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GC Flow Path Inertness Ensuring Reliable Results
Page 1
What is GC Flow Path Inertness?
Page 2
Whatever goes in here…
Makes it all the way over here!
With no loss and no peak shape distortion (tailing)!!!
Peak Tailing – Why does it Happen?
Turbulent Flow Problem
-Dead volume, obstruction, poor installation, or severe column contamination
Active Sites in Injector, Column, and/or Flow Path
- Reversible adsorption of active compounds (-OH, -NH, -SH)
Page 3
Where does liner and column activity come from?
Isolated Geminal Vicinal Siloxane
- Sterically difficult to “cap” all of them(estimate 40-65% older traditional deactivations.)
- Oxidation of Stationary Phases from air leaks
- Injecting Reactive Samples or Non-volatile Contamination
Page 4
Agilent Inert Flow Path Solution
Ultimetal Plus– FPD
Ultimetal Capillary Flow Technology Devices Ultra Inert GC ColumnUltra Inert Gold Seal
Ultra Inert Inlet Liner
Flexible Metal Ferrules
Ultimetal Plus Inlet Weldments,Shell and Transfer Lines
Page 5
Top 5 Inertness Tips
1. Use Good Gas Purifiers2. Regular Inlet Maintenance3. Use Inert Liners, Seals,
Ferrules, etc. in Inlet
3. Select an Ultra Inert Column
4. Maintain an Inert Detector
Page 6
Agilent Ultra Inert Inlet Liners
Touchless PackagingEasy installation of new, clean liner without risk of contamination from touching.
Includes non-stick plasma treated o-ring
Page 7
Ultra Inert deactivation passes Endrin/DDT decomposition test after 100 injections
Endrin Decomposition Test : Robustness
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3 4
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Agilent Ultra Inert single taper liner (p/n 5190-2292)
%Breakdown
Endrin DDT Agilent UI liner 1st injection: 1.2 2.5
101st injection: 12.2 3.0
Competitor’s liner 1st injection: 1.1 1.7101st injection: 33.8 2.2
Competitor’s single taper deactivated liner
Peak identification: 1. DDE*2. Endrin3. DDD*4. Endrin aldehyde*5. DDT6. Endrin ketone*
* Breakdown products
1st injection101st injection
101st injection
1st injection
Page 8
IS 1
12 3
4
5
IS2
IS1
12
3
4
5
IS2
Agilent Ultra Inert single taper liner with wool (p/n 5190-2293)
Competitor’s deactivated gooseneck liner with deactivated wool
Higher responses
Peaks:1. 2,4-Dinitrophenol 2. 4-Nitrophenol3. 4,6-Dinitro-2-methylphenol4. 4-Aminobiphenyl5. Pentachlorophenol IS1. Acenaphthene-d10IS 2. Phenanthrene-d10
Even with glass woolUltra Inert liners provide high responses for sensitive semivolatile acidic compounds.
Semi-Volatiles Suitability
Page 9
Drug of abuse are shown on GC/MS SIM chromatograms 5 ng of checkout standards on column
Basic Drug Suitability
Agilent UI single taper liner with wool (p/n 5190-2293)
Competitor’s deactivated gooseneck liner with deactivated wool
12
34
56
7
1
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3 4
5 6
7
Higher response
Better peak shape
Peaks:1. Oxycodone2. Temazepam3. Flunitrazepam4. Heroin5. Nitrazepam6. Clonazepam7. Alprazolam
Page 10
1. 1-Propionic acid
2. 1-Octene
3. n-Octane
4 4-Picoline
5. n-Nonane
6. Trimethyl phosphate
7. 1,2-Pentanediol
8. n-Propylbenzene
9. 1-Heptanol
10. 3-Octanone
11. n-Decane
DB-5ms Ultra Inert vs. Competitors
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4 5
6 7
8
9 10 11
min0 2 4 6 8 10
pA
10
12.5
15
17.5
20
22.5
25
27.5 Agilent J&W DB-5msUI
30m x 0.25mm x 0.25um(P/N 122-5532UI)
1
2 34
5
67
8
9 1011
min0 2 4 6 8 10
pA
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8
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20
1
2 34
5
67
8
9 1011
min0 2 4 6 8 10
pA
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8
10
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1
2 3
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5
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9 1011
6min0 2 4 6 8 10
pA
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CompetitorColumn
CompetitorColumn
Page 11
Ultra Inert Test Mix
Semivolatiles Prone to Peak Tailing(App. Note 5990-3416EN)
Page 12
Semivolatiles Prone to Peak Tailing(App. Note 5990-3416EN)
Page 13
Resolution of benzo-b & k fluoranthene isomers
19.00 19.500
100000
500000
1000000
1500000
Time-->
Abundance
Benzo-b-fluoranthene
Benzo-k-fluoranthene
Resolution of 1.2
As good as it gets…it only gets worse!
Page 14
Agilent J&W DB-624 UI vs. Competitor 624ms Organic acid performance at 200 ppm
Column: Agilent J&W DB-624UI 30 m x 0.32 mm x 1.8 um vs Rxi-624Sil MSOven: 35C 7.45 min hold, 6.72/min to100C (2.23min hold),10.08 /min to 220C(4.47 min hold), 16.79 /min (4.17 min hold)Carrier : Helium 39.6 cm/s (approx. 2.6 mL/min) set at 35C, EPC-Constant FlowInlet: Split, 20:1 at 250C (total flow approx 51 mL/min, and 11.2 psi)Inlet liner: Ultra Inert with wool Detector: FID at 280C, H2 @ 40 mL/min, Air @ 400 mL/min, N2 makeup @ 30 mL/min
min10 12 14 16 18 20 22 24 26
pA
2
4
6
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10
12
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Acetic acid
propionic acidbutanoic acid Octanoic acid
No detection on Competitor’s 624ms
Severe tailing on competitor’s 624ms
Page 15
New Flexible Metal Ferrule - Design FeaturesGroovesreduce bulk stiffness during compression and improves ID constriction.
Angle eliminates wall frictional contact to allow the material to flow into the ID area for larger range of constriction.
Tighter ferrule ID specification and tolerances (30%)
Wider opening allows for easier column insertion
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Page 16
Current vs. New Agilent Flexi-Metal Ferrule
Current Ferrule
Stiff- prone to cause damage
Poor installation Can lead to: column crushing leakage thread damage
Small ID compression (40 to 60um) seals at tip
Tight pinch point
Agilent Flexi-Metal Ferrule
More forgiving
Easier to use
Large ID compression (100 to 120um)
Broad lamp shadesealing surface
Forgiving pinch point
Page 17
New Touchless Dial Packaging
Easy column insertion
No lost ferrules
No contamination risks
Page 18
1 ng on Column Forensic/Toxicology Check Out Mix Flexible metal Ferrules vs. Siltite installed post column
min15 16 17 18 19
pA
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6.2
6.4
6.6
6.8
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7.4
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Blue = Flexible Metal Ferrules in Ultimate Union Red = Siltite Ferrules in Ultimate Union
Improved Response forBenzodiazepines
12 SKF‐525a, proadifen13 Oxazepam14 triphenyl phosphate 15 Codeine16 Lorazepam17 Diazepam18 Hydrocodone19 Dronabinol20 Oxycodone21 Temazepam22 Flunitrazepam23 Diacetylmorphine24 Nitrazepam25 Clonazepam26 Alprazolam
Page 19
Enlarged chromatograms for sensitive pesticides
UltiMetal Plus on Flexible Metal FerruleIs deactivation needed for such small surface?
4x10
0
1
2
4x10
0
1
2
Counts vs. Acquisition Time (min)4.5 5 5.5 6 6.5 7 7.5
Untreated FMFPost column Std 500ppb
FMF + UltiMetal PlusPost column Std 500ppb
AcephateOmethoate
Demeton-S
AcephateOmethoate
Demeton-S
Page 20
Agilent UI Gold Seal: Deactivated Gold Surface
• Soft gold plating is essential for proper sealing
• Ultra Inert chemistry blocks active sites (gold is NOT inert)
• Smooth surface doesn't leak
Agilent MIM seal Alterative vendor machined seal
Reliable ppb and ppt measurements require
attention to the little things!
Page 21
Response Comparison for Sensitive Pesticides
3x10
0
1
Standard gold seal
3x10
0
1
Ultra Inert Gold Seal
3x10
0
1
Counts vs. Acquisition Time (min)4 4.5 5 5.5 6 6.5 7 7.5
3x10
0
4
8
treaded SS
3x10
0
4
8
3x10
0
4
8
Standard gold seal
Counts vs. Acquisition Time (min)4 4.5 5 5.5 6 6.5 7 7.5
Acephate Omethoate
Acephate Omethoate
Acephate Omethoate
Acephate Omethoate
Acephate Omethoate
Acephate Omethoate
100 ppb STD 500 ppb STD
Ultra Inert Gold Seal
treaded SS
Page 22
New Product: Agilent Inert Inlet
UltiMetal Plus treatment forinert surface 7890 inlet shell & top weldments
•Limits adsorption/degradation of active analytes
•GC/MS and GC-ECD pesticide analysis
or Any Active Analyte Analyses
Agilent’s proven proprietary Ultimetal
Plus surface treatment
Page 23
Putting It All Together –Inert Flow Path vs. Standard Flow Path
20.20 20.40 20.60 20.80 21.00 21.20 21.40 21.60
10000
20000
26000
Green = Inert Flow PathBlue = Standard Flow Path
Column: Agilent J&W HP-5ms UI 30 m x 0.25 mm x 0.25 um Oven: 100C 4 min hold, 10/min to 280C, 6 /min to 300C (4.67 min hold),Carrier : Helium 52.7 cm/s (2 mL/min) set at 100C, EPC-Constant FlowInlet: Pulsed Splitless 35 PSI pulse until 0.73 min, 0.75 min purge 50 ml/min, gas saver 20, ml/min at 2 minInlet liner: Ultra Inert with wool / Standard single taper liner with wool (p/n 5190-3165)Gold Seal: UI Gold Seal / Standard gold sealDetector: MSD Scan mode 40 t0 450 m/z, 230 C source temp, 150 C Quad temp, 310 C transfer line
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1. Dronabinol2. Oxycodone3. Temazepam4. Flunitrazepam5. Diacetyl morphine
Drugs of Abuse 250 ppb using HP-5ms UI
Page 24
So Remember…
1. Use Good Gas Purifiers2. Do Regular Inlet Maintenance3. Use Inert Liners, Seals,
Ferrules, etc. in Inlet
3. Select an Ultra Inert Column
4. Maintain an Inert Detector
Page 25
AND Don’t Touch Anything!!! French Fries!
Column: DB-5ms, 30m x 0.25mm, 0.25umCarrier: H2, 60 cm/sec, constant flowInjector: split 1:20, 250oCDetector: FID, 320oC, N2 makeup gasOven: 40oC for 0.75 min, 40-325oC at 20oC/min,
325oC 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 40oC.(6) Started oven temperature program as soon as oven reached 40oC.
Page 26
Contamination from Liquid Soap
Column: DB-5ms, 30m x 0.25mm, 0.25umCarrier: H2, 60 cm/sec, constant flowInjector: split 1:20, 250CDetector: FID, 320C, N2 makeup gasOven: 40C for 0.75 min, 40-325C at 20C/min,
325C for 30 min
Red: Liquid Soap
Blue: system blank
Procedure:(1) One very small drop of liquid soap 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 27
Contamination from Hand Lotion
Column: DB-5ms, 30m x 0.25mm, 0.25umCarrier: H2, 60 cm/sec, constant flowInjector: split 1:20, 250CDetector: FID, 320C, N2 makeup gasOven: 40C for 0.75 min, 40-325C at 20C/min,
325C for 30 min
Procedure:(1) One very small drop of hand lotion 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.
Red: Hand Lotion
Blue: system blank
Page 28
