GC and GCMS Fundamentals of Instrument Troubleshooting and Maintenance. Kirk Lokits Ph.D. Applications Chemist
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1 GC and GCMS Fundamentals of Instrument Troubleshooting and Maintenance Kirk Lokits Ph.D. Applications Chemist August 1, 2016
2 A with Oscilloscope and Strip Chart Timeline: Intel introduces first microprocessor, 4004 IBM introduces 8 floppy disk Page 2
3 Page B/7890B with Sampler Tower and Tray
4 Everything was just fine and then this happened! How do I go about TROUBLESHOOTING? Page 4
5 Everything was just fine and then this happened! Logic = Something changed (slowly or sudden) = Something is different Track Events log book -Changed column, liner, septum, syringe, etc. -Injected samples, other method, etc. -Did maintenance, cut column, inlet flush, etc. Page 5
6 Logical Troubleshooting Troubleshooting Starts with Isolating the problem There are 5 basic areas from where the problem arises FLOW INJECTOR COLUMN DETECTOR ELECTRONICS But of course it can always be some COMBINATION Knowing what can & can t cause the symptom is the key Page 6
7 Typical Problems of Optimized Methods becoming Unoptimized and the Reason Why. Column Installation Correct Process Peak Tailing Flow Path or Activity Bonus Peaks In Sample or Back Flash (Carry Over) Split Peaks Injector Problems, Mixed Solvent No Peaks Wasn t Introduced, Wasn t Detected Response Changes Activity, Injector Discrimination, Detector Problem Peak Fronting Overload or Solubility Mismatch, Injector Problems Shifting Retention Leaks, Column Aging, Contamination or Damage Loss of Resolution Separation Decreasing, Peak Broadening Baseline Disturbances Column Bleed, Contamination, Electronics Noisy or Spiking Baseline Electronics or Contaminated Detector Quantitation Problems Activity, Injector or Detector Problems Page 7
8 Column Installation Procedure Install the column Leak and installation check Column conditioning Bleed profile Test mix Page 8
9 Column Installation What type of ferrule should I use? Graphite Graphite/Vespel Page 9
10 Self Tightening Column Nuts For inlet or detector p/n For mass spec transfer line p/n Page 10
11 What to Use When? Application Requirement Ease of Use - finger tighten / no wrench Inertness for active analytes Installed or used hardware Self Tightening Column nut with short Graphite/Polyimide blend ferrule x x UltiMetal Plus Flexible Metal ferrule Same style ferrule at inlet and MS interface x High temp above 350 x Mass Spec Interface fitting x Capillary Flow Technology device x Pre-swage for precise height into fitting x x Re-use of ferrule x x Page 11
12 Solving Shrinking Ferrule Syndrome Page 12
13 Column Installation Measuring the right distance White out Septa Page 13
14 Cutting The Column Gently scribe through the polyimide coating. Do not attempt to cut the glass. Recommended tools: Diamond or carbide tipped pencil; or sapphire cleaving tool, ceramic wafer Ocular Do not use: Scissors, file, etc. Page 14
15 Page 15 Example of a Bad Cut
16 Examples of Column Cuts Bad Good Page 16
17 Column Installation How tight is tight? Page 17
18 Page 18 Overtightened Ferrule
19 Column Installation Leak Check DO NOT USE SNOOP Electronic leak detector IPA/Water (50:50) Inject a non-retained peak Page 19
20 Leak and Installation Check Inject a non-retained compound vs DB-1 Detector FID Compound Methane or Butane ECD MeCl 2 (headspace or diluted) NPD TCD MS CH 3 CN-acetonitrile (headspace or diluted) Air Air or Butane The peak should be sharp and symmetrical Page 20
21 Non-Retained Peak Shapes Good Installation Improper Installation or Injector Leak Check for: -Too low of a split ratio -Injector or septum leak -Liner problem: (broken, leaking, misplaced) -Column position in injector and detector Page 21
22 Column Conditioning System must be leak free before conditioning column Heat the column to the lower of: Isothermal maximum temperature OR 20 to 30 C above highest operation temperature Temperature programming is not necessary Stop conditioning when the stable baseline is obtained: 1 to 2 hours in most cases Page 22
23 Generating a Bleed Profile Temperature program the column without an injection* 1.3e4 1.2e4 1.1e4 1.0e Time (min.) *DB-1 30m x.32mm I.D.,.25µm Temperature program // 40 C, hold 1 min // 20 /min to 320 C, hold 10 min. Page 23
24 Peak Tailing INJECTOR or COLUMN is Active -Reversible adsorption of active compounds (-OH, -NH, -SH) FLOW problem - dead volume, obstruction, poor installation, or severe column contamination Miscellaneous - co-elution, polarity mismatch between phase, solute or solvent, and some compounds always tail *Tip = Inject a light hydrocarbon, should not tail unless flow path problem. Page 24
25 Bonus Peaks or Ghost Peaks Contamination in INJECTOR, COLUMN or FLOW (carrier gas) -Carry-over from a back flash or previous sample -Bad tank of gas or traps have expired -Septum bleed *TIP = Run a blank run it should be blank! Page 25
26 Ghost Peaks Back flash Back flash occurs when vapor condenses on a cooler part of the injector. This condensed sample will still have a headspace which can be swept forward to the column and cause ghost peaks. Page 26
27 Ghost Peaks Steps to Prevent Backflash Reduce injection volume Lower inlet temperature Consider a large volume liner Pressure pulse the injection (if possible) Change solvents Page 27
28 Split Peaks INJECTOR (poor sample introduction) -Injecting the sample twice (some how?) -Mixed sample solvent (polarity difference) -Sample in syringe needle (manual inject) INJECTOR (activity) -Breakdown (not really a split peak, 2 peaks) -Sample degradation in injector VOLATILITY High boilers dropping out on Cold Spots -Transfer line temps -Unions or fittings not tracking column temp Page 28
29 Logical Troubleshooting Tips Look and Ask Which peaks? Early or late? Trends? = Injection technique - erratic Page 29
30 No Peaks DETECTOR (not on or not operational) INJECTOR (not working) -Plugged syringe/plunger not moving -Wrong injector (or detector) -Huge leak (older systems) -No carrier gas flow NOT the COLUMN Unless -Broken column or No column Page 30
31 30 A Real Troubleshooting Example No Peaks Page 31
32 Is the flame Lit? put glass piece over FID outlet----answer in this case, Water condensation look at output in instrument gauge-- is the digital value greater than 0.0? Answer in this case is approximately 16.2 pico amps Is there flow through the column? Logical Steps Taken to Find Peaks (most of our problems are leaks and plugs) disconnect column from detector and measure flow with a meter Answer in this case was YES THERE IS FLOW Assess the observations Flame is lit and we have flow from end of column Hypothesis: Sample not getting on column-syringe plugged? Take syringe out and make injection manually on a dry paper towel Answer towel stays dry (Syringe was clogged with septum) Pull plunger out top, add solvent and replace plunger will usually dislodge septum particle (should hear a little pop) If you can t dislodge plug, Replace syringe Reassemble the Injector & Re-inject Page 32
33 Peak Response All Change in Size INJECTOR -Leaky syringe -Split ratio set incorrectly -Wrong purge activation time -Septum purge flow too high -Injector temperature too low* DETECTOR (response problem) -Settings or flows changed -Electronics failing *Tip = Is it all of them or some of them, if all then injector or detector Page 33
34 Peak Response Some Change in Size INJECTOR or COLUMN is active/contaminated -Irreversible adsorption of active compounds (-OH, -NH, -SH) -Decomposition of sample -Temperature Change Discrimination -Evaporation from sample *Tip = If only some change, then which ones? If active compounds then activity. If tracks volatility then cold spots or inlet discrimination. Page 34
35 Peak Fronting Shark Fin Shaped or Just Slight COLUMN (contaminated) -Overload (More pronounced with large solute and phase polarity differences) INJECTOR -Column installation -Compound very soluble in injection solvent (need retention gap) -Mixed sample solvent OTHER -Co-elution -Breakdown Page 35
36 Retention Time Shift INJECTOR -Leak in the septum -Change in injection solvent -Large change in sample concentration FLOW -Change in gas velocity COLUMN -Contamination -Damaged stationary phase -Loss of stationary phase -Change in temperature Page 36
37 Effect of Sample Overload on Retention Time and Peak Shape 1400 ng 7 ng min Page 37
38 Loss of Resolution Separation Peak Width Resolution is a function of separation and peak width Page 38
39 Loss of Resolution - Separation Decrease COLUMN -Different column temperature -Contamination (more phase?) Separation -Matrix components co-eluting -Different column phase? Peak Width Page 39
40 Loss of Resolution - Peak Broadening FLOW -Change in carrier gas velocity -Make-up gas Separation COLUMN -Contamination -Phase degradation Peak Width INJECTOR (efficiency) -Settings, Liner, Installation, etc. Page 40
41 Baseline Disturbances Sudden Changes, Wandering, or Drifting WANDER DRIFT COLUMN or DETECTOR -Not fully conditioned or stabilized (electronics) -Contamination FLOW -Changes in carrier and/or detector gas flows -Valves switching, leaks Page 41
42 Noisy Baseline MILD SEVERE FLOW -Contaminated gas -Incorrect detector settings COLUMN -Bleed if at high temperature -In detector flame (poor installation) DETECTOR -Air leak - ECD, TCD -Electronics malfunction Page 42
43 Spiking Baseline DETECTOR -Particles entering the detector -Random: poor connection -Regular: nearby "cycling" equipment (electronics) Page 43
44 Quantitation Problems DETECTOR -Poor stability (electronics) or Baseline disturbances (contamination) -Outside detector's linear range or wrong settings Activity (adsorption) in INJECTOR or COLUMN INJECTOR -Technique, settings, conditions -Syringe worn OTHER -Co-elution -Matrix effects -Sample evaporation leaky vials -Sample decomposition Page 44
45 TROUBLESHOOTING TOOLS Bleed Profile: baseline problems Inject a non-retained peak: peak shape problems Test mix: all problems Isolate the components: all problems Jumper Tube Test: baseline problems Static Pressure Test: check for leaks Page 45
46 GENERATING A BLEED PROFILE 1.3e4 1.2e4 Use when the column is new (for future reference) or there is a baseline problem 1.1e4 1.0e *DB-1 30m x.32mm I.D.,.25µm Temperature program // 40 C, hold 1 min // 20 /min to 320 C, hold 10 min Time (min.) Page 46
47 NON-RETAINED PEAK SHAPES Used to Check Flowpath Good Installation Improper Installation or Injector Leak Potential problems: Injector or septum leak Too low of a split ratio Liner problem (broken, leaking, misplaced) Column position in injector and detector Page 47
48 Test Mixes Used to determine how "good" the column is #1 Page 48
49 Column Performance Summary PART NO: COLUMN I.D. NO.: LIQUID PHASE: FILM THICKNESS: DB µm COLUMN DIMENSIONS: 30 m X mm TEMPERATURE LIMITS: -60 C TO 325 C ( 350 C PROGRAM) COMPOUND IDENTIFICATION 1,6-HEXANEDIOL 4-CHLOROPHENOL METHYL NONANOATE 4-PROPYLANILINE RETENTION TIME (T R) PARTITION RATIO (k) PEAK WIDTH (W 1/2) THEORETICAL PLATES/METER: PENTADECANE MIN SPEC ACTUAL TRIDECANE 1-UNDECANOL COATING EFFICIENCY: PENTADECANE RETENTION INDEX: MIN SPEC MAX SPEC ACTUAL ACENAPHTHYLENE PENTADECANE UNDECANOL ACENAPHTHYLENE PEAK HEIGHT RATIO: 4-CHLOROPHENOL/ METHYL NONANOATE 0.83 Approximately 5-10 ng on column 4-PROPYLANILINE/ METHYL NONANOATE 1.14 (t o) 1.29 Page 49
50 TEST MIX Used to determine how good the column is or if the problem is related to the chemical properties of the analytes. TEST TEMPERATURE: 135 C cm ml CARRIER GAS: (H 2) 38.7 sec ( 1.2 min ) INJECTION: SPLIT ANALYST: ERIK Max. Bleed 10.0 pa pa RETENTION TIME (MIN) Page 50
51 Test Mixture Components Compounds Hydrocarbons FAME s, PAH s Alcohols Acids Bases Purpose Efficiency Retention Retention Activity Acidic Character Basic Character Page 51
52 Own Test Mixture More specific to your application Selective detectors Concentrations specific to your application Use same instrument conditions Easiest to simply inject a calibration standard Store for future measure of column performance Page 52
53 ISOLATE THE COMPONENTS Put in a known good column Move column to a different GC, inlet or detector Simplify the system: example - Direct injection instead of P&T sample introduction Page 53
54 JUMPER TUBE TEST Purpose Helps to locate the source of contamination or noise Isolates GC components Page 54
55 JUMPER TUBE TEST Isolate the Detector Remove column from the detector Cap detector and turn on Blank run Page 55
56 JUMPER TUBE TEST Isolation of Detector - Results Detector OK Detector is the problem Page 56
57 JUMPER TUBE TEST Isolate the Injector Connect the injector and detector 1-2 meters deactivated fused silica tubing Turn on carrier gas Blank run Page 57
58 JUMPER TUBE TEST Isolate the Injector - Results Injector OK Injector, lines or carrier gas contaminated Page 58
59 JUMPER TUBE TEST Isolate the Column Reinstall the column Setup as before Blank Run Page 59
60 JUMPER TUBE TEST Isolate the Column - Results Problem returns: It s the column Problem gone: Previous leak, solid debris, or installation problem Page 60
61 STATIC PRESSURE CHECK Checks for Leaks in Injector or Gas Lines Seal all injector outlets Supply pressure from gas cylinder up to 20psi higher than analysis Turn off cylinder <2 psig per hour drop if leak free Page 61
62 Common Causes of Column Performance Degradation and or Short Column Life Physical damage to the polyimide coating Thermal damage Oxidation (O 2 damage) Chemical damage by samples Contamination Page 62
63 Physical Damage to The Polyimide Coating The smaller the tubing diameter, the more flexible it is. Avoid scratches and abrasions Immediate breakage does not always occur upon physical damage Page 63
64 NOT what you want your column to look like! Page 64
65 Thermal Damage Degradation of the stationary phase is increased at higher temperatures. Breakage along the polymer backbone. CH 3 CH 3 CH 3 Si Si Si O O O O CH 3 CH 3 CH 3 Dimethylpolysiloxane Page 65
66 Thermal Damage What To Do If It Happens Disconnect column from detector Bake out overnight at isothermal limit Remove cm from column end Page 66
67 Thermal Damage Rapid degradation of the stationary phase caused by excessively high temperatures Isothermal limit = Indefinite time Programmed limit = 5-10 minutes Temporary "column failure" below lower temperature limit Page 67
68 Oxidation (O2 Damage) Oxygen in the carrier gas rapidly degrades the stationary phase. The damage is accelerated at higher temperatures. Damage along the polymer backbone is irreversible. CH 3 CH 3 CH 3 Si Si Si O O O O CH 3 CH 3 CH 3 Dimethylpolysiloxan e O 2 Page 68
69 Oxygen Damage What To Do If It Happens Rapid damage to the column Usually results in irreversible column damage Page 69 Group/Presentation Title Agilent Restricted
70 How to Prevent Column Damage by Oxygen High quality carrier gas (4 nine's or greater) Leak free injector and carrier lines Change septa Maintain gas regulator fittings Appropriate impurity traps Page 70
71 Configurations for Carrier Gas Purifiers Indicating Moisture Trap High Capacity Oxygen Trap OVEN TEMP 100 Indicating Oxygen Trap GC Page 71
72 Common Causes of Leaks Re-use and mis-installation. Leak from O-ring, Gold Seal, ferrules, column nuts O-rings are elastomer compression fittings designed for one use, not perfectly elastic. Gold seals are designed for one use, knife edge cuts into gold layer giving leak tight seal w/o shrinkage or potential organic contaminants from polyimide out-gassing/degradation. Re-using could result in overlap in seal rings, resulting in a leak. Over-tightening of fittings Page 72
73 Leaks Due to Septum Nut With repeated use, conical needle guide gets worn, out of round, and needs replacement as septum can begin to bulge out, especially with excessive tightening, Septa fail faster because needle is not guided with as much precision. Under or Over tightening tighten nut until c-clamp on top stops turning, then ½ to ¾ turn more. Non-Agilent septa may be too thin, too thick, or out of round like die-cut septa and may not seal as well. Use Environments that decrease lifetime, like using non-agilent Autosamplers (ours are precisely aligned), manual injection, larger gauge syringes Replace septum nut annually for peace of mind. Page 73
74 Avoid High Temperatures Hotter temperatures degrade the phase faster Maintain column at or below isothermal limit Minimize time at programmable temperature limit Lower temperature limit is performance related and not related to phase damage Page 74
75 Avoid Chemical Damage There are more things that don t go through the column than do. There are nasty things in samples. Inorganic acids and bases will react with and damage most stationary phases. i.e. HCl, H 2 SO 4, KOH, NaOH, etc. CONCLUSION: Don t inject anything on the column! - It will last much longer! Page 75
76 Chemical Damage What To Do If It Happens Remove 1/2-1 meter from the front of the columns Severe cases may require removal of up to 5 meters Page 76
77 Contamination of system by residue on fingers during column installation Column: DB-5ms, 30m x 0.25mm, 0.25um Carrier: H2, 60 cm/sec, constant flow Injector: split 1:20, 250C Detector: FID, 320C, N2 makeup gas Oven: 40C for 0.75 min, C at 20C/min, 325C for 30 Red: WD-40 Blue: system blank Procedure: (1) One very small drop of liquid placed on one fingertip. (2) Fingertip was wiped with paper towel to remove as much of the offending material as possible. (3) Lightly touched the part of the column sticking up above the ferrule. (4) Installed column into injector. (5) Set oven temperature to 40C. (6) Started oven temperature program as soon as oven reached 40C. Page 77
78 Contamination from Liquid Soap Column: DB-5ms, 30m x 0.25mm, 0.25um Carrier: H2, 60 cm/sec, constant flow Injector: split 1:20, 250C Detector: FID, 320C, N2 makeup gas Oven: 40C for 0.75 min, C at 20C/min, 325C for 30 Red: liquid soap Blue: system blank Procedure: (1) One very small drop of liquid placed on one fingertip. (2) Fingertip was wiped with paper towel to remove as much of the offending material as possible. (3) Lightly touched the part of the column sticking up above the ferrule. (4) Installed column into injector. (5) Set oven temperature to 40C. (6) Started oven temperature program as soon as oven reached 40C. Page 78
79 Contamination from Hand Lotion Column: DB-5ms, 30m x 0.25mm, 0.25um Carrier: H2, 60 cm/sec, constant flow Injector: split 1:20, 250C Detector: FID, 320C, N2 makeup gas Oven: 40C for 0.75 min, C at 20C/min, 325C for 30 Red: hand lotion Blue: system blank Procedure: (1) One very small drop of liquid placed on one fingertip. (2) Fingertip was wiped with paper towel to remove as much of the offending material as possible. (3) Lightly touched the part of the column sticking up above the ferrule. (4) Installed column into injector. (5) Set oven temperature to 40C. (6) Started oven temperature program as soon as oven reached 40C. Page 79
80 Contamination of system by residue on fingers during column installation Column: Carrier: Injector: Detector: Oven: DB-5ms, 30m x 0.25mm, 0.25um H2, 60 cm/sec, constant flow split 1:20, 250 o C FID, 320 o C, N2 makeup gas 40 o C for 0.75 min, o C at 20 o C/min, 325 o C for 30 min Red: French Fry Blue: system blank Procedure: (1) Held French fry for 5 seconds. (2) Fingertip was wiped with paper towel to remove as much of the offending material as possible. (3) Lightly touched the part of the column sticking up above the ferrule. (4) Installed column into injector. (5) Set oven temperature to 40 o C. (6) Started oven temperature program as soon as oven reached 40 o C. Page 80
81 Tips to Maximize Septum Life, Minimize Septum Leaks Use Agilent Gold Standard, HP Point, gauge taper syringes. The point style cores septa significantly less when used with CenterGuide Septa. Taper minimizes septum coring/wear. HP-Point Style Use Agilent CenterGuide Septa. The molded hole minimizes septa coring, counter-intuitive, but true. Solid Septum CenterGuide Septum Page 81
82 What Does GC System Inertness Look Like? Easier question: What does poor inertness loo Symptoms of poor GC system inertness: * Tailing peaks * Reduced peak response * No peak response * Extra peaks! * Poor linearity of a peak usually at low concentrations Page 82
83 Possible Inertness Problem Areas Inlet -liner, liner packing, gold seal, stainless steel Consumables - septa, syringe, vial, caps, inserts, solvents Column GC Detector - source geometry, material, column interface, acquisition rates? Temperatures - inlet, xfer line, source, quads, oven Other method factors, i.e. standards & sample preparation Page 83
84 How important is each component s inertness to overall Flowpath Inertness? GC Flowpath Surface Areas Surface Area l (cm) d (cm) pi (cm 2 ) Liner Seal Column Page 84
85 Split Liners What s What? Straight tube Straight tube with glass wool Fixed glass wool Inverted cup Baffle Page 85
86 Splitless Injection Liners Liner Part No. Comments Side hole G G Single taper, deactivated, 900 L volume. Taper isolates sample from metal seal, reducing breakdown of compounds that are active with metals. For trace samples, general application. Single taper, deactivated, with glass wool, 900 L volume. Glass wool aides volatilization and protects column. For trace (dirty) samples. Double taper, deactivated, 800 L volume. Taper on inlet reduces chance for backflash into carrier gas lines. High efficiency liner for trace, active samples. Direct connect liners, single and dual taper, deactivated. Capillary column press fits into liner end, eliminating sample exposure to inlet. Ultimate protection for trace, active samples. Side hole permits use with EPC. Page 86
87 Liner Maintenance Liners become contaminated with use, collecting non-volatiles, salts, excess reagents, etc., or become damaged/cracked. Should inspect and replace liners often. Handle with gloves and forceps. Insert into or remove liners only from cool injection ports. Replacing with a new liner is recommended, to ensure reproducibility Page 87
88 What about Baking Out Columns? SURE! But Only removes semi-volatile residues Limit to 1-2 hours May polymerize some contaminants Reduces column life Page 88
89 Common Care and Maintenance Scheme 1. Bake out the column for no more than 2 hours. 2. Change the Liner and cut off 6-1ft of the inlet end of the column. (Change gold seal) 3. Cut off more column. (repeat as necessary) 4. Periodically clean the injector. Page 89
90 MS Troubleshooting Process (same as GC) 1. Isolate the problem. (Blank Run, Inject Un-retained Compound, Jumper Tube Test) 2. Change only one variable at a time. 3. Compare before/after chromatograms. (Peak shape, response, retention, baseline rise, background, look for trends, etc.) 4. Utilize Technical Support. Page 90
91 Page 91
92 Page 92
93 Page 93
94 Page 94
95 Page 95
96 Tuning Parameters - EI Inert Source Ion Source Volume Filament Inlet (column) Ion Focus Guide Rod or DIF HED Repeller Filament Drawout Entrance Lens, offset AMU gain, offset Mass axis gain, offset Element Voltages Effect Filament Emission 0-315ua Electron Energy volts Energy of electron beam Number of electrons generated Electron Multiplier Repeller volts Pushes ions out of the source Drawout Ground potential Entrance aperture to lens stack Ion Focus volts Relative abundance Entrance Lens mv / amu Relative abundance Entrance Lens Offset volts Relative abundance AMU Gain Peak Width AMU Offset Peak Width Guide Rod or DIF volts Focus / Guide Ions HED +-10,000 volts Converts ions to electrons Electron Multiplier volts Sensitivity Mass Axis Gain 2047 Mass assignment Mass Axis Offset 499 Mass assignment Page 96
97 Tuning Parameters - EI Extraction Source 5977 Ion Source Volume Filament Inlet (column) Ion Body Ion Focus Quadrupole Guide Rod HED Repeller Filament Extractor Entrance Lens AMU gain, offset Mass axis gain, offset Electron Multiplier Element Voltages Effect Filament Emission current 0-315ua / Electron Energy volts Number of electrons generated / Energy of electron beam Ion Body volts Reference for Electron Energy Repeller volts Pushes ions out of the source Extractor volts Entrance aperture to lens stack Ion Focus volts Relative abundance Entrance Lens mv / amu Relative abundance Entrance Lens Offset volts Relative abundance AMU Gain Peak Width AMU Offset Peak Width Guide Rod or DIF volts Focus / Guide Ions HED +-10,000 volts Converts ions to electrons Electron Multiplier volts Sensitivity Mass Axis Gain 2047 Mass assignment Mass Axis Offset 499 Mass assignment Page 97
98 Autotune report evaluation Symmetrical smooth peak shapes No split peaks 10% Total peak height Appropriate EM voltage 3000 maximum Consistent mass peak widths ±0.05 of each other ( ) Low water and air 18 to 69 20% 28 to 69 10% Correct mass assignments ±0.1 a.m.u. Proper absolute abundance Minimum usually set to 400, ,000 for 69 Typical relative abundance Base peak should be 69 or % Proper isotope ratios 1.1, 4.4, 10.1% respectively ±20% Correct mass assignments ±0.1 a.m.u. Page 98
99 Good Source Cleaning Practices Use aluminum oxide sand powder, green sandpaper, Bar Keepers Friend, flexible sand sticks (LCMS), Soft Scrub Lightly clean flat surfaces and focus on inside surface of lens openings Examine repeller surface and ensure flat rounded surface Solvent wash cleaned source parts in 1 water, 2 acetone or methanol, 3 dichloromethane or hexane (don t solvent wash ceramics or polymer insulators) Change your filaments Page 99
100 Troubleshooting Tools Needed for MS Know good pressure readings for your system (high/rough vacuum) Known good tune voltages of a clean well functioning system Know your background abundances (H 2 O, N 2, CO 2, column bleed ions i.e. m/z 207) Good column background of blank baseline of column bleed Good chromatogram of your mid to low standard or calibrator (prefer in matrix) Page 100
101 Potential MS Leak Sites O-ring around analyzer MS column interface connection GC inlet Pumping system problems Page 101
102 Vacuum Leak Troubleshooting Process Isolate the system compartments (Gas flow, GC inlet, column, MS interface, MS) Check age of gas traps, isolate from flow path (can become saturated) Check septa, liner O-ring, Au seal, ferrule/column installation Use dust off and manual tune window to monitor at m/z 51 and 65 Cap column off from inlet with a septa and allow MS to pump for ~ 30 mins. Cap off MS with solid blank ferrule Measure the flow coming out of rough pump Page 102
103 Questions Thank you for your attention 103
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