Agilent Gcms
Agilent Gcms
GC AND GC/MS
AGILENT PARTS AND SUPPLIES
Maintenance Schedule
Every
Task Every week 6 months Every year As needed
Tune the MSD 3
Change injection port liners 3
Check the foreline pump oil level 3
Gas ballast the foreline pump 3
Check the calibration vial 3
Replace the foreline pump oil 3
Check the diffusion pump fluid 3
Replace the diffusion pump fluid 3
Replace the dry pump tip seals (IDP3) 3
Replace the traps and filters 3
Clean the ion source 3
Replace worn out parts 3
Lubricate seals (where appropriate) 3
Replace column 3
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AGILENT PARTS AND SUPPLIES
MSD Contamination
Contamination is usually identified by excessive background in the mass spectra, which can come from
the GC or MSD. The source of contamination can sometimes be determined by identifying the
contaminants. Some contaminants are much more likely to originate in the GC, while others are likely
to originate in the MSD.
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AGILENT PARTS AND SUPPLIES
Air Leaks
Air leaks are a problem for any instrument that requires a vacuum to operate. Leaks are generally caused by
vacuum seals that are damaged or not fastened correctly.
Symptoms of leaks
• Higher than normal vacuum manifold pressure or foreline pressure
• Higher than normal background
• Peaks characteristic of air (m/z 18, 28, 32, and 44 or m/z 14 and 16)
• Poor sensitivity
• Low relative abundance of m/z 502 (this varies with the tune program and MSD used)
Remedy
• Check interface nut for tightness. Replace if necessary.
• Check and leak test the GC injection port.
Leaks can occur in other places in the MSD, including the following:
• GC/MSD interface column nut
• Side/top plate O-ring (all the way around)
• Vent valve O-ring
• Calibration valve
• High vacuum gauge tube/controller fitting
• Cracked ion gauge tube
• Front and rear end plate O-rings
• GC/MSD interface O-ring (where the interface attaches to the vacuum manifold)
• Diffusion pump co-seal
• Baffle adapter O-ring
• Turbomolecular pump O-ring
• Polyimide/graphite ferrules, when heated
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AGILENT PARTS AND SUPPLIES
Cleaning Solvents
It is common to see cleaning solvent peaks in the mass spectra shortly after the ion source is cleaned.
Remedy
• Dry all cleaned metal parts in the GC oven before reassembling and reinstalling them.
Refer to specific cleaning procedures in your MSD Hardware Manual or MSD Maintenance
and Troubleshooting Manual.
• Use a temperature above the boiling point of the solvent but below the limit of the column.
Fingerprints
Fingerprints contain hydrocarbons that can appear in mass spectra. Hydrocarbon contamination is
characterized by a series of mass peaks 14 m/z apart. The abundance of these peaks decrease as peak
mass increases. Fingerprint contamination is usually caused by the failure to wear clean, nylon gloves
during ion source handling or cleaning, GC inlet maintenance, or from installing the column. Use special
care to avoid recontamination of parts after you clean them. This typically occurs after some maintenance
or part replacement.
Remedy
Reclean using clean, nylon gloves and proper cleaning techniques.
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AGILENT PARTS AND SUPPLIES
Common Contaminants
Ions (m/z) Compound Possible Source
13, 14, 15, 16 Methane CI gas
18, 28, 32, 44 or 14, 16 H20, N2, O2, CO2, CO2 or N, O Residual air and water, air leaks,
outgassing from Polyimide ferrules
31, 51, 69, 100, 119, 131, 169, PFTBA and related ions PFTBA (tuning compound)
181, 214, 219, 264, 376, 414,
426, 464, 502, 576, 614
31 Methanol Cleaning solvent
43, 58 Acetone Cleaning solvent
78 Benzene Cleaning solvent
91, 92 Toluene or xylene Cleaning solvent
105, 106 Xylene Cleaning solvent
151, 153 Trichloroethane Cleaning solvent
69 Foreline pump fluid or PFTBA Foreline pump oil vapor or
calibration valve leak
73, 147, 207, 221, 281, 295, Dimethylpolysiloxane Septum bleed or methyl silicone
355, 429 column coating
77, 94, 115, 141, 168, 170, 262, Diffusion pump fluid Diffusion pump fluid
354, 446 and related ions
149 Plasticizer (phthalates) Vacuum seals (O-rings) damaged
by high temperatures, use of vinyl
or plastic gloves
Peaks spaced 14 amu apart Hydrocarbons Fingerprints, foreline pump oil
The easiest way to insure that you minimize background contamination and remove damaging oxygen from
your carrier gas system is to use a carrier gas purifying trap right before the gas enters your GC system.
Column bleed generally appears as a continuous and increased rise in the baseline at higher column
temperatures, especially at or near the upper temperature limit of the GC column. Septum bleed usually
appears as discrete peaks, and can occur at any temperature.
A crude sign of a "leak-free" MS system is when the ion ratio of m/z 28 (nitrogen) over m/z 32 (oxygen)
is approximately two or greater.
Even preconditioned ferrules can shrink slightly at very high temperatures. If leak problems persist upon
a new column installation, check this fitting first.
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AGILENT PARTS AND SUPPLIES
(Continued)
Cloths, lint-free, 05980-60051
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AGILENT PARTS AND SUPPLIES
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AGILENT PARTS AND SUPPLIES
By using tools, supplies and best practices that provide a leak-free GC or GC/MS, analysts can improve
performance and productivity of their system. The Agilent innovative Self Tightening column nuts using
standard short polyimide/graphite ferrules eliminate the need to retighten GC column fitting at the mass
spec transfer line, even after repeated heat cycling. Agilent UltiMetal Plus Flexible Metal ferrules provide
robust leak-free column connections, along with an inert surface for fittings in the sample flow path.
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AGILENT PARTS AND SUPPLIES
Ion Source
The ion source operates by electron ionization (EI) or chemical ionization (CI). The sample enters the ion
source from the GC/MSD interface. Electrons emitted by a filament enter the ionization chamber, guided by
a magnetic field. The high-energy electrons interact with the sample molecules, ionizing and fragmenting
them. The positive voltage on the repeller pushes the positive ions into the lens stack, where they pass
through several electrostatic lenses. These lenses concentrate the ions into a tight beam, which is directed
into the mass filter.
Electron Impact (EI) Ion Source
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AGILENT PARTS AND SUPPLIES
Preparing to Clean
Prior to cleaning, the mass spectrometer must be vented and the ion source must be removed.
Before venting the system, the following conditions must be met:
• Heated zones are less than 100 °C
• The diffusion pump is off and cool (if applicable)
• The turbo pump is off and not spinning (if applicable)
• The rough pump is off
Always allow the automatic venting routine to run its full course. Improper venting may cause diffusion
pump fluid to be deposited into the analyzer (backstreaming). It can also reduce the life of the multiplier
or other sensitive MS parts.
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AGILENT PARTS AND SUPPLIES
Aperture Diameters Availabe for the Agilent 5977A Series Ion Sources
Aperture Diameter 3 mm 6 mm 9 mm
Stainless Steel Source 05971-20134 G3136-20530 --
Inert Source G2589-20100 G2589-20045 --
Extractor EI Source G3870-20444 G3870-20448 G3870-20449
Having trouble selecting the appropriate aperture diameters for the Agilent 5977A Series Ion Sources? Download publication
number 5991-2106EN at www.agilent.com/chem/library
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AGILENT PARTS AND SUPPLIES
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AGILENT PARTS AND SUPPLIES
EI Tune Options
In the Tune menu, and in the Tune and Vacuum Control view there are several options for tune selection.
The top two options are mechanisms to run part or the entire active tune. The remaining menu options are
tunes for specific purposes and are described below.
Description of the Tune Options for the Agilent 5977A Series Ion Source
Tune menu items
(default tune filenames as *.U) Description
Tune MSD Performs the type of tune that is embedded in the active tune.
QuickTune Provides a fine tuning to ensure acceptable response, resolution and accurate mass assignment.
Autotun (Atune.U) The standard repeller-based tune of the Agilent 5973 inert MSD and Agilent 5975 Series.
Extraction source tune (Etune.U) Used with the Extractor EI Source to provide the highest sensitivity. Equivalent to Atune when used with inert
or stainless sources.
BFB Autotune (BFB_Atune.U) Used in conjunction with Atune to meet US EPA BFB tuning criteria. Requires the use of 6 mm drawout/extraction lens
and operates in standard repeller-based tuning mode.
Low Mass Autotune (Lomass.U) Identical to Autotune, except it tunes on masses 69, 131, and 219 instead of 69, 219, and 502. Intended for low
molecular weight applications and natural gases under 250 daltons.
Standard Spectra Tune (Stune.U) Ensures standard response over the full mass range. Specifically, PFTBA mass 69 is the base peak, mass 219 is between
35 and 99%, and mass 502 is >1%. This is a lower sensitivity tune used to better match legacy libraries created using
the Agilent 5971 or 5972 MSDs.
DFTPP A specific target tune used for US EPA semivolatile analyis (8270 methods).
BFB A specific legacy target tune used for VOC analysis. It does not provide the same sensitivity and stability
as BFB Autotune. Provides continuity for established SOPs and for users with a preference for target tuning.
See Application Note 5991-0029EN for a description of the recommended procedure for VOC analysis at
www.agilent.com/chem/library
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AGILENT PARTS AND SUPPLIES
10
9
1 11
5
6
4
7
14 13
Lens insulator, G3170-20530 2 12
17
8
3
16
15
14
12
14
2
2
14
7
Repeller insulator, G1099-20133
2
EI Ion Source Parts
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AGILENT PARTS AND SUPPLIES
10
9
1 11
5
6
4
7
14 13
2 12
8
3
16
15
14
12
14
2
2
14
7
2
5977/5975/5973 Inert Ion source parts (EI)
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AGILENT PARTS AND SUPPLIES
Extractor EI Source
This innovative ion source has an extractor lens in place of the drawout plate used in the other EI sources
and it is made of an inert material. It is programmable up to 350 ºC to deliver enhanced response for active
compounds and late eluters. These unique features provide maximum, ultratrace level sensitivity for a wide
variety of compounds. The extractor lens provides additional focus to the ion beam into the mass analyzer.
A potential is applied to the extractor lens which pulls the ions out of the ionization chamber, adding to the push
Extractor EI Source provided by the repeller voltage. The result is a significant increase in the number of ions analyzed, improving
the true sensitivity of the instrument. There are three available aperture sizes for the Extractor EI Source, as well
as the two other sources: 3, 6, and 9 mm. Generally, the 3 mm aperture provides the best sensitivity. Selecting
one of the larger aperture sizes enables analysis of higher concentrations of target compounds. Increasing
aperture diameters also reduces the residence or interaction time and provides higher effective inertness for
fragile compounds.
The Extractor EI Source can be operated in the higher sensitivity mode of extraction tuning or in standard mode
in which it behaves in the same way as the standard stainless and inert sources. The ability to change between
extractor and repeller-only mode is controlled by the software and does not require any physical changes.
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AGILENT PARTS AND SUPPLIES
9
8
1 10
4
5
6
7 12
2
17 11
16
1*
14 13
15
11*
7*
2* 18
7*
2*
6*
7*
2*
Extractor Ion Source Parts
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9
5
11
6
1
7
10
13
12
2 4
8
3
14
2
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Analyzer chamber
MSD GC
EI Transfer Line
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AGILENT PARTS AND SUPPLIES
MSD Filaments
Like the filaments in an incandescent light bulb, the ion source filaments will eventually burn out.
Certain practices will reduce the chance of early failure.
• When setting up data acquisition parameters, set the solvent delay so that the analyzer
will not turn on while the solvent peak is eluting
• When the software prompts 'Override solvent delay at the beginning of a run' always select 'No'
• Higher emission current will reduce filament life
• If you control your MSD from the Edit Parameters screen, always select 'MS Off' before changing
any of the filament parameters
MSD Filaments
Description 7200 Series 7000 Series 5977 Series 5975 Series 5975T Series 5973 Series
Filament assembly, high temperature (EI) G7005-60061 G7005-60061 G7005-60061 G7005-60061 G7005-60061 G7005-60061
Filament assembly (CI), 2/pk G7005-60072 G7005-60072 G7005-60072 G7005-60072 G7005-60072
Micro ion vacuum gauge G3170-80001 G3170-80001 G3170-80001 G3170-80001
Triode gauge tube for measuring vacuum 0960-0897
Ion gauge controller G3397B G3397A G3880-80010
Ion gauge tube G3880-80011
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AGILENT PARTS AND SUPPLIES
CI Valve Supplies
Item Description Unit Part No.
1 PFDTD calibrant, for GC/MS, perfluoro-5,8-dimethyl-3, 6,9-trioxidodecane 1 mL 8500-8510
2 CI Cal valve assembly G1999-60452
3 Certified non-stick fluorocarbon O-ring 10/pk 5188-5365
4 5975 Calibrant bulb G3170-80002
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AGILENT PARTS AND SUPPLIES
Gas Filters
Description Part No.
Replacement Agilent Gas Clean carrier gas filter, Chemical ionization gas purifier G1999-80410
CP17973 Gas Clean carrier gas starter kit for 7890 CP17988
Replacement Agilent Gas Clean carrier gas filter CP17973
Big universal trap, 1/8 in fittings, nitrogen, for 7000 and 7200 Series RMSN-2
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