shift, fewer counts fall within the region of interest (ROI) boundaries,
causing the reported Peak counts to decrease. In this case, the Peak and Centroid
graphs will track each other, while the Total counts would remain constant.
When the problem is a resolution change, the peak width increases. Since the total
number of peak X-rays does not change (i.e., peak area remains the same), the peak
would become shorter, causing fewer counts to fall within the ROI. In this case, the
Peak graph would be a mirror image of the FWHM graph, while the Total counts would
be constant.
Fig. 5 - 10
Of course, it is also possible for both the Generation and Detection systems to be un-
stable at the same time. In that case, interpretation of the results becomes more diffi-
cult, since a change in Peak counts, for example, may be due to any one of several
unrelated factors. In such cases, it is especially useful to have a record of hardware
performance during the test. The history of over 20 system parameters is shown in the
bottom frame of the Stability Test Chart and also saved as "HardwareLog.csv" in the
test data folder. Each parameter’s history can be displayed by clicking on that parame-
ter in the list.
In summary, the interpretation of the test results relies on the following logic:
Total deviation affects the Peak, but Peak deviation does not affect the Total.
• If Total stability is poor, then investigate components such as the X-ray tube, X-ray
high voltage power supply, or the X-ray control board. Look for correlations be-
tween the Total counts and the recorded history of X-ray Tube Monitor and Control
Voltages, Tube Current, and the H.V. power supply voltage.
• If the Peak stability is poor, and it does not parallel the Total chart, then look for
correlations with the Centroid and FWHM charts. Peak instability is most often as-
sociated with detector problems, noise pickup, or a faulty EDS board. Thus, study
the histories of Detector Temperature, Heat Sink Temperature, system voltages, as
well as parameters such as dead time and Fast Discriminator, which often shed
light on noise issues
• Adjustable ROI
Access the advanced options by clicking Change Test Parameters. By speci-
fying the Peak Position, Peak Search and Stability Width parameters, you have un-
limited flexibility to select the element, line or region for stability calculations. Click
Calculate to re-analyze any existing set of stability spectra after changing the test
parameters.
• Data Evaluation and Manipulation
The stability and hardware charts can be scaled vertically and horizontally. To scale
the charts vertically, click the Up or Down buttons corresponding to the chart to
contract or expand the scale, respectively. For the stability chart only, the Display
Scale options can also be used to display the results scaled to the data or on a
"standard" scale based on maximum permissible deviation for a "typical" system.
(Note: the vertical scale buttons are only enabled when chart is scaled "To Data").
To scale either chart horizontally, press and hold the SHIFT key, then click the left
mouse button and drag the mouse to highlight a subset of data points, which may
contain as few as three points. Both charts will be expanded to show only the se-
lected subset of the data. The Peak and Total RSDs shown in the chart window will
also be recalculated for the subset. To view the full dataset, press and hold SHIFT
and click the right mouse button.
Left-click the Results chart to turn on the cursor; right-click to turn the cursor off.
Use the keyboard arrow keys to move the cursor and examine the results for each
individual point.
Repeatability
The purpose of this test is to check whether the output of the X-ray tube is affected by
cycling. The output is first measured at a given kV and mA setting and then compared
to the output after the tube power is cycled or momentarily set to different voltage and
current.
Test Equipment
• Copper (Cu) sample
• 8.8 mm X-ray tube collimator (standard)
Test Conditions
The spectrometer must pass Stability.
Procedure
To test for repeatability:
1. Install the standard X-ray tube collimator (8.8 mm) and place the Cu sample in
Position 1.
2. Start QUANT’X Diagnostics.
3. Choose the Repeatability Test option and click Next.
4. Click Start.
The program will run the WinTrace Software automatically.
5. Adjust the dead time to approximately 50% by changing the current in Edit >
Condition Properties.
Do not use auto-current.
6. Choose Analyze > Next Sample.
Analysis will stop with a prompt for the next tray.
7. Click OK to continue the test.
8. While measurement #6 is being analyzed, choose Edit > Condition Properties
and set.
a. Tube Voltage to twice the present value (e.g., 40 kV instead of 20 kV).
b. Tube Current to half the present value (e.g., 0.06 mA instead of 0.12 mA.
c. Filter to Cu thick.
After 15 seconds, change the three parameters back to their original values
and click OK.
9. Wait for 20 seconds, choose Spectrum > Clear.
10. When the system prompts for "Tray 2", wait for 2 minutes and click OK.
Do not change trays or otherwise disturb the sample.
The test results consist of:
Test Equipment
• Thin washers (about 0.010 in.)
• Copper (Cu) sample
• 8.8 mm X-ray tube collimator (standard)
Test Conditions
The spectrometer must pass Stability.
Procedure
To adjust the sample tray height:
1. Remove all washers from under the tray pads.
2. Install the standard X-ray tube collimator (8.8 mm) and place the Cu sample in tray
position 1.
3. Start QUANT’X Diagnostics.
a. Click Service Technician and enter service for the password.
b. Select the Tray Height Adjustment option and click Next.
c. Click Start.
The program will run the WinTrace Software automatically.
d. Adjust the current to achieve a dead time of approximately 50%.
Do not use auto-current.
e. Choose Analyze > Next Sample.
Analysis will stop with a prompt for the next tray.
f. Add one washer under each tray pad and replace the tray.
g. Click OK to continue the test.
After measuring with the first washer, the program will show graph of the re-
sults. All subsequent measurements will be shown.
4. Repeat Step 3 until the correct tray height is determined.
The signal intensity should start low, achieve a maximum and start dropping as more
washers are added. The correct tray height corresponds to the highest intensity.
The adjustment allows for up to 9 washers to be added. If the maximum is not
achieved by then, the spectrometer is not functioning correctly.
5. After finding the correct number of washers, click Cancel when prompted for the
next tray and click Stop on the status window.
The test results consist of:
• Test Conclusion: The number of washers producing the maximum signal inten-
sity.
• Chart of the results, shown as Intensity versus Number of Washers.
• Display of detailed test results. All results and test data are stored in the default
folder C:\QUANT’X\Diagnostics\THA.
6. Install the correct number of washers under the tray pads.
Tray Accuracy
This test verifies that the system produces the same results when analyzing the same
sample in any position of the sample tray. The test analyzes a set of identical brass
plugs, one in each tray position, and calculates the deviation in counts between posi-
tions. The single-sample stage does not require this test.
Test Equipment
• Twenty (20) identical 1.25 in brass plugs (cut from the same bar)
• 8.8 mm X-ray tube collimator (standard)
Test Conditions
The system must pass the Stability and the Tray Height Adjustment must be performed.
Procedure
To perform the sample tray accuracy test:
1. Install the standard X-ray tube collimator (8.8 mm) or the collimator that will be used
for analytical measurements.
2. Load the identical brass samples into the tray to be tested.
If the system has more than one type of tray, then test each tray separately.
3. Start QUANT’X Diagnostics.
a. Click Service Technician and enter service for the password.
b. Select the Tray Accuracy Test option and click Next.
c. Click START.
The program will run the WinTrace software automatically.
d. Test the (optional) sample spinner, if necessary, by clicking Yes when
prompted.
e. During the spinning, verify that the spinner motor is turning and that a spinner
cup turns smoothly when empty or with a brass sample.
f. The spinning continues for 20 seconds, then the program returns you automat-
ically to Step c. If you are ready sooner, continue with the test by clicking
START again.
g. Adjust the current to achieve a dead time of approximately 50%.
Do not use auto-current.
The test will run until completion at which time you will see the result, which will
consist of:
• Test Conclusion: ON or OFF Spec.
• Graphical Display of test results, shown as Intensity versus Tray Position.
• Display of detailed test results. All results and test data are stored in the default
folder C:\QUANT’X\Diagnostics\STA.
4. Verify that both of the following criteria are met:
• The overall relative standard deviation,% RSD, is ± 0.30%.
• The relative error, % Error, for any single position is ± 0.50%.
If the system fails this test, perform the Sample Tray Height Adjustment. Optimal tray
height greatly minimizes the sensitivity to tray flatness.
Test Equipment
Sample cup with copper foil (approximately 0.150-in diameter disk) fixed in place be-
tween two stretched mylar sheets and MnO2 powder.
Test Conditions
The DPP Calibration (DPP Cal) must be performed.
Procedure
To perform a live time correction test:
1. If the test sample has not been assembled, see Test Sample Assembly.
2. Pour MnO2 powder into the test sample cup, enough to completely cover the bottom
of the cup with a thick layer.
3. Place the test sample in tray position 1.
4. Start QUANT’X Diagnostics.
a. Click Service Technician and enter service for the password.
b. Select the live time Correction Test option and click Next.
c. Click START.
The program will run the WinTrace software automatically.
d. Adjust the current to achieve a dead time of approximately 50%.
Do not use auto-current.
e. Choose Analyze > Next Sample.
Analysis will stop with a prompt for the next tray.
f. Pour the MnO2 powder out of the sample cup and into an empty container.
g. Return the sample cup to the tray and click OK to continue the test.
The dead time should now be 15 to 20%. If not, the size of the copper foil must
be adjusted and the test re-started.
h. When prompted for "Tray 3", return the MnO2 powder to the test sample cup.
Take care to not move the Cu foil and/or sample cup when the powder is
poured in, otherwise the test must be re-started.
i. Click OK to analyze the last test spectrum.
The test results will consist of:
• Test Conclusion: ON or OFF Spec. -
• Display of detailed test results. All results and test data are stored in the default
folder C:\QUANT’X\Diagnostics\LIV.
5-36 ARL Quant'X Technical Manual– Preliminary Version Thermo Scientific
Chapter 5 | Test and Adjustment Procedures
Make sure the adhesive does not contain metals detectable by XRF.
3. Place a second piece of X-ray film over the Cu disk and lock the film in place using
the standard locking ring supplied with the cup.
Step 3
Step 2
Step 1
Stray Lines
This test verifies the intensities of any spectrometer-sourced contamination in the X-ray
spectrum are below specified limits. The test involves analysis of a sample known to
contain only low atomic number elements (such as C, H and O), which the spectrometer
cannot detect.
Test Equipment
Lucite sample or another plastic sample known to be free of inorganic contaminants and
an 8.8 mm X-ray tube collimator (standard).
Test Conditions
None.
Procedure
To perform the stray lines test:
1. Install the standard X-ray tube collimator (8.8 mm) or the collimator intended to be
used for analytical measurements.
2. Place the test sample in tray position 1.
3. Start QUANT’X Diagnostics.
a. Click Service Technician and enter service for the password.
b. Select the Stray Lines Test option and click Next.
c. Click START.
The program will run the WinTrace Software automatically.
d. Allow auto-current to run and adjust for the appropriate dead time for the de-
tector type.
The test results will consist of:
• Test Conclusion: ON or OFF Spec.
• Display of detailed test results. All results and test data are stored in the default
folder C:\QUANT’X\Diagnostics\SLT.
4. Verify that the calculated ratio percentages are below the following limits for the
detector type:
Low-Energy Lines High Energy Lines
Cu Fe W Background Ag Sn Background
If the system fails this test, clean the surface of the test sample with a solvent and
repeat the test. Any contamination of the surface may cause high results. Also, con-
firm that the detector collimator is installed and properly aligned.
Test Equipment
Standard liquid sample cup containing Conostan standard S-12 100 ppm trace ele-
ments in oil and an 8.8 mm X-ray tube collimator (standard).
Test Conditions
None.
Procedure
To perform the minimum detection limits test:
1. Install the standard X-ray tube collimator (8.8 mm).
2. Shake the sample cup with the oil to mix the elements thoroughly.
3. Place the sample cup in tray position 1.
4. Start QUANT’X Diagnostics.
a. Click Service Technician and enter service for the password.
b. Select the Minimum Detection Limits option and click Next.
c. Click START.
The program will run the WinTrace software automatically.
d. Allow auto-current to run and adjust for the appropriate dead time for the de-
tector type.
The test results will consist of:
• Test Conclusion: ON or OFF Spec.
• Display of detailed test results. All results and test data are stored in the default
folder C:\QUANT’X\Diagnostics\MDL.
5. Verify that the calculated MDL values are below the following limits:
Fe Pb
where: Cstd = Concentration in the standard (100 ppm for Conostan S-12)
Chamber Vacuum
This procedure tests and adjusts the sample chamber vacuum subsystem. The test
includes setting the vacuum sensor trip point and measuring the chamber pump down
speed.
Test Equipment
• Copper (Cu) sample
• 200 liter per minute vacuum pump
• Varian 801 vacuum thermocouple meter (or equivalent)
• Vacuum hose tee with a Varian™ TYPE 0531 (or equivalent) thermocouple gauge
installed
Test Conditions
Do not use liquid samples in the sample chamber.
Procedure
To perform the chamber vacuum test:
1. Install the tee in line with the vacuum pump hose. Connect the vacuum pump hose
and power cord to the QUANT’X back panel.
2. Connect the meter to the thermocouple mounted in the tee.
3. Place the test sample in tray position 1.
4. Start QUANT’X Diagnostics.
a. Click Service Technician and enter service for the password.
b. Select the Chamber Vacuum Test option and click Next.
c. Click START.
The vacuum pump will turn on. The sensor status bar will show the sensor
voltage relative to the current trip point setting. A time status bar will also show
the elapsed seconds since the pumping started.
Note: If the everything is functioning correctly, the lid will get pressed down and
sealed as the chamber is pumped down. However, the chamber must seal itself,
without pressing on the lid. If the lid does not seal, the vacuum fails to hold or hissing
of any kind is audible, then the chamber lid, baseplate or the o-ring must be adjusted
or replaced.
d. As soon as the sensor reading reaches the trip point, note the vacuum meter
reading.
e. If the pressure is between 750 and 1000 mTorr, go on to Step h, If not continue
with Step f.
f. Type the vacuum meter reading into the Pressure Gauge Reading text
box.
The new vacuum sensor trip point will be calculated. This value can also be ed-
ited manually.
g. Click Set Trip Point.
- Repeat Steps c through g until the vacuum level at the sensor trip point is
within the specified values.
- Note the time (seconds) elapsed since pumping started and confirm that it
does not exceed 90 seconds.
h. Click Analyze spectrum under vacuum…
The program will run the WinTrace Software automatically.
i. Allow spectrum collection to continue for at least 10 minutes and examine the
spectrum.
5. Verify that all of the following criteria are met:
• Spectrum analysis starts in less than 90 seconds after the vacuum pump turns
on.
• There is no Argon (Ar) peak in the spectrum.
• The pressure reading is less than 500 mTorr after 10 minutes of pumping.
Note: The vacuum sensor trip point can also be accessed or set through the Sys-
tem Configuration program in the Chamber Parameters tab.
Test Equipment
Printer.
Test Conditions
Complete, fully functional system.
Procedure
To perform a system status voltages test:
1. Start Acquisition Manager and choose File > New > Qualitative Tray List.
2. Type anything for a sample name and press the <Down> arrow key.
3. Click inside the Condition cell, choose Edit > Condition Properties.
Set up the following conditions:
Parameter Setting
Tube Voltage 25 kV
Filter Cu thin
Atmosphere Air
Warm-up 0 sec
Helium Flush
Use the helium flush test to perform a basic operational test and a high-pressure stress
test of the helium flush feature. This test needs to be performed only if the system is
equipped with this option.
Test Equipment
• 10–80 psi variable-pressure compressed air source
• Flow meter or equivalent (if a meter not available, see Alternate Procedure)
Test Conditions
The helium flush manifold must be adjusted per its subassembly level test procedure.
Procedure
To perform a helium flush test:
1. Set the compressed air source to 80 psi.
2. Insert the flow meter in the compressed air line.
3. Connect the compressed air to the rear panel HELIUM input nipple.
4. Verify that the flow meter reads zero flow.
5. Start Acquisition Manager and choose File > New > Qualitative Tray List.
a. Type anything for a sample name and press the <Down> arrow key.
b. Click inside the Condition cell, choose Edit > Condition Properties.
c. Set Atmosphere to Helium, Live Time to 0 sec, and Current to 0.02 mA.
d. Choose Analyze > Start to start the analysis.
6. Verify that the flow meter reads 7.0 ± 1.0 SCFH during the 2 minute purge.
7. Verify that the flow meter reads 1.5 ± 0.5 SCFH during the analysis.
Alternate Procedure
If a flow gauge is not available, a simple test of the basic operation may still be per-
formed.
1. Set the compressed air source to 80 psi.
2. Connect the compressed air to the rear panel HELIUM input nipple.
3. Start System Configuration.
a. Select the Service Mode check box.
b. Click OK to exit.
4. Open the sample chamber lid.
5. Start Spectrometer Manager and click the ?? tab.
a. Low flow solenoid:
- Type ?? and click Send to turn on helium low flow. Listen carefully for the sound
of air flowing inside the sample chamber.
- Type ?? to turn off low flow. The air flow should stop.
b. High flow solenoid:
- Type ?? and click Send to turn on helium high flow. Listen for the air flow sound
again. This time is should be significantly louder than before.
- Type ?? to turn off high flow. The air flow should stop.
c. Pressure switch:
- Type ?? and click Send to turn on low flow again
- Type ?? and click Send. The response should be "AUL" (low flow valve on).
- Reduce the air pressure gradually.
- Repeat steps ii and iii until the response reads "AUX" (low pressure).
Test Conditions
No open flames or other ignition sources may be in the area.
Test Equipment
A laboratory grade aerosol can of air, Methanol in a small squirt bottle, and a small
vacuum.
Safety Precautions
WARNING Avoid personal injury. Do not touch or otherwise handle the foil. Do
not touch, breathe or swallow the particles and do not allow the particles to come into
contact with your skin or clothing.
The beryllium windows on the X-ray tube and detector are extremely fragile and brittle.
When installing, replacing, or working around the X-ray tube and the detector assem-
blies, proceed with great caution.
• DO NOT touch jar, or subject the beryllium windows to mechanical or thermal
shock.
• DO NOT expose the beryllium windows to corrosive substances such as acid, acid
vapor (such as from caustic samples), water, water vapor, or others substances.
• Protect the surface of the beryllium window by installing a collimator with a protec-
tive mylar window attached.
• Exercise caution when handling materials and samples in the vicinity of the beryl-
lium window. Any physical contact with the window will almost certainly rupture it,
even small particles can puncture the beryllium window.
The beryllium window on the X-ray detector assembly is approximately 0.00035 inches
(8 microns) thick. It is also under one atmosphere of pressure since the detector hous-
ing is evacuated. The beryllium window on the PCD is 0.00035 thick (8 microns), and
the SDD is .0005 thick (12.5 microns).
IMPORTANT The window is highly fragile and will be destroyed by any physical
contact.
Do not attempt to clean the window with a cotton swab or to pick debris off of it using
tweezers.
Beryllium metal is also very susceptible to corrosion from water, acid, or other caustic
substances. Corrosion destroys the vacuum integrity of the window. Do not use clean-
ing solvents other than those specified without contacting the Customer Service de-
partment first.
Rupture of the window destroys the detector assembly necessitating its complete re-
placement. Replacement due to window damage is not covered under warranty or ser-
vice contract and costs several thousand dollars.
Emergency Measures
Avoid personal injury. Do not touch, breathe or swallow the particles and do not allow
the particles to come into contact with your skin or clothing. Do not touch or other-
wise handle the foil.
Procedure
To clean the X-ray detector window:
1. Remove the sample tray and the metal plate covering the components of the sam-
ple chamber.
2. Remove the two socket head screws holding the filter wheel assembly in place.
Move the assembly to the side, it is not necessary to disconnect its cables.
3. Loosen the nylon screw(s) holding the detector collimator in place.
4. Gently remove the collimator.
5. If the contamination is particulate in nature (rather than liquid or oil), an air stream
may be sufficient to remove the particles.
a. Use the canned air to blow a stream of air parallel to the surface of the window
as much as possible.
b. Start with the nozzle about 6 inches (15 cm) away and slowly move it closer to
the window until the particles are removed.
Do not allow the nozzle to come closer than 2 inches (5 cm) to the window.
6. If an air stream is not sufficient to clean the window, a liquid wash is required.
a. Place an absorbent towel in the sample chamber, under the window area.
b. Using the squirt bottle of methanol, direct a fine stream of liquid at the metal
area above the window.
Do not allow the stream to strike the beryllium material directly.
c. Dry the window using the canned air as described above.
This process may be repeated if required.
7. If the window still is not clean, a stronger solvent or factory assistance is required.
Please contact us for advice.
8. If the window appears clean, replace the collimator and filter wheel assembly.
The flat portion of the collimator snout should be horizontal (parallel to the plane of
the sample tray).
To clean the X-ray tube window:
The X-ray tube window is approximately 10 times thicker than the detector window.
Therefore it is not as fragile as the detector window, but caution must still be exercised.
Tip For particulate matter removal without removing the X-ray tube, a small vac-
uum may be used.
h. Remove the two socket head screws that fasten the filter wheel assembly to
the baseplate.
Move the assembly aside, it is not necessary to disconnect its cables.
i. While supporting the tube with one hand, remove the two screws holding it in
place.
These screws are accessed from inside the sample chamber, on either side of
the tube collimator. These are special vacuum sealing screws with an integral
o-ring, save them for reuse
j. Remove the X-ray tube and shroud.
k. Reassemble after cleaning the window.
4. Follow the procedure outlined above for the detector window; hold the tube with the
window down so the liquid drains out.
5. Replace the tube and other components.
QUANT’X Diagnostics
QUANT’X Diagnostics is a utility program designed to facilitate the performance of
many tests and adjustments.
Fig. 5 - 11
During startup, the program will attempt to establish and test a connection with the
QUANT’X hardware.
If the connection fails, you will not be allowed to analyze any test data, although you
will be allowed to re-process any existing test data.
Access to advanced adjustments and procedures can be obtained by clicking Ser-
vice Technician. The password is service.
A typical individual test interface is shown below:
START will not be enabled if the hardware connection is not established or the
self-test fails.
Whenever a calculation is performed, the test results are automatically saved into a
new text file named "Test_n.txt", where n is incremented to the next number after
the existing reports in the test data folder. The very first test result file would be
named "Test_1.txt"
During data analysis, the following status window is typically shown:
STOP can be pressed at any time during data analysis or re-calculation. If X-rays
are on when the Stop button is pressed, QUANT’X Diagnostics should automatical-
ly choose Analyze > Stop in Acquisition Manager, uncheck the "Save Spectrum"
box and click Yes. If this sequence of events does not complete properly, you
should perform/repeat them manually.
The Lock icon may be clicked to Lock the system during a test and prevent unau-
thorized or unintentional interruption. The user will be prompted for a temporary
password (case-sensitive). A blank password will not be accepted; if entered, the
system will return to unlocked mode. The same password would have to be entered
later to unlock the system and return to the test. In case the original password is
forgotten, the user can always unlock the system by entering the following pass-
word: "service" (case sensitive).
Finally, the Test Report screen shown below is used to display the results of all
tests.
Test Equipment
None.
Test Conditions
The ARL QUANT’X front end must be on and initialized.
Procedure
To perform the system noise spectrum measurement:
1. Close all instances of WinTrace and confirm that Spectrometer Manager is not
running.
2. Navigate to WinTrace > Service and start GSTest.
GSTest.exe is a special advanced diagnostics program in the WinTrace software
suite. It is used to monitor low-level communications between the computer and the
DPP module and to provide event data related to detector performance.
3. Ensure that the IP address shown matches that specified in System Configuration.
The default IP address is 192.168.18.10.
4. Click Connect.
If the connection is successful, you should note that some parameters will be up-
dated. In particular, the ZeroFWHM should be a non-zero value. If the connection is
not successful, then confirm the IP Address and click the Connect button again. If
you still do not connect, exit from GSTest.exe, reboot the QUANT’X front-end, and
run Spectrometer Manager to confirm that the computer can communicate with the
DPP.
5. Set the following parameters:
PPADC Variable
Mode MCA
MCA Variables
Mode Waveform
Options
Decimate 10
Average 20
Blocks 2500
FFT Checked
Note: To make another measurement, repeat Step 5 through Step 9. Clicking Start
by itself will not work.
10. To exit GSTest and ensure normal spectrometer function, perform the following
steps:
a. Set the Mode in MCA Variables to Normal.
b. Click Write Vars.
c. Click Exit to close the program.
Noise spectra (FFT) are archived for all systems before shipment to customers, and are
available for diagnostics. Contact us for help evaluating your system’s noise character-
istics.
Signs of noise problems include:
• The presence of peaks other than normal for the detector installed (see below).
• Any peak height greater than 40 K vertical scale.
• Incorrect peak ratios.
• Background that is too high or not flat.
Periodic Maintenance
The ARL QUANT’X spectrometer is inherently a low maintenance spectrometer. The
maintenance procedures prescribed in this section are of a preventative nature. By
periodically performing inspections, unscheduled down-time will be reduced. Detailed
instructions for performing these procedures are given in the ARL QUANT'X Technical
Manual AA83826.
This section does not include procedures for application related operational mainte-
nance tasks such as standardization of the spectrometer. Refer to an applications spe-
cialist for information on operational maintenance.
The maintenance requirements are presented by frequency of service.
Maintenance item Daily Weekly Monthly Every 6 Yearly
Months
Energy Adjustment Perform
Run a check standard Perform
Resolution Test Perform
Overnight Stability Test Perform
System Status Screens: Print
- System Information
- System Status
- EDS Status
Vacuum Pump oil level Check
Air filters on the right side of the Clean
spectrometer
Interlock circuit Test Perform
Vacuum pump oil Replace
Procedure
To perform Energy Adjustment:
1. Start Acquisition Manager and choose File > New > Qualitative Tray List.
2. In the System Manager, verify that the analysis parameters are correctly set and
click OK.
- for instruments with Rh target X-ray tube:
Fig. 6 - 1
4. Upon completion, a Fine Gain Adjustment Report opens on the screen. Verify
whether the parameter values meet the specifications:
Item Values
Final Fine Gain Setting between 25.000 and 30.000
Fig. 6 - 2
The Fine Gain Adjustment Report is saved automatically and can be found in the
C:\QUANT'X\Diagnostics directory.
The Energy Adjustment procedure is now completed.
Procedure
To perform the Resolution Test
Note These settings remain as the default test configuration until changed.
Procedure
To perform the stability test:
Note These settings remain as the default test configuration until changed.
Note The system should be stable regardless of dead time, as long as the peak
counting statistics are sufficient. Typically, a peak should have at least 500,000 to 1
million counts to qualify.
Note The Stop button is disabled and blinks red when the test collects hardware
status readings. Do not stop the analysis at this time, as it may freeze the system.
8. The test report shows the total system error (instability) and the spectrometer con-
tribution to the instability. The spectrometer contribution is calculated using the fol-
lowing formula:
Diagnostic Software
Diagnostic programs allow the service technician to evaluate the performance of various
subsystems of the ARL QUANT’X. This capability makes them useful tools for verifying
proper spectrometer operation as well as malfunctions.
The status pages within the ARL QUANT’X WinTrace Spectrometer Manager program
provide system diagnostics. Both pass/fail status messages and numerical values for
various system parameters, such as voltages and temperatures, are displayed on these
pages. By viewing them, the technician may quickly spot abnormal conditions.
This section describes the Diagnostic command page of Spectrometer Manager. Diag-
nostic commands are found in this technical manual to test and diagnose system func-
tionality such as in Helium Flush.
Diagnostic Page
The Diagnostic page allows the service technician to exercise various spectrometer
hardware functions by sending simple commands to the chamber control board. This
capability is useful for troubleshooting specific hardware malfunctions.
The Diagnostic page is accessed by setting Service Mode (see WinTrace Service
Mode). Spectrometer Manager automatically adds the Diagnostic page if it is running
already.
Component Replacement
This section contains procedures for the field replacement of components in the ARL
QUANT’X chassis. The special precaution section as well as the specific procedure for
the component of interest should be read before beginning the actual repair work. This
will provide insight on the scope of the task and allow the service technician to properly
plan the time and materials required.
New figure: ARL QUANT'X DPP components
Circuit Boards
Replacement of the PC boards located in the ARL QUANT’X DPP assembly and else-
where is detailed below.
EDS Board
To replace the EDS board:
1. With the Chamber/Spectrometer Control board (CSC) removed from the assembly,
locate the four hex standoffs at the corners of the EDS divider panel and remove.
2. Remove the inverted hex standoff located next to the PC-104 connectors.
3. Remove the screw located near the middle of the right side of the EDS divider pan-
el.
4. Remove the three hex standoffs from the corners of the EDS board.
5. Remove the inverted standoff located near the PC-104 connectors.
6. Carefully lift the board straight off the PC-104 and PC-104-Plus connectors.
7. Remove the 120 pin PC-104-Plus extender connector and put into the replacement
EDS board.
8. Repeat the previous steps in reverse order.
The DPP includes a replaceable lithium coin battery. If replaced, dispose of the old
battery properly according to local and national regulations.
Power Supplies
Replacement of all the system power supplies is detailed below. It is possible to replace
the entire power supply tray as one assembly however these procedures address each
supply individually.
Fig. 7 - 1
1. Turn off the spectrometer power.
2. Remove panel screws that hold the right side cover in place.
3. Remove the enclosure cover by grasping it on the bottom, pulling out and sliding
back.
4. Remove the screws that hold the L-bracket in place.
5. Disconnect the high voltage cable and ground connectors from the front of the
power supply.
Do not touch the end of the high voltage cable or allow it to become dirty. If re-
quired, it may be cleaned with isopropyl alcohol.
6. Rotate the supply away from the back panel and unplug connectors.
7. Install the replacement by following the previous steps in reverse order.
8. Perform the following procedures:
a. MNX high voltage Power Supply Setup
b. Run at several voltages and verify that the high voltage MONITOR value on the
System Status screen in Spectrometer Manager approximately matches the
voltage selected.
c. Stability
d. System standardization is required before beginning quantitative analysis.
The tray drive wheel should rotate, change direction to locate the home flag center,
and stop.
Miscellaneous Items
Use the following procedures to replace X-ray Tubes, X-ray Cooling Fans, Enclosure
Cooling Fans, Sample Chamber Lid Latch Assembly, and the Vacuum Power Pump
Relay.
X-ray Tube
To remove and replace the X-ray tube:
1. Turn off the instrument power.
2. Remove the two back panel screws that hold the right side enclosure cover in
place.
3. Disconnect the panel fan cable.
4. Remove the X-ray high voltage power supply as described in the "X-ray High Volt-
age Power Supply" section.
5. Detach the hose from the X-ray tube cooling shroud.
6. Remove screw securing temperature sensor.
Can be removed after lower X-ray tube if unable to access.
7. Remove the sample tray and the metal plate that covers the sample chamber
components (or the special sample handling stage if installed).
The cover plate is secured with special vented screws, save these for reuse.
8. Remove the two socket head screws that fasten the filter wheel assembly to the
baseplate.
Move the assembly aside, it is not necessary to disconnect its cables.
9. While supporting the tube with one hand, remove the two screws holding it in place.
These screws are accessed from inside the sample chamber, on either side of the
tube collimator. These are special vacuum sealing screws with an integral o-ring,
save them for reuse.
10. Remove the X-ray tube and shroud.
11. Install the tube and shroud by following the previous steps in reverse order.
12. Verify that the tube flange depresses the interlock switch lever located on the
chamber port.
13. Perform the procedure in "Stability."
If the tube has not been operated for a long period, an overnight burn-in at moder-
ate power may be required to improve its stability.
14. Perform the MNX high voltage Power Supply Setup appropriate to the tube model
number.
Optional Equipment
This chapter provides an overview of the some of the standard options (Helium Flush,
Camera) available on the ARL QUANT’X. Each subsection includes a functional de-
scription and an installation guide if applicable.
Helium Flush
The Helium Flush option is required for light-element analysis of liquid samples. Be-
cause low energy X-rays are absorbed by the air in the chamber, the air must be re-
moved to perform the analysis. With non-liquid samples the chamber is evacuated with
a vacuum pump. Since liquid samples vaporize in a vacuum, the air is displaced using
helium gas.
The hardware consists of a manifold with a pressure regulator, pressure switch, and two
solenoid valves mounted to it. The figure below is an illustration of the manifold. A hose
is attached between the manifold and the sample chamber wall to carry the helium. The
two valves are used to provide dual flow rates. When an analysis is started, a large
volume of air must be displaced from the sample chamber. A two-minute high flow, or
purge, cycle is initiated by the analysis program. After the two minute period, the high
flow valve turns off and the low flow valve turns on. Only a small flow is required during
the analysis to maintain the chamber environment.
The pressure regulator is used to provide a known, stable pressure inside the spec-
trometer regardless of the helium inlet pressure (within the specified limits). The flow
rates are then set by the manifold orifices. The pressure switch is used to detect a low
flow condition that would adversely affect the analysis performance. If the helium tank
runs out, the analysis program does not allow an analysis to begin or stops an analysis
already in progress and display a warning message.
Specifications
The helium flush option has the following specifications:
• Inlet fitting: ¼ inch hose barb
• Inlet pressure: 15 to 65 psig (103-448 kPa)
• Consumption (flow rate):
• high flow cycle - 15 SCFH (425 l/h)
• low flow cycle - 5 SCFH (142 l/h)
Fig. 8 - 1
Installation
Disregard this section if the option was installed at the factory. Otherwise, use the fol-
lowing steps to install the Helium Flush option.
1. Remove the detector assembly as detailed in the Detector Assemblies. This is
required to gain access to the chamber wall fitting.
2. Remove the brass hole plug from the chamber wall.
It is located next to the detector port opening.
3. Install the hose barb nipple in the chamber wall.
Use sealant on the threads.
4. Remove the six screws securing the AC Distribution box and slide box out.
This is required to gain access to the chamber wall fitting.
5. Remove the brass hole plug from the chamber wall.
It is located directly behind the AC distribution box.
6. Install the pressure relief valve in the chamber wall.
Use sealant on the threads.
7. Remove the vacuum/helium panel from the rear panel of the spectrometer.
This is the middle panel with the vacuum nipple. Allow the panel to hang from the
large vacuum hose.
8. Remove hole plugs and dummy screws as required from the panel and install the
helium manifold.
9. Remove the motherboard access panel from the back panel.
10. Connect the helium manifold cable to the motherboard J6 connector.
This is the white 6-pin connector located behind the large black J7 connector. Align
the connector locking ramps for proper orientation. Also check that it is not one pin
off (front to rear) as the connector has no protection against this.
11. Connect the small hose from the helium manifold to the hose barb fitting on the
sample chamber.
12. Reinstall the vacuum/helium panel.
Make sure the helium hose is not kinked.
13. Reinstall the detector assembly per procedure.
14. Run System Configuration and check the Helium check box.
15. Test the operation per Helium Flush.