Agilent 1100MSD GettingStarted
Agilent 1100MSD GettingStarted
Agilent 1100MSD GettingStarted
HP 1100 Series
LC/MSD System
Getting Started
Gsbook4pdf.fm Page 2 Thursday, May 14, 1998 8:45 AM
Item Description
Contents Displays the list of help topics
(shown to the right).
Index Lets you use keywords to
search the help index for a
particular topic.
Find Lets you type a word or phrase
and then displays a list of all
the topics in the online help
that contain those words.
Open Opens the selected book or help
topic. When you open a book or
select a book that is already
open, this button changes to Help Icons
Close.
Print Prints the selected book or help Indicates a book containing more help topics.
topic for future reference. If you To open a book, select it then double-click or
select a book, then all the help click the Open button.
topics contained in the book are
printed. To print a popup, click Indicates an open book of help topics. To close
on it with the right mouse an open book, select it then double-click or
button and select Print from click the Close button.
the menu.
Indicates a help topic. To jump to a help topic,
Cancel Closes the Help Topics window. select it then double-click or click the Open
button.
— 2 —
Gsbook4pdf.fm Page 3 Thursday, May 14, 1998 8:45 AM
ChemStation Views
The ChemStation software consists of several Verification (OQ/PV) View
views. The available items in the menus and In this view you can determine if your system is
toolbar depend on the current view. Each view operating in a predictable manner. This is useful
allows you to perform a certain set of tasks. to show Good Laboratory Practice (GLP)
compliance. This may be required by some
You can switch views using the View menu or by government agencies.
using the pulldown menu in the upper left corner
of the screen.
Diagnosis View
This view lets you run tests to diagnose
instrument problems and access information on
how to resolve these problems. The early
maintenance feedback (EMF) feature can be used
to notify you when it is time to perform system
maintenance before a problem occurs. Videos of
the various maintenance procedures are provided
on the LC/MSD maintenance CD-ROM.
Each view is briefly described below and on the
following pages. MSD Tune View
This view lets you calibrate your LC/MSD
Method and Run Control View automatically. You can also set parameters
manually for specific types of molecules.
In this view, you can set up methods and adjust
instrument parameters to inject samples and
acquire data one sample at a time or in
automated sequences.
— 3 —
Gsbook4pdf.fm Page 4 Thursday, May 14, 1998 8:45 AM
Method and Run Control View (configured with LC/MSD and DAD)
System
View Selection Title Bar Top Toolbar Diagram
Status Bar
Start/Stop Run
Sampling Diagram
Online Plot
Message Line
Method Overview
— 4 —
Gsbook4pdf.fm Page 5 Thursday, May 14, 1998 8:45 AM
— 5 —
Gsbook4pdf.fm Page 6 Thursday, May 14, 1998 8:45 AM
DAD Signal
LC/MSD Signal
Message Line
— 6 —
Gsbook4pdf.fm Page 7 Thursday, May 14, 1998 8:45 AM
— 7 —
Gsbook4pdf.fm Page 8 Thursday, May 14, 1998 8:45 AM
The following cursor tools are for manual Delete peaks from the calibration table
integration and working in the signal window:
Add peaks to the calibration table
Graphics tools (available in all tool sets)
Recalibrate peaks in the calibration table
Zoom in (available in all tool sets)
Set calibration table options
Zoom out (available in all tool sets)
Show/hide current chromatogram
Pointer tool (available in all tool sets)
Zoom in on MS window
Draw baseline
Extract ion chromatogram
Draw baseline for negative peaks
Hide extracted ion chromatogram
Tangent skim
Split peaks
— 8 —
Gsbook4pdf.fm Page 9 Thursday, May 14, 1998 8:45 AM
— 9 —
Gsbook4pdf.fm Page 10 Thursday, May 14, 1998 8:45 AM
View Selection Title Bar Calculation Technique Report Template Top Toolbar
Report Section
Insertion Triangle
Click a blue triangle to activate
the new section menu (triangle
turns red)
Message Line
— 10 —
Gsbook4pdf.fm Page 11 Thursday, May 14, 1998 8:45 AM
Template Description
SIMPLE.FRP Includes a chromatogram and calibration
curves per calibrated compounds.
NESTED.FRP Shows how to nest subsections.
SPECTRA.FRP Shows how to include spectra.
PURITY.FRP Shows how to include peak purity data.
ESTD.FRP Uses the same elements as the standard
Print Preview button
ESTD reports so you can customize your
external standard reports.
AREAPCT.FRP Uses the same elements as the standard
area percent report so you can customize
your area percent reports.
LIBRARY.FRP A customized report that uses library search
results. You must have a method loaded that
specifies the spectra library.
— 11 —
Gsbook4pdf.fm Page 12 Thursday, May 14, 1998 8:45 AM
System
View Selection Title Bar Verification Toolbar Diagram
Status Bar
Start/Stop Run
Sampling Diagram
Online Plot
Message Line
Method Overview
— 12 —
Gsbook4pdf.fm Page 13 Thursday, May 14, 1998 8:45 AM
Verification Toolbar
Print a report of the current
The Verification Toolbar, which is located at the instrument verification results.
top of the Verification screen, is displayed when
you select Show Top Toolbar from the View menu.
About This View
Set up a new verification. The Verification (OQ/PV) view lets you test
whether your analytical instruments and the
ChemStation software are operating correctly
according to predefined performance criteria.
Load a previously-stored instrument
verification. • Operation Qualification (OQ)
Operation Qualification is the documented
verification that the equipment-related
Save the current instrument
verification to disk. system or subsystem performs as intended
throughout representative or anticipated
operating ranges.
Edit the current instrument • Performance Verification (PV)
verification.
Performance Verification is the documented
verification that the process and or the total
Run the current instrument process-related system performs as intended
verification. throughout all anticipated operating ranges.
Available Tests
Toggle the display of the Verification
The following verification tests are supplied with
Logbook.
your ChemStation software. Refer to the online
help for more information on how to run, edit, or
Toggle the display of the current create new verification tests.
online Logbook.
o VWD Wavelength Accuracy
o Intensity
Toggle the display of the current o Holmium
Sequence Logbook. o Temperature Accuracy
o Noise, Flow, Temperature
o DAD Wavelength Accuracy
Display the Instrument Verification
o Injector Precision*
Test Report.
o Detector Linearity/Carry-over*
o Injector Linearity*
o Gradient Composition
* These tests can be used to verify LC/MSD performance.
— 13 —
Gsbook4pdf.fm Page 14 Thursday, May 14, 1998 8:45 AM
Diagnosis View
Instrument Panel
Variables Display
Message Line
Help
Link to Maintenance
CD-ROM
— 14 —
Gsbook4pdf.fm Page 15 Thursday, May 14, 1998 8:45 AM
Status Bar
Message Line
— 15 —
Gsbook4pdf.fm Page 16 Thursday, May 14, 1998 8:45 AM
APCI
— 16 —
Gsbook4pdf.fm Page 17 Thursday, May 14, 1998 8:45 AM
— 17 —
Gsbook4pdf.fm Page 18 Thursday, May 14, 1998 8:45 AM
— 18 —
Gsbook4pdf.fm Page 19 Thursday, May 14, 1998 8:45 AM
To Use Deconvolution
Deconvolution is a process that transforms 8 You can look at individual components or
mass spectra from multiply-charged ions into a groups of components by selecting specific
calculated molecular weight. components from the Component list.
— 19 —
Gsbook4pdf.fm Page 20 Thursday, May 14, 1998 8:45 AM
Operating Tips
❏ Back up your data and methods regularly to ❏ Use only filtered, HPLC-grade mobile phase.
avoid loss of data if the files are accidentally
overwritten, deleted, or if a hardware problem ❏ If a UV detector is available, use it in series
develops with your disk drive. with the LC/MSD. Try to minimize
chromatographic peak broadening by using
❏ Put the system in standby mode overnight or low dispersion tubing.
whenever you won’t be analyzing samples for
an extended time. ❏ To avoid chromatographic band broadening,
make sure all tubing connections are free of
❏ Make sure the tune file you are using is dead volume. Use zero dead-volume (ZDV)
appropriate for your samples. fittings when possible. If using fingertight
fittings, force tubing into unions and tees
❏ Save Tune reports in an MS Logbook for while tightening the fittings.
future reference.
❏ Use the following table as a guide to using
❏ Regular system maintenance can reduce SIM, condensed scan, and full scan
problems. Maintenance tasks are described acquisition modes.
on the HP 1100 Series LC/MSD Maintenance
CD-ROM. Keep a maintenance record. Task Mode
❏ Flush the sample path and clean the spray Analyze a mixture with known Scan or SIM
components in unknown amounts
chamber, capillary tip, and spray shield daily (quantitate).
or at the end of each shift. Check the pump
fluid level every week. Identify the presence of a few known SIM
compounds at low levels within a
mixture.
❏ The spray chamber vent hose must be
connected to a lab vent that is used only for
the source (completely separate from the ❏ If you are using APCI, the optimal flow rate is
vent hose for the foreline pump). Otherwise, 1.0 ml/min. The range is 0.5 to 1.5 ml/min.
waste products can migrate into the spray
chamber vent producing chemical noise.
— 20 —
Gsbook4pdf.fm Page 21 Thursday, May 14, 1998 8:45 AM
Troubleshooting Tips
No peaks High spectral noise
o Make sure there is spray from the nebulizer. o Use appropriate mass filter values.
o Make sure the capillary voltage is set correctly. o Check the spray shape. Nebulizer may be
damaged or incorrectly set.
o Make sure the LC/MSD is tuned correctly.
o Make sure drying gas flow and temperature are
o Make sure LC/MSD pressures are within normal correct for the solvent flow you are using.
ranges.
o Make sure the solvent is thoroughly degassed.
o Check the drying gas flow and temperature. Do not use ultrasonic degassing with protein
o Make sure the fragmentor is set correctly. samples.
o Make sure the LC backpressure is steady; this
Poor mass accuracy indicates a steady solvent flow.
o Recalibrate the mass axis. o If you are using water as part of the mobile
phase, make sure it is de-ionized (>18MΩ).
o Make sure the ions used for tuning span the
mass range of the sample ions and that they
show strong, stable signals. Droplets, not spray, exiting the nebulizer
o Make sure the nebulizing gas pressure is set
Low signal high enough for the LC flow being used.
o Check the solution chemistry. Make sure the o Check the position of the needle in the nebulizer.
solvent you’re using is appropriate for your o Stop the solvent flow and remove the nebulizer
sample. Mixed samples can exhibit signal assembly. Use a magnifying glass to examine
suppression of one or more components. the end of the nebulizer for damage.
o Make sure the sample is fresh and has been
stored correctly. No flow
o Make sure the LC/MSD is tuned correctly. o Make sure the LC is on and there is sufficient
o Check the nebulizer condition. solvent in the correct bottle.
o Clean the capillary entrance. o Check for LC error messages.
o Check the capillary for damage and o Check for blockages. Repair or replace any
contamination. blocked components.
o Check for leaks.
Unstable signal o Make sure the MS stream selector valve is set
to LC to MSD.
o Make sure the drying gas flow and temperature
are correct for the solvent flow you are using.
Undesired fragmentation
o Make sure the solvent is thoroughly degassed.
Do not use ultrasonic degassing with protein o Fragmentor is set too high.
samples. o Ionization is causing fragmentation (APCI vs.
o Make sure the LC backpressure is steady; this Electrospray).
indicates a steady solvent flow. o APCI temperature is too high.
— 21 —
Gsbook4pdf.fm Page 22 Thursday, May 14, 1998 8:45 AM
HP 1100 Series LC
Solvent bottles
Solvent cabinet
Vacuum degasser
Pump
Control module
(optional)
Autosampler
Column
compartment
LC Detector
(DAD or VWD)
— 22 —
Gsbook4pdf.fm Page 23 Thursday, May 14, 1998 8:45 AM
LC Cabling
Remote cable
AC power
Analog signal
to recorder
HP-IB to ChemStation
— 23 —
Gsbook4pdf.fm Page 24 Thursday, May 14, 1998 8:45 AM
— 24 —
Gsbook4pdf.fm Page 25 Thursday, May 14, 1998 8:45 AM
Corona needle
— 25 —
Gsbook4pdf.fm Page 26 Thursday, May 14, 1998 8:45 AM
Electronics cabinet
MS selection valve
Vacuum manifold
Electrospray nebulizer
Nitrogen inlet
Electrospray
spray
chamber
Pressure
sensor
Manual injection
valve
LC inlet
Calibrant delivery system
— 26 —
Gsbook4pdf.fm Page 27 Thursday, May 14, 1998 8:45 AM
Calibrant delivery
system gas (N2)
LC tubing
Remote start
Network cable
Spray chamber
high voltage
HP-IB cable
Calibrant delivery
system control
Drain tubes
Foreline pump
power cord Foreline hose
LC/MSD
power cord
— 27 —
Gsbook4pdf.fm Page 28 Thursday, May 14, 1998 8:45 AM
Electronics cabinet
MS selection valve
Nitrogen inlet
APCI spray
chamber
Pressure
sensor
Manual injection
valve
(optional)
LC inlet
Calibrant delivery system
— 28 —
Gsbook4pdf.fm Page 29 Thursday, May 14, 1998 8:45 AM
Calibrant delivery
system gas (N2) Nebulizing gas
LC tubing
Remote start
Network cable
Spray chamber
high voltage
HP-IB cable
Calibrant delivery
system control
Drain tubes
Foreline pump
power cord Foreline hose
LC/MSD
power cord
— 29 —
Gsbook4pdf.fm Page 30 Thursday, May 14, 1998 8:45 AM
Chemical Consumables
Calibrant, Electrospray G2421A
Calibrant, APCI G2422A
Evaluation Sample, APCI Negative Mode G2425A
Evaluation Sample, ES Negative Mode G2424A
Evaluation Sample, Positive Mode G2423A
Myoglobin Standard (Multiply-charged) G2426A
OQ/PV Chemical Kit (Caffeine) 8500-6917
Instrument Consumables
Capillary G1946-80009
Corona Needle, APCI G2429A
Electron Multiplier Replacement Horn 05971-801
Ferrule, Nebulizer Needle G1946-20213
Fitting, F120 (Fingertight PEEK Fitting) 0100-1920
Front Capillary Bal Seal, 1/4” ID 0100-1516
Manual Sample Injector 0905-1475
Nebulizer Needle, Electrospray 0101-0941
Nebulizer Needle, APCI G2427A
Nitrogen Gas Conditioner G1946-80047
Tubing (PEEK) 0.005” ID, 1/16” OD 5182-3441
Vacuum Pump Fluid 0890-1915
6040-0834
General Supplies
Abrasive Mesh (micro-grit paper) 8660-0852
Cloth, Clean 05980-60051
Nitrile Rubber Glove, Medium 9300-1751
— 30 —
Gsbook4pdf.fm Page 31 Thursday, May 14, 1998 8:45 AM
Safety Warnings
Intended Purpose Safety Symbols
Use of the HP 1100 Series LC/MSD in a manner
not intended by the manufacturer is prohibited.
; Refer to operating instructions.
+
The HP 1100 Series LC/MSD is a Safety Class 1
instrument and has been designed and tested in Indicates hot surfaces.
accordance with IEC Publication 1010-1, Safety
Requirements for Electrical Equipment for
Measurement, Control, and Laboratory Use. 3 Indicates earth (ground) terminal.
Stack Configuration WA RN IN G
Connecting the LC/MSD to a power source that is not
WA RN IN G equipped with a protective earth contact creates a
While it is possible to stack the HP 1100 Series LC shock hazard for the operator and can damage the
modules on top of the LC/MSD without damaging it, instrument. Likewise, interrupting the protective
this arrangement is potentially unstable and dangerous conductor inside or outside the LC/MSD or
and is not recommended. disconnecting the protective earth terminal creates a
shock hazard for the operator and can damage the
instrument.
Placing the LC modules on top of the LC/MSD is
also inconvenient. It puts the solvent bottles
and some LC controls out of easy reach and
requires the LC stack to be disassembled and
WA RN IN G
removed for LC/MSD maintenance.
Any adjustment, maintenance or repair of the opened
instrument while it is connected to a power source
should be avoided and, if required, should be performed
WA RN IN G only by trained persons who are aware of the hazards
Nitrogen is the only acceptable drying and nebulizer gas. involved.
Use of air, oxygen, or other gases, when combined with
solvents and high voltages in the spray chamber, could
result in an explosion.
WA RN IN G
The power switch on the front of the LC/MSD does not
completely cut power to the instrument. You must also
turn off the main circuit breaker and disconnect the
power cord before performing maintenance on the
electronics or turbo controllers.
— 31 —
Gsbook4pdf.fm Page 32 Thursday, May 14, 1998 8:45 AM
H
Document History
*G1946-90035*
*G1946-90035*
Copyright © 1998
Manual Part Number Hewlett-Packard Company
G1946-90035 Printed in U.S.A. 5/98