2°C/min. 160°C. 3°C/min. 1. Isobutyric acid. 2. Butyric acid. 3. Valerolactone. 4. ... 3. 4 5. Sample. 0.07 to 0.14% in acetic acid and acetone. Carrier: Helium 42 cm/sec, 24 psi (120°C), 1.8 ml/min constant flow ...... Dichlorobenzidine, 3,3'-. 37. .... 4,4'-DDD. 14. Endrinaldehyde. 15. Endosulfan sulfate. 16. 4.4'-DDT. 25 min.
Applications
Chemical/Industrial
GC and GC/MS Applications
GC and GC/MS Applications Chemical/Industrial Free Fatty Acids in Water 1. 2. 3. 4. 5.
6. 7. 8. 9.
Acetic Propionic Isobutyric Butyric Isovaleric
Free Organic Acids in Water
Valeric Iso-caproic Caproic Heptanoic
120°C 20°C/min
80°C
205°C 2 min 6.13°C/min
1. 2. 3. 4. 5.
Acetic acid Propionic Isobutyric n-Butyric Isovaleric
6. 7. 8. 9.
Valeric Isocaproic Caproic Heptanoic
265°C 2 min
7
1 min 5
9 5 2
1 0
2
Sample: Column: Carrier: Split Ratio: Injector Temp: Injection Size: Liner: Oven: Detector temp:
4
3
6
7 8
1
6. 7. 8. 9.
6
8
110°C
5
6
4
0
2
Sample: Carrier: Column:
4
Time (min)
6
8
10
0.06 to 0.13% each acid in water Helium, 42 cm/sec, 24 psi (120°C) 1.8 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (40:1), 1 l, inlet 250°C Temperature program listed above Pub No.: 5091-6687E FID 300°C
Injection: Oven: Detector:
Cis/Trans Cyclohexanoic Acids
4-Pentenoic acid trans-2-Methyl-2-butenoic acid trans-3-Pentenoic acid trans-2-Pentenoic acid 133°C
3 4
6
10
220°C 160°C
150°C 1 min
3°C/min
10°C/min
185°C 3°C/min
2°C/min
1 min 1 2
8
2
10 mM each acid in water 25 m x 0.32 mm x 0.5 m FFAP (Part No. 19091F-112) Helium @ 10.8 psi (42 cm/sec), constant flow 20/1 260°C 0.5 l Deactivated with glass wool plug Temperature program listed above 260°C
Isobutyric acid Butyric acid Valerolactone 2-Methyl butyric acid Valeric acid
9
10°C/min
4
Free Organic Acids/C4-C5 Isomers 1. 2. 3. 4. 5.
3
120°C 1 min
cis/trans m-Methyl cyclohexanoic acid
cis/trans p-t-Butyl cyclohexanoic acid
89
7
0
Carrier: Column: Injection: Oven: Detector:
400
5
10 Time (min)
15
2
20
Helium 42 cm/sec, 24 psi (120°C) 1.8 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (40:1), 1 l, inlet 250°C Temperature program listed above Pub No.: 5091-6687E FID 300°C
Sample: Carrier: Column: Injection: Oven: Detector:
4
6
8 Time (min)
10
12
14
0.5 to 1% in acetone Helium 46 cm/sec, 27.7 psi (150°C), 2 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (150:1), 1 l, inlet 250°C Temperature program listed above FID 270°C
Chemical/Industrial
Free Fatty Acids 1. 2. 3. 4.
Acrylates
5. 6. 7. 8.
C10 C12 C13 C14
9. 10. 11. 12.
C15 C16 C1 C18
C19 C20 C21 C22
265°C (10 min) 200°C 1 min
10°C/min
1. 2. 3. 4. 5.
Methyl methacrylate Ethyl methacrylate sec-Butyl methacrylate Allyl acrylate n-Butyl acrylate
6. 7. 8. 9.
Hexyl methacrylate Cyclohexyl methacrylate Hydroxypropyl acrylate Unknown
2 4 5 6
1
160°C 15°C/min
60°C 10°C/min
35°C 1 min
3 7
8
5
9 10 11
0
5
Sample Carrier: Column:
12
1
10 Time (min)
15
2 3
9
11 min
Carrier: Column: Injection: Oven: Detector:
Hydrogen HP-FFAP (Cross-Linked PEG-TPA), 10 m x 0.53 mm x 1.0 m (Part No. 19095F-121) On-column, 1 l Temperature program listed above FID
Alcohols
Air Methanol (Solvent) Water 1-Butanol, 0.046%
5. 1-Pentanol, 0.022% 6. 1-Hexanol, 0.018% 7. 1-Heptanol, 0.014%
160°C
45°C
20°C/min
1. 2. 3. 4. 5.
1-Propanol iso-Butanol 3-Methyl-3-pentanol 1-Butanol 4-Methyl-2-pentanol
6. 7. 8. 9. 10.
1-Pentanol 2-Ethyl-1-Butanol 1-Hexanol Cyclohexanol 1-Heptanol 4
4
2
10°C/min
10 8
6
5
7
9
7
1
1 2
3
10 min
Injection: Oven: Detector:
45°C 1 min
6
5
Carrier: Column:
150°C
Applications
Alcohols 1. 2. 3. 4.
8
4
20
0.07 to 0.14% in acetic acid and acetone Helium 42 cm/sec, 24 psi (120°C), 1.8 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (40:1), 1 l, inlet 250°C Temperature program listed above FID 300°C
Injection: Oven: Detector:
7 6
0
Helium, 4 ml/min at 45°C HP-5 (5% Phenyl Methyl Silicone), 30 m x 0.53 mm x 2.65 m (Part No. 19095J-123) On-column, 2 l Temperature program listed above FID 350°C
Carrier: Column: Injection: Oven: Detector:
2
4
3
6 Time (min)
8
10
12
Helium, 29 cm/sec, 3.0 psi (45°C) 4 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.53 mm x 1.0 m (Part No. 19095N-123) Split (25:1), 1 l, inlet 250°C Temperature program listed above FID 250°C
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401
Applications
Chemical/Industrial
GC and GC/MS Applications
Ethylene Glycol Mixture 1. 2. 3. 4. 5.
Volatile Alcohols
Diethylene glycol Triethylene glycol Polyethylene glycol 200 Polyethylene glycol 400 Polyethylene glycol 600
200°C 100°C
20°C/min
1. 2. 3. 4. 5.
Acetone Methanol isopropanol Ethanol n-Propanol
110°C 45°C 5
20°C/min
2.5 min
0.5 min 1
3
1 3 2
4 2
4 5
7 min
Carrier: Column: Injection: Oven: Detector:
0
Helium, 25 cm/sec Ultra-1 (Cross-Linked Methyl Silicone),12 m x 0.2 mm x 0.33 m (Part No. 19091A-101) Split (100:1) inlet 250°C, 1 l Temperature program listed above FID
Glycols/Diols 1. 2. 3. 4. 5. 6.
Ethylene glycol 1,3-Butanediol Ethylene glycol phenyl ether 1,7-Hepatanediol 1,9-Nonanediol 1,10-Decanediol 2 1
1
Carrier: Column:
2
Time (min)
3
4
5
Helium, 46 cm/sec, 1.8 3.0 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 15 m x 0.25 mm x 0.5 m `(Part No. 19091N-231) Split (300:1), 0.5 l, inlet 250°C Temperature program listed above FID 275°C
Injection: Oven: Detector:
Aldehydes 180°C 50°C 3 min
8°C/min
1. 2. 3. 4. 5.
Hexanal Nonanal Dodecanal Tetradecanal Hexadecanal
35°C 0 min
3 1
150°C 10 min 10°C/min
1 2
(A)
(B)
2 4
5 5
3
6
4
15 min
3 5 4
15 min
20 min. Carrier: Column: Injection: Oven: Detector:
402
Helium, pressure program: 10 psi to 25 psi (4.25 min) at 1 psi/min HP-1 (Cross-Linked Methyl Silicone), 30 m x 0.53 mm x 0.88 m (Part No. 19095Z-023) On-column, 1 l, inlet program: 50°C (0 min) to 180°C (8.45 min) at 12°C/min Temperature program listed above FID 250°C
Carrier:
Helium, 7 psi at 35°C, (A) use constant flow mode, (B) use pressure program 7 psi to 18 psi (10 min) at 1 psi/min Column: HP-1 (Cross-Linked Methyl Silicone), 30 m x 0.53 mm x 0.88 m (Part No. 19095Z-023) Injection: On-column, 1 l Oven: Temperature program listed above Detector: FID 250°C
Chemical/Industrial
Aldehydes and Acids 7. 8. 9. 10. 11. 12.
Butanal 2-Methyl butanal Pentanal Hexanal Heptanal Octanal
Acetic acid Decanal Propanoic acid so-Butyric acid Butyric acid so-Valeric acid
13. 14. 15. 16. 17.
Valeric acid Hexanoic acid Heptanoic acid Octanoic acid Decanoic acid 250°C
2 1
10
11 12
13
7
5
0
Carrier: Column:
3
8
6
5
17
14 15
3 4
16
10
15
Aromatic Amines 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
11. 12. 13. 14. 15. 16. 17. 18. 19.
14
Beta-phenylethylamine N-ethylaniline 2,4-dimethylaniline N,N-dimethylaniline o-phenylenediamine m-phenyleneadiamine 1-naphthylamine 150°C Dibenzylamine Tribenzylamine 70°C 10°C/min 1 min 18
7 8 13
2 1 2 4 Sample: Carrier: Column: Injection: Oven: Detector:
3 4
Helium, 21 cm/sec HP-1 (Cross-Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 m (Part No. 19095Z-121) Split 20:1, 1 l 80°C FID
Injection: Oven: Detector:
1. 2. 3. 4. 5. 320°C 5 min 35°C/min
n-Octylamine n-Nonylamine n-Decylamine Benzylamine Dicyclohexylamine
counts
19
6. 7. 8. 9. 10.
2 3
3000
17
n-Heptadecane Trihexylamine n-octyldecane 2,6-Dimethylaniline 2,4-Dimethylaniline
1
5000 4000
4
5
2000
12 9 10
6
7
8
9
1000
6 11
Carrier: Column:
HP Basic Wax Column Amines
Piperidine 2-methyl piperidine Aniline Benzylamine Alpha-phenylethylamine N-methyl aniline N,N-dimethyl aniline p-toluidine o-toluidine m-toluidine
5
8 min
20
Helium, 40 cm/sec, 11.7 psi (60°C), 2.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.32 mm x 0.5 m (Part No. 19091N-213) Split (40:1), 0.5 l, inlet 250°C Temperature program listed above FID 275°C
Injection: Oven: Detector:
2
1
10°C/min
60°C 1 min 9
1. n-Butylamine, 10% 2. n-Hexylamine, 89% 3. Cyclohexylamine, 1%
Applications
1. 2. 3. 4. 5. 6.
Amines
15
16
0
6 8 10 12 14 16 18 100-250 g/ml each Helium, 1.1 ml/min, constant flow HP-35MS, 30 m x 0.25 mm x 0.25 m (Part No. 19091G-633) Split (50:1), 1 ul, 275°C Temperature listed above MSD
2
Sample: Column: Injection: Oven: Detector:
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4
6
8
10
12
14
16
10
18 min
0.5 mg/ml in Hexane HP-Basic Wax, 30 m x .32 mm x 0.25 m (Part No. 19091N-613) Split (ratio) 100:1, 250°C 120°C FID 250°C
403
Applications
Chemical/Industrial
GC and GC/MS Applications
Primary Amines 1. 2. 3. 4. 5.
Aromatic Amines
n-Butylamine n-Amylamine n-Hexylamine Cyclohexylamine n-Heptylamine
6. 7. 8. 9.
n-Octylamine n-Decylamine n-Dodecanylamine n-Tetradecanylamine
220°C 25°C/min
45°C 2 min
1. 2. 3. 4. 5. 6.
Xylene Aniline Dichlorotoluene p-Nitrochlorobenzene N-Methylformamide Formamide
7. 8. 9. 10. 11.
Phenazine 2-Nitrodiphenylamine 4-Nitrodiphenylamine 4,4'-Dinitrodiphenyl ether 4,4'-Dinitrophenlamine
4 7
6
50°C 2 min
8 9
3 4
5
1
250°C 5 min 10°C/min
1
3
6
2
2
9 5
1 1
7 8 10
2
4
6
8
10 min 35 min
Sample:
1 l split (ratio 30:1), 0.1 to 0.35% aliphatic amines in methanol Helium, 1.5 ml/min constant flow HP-35,15 m x 0.25 mm x 0.25 m (Part No. 19091G-131) Temperature program listed above FID 310°C
Carrier: Column: Oven: Detector:
Carrier: Column: Injection: Oven: Detector:
Esters 1. 2. 3. 4. 5. 6. 7.
Ethyl Esters 8. 9. 10. 11. 12. 13.
Ethyl propionate Propyl acetate Ethyl butyrate Propyl propionate Propyl butyrate Ethyl valerate Butyl propionate
1
6 2 4 3 5
Carrier: Column: Injection: Oven: Detector:
404
5
14. 15. 16. 17. 18. 19.
Propyl valerate Ethyl caproate Butyl valerate Propyl caproate Methyl decanoate Butyl caproate
Methyl dodecanoate Butyl heptanoate Methyl tetradecanoate Methyl hexadecanoate Methyl octadecanoate Methyl eicosenoate
1. 2. 3. 4. 5.
C4 C5 C6 C7 C8
6. 7. 8. 9.
C9 C10 C10 C12
200°C 5°C/min
45°C 1 min
200°C
8
5°C/min
45°C 1 min
9
7
0
Helium, 70 kPa HP-1 (Cross-Linked Methyl Silicone), 30 m x .53 mm x 2.65 m (Part No. 19095Z-123) On-column 1 l Temperature program listed above FID
11
4
15 13
10 12 14
2 16 17
10 15 Time (min)
18
20
19
3
5
6
9
7 8
1
0
25
Helium 29 cm/sec, 3.0 psi (45°C) 4 ml/min constant flow HP-INNOWax (Crossed-Linked PEG), 30 m x 0.53 mm x 1.0 m (Part No. 19095N-123) Split (25:1), 1 l, inlet 250°C Temperature program listed above FID 250°C
Carrier: Column: Injection: Oven: Detector:
5
10 15 Time (min)
20
25
Helium, 29 cm/sec, 3.0 psi (45°C) 4 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.53 mm x 1.0 m (Part No. 19095N-123) Split (25:1), 1 l, inlet 250°C Temperature program listed above FID 250°C
Chemical/Industrial
Phthalic Acid Esters 1. 2. 3. 4. 5.
Methyl Esters of Dibasic Acids
Dimethyl phthalate Diethyl phthalate Dibutyl phthalate Dicyclohexyl phthalate Dioctyl phthalate
200°C (2 min) 10°C/min
50°C 5 min
1. 2. 3. 4. 5.
6. 7. 8. 9.
C2 C3 C4 C5 C6
C7 C8 C9 C10
240°C (5 min)
8 9
6 1
2
3
5°C/min
45°C 1 min
5
45
7
4 1
2
3
30 min 0
15
20
25
30
35
Time (min)
Injection: Oven: Detector:
Helium, 20 ml/min HP-1 (Cross-Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 m (Part No. 19095Z-121) On-column, 1 l Temperature program listed above FID
Fast Analysis of Laboratory Air
Carrier: Column: Injection: Oven: Detector:
Helium, 29 cm/sec, 3.0 psi (45°C) 4 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.53 mm x 1.0 m (Part No. 19095N-123) Split (25:1), 1 l, inlet 250°C Temperature program listed above FID 250°C
Chiral Compounds in Essential Oils and Gases 1. 2. 3. 4. 5. 6. 7.
1. Oxygen 2. Nitrogen
2
1,2-Dimethylbenzene Myrcene (-)-Camphene (+)-Camphene (+)--pinene 1S-(-)--pinene Cineole
pA
8. 9. 10. 11. 12. 13. 14.
(R)-(+)-Citronellal 1S, 2R,5S-(+)-Menthol 1R, 2S,5R-(-)-Menthol -Terpineol (+/-)-isoborneol (+)-borneol trans-Cinnamaldehyde 65°C 1 min 8
1
170°C
Applications
Carrier: Column:
5°C/min
14
100 2
80
1
5
7
10 13 9 11
6
60
12 34
40 0.00
0.20
0.40 Time (min)
0.60
20 5
Sample: Carrier: Column: Oven:
25 l, split (ratio 4:1) Helium, 87 ml/min HP-PLOT/MoleSieve, 15 m x 0.53 mm x 25 m (Part No. 19095P-MS5) 40°C
Sample: Carrier: Column: Injection: Oven: Detection:
10
Time (min)
15
20
0.25 ng/l each analyte in Hexane Hydrogen, 39 cm/sec, Constant pressure HP-Chiral , 30 m x 0.25 mm x 0.25 m (Part No. 19091G-B233) Split 30:1, 1 l, 250°C Temperature program listed above FID 300°C Pub No.: 5965-7873
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405
Applications
Chemical/Industrial
GC and GC/MS Applications
Noble Gases 1. 2. 3. 4. 5. 6.
Inorganic Hydride Gases
Neon Argon Oxygen Nitrogen Krypton Xenon
120°C 5 min 25°C/min
35°C 3 min
4
1. 2. 3. 4.
5. Tetraborane 0.10 ppm 6. Pentaborane 0.10 ppm 7. Dihydropentaborane 0.60 ppm
Arsine 0.1% Phosphine 0.1% Selenide 0.1% Diborane 0.10 ppm
(A)
2 5
-70°C
1
(B)
4
30°C
6
1
2
3
5 6 2
GC: Sample: Carrier: Column: Oven:
4
Time (min)
6
5890 Series II GC EPC and TCD 250 l, split (ratio 50:1) Helium, 4 ml/min HP-PLOT/MoleSieve, 30 m x 0.53 mm x 50 m (Part No. 19095P-MSO) Temperature program listed above Pub No.: 5963-2466
Aromatic Compounds 1. 2. 3. 4. 5.
Benzene Toluene m-Xylene o-Xylene p-Cymene
3
8
Carrier: Column: Injection: Oven: Detector:
7
Helium, 35 cm/sec HP-1 (Cross-Linked Methyl Silicone), 50 m x 0.2 mm x 0.5 m (Part No. 19091Z-205) Split (25:1), 1 l A: -70°C isothermal; B: 30°C isothermal FPD (535 m filter)
Chlorinated Isooctane 1. 2. 3. 4.
1 2 34
1-Chloro isooctane 4-Chloromethyl 2,2'-dimethyl pentane 3-Chloro isooctane 4-Chloro isooctane 4 2 3 Monochloro isomers
5
1
3
4
5 Time (min)
6
8 min Carrier: Column: Injection: Oven: Detector:
406
Hydrogen HP-FFAP (Cross-Linked PEG-TPA), 50 m x 0.32 mm x 0.52 m (Part No. 19091F-115) Split (150:1), 1 l 110°C FID
Carrier: Column: Injection: Oven: Detector:
Helium, 33 cm/sec, 35.7 psi (80°C) 2 ml/min HP-INNOWax (Cross-Linked PEG), 60 m x 0.25 mm x 0.25 m (Part No. 19091N-136) Split (150:1), 0.5 l, inlet 250°C 80°C isothermal FID 300°C
7
Chemical/Industrial
Butadiene and Aromatics
1
Ketones 1. 2. 3. 4.
2
1,3-Butadiene Cyclopentene Benzene Toluene
1. 2. 3. 4.
3-Pentanone 4-Methyl-2-pentanone 4-Heptanone 5-Methyl-3-heptanone
5. 2,6-Dimethyl 4-heptanone 6. 2-Heptanone 7. 5-Methyl-2-hexanone
250°C
60°C 1 min
15°C/min
150°C 2 min
150°C
75°C 2°C/min
20°C/min
5 6
4
7
1 3 3
1
2
3
GC: Carrier: Column:
4
5 6 Time (min)
7
8
9
10 2
6890 Helium, 25 psig HP-PLOT Q, 30 m x 0.53 mm x 40 m (Part No. 19095P-Q04) Temperature program listed above FID, 275°C
Carrier: Column:
Oven: Detector: Butadiene Concentration: 200 ppm (v/v)
7. 8. 9. 10. 11.
2,4,6-Trinitrophenol 2,4-Dinitrophenol 4-Nitrophenol 2-Methyl-4,6-dinitrophenol Pentachlorophenol
1. 2. 3. 4. 5. 6. 7. 8. 9.
4 1 2
5 3
7
9
10
Time (min)
15
20
8
4,5
10 11
2 3
10
4-chloro-3-methylphenol 2,4,5-trichlorophenol 2,4,6-trichlorophenol Dinoseb 4-nitrophenol 2,4-dinitrophenol 2-methyl-4,6-dinitrophe nol 17. 2,3,4,6-tetrachlorophenol 18. Pentachlorophenol
25
20 g/ml phenols in methylene chloride HP 5MS (Part No. 19091-5433) 30 m x 0.25 mm x 0.25 m Helium, 33 cm/sec, constant flow 35°C (5 min), 8°C/min to 220 (2 ml) 1 l, Splitless, 250°C 0.75 min FID 300°C Pub No.: 5952-6971
3.0 Sample: Column: Inlet: Oven: Detector:
240°C 5 min 20°C/min
13
10
17 18
7 14,15
4.0
180°C 1 min 25°C/min
50°C 1 min
11 12
9
6
1
Sample: Column: Carrier: Oven: Injection: Purge Time: Detector:
8
10. 11. 12. 13. 14. 15. 16.
Phenol 2-chlorophenol o-cresol m-cresol p-cresol 2,4-dimethylphenol 2-nitrophenol 2,4-dichlorophenol 2,6-dichlorophenol
6
8
5
6 Time (min)
Phenols
Phenol 2-Chlorophenol 2-Nitrophenol 2,4-Dimethylphenol 2,4-Dichlorophenol 4-Chloro-3-methylphenol
0
4
Helium, 30 cm/sec, 8.8 psi (60°C) 21.75 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.32 mm x 0.5 m (Part No. 19091N-213) Split (50:1), 0.5 l, inlet 250°C Temperature program listed above FID 275°C
Injection: Oven: Detector:
Phenols on HP-5MS 1. 2. 3. 4. 5. 6.
4
Applications
0
2
5.0
6.0 7.0 Time (min)
16
8.0
9.0
10.0
20 M/ml each HP-35MS, 30 m x 0.25 mm x 0.25 m (Part No. 19091G-633) 240°C, split 10:1, flow 1.1 ml/min Temperature program listed above MSD, 260°C
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407
Applications
Chemical/Industrial
GC and GC/MS Applications
Free Phenols 1. 2. 3. 4. 5. 6.
Monomers in Latex Paint by Headspace
Phenol 2-chlorophenol 2,4-dimethylphenol 2-nitrophenol 2,4-dichlorophenol 4-chloro-3-methylphenol
7. 8. 9. 10. 11.
2,4,6-trichlorophenol 2,4-dinitrophenol 4-nitrophenol 2-methyl-4,6-dinitrophenol Pentachlorophenol
100°C 1 min 3
Acrylonitrile Methyl acrylate Butyl acrylate Styrene
40°C
250°C 1 min 15°C/min
3
10
5
4
2
9
4
200°C 30°C/min
90°C 15°C/min
5 min
6
1 2
1. 2. 3. 4.
1
7 8 11
GC: Carrier Gas: Column: Injector: Oven: Detector:
8
10 Time (min)
12
14
2
Sample: Carrier: Column:
6890 Hydrogen, constant flow 45 cm/sec HP-50+, 30 m x 0.25 mm x 0.25m (Part No. 19091L-433) Split 100:1 Temperature program listed above FID 300°C
8. 9. 10. 11. 12. 13.
Propylene Propane 1-Butene Butene Pentane Toluene Styrene
C2H5-C(Ph) = CH2 C4H9-CH2CH2-Ph C4H9-C(Ph) = CH2 C4H9-CH=C(Ph)CH3 Styrene dimer 0°C Styrene trimer
280°C 60°C 5°C/min
3
1 4
0
Sample: Carrier: Column: Injection: Oven: Detector:
408
8
5 10
20
1. 2. 3. 4. 5. 6.
1-Propene Butene Acetonitrile Acrylonitrile Propanenitrile 1,5-Hexadiene
12
30 Time (min)
7. 8. 9. 10. 11. 12.
1-Hexene Butylamine Cyclopentanone Cyclohexenone Hexylamine Caprolactam
1
13
10 2
8
12
10
Pyrolysates of Nylon 66
7
6
6
0.200 gm sample with 1 gram sodium sulfate in 5 ml water Helium, 45.5 cm/sec (40°C), 6 ml/min constant flow HP-INNOWax (Cross-Linked PEG) 30 m x 0.53 mm x 1.0 m (Part No.19095N-123) Split (10:1), 1 ml headspace, inlet temp 220°C Temperature program listed above FID 300°C
Injection: Oven: Detector:
Pyrolysates of Polystyrene 1. 2. 3. 4. 5. 6. 7.
4
Time (min)
Abundance
6
6
5 50
100 mg pyrolyzed Helium, 30 psi, 12 ml/min HP-Ultra 1 (Cross-Linked Methyl Silicone), 50 m x 0.20 mm x 0.33 m (Part No. 19091A-105) Split (30:1), inlet 280°C, Pyrolyzer 600°C Temperature program listed above FID 300°C
60
Carrier: Column: Injection: Inlet: Oven: Detector:
A900°C Pyrolysis
9
10
40
15°C/min
0°C 1 min
2 34 5 7 8
9 11
275°C (2 min)
10
B700°C Pyrolysis 11 15 Time (min)
12 20
25
Helium, 5 psi HP-5 (5% Phenyl Methyl Silicone), 30 m x 0.53 mm x 2.65 m (Part No. 19095J-123) Direct interface to pyrolyzer (1000°C, 10 seconds) -10°C (0.5 min) to 300°C (1 min) at 120°C/min Temperature program listed above MSD 300°C
Chemical/Industrial
Pyrolysates of Kraton 1107 2-Methyl-1-propene 2-Methyl-1-butene 2-Methyl-1,3-butadiene 2-Methyl-2-butene 2,3-Dimethyl-2-butene 1,3,5-Hexadiene 3-Methyl-1,3-pentadiene Toluene Ethyl benzene
10. o-Xylene 11. Styrene 12. 1,4-Dimethyl-4-vinyl cyclohexene (ethyl methyl benezene co-elutes) 13. 1-Propenyl benzene 14. 1-Methyl-4-isopropenyl cyclohexene (dipentene) 275°C
3
0°C 1 min
TIC
10
4 1
5
2
2
4
Carrier: Column:
6 6
8
1
13 0
10 12 Time (min)
14
2
5
3
4
5
15°C/min
16
18
2
1
7
6 4
0
7
6 0.5
1
1.5
Time (min)
20 Carrier:
Helium, 27.5 psi (0.2 ml/min), 27 cm/sec Column: HP-Wax, 10 m x 100 m x 0.2 m (Part No. 19091X-241) Injection: 1000/1, 0.1 l Oven: 60°C (1.5 min), 30°C/min, 150°C (2 min)
Carrier:
Hydrogen, 33.7 psi (0.6 ml/min), 69 cm/sec Column: HP-Wax, 10 m x 100 m x 0.2 m (Part No. 19091X-241) Injection: 1000/1, 0.1 l Oven: 60°C (.56 min), 80°C/min, 150°C (0.1 min) Pub No.: 5965-6692
Solvents 1. 2. 3. 4. 5.
34
2 min
Helium, 5 psi HP-5 (Cross-Linked 5% Phenyl Methyl Silicone), 30 m x 0.53 mm x 2.65 m (Part No. 19095J-123) Direct interface to pyrolyzer (10 seconds) -10°C (0.5 min) to 300°C (1 min) at 120°C/min Temperature program listed above MSD 300°C
Injection: Inlet: Oven: Detector:
2
9 12
7
5. Toluene 6. C8 aromatics 7. 4-hydroxy-4methyl 2-pentanone
Propylene oxide Acetone Methanol Methylene chloride
14
11
8
1. 2. 3. 4.
Solvents
Methane Acetone Isopropanol Methylene chloride Methyl ethyl ketone
6. 7. 8. 9. 10.
1,1,1-Trichloroethane Isopropyl acetate Trichloroethylene Toluene n-Butyl acetate
11. 12. 13. 14.
150°C 10°C/min
40°C 3 min
1. 2. 3. 4. 5. 6. 7. 8. 9.
Perchloroethylene Xylene Xylene Xylene 180°C 20°C/min
Ethanol Acetonitrile Acetone Dichloromethane Diethyl ether Pentane Ethyl acetate Hexane Benzene
Applications
1. 2. 3. 4. 5. 6. 7. 8. 9.
Solvents in Paint Thinner
4 6 7 2
3
4
8
5
9 10
9
5 6
11 13
1
1
3 2
7
12
8
14 0
1
10 min Carrier: Column: Injection: Oven: Detector:
Helium, 24 cm/sec PONA (Cross-Linked Methyl Silicone), 50 m x 0.2 mm x 0.5 m (use 25 m only) (Part No. 19091S-001) Split (150:1); 0.1 l 250°C Temperature program listed above MSD 280°C Pub No.: 5953-8065
GC: Sample: Carrier: Column: Injection: Oven: Detector:
2
3 4 Time (min)
5
6
6890 1 l 0.1-0.3% solvents in methanol Hydrogen 9 ml/min HP-PLOT Q, 30 m x 0.53 mm x 40 m (Part No. 19095P-Q04) 250°C Split mode (12:1) 150°C Isothermal FID 250°C Pub No.: 5965-7872
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409
Applications
Chemical/Industrial
GC and GC/MS Applications
Common Industrial Solvents 1. 2. 3. 4. 5. 6. 7.
MeOH Methyl formate EtOH Acetone i-PrOH CH2CI2 n-PrOH
8. 9. 10. 11. 12. 13.
Headspace Analysis of Common Solvents 1,4-Dioxane Toluene Mesityl oxide Diacetone-alcohol m-Xylene Cyclohexanone
14. 15. 16. 17. 18. 19.
MEK s-BuOH EtOAc i-BuOH i-PrOAc Nitropropane
140°C
10°C/min
1 2 45 3
58
19 2
17
14
8 6 7
1
11
16
9 15
Headspace Analysis of Common Solvents on Fast GC Residual Solvent Column
40°C 1.7 min
17. Benzene Hexane 18. Heptane Propanol 19. Trichloroethylene Methylethylketone 20. 1,4-Dioxane Ethylacetate Tetrahydrofuran 21. Pyridine s-Butanol 22. Toluene Chloroform Cyclohexane Vial Equilibration Time: 10 min Pressurization Time: 0.2 min 250°C Loop Fill Time: 0.15 min 90°C 30°C/min Loop Equilibration Time: 0.05 min 6°C/min 8 Injection Time: 1.00 min 45 19 10 11 6 15 7 23 1
1 GC: Column:
Carrier: Oven: Injection: Detector:
410
2
9. 10. 11. 12. 13. 14. 15. 16.
9
3
12
16 17 18
4 Time (min)
6890 HP-Fast GC Residual Solvent Column (Part No. 19095V-420) Helium, 35 cm/min, constant flow Temperature program listed above Headspace, 180°C, Split 7/1 FID, 260°C
GC: Column: Carrier: Oven: Injection: Detector:
5
12
16
19
18
22 21
20
21
6
8 Time (min)
6890 HP-624 30 m x 0.53 mm x 3.0 m (Part No. 19095V-423) Helium, 35 cm/min, constant flow 40°C (5 min) to 90°C at 2°C/min 90°C to 250°C at 30°C/min Headspace, 180°C, Split 7/1 FID, 260°C
12
14
Headspace Conditions Carrier Gas Pressure: Oven Temp: Loop Temp: Transfer Line Temp: Vial Pressure:
40°C 5 min
1. 2. 3. 4. 5.
30°C/min
90°C 2°C/min
3.5 psi 85°C 95°C 110°C 10 psi
Methanol Chloride (25 ppm) Chloroform (12 ppm) Benzene (25 ppm) Trichloroethylene (25 ppm) 1, 4-Dioxane (25 ppm) 3
1 4
2 2
4
6 Time (min)
HP-624, 30 m x 0.53 mm x 3.0 m (Part No. 19095V-423) Carrier: Helium, 35 cm/min, constant flow Oven: Temperature program listed above Injection: Headspace, 180°C, Split 7/1 Detector: FID, 260°C 3.5 psi 85°C 95°C 110°C 10 psi
10
250°C
Column:
6
Headspace Conditions Carrier Gas Pressure: Oven Temp: Loop Temp: Transfer Line Temp: Vial Pressure:
4
Headspace Analysis of USP 467 Solvents
22 20
9 10
15
2
Helium, 35 kPa HP-1 (Cross-Linked Methyl Silicone), 25 m x 0.32 mm x 1.0 l Part No. 19091Z-212) Split (200:1), 1 l Temperature program listed above IRD 200°C Pub No.: 5954-0657
Methanol Ethanol Ether Acetone i-Propanol Acetonitrile Methylene Chloride t-Butanol
6 7
18
12 min
1. 2. 3. 4. 5. 6. 7. 8.
9. Benzene Hexane 10. Heptane Propanol 11. Trichloroethylen Methylethylketone 12. 1,4-Dioxane Ethylacetate s-Butanol 13. Pyridine Tetrahydrofura 14. Toluene Chloroform Cyclohexane Vial Equilibration Time: 10 min Pressurization Time: 0.2 min Loop Fill Time: 0.15 min 13,14 Loop Equilibration Time: 0.05 min 17 Injection Time: 1.00 min 11
20. 21. 22. 23. 24. 25. 26. 27.
4
10 13
Injection: Oven: Detector:
Methanol Ethanol Ether Acetone i-Propanol Acetonitrile Methylene Chloride t-Butanol 3
12
30°C
Carrier: Column:
1. 2. 3. 4. 5. 6. 7. 8.
8
10
Headspace Conditions Carrier Gas Pressure: Oven Temp: Loop Temp: Transfer Line Temp: Vial Pressure:
Vial Equilibration Time: Pressurization Time: Loop Fill Time: Loop Equilibration Time: Injection Time:
10 min 0.2 min 0.15 min 0.05 min 1.00 min
5
3.5 psi 85°C 95°C 110°C 10 psi
Chemical/Industrial
Fast GC Analysis of USP Solvents 1. 2. 3. 4. 5.
Methanol Chloride (25 ppm) Chloroform (12 ppm) Benzene (25 ppm) Trichloroethylene (25 ppm) 1, 4-Dioxane (25 ppm)
Solvent Paint Thinner 250°C 30°C/min
90°C 40°C 1.7 min
6°C/min 3
1. 2. 3. 4. 5. 6.
7. 8. 9. 10. 11. 12.
Methanol Ethanol Ethyl ether Acetone Isopropanol Cyclohexane
Methyl acetate n-Propanol MEK Hexane Isobutanol Benzene
1 23 56 8 9 4
n-Butanol MIBK n-Butyl acetate Ethyl benzene m, p-Xylene o-Xylene 100°C 5°C/min
250°C 15°C/min
50°C 2°C/min
35°C (2 min)
1
13. 14. 15. 16. 17. 18.
11 12 13
14
15
16 17 18
10 7
4
5
2
2 4 Time (min) 6890 HP-Fast GC Residual Solvent Column (Part No. 19095V-420) Helium, 30 cm/min, constant flow Temperature program listed above Headspace, 180°C, Split 7/1 FID, 260°C
Carrier: Oven: Injection: Detector:
6 Carrier: Column:
Rapid Analysis of Water in Organic Solvents
Ethylene oxide Ethyl formate Ethyl alcohol Water 2-Ethoxyethanol 2-Ethoxyethyl acetate
7. 8. 9. 10. 11.
Hydroxy acetate Acetic acid Formic acid Ethylene glycol/monoformate Ethylene glycol/monoacetate
87 ppm Water in Aniline
210°C 10°C/min
100°C
5°C/min
60°C 1 min
0 TIC (MSD)
5 2 1
0
Carrier: Column: Injection: Oven: Detector:
Helium, 25 psi HP-1 (Cross-Linked Methyl Silicone), 50 m x 0.32 mm x 1.0 m (Part No. 19091Z-215) Split, 1 l Temperature program listed above FID
Injection: Oven: Detector:
Ethoxyethanol 1. 2. 3. 4. 5. 6.
12 min
Applications
GC: Column:
6
10
0.2
0.4
11
0.6
0.8
1
1.2
Time (min)
4 3
78 9 5
10 Time (min)
Column:
15
20
Helium, 10 ml/min HP-FFAP (Crossed-Linked Polyethylene Glycol), 30 m x 0.53 mm x 1.0 m (Part No. 19095F-123) Split (10:1) Temperature program listed above MSD (280°C)
Carrier: Oven: Inlet: Inlet temperature Injection volume: Detector:
Pub No.: 5054-8215
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HP-INNOWax 530 m x 15 m 1.0 m (Part No. 19095N-121) 15 mL/min helium, constant flow mode 100°C (1.5 min), post temp: 175°C (2.5 min) Purge packed; 240°C 0.5 l Thermal conductivity (TCD), 240°C
Pub No.: 5966-4131
411
Applications
Chemical/Industrial
GC and GC/MS Applications
Solvents 1. 2. 3. 4. 5. 6. 7. 8.
Solvent Purity Chloroform 9. 10. 11. 12. 13. 14. 15.
Isopropanol Unknown Methyl ethyl ketone Ethyl acetate n-Butyl alcohol Ethyl cellosolve Methyl isobutyl ketone Toluene
n-Butyl acetate Diacetone alcohol p-Xylene Cellosolve acetate o-Xylene Butyl cellosolve Butyl cellosolve acetate
1. Chloroform 2. Tetrachloromethane
100°C (2 min) 20°C/min
30°C 12 min
200°C (2 min) 5°C/min
70°C 3
1 2
45 6
12 13 14
10 7 8 9
11
15
1
17 min Carrier: Column:
25 min Carrier: Column: Injection: Oven: Detector:
Helium, 30 psi HP-1 (Cross-Linked Methyl Silicone), 50 m x 0.2 mm x 0.52 m (Part No. 19091Z-205) Split, 1 l Temperature program listed above TCD
Purity of Ethylbenzene
Styrene
ASTM Method D5060 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
60°C 1 min
4°C/min
290°C 6°C/min 120°C
4 1 6
6
12 1 0
Injection: Oven: Detector:
1. Styrene 2. Diphenyl cyclobutane 3. Triphenyl hexanes
4
1
Sample: Carrier: Column:
220°C 20°C/min
92°C (4.5 min)
Hydrocarbon Benzene Toluene Ethylbenzene p-Xylene m-Xylene Cumene o-Xylene Propylbenzene Styrene
Injection: Oven: Detector:
Helium, 4.4 ml/sec HP-1 (Cross-Linked Methyl Silicone), 30 m x 0.53 mm x 2.65 m (Part No. 19095Z-123) Split (50:1), 1 l Temperature program listed above TCD
3 2
5 5
3
10 Time (min)
7 8
9 10
10
11 Time (min)
31 min
15
Neat, 99%+ Helium, 32 cm/sec, 19.9 psi (60°C), 2.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 60 m x 0.32 mm x 0.5 m (Part No. 19091N-216) Split (100:1), 0.5 l, inlet 220°C Temperature program listed above FID 270°C
Carrier: Column: Injection: Oven: Detector:
Hydrogen, 55 cm/sec HP-101 (Methyl Silicone Fluid), 50 m x 0.32 mm x 0.3 m (Part No. 19091Y-015) On-column, 1.5 l Temperature program listed above FID Pub No.: 5953-1540
412
BioPharmaceutical
BioPharmaceutical Purity of p-Xylene: ASTM Method D3798 1. 2. 3. 4. 5. 6.
Hydrocarbon Toluene Ethylbenzene p-xylene m-Xylene o-xylene
Styrene 220°C 20°C/min
92°C (4.5 min) 60°C 1 min
4°C/min 4
1. 2. 3. 4. 5.
Vinyl acetate Ethyl benzene o-Xylene Styrene a-Methyl styrene 3
1
5
100°C (2 min) 85°C 1 min
4
5°C/min
4 5
5 3
6
2
Sample: Carrier: Column:
5
10
10 Time (min)
11 12 Time (min)
15
Neat, 99%+ Helium, 32 cm/sec, 19.9 psi (60°C), 2.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 60 m x 0.32 mm x 0.5 m (Part No. 19091N-216) Split (100:1), 0.5 l, inlet 220°C Temperature program listed above FID 270°C
Injection: Oven: Detector:
Pub No.: 5953-1543
Analysis of Ethylene Oxide in a Pharmaceutical Formulation 200°C 25°C/min
75°C 50°C
5°C/min
Carrier: Column: Injection: Oven: Detector:
3 min Hydrogen HP-FFAP (Cross-Linked PEG-TPA), 10 m x 0.53 mm x 1.0 m (Part No. 19095F-121) On-column, 1 l Temperature program listed above FID
Underivatized Drugs 1. 2. 3. 4. 5. 6. 7.
Ethosuximide Methylpropylsuccinimide Barbital Amobarbital Pentobarbital Secobarbital Mephobarbital
8. 9. 10. 11. 12. 13. 14.
Phenobarbital Procaine Methadone Amitriptyline Cocaine mipramine Nortriptyline
15. 16. 17. 18. 19. 20. 21.
Carbamazepine Desipramine Primidone Phenytoin Codeine Phenytoin Quinine
acetonitrile
280°C 80°C
20°C/min
ethylene oxide 1 2
8
3 2
3
4
5 Time (min)
4
5 7 6
13 11 12 9 10
6
14 15 16 18 17 19 20 21
Inlet: Column:
Split/10:1, 1 l, 250°C HP-WAX, 60 m x 0.53 mm i.d. x 1 m (Part Number 19095X-126) Carrier Gas: Hydrogen Head Pressure: 25 kPa at 50°C constant flow mode Flow: 5.2 ml/min Oven Temperature: Temperature program listed above GC System: FID, 250°C Pub No.: 5968-0322E
27 min Carrier: Column: Injection: Oven: Detector:
Hydrogen, 50 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.32 mm x 0.52 m (Part No. 19091B-112) On-column, 5 ng/component, 1 l Temperature program listed above FID
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413
Applications
1
0
2
3
Applications
BioPharmaceutical
GC and GC/MS Applications
Underivatized Drugs 1. 2. 3. 4. 5. 6. 7. 8.
Opiates
9. 10. 11. 12. 13. 14. 15.
Ethosuximide MPS Barbital Probarbital Aprobarbital Talbutal Meprobamate Pentobarbital
16. 17. 18. 19. 20. 21. 22.
Methapyrilene Phenobarbital Amitriptyline Imipramine Nortriptyline Primidone Desipramine
Carbamazepine Primidone/phenytoin Diazepam Desmethyl diazepam Phenytoin Flurazepam Librium
1. 2. 3. 4. 5.
20°C/min
45°C 1 min
1 2
6
8 34
2°C/min
5
1
14 17 13 15 16 12 11
10
3 4
1819 20
9
50°C/min
200°C 1 min
2
7
5
21
1
22
1.5
GC: Carrier: Column: Injection: Oven: Detector:
5 min Helium, 30 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.32 mm x 0.17 m (Part No. 19091B-012) Split, 1 l, 10 ng/component Temperature program listed above FID
Injection: Oven: Detector:
300°C
210°C 200°C (5 min)
Carrier: Column:
Meperidine Methadone Codeine Ethyl morphine Morphine
2 Time (min)
2.5
6890 Helium, 0.5 ml/min constant flow HP-1, 10 m x 100 m x 0.1 m (Part No. 19091X-141) 1 l sample, split (10:1) Temperature program listed above MSD
Pub No.: 5965-6692
Drugs of Abuse GC: Carrier: Column:
6890 Helium, 0.5 ml/min constant flow HP-1, 10 m x 100 m x 0.1 m, (Part No. 19091X-141) Split (10:1), 1 l sample Temperature program listed above FID (325°C)
Injection: Oven: Detector: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
Caffeine Glutethimide Lidocaine Phenobarbital EDDP Methaqualone Methadone Cocaine Desipramine Carbamazepine
300°C 50°C
50°C/min
1 min
6
9 7 10
3 2 5
4 1
8
1
1.5
2
2.5
3
3.5
Time (min) Pub No.: 5965-6692
414
BioPharmaceutical
Underivatized Drugs 1. 2. 3. 4. 5.
6. 7. 8. 9. 10.
Barbital Pentobarbital Diphenhydramine Phenobarbital Methazualone
Codeine Morphine Quinine Haloperidol Strychnine
1. Phenobarbital, 100 ng 2. Primidone, 200 ng 300°C 160°C (5 min)
Carrier: Column:
3 2
Helium, 0.8 ml/min HP-1 (Cross-Linked Methyl Silicone), 12 m x 0.2 mm x 0.33 m (Part No. 19091-60312) Splitless, 1 l, 50 ng/ml Temperature program listed above MSD
Injection: Oven: Detector:
1
2
1
40°C/min
50°C 2 min
5
8°C/min
6 10 4
3 min
9 7
Carrier: Column:
8 Injection: Oven: Detector:
24 min
Helium, 30 cm/sec HP-1 (Cross Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 m (use 5 m only) (Part No. 19095Z-121) Splitless, 1 l 220°C FID Pub No.: 5953-8066
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.
Barbiturate and Acidic Drugs
Methabarbital Barbital Allobarbital Aprobarbital Butabital Amobarbital Pentobarbital Methohexital Secobarbital Hexobarbital Phenobarbital Mephobarbital
40°C/min
150°C 1 min
8
4 3
1
1. 2. 3. 4. 5. 6.
280°C
10
7. 8. 9. 10. 11.
Ethosuximide Barbital Methyprylon Aprobarbital Butalbital Amobarbital
100°C
11
6
11
1
9
Phenobarbital Methaqualone Primidone Carbamazepine Dipenyhydanation 280°C 8 min 10°C/min
1 min
7
5
12. 13. 14. 15. 16.
Pentobarbital Secobarbital Meprobamate Carisoprodal Glutethimide
13
3
12
4
2
57 6 8
12 15
2
14
10 9
1 GC: Carrier: Column: Injection: Oven: Detector:
1.5
2 Time (min)
6890 Helium, 0.6 ml/min constant flow HP-1, 10 m x 100 m x 0.1 m, (Part No. 19091X-141) Split (10:1), 1 l sample Temperature program listed above FID (300°C)
2.5
Applications
Barbiturates
3
Pub No.: 5965-6692
0
Column: Carrier: Oven: Injection: Detector:
5
10
Time (min)
15
HP-35, 30 m x 0.53 mm x 1.0 m Helium, 40 cm/sec, constant flow Temperature program listed above Splitless, 1 l, 62 g/ml per compound FID (300C)
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20
16
25
Pub No.: 5965-1622
415
Applications
BioPharmaceutical
GC and GC/MS Applications
Urine Drug Screen 1. 2. 3. 4. 5. 6. 7.
Amphetamine Methamphetamine Meperidine Phencyclidine (PCP) Methadone Proposyphene Amitriptyline 12
Serum Drug Screen 8. 9. 10. 11. 12. 13.
3
Cocaine Imipramine Cyheptamide (ISTD) Codeine Diazepam Flurazepam 45°C 1.5 min 4
300°C
1. 2. 3. 4. 5.
Ethchlorvynol Methprylon Butalbital Amobarbital Pentobarbital
6. 7. 8. 9. 10.
11. 12. 13. 14.
Secobarbital Glutethimide Phenobarbital Methaqualone Amitriptyline
Imipramine Cyheptamide (ISTD) Phenytoin Diazepam 300°C (2 min)
6°C/min
5
1
2
45 6 7
8 9
3
6°C/min
45°C 1.5 min 12
8 10 6
13 7
13
9
11
14 10 11
12
22 min
12 min Carrier: Column: Injection: Oven: Detector:
Carrier: Column:
Hydrogen 80 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 50 m x 0.32 mm x 0.52 m (Part No. 19091B-115) Splitless, 1 l Temperature program listed above FID
Injection: Oven: Detector:
Alkaloids/Barbiturates 1. 2. 3. 4. 5. 6.
Barbital NC16 Amobarbital Pentobarbital Secobarbital Phenobarbital
7. 8. 9. 10. 11.
Hydrogen, 80 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 50 m x 0.32 mm x 0.52 m (Part No. 19091B-115) Splitless, 1 l Temperature program listed above FID
Alkaloid Street Drugs
Procaine Methadone Cocaine Codeine Heroin
280°C 14°C/min
50°C 1.5 min
1. 2. 3. 4. 5. 6. 7.
Procaine Methadone Cocaine Codeine Morphine Heroin Quinine
280°C 15°C/min 170°C 1 7 2
5
3 2
1
4
8 3
4
5
6
9
10
6 11
7
8 min 13 min Carrier: Column: Injection: Oven: Detector:
416
Hydrogen, 165 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.32 mm x 0.17 m (Part No. 19091B-012) Splitless, 1 l Temperature program listed above FID Pub No.: 5963-1708
Carrier: Column: Injection: Oven: Detector:
Helium, 20 ml/min HP-1 (Cross-Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 m (Part No. 19095Z-121) Direct Injection,1 l, 12 ng/component, (packed column injection port) Temperature program listed above NPD
BioPharmaceutical
Drug Standard Mixture 1. 2. 3. 4. 5. 6.
Drugs in Urine
Caffeine Methadone Cocaine Codeine Monoacetyl morphine Diacetylmorphine
280°C (2.4 min) 50°C/min
50°C
1 2
1. 2. 3. 4. 5.
Amobarbital Phencyclidine Glutethimide Imipramine (IS) Codeine
260°C (5 min) 160°C 1 min
25°C/min
3 3 6
2 4
4 5 1 5.0 Time ( min)
6.0
5
7.0
0 Carrier: Column: Injection: Oven: Detector:
Helium, 0.8 ml/min HP-1 (Cross-Linked Methyl Silicone), 12 m x 0.2 mm x 0.33 m (Part No. 19091-60312) Splitless, 1 l, inlet 250°C Temperature program listed above MSD Pub No.: 5956-4809
Drug Standard 1. 2. 3. 4.
d-Amitriptyline d-Imipramine Cyheptamide d-Valium 130°C (.5 min)
Carrier: Column: Injection: Oven: Detector:
2
4 Time (min)
6
8
Helium 65 cm/sec, 8.5 psi, constant flow HP-50+ (Cross-Linked 50% Phenyl Methyl Silicone), 30 m x 0.53 mm x 1.0 m (Part No. 19095L-023) Splitless, 1 l, inlet 275°C Temperature program listed above FID 300°C
Drugs in Urine 275°C (5 min) 230°C (.5 min)
18°C/min
16°C/min
180°C (.5 min) 25°C/min
30°C/min
1. 2. 3. 4. 5. 6. 7.
Nicotine PCH-(1-phenylcyclohexene) Phenmetrazine Cocaine metabolite I Phendimetrazine Nicotine metabolite I
8. 9. 10. 11. 12. 13.
Nicotine metabolite II Caffeine Phenobarbital Cocaine Homocaine Phenytoin
290°C (5 min)
260°C (5 min)
55°C (1 min)
5°C/min
13°C/min 110°C 3
3 4 6
1
2
2 5
21 min Carrier: Column: Injection: Oven: Detector:
11
8
4 7
9
10
12 13
17 min
Helium flow adjusted to maintain Cyheptamide RT = 15.00 min Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.32 mm x 0.52 m (Part No. 19091B-112) Splitless, 1 l Temperature program listed above FID Pub No.: 5956-4809
Carrier: Column: Injection: Oven: Detector:
Helium, 28 cm/sec Ultra 1 (Cross-Linked Methyl Silicone), 25 m x 0.32 mm x 0.52 m (Part No. 19091A-112) Splitless, 1 l Temperature program listed above MSD
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417
Applications
4.0
Applications
BioPharmaceutical
GC and GC/MS Applications
Barbiturates and Antidepressants 1. 2. 3. 4. 5.
6. 7. 8. 9. 10.
Barbital Amobarbital Phenobarbital Secobarbital Meprobamate
Phenobarbital Amitriptyline Imipramine cis-Doxepin Nortriptyline
Tricyclic Antipsychotics 11. 12. 13. 14. 15.
trans-Doxepin Despiramine Protiptyline Desmethyl doxepin Clomipramine 230°C (10 min)
23 5 4
9 6 10 11
Triflupromazine Promethazine Promazine Chlorpothixene Thioridazine
290°C (10 min) 250°C
1
10°C/min
10°C/min
3 min
4
3
10°C/min
225°C (6.5 min) 115°C 1 min
1
1. 2. 3. 4. 5.
2
5
7 8 12 13 14 15
12 min
Carrier: Column: Injection: Oven: Detector:
10 min
Hydrogen, 80 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.32 mm x 0.17 m (Part No. 19091B-012) Splitless, 1 l, 15 ng/component Temperature program listed above FID
Carrier: Column: Injection: Oven: Detector:
Antipsychotics 1. 2. 3. 4.
Hydrogen, 106 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 12 m x 0.2 mm x 0.33 m (Part No. 19091B-101) Split (75:1), 1 l Temperature program listed above Pub No.: 5954-7614 FPD
Antiepileptic Drugs
Promethazine Promazine Chlorpromazine Trifluoroperazine
290°C
2 250°C 3 min
20°C/min
1. 2. 3. 4.
Ethotoin PEMA n-Des Phenobarbital 1
1
5. 6. 7. 8.
2
Carbepoxide 10/11 Primidone Phenyltoin 100°C ISTD
3 4
6
14 min
5 min
Injection: Oven: Detector:
418
8 7
3
Hydrogen, 106 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 12 m x 0.2 mm x 0.3 m (Part No. 19091B-101) Splitless, 1 l Temperature program listed above NPD
15°C/min
4
5
Carrier: Column:
230°C
Carrier: Column: Injection: Oven: Detector:
Helium, 14 psi Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 12 m x 0.32 mm x 0.17 m (Part No. 19091B-012) Split (35:1), 1 l Temperature program listed above NPD
BioPharmaceutical
Antiepileptic Drugs in Plasma 1. 2. 3. 4.
Valproic acid Ethosuximide Phenobarbital Primidone
Anticonvulsants
5. Carbamazepine 6. Phenytoin 7. Clonazepam
200°C (16 min) 10°C/min
1. 2. 3. 4.
5. 6. 7. 8.
Ethosuximide Methylpropylsuccinimide Mephobarbital Phenobarbital
Carbamazepine Primidone Phenytoin Methylphenytoin
260°C
100°C 10°C/min
75°C
1
12 3
2
7
5
3 4
6
12 min Carrier: Column: Injection: Oven: Detector:
8
20 min
Nitrogen at 4 ml/min HP-1 (Cross-Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 m (Part No. 19095Z-121) Splitless, 1 l, 0.1 mg/ml Temperature program listed above FID Pub No.: 5954-9183
Antiepileptic Drugs in Plasma 1. Caproic acid 2. Valproic acid 3. Ethosuximide
7
Carrier: Column: Injection: Oven: Detector:
Hydrogen, 50 cm/sec HP-1 (Cross-Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 m (Part No. 19095Z-121) On column, 1 l Temperature program listed above Pub No.: 5956-4809 FID
Amphetamines Injected as Salts 140°C 2 min 80°C 2 min
1. Amphetamine sulfate 2. Methamphetamine HCl
10°C/min 2
Applications
4
6 5
1
2 1
0 Carrier: Column: Injection: Oven: Detector:
3
5 10 Time (min)
1.5 min
Helium, 20 ml/min HP-1 (Cross-Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 m (Part No. 19095Z-121) Splitless, 1 l Temperature program listed above FID Pub No.: 5954-9183
Carrier: Column: Injection: Oven: Detector:
Helium, 30 ml/min HP-1 (Cross-Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 m (Part No. 19095F-121) Split (30:1), headspace 50°C isothermal FID
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419
Applications
BioPharmaceutical
GC and GC/MS Applications
Cholesterol
Blood Alcohols 4. Palmitic acid 5. Stearic acid 6. Cholesterol
1. C6 2. C8 3. C10
300°C (5 min) 200°C (1 min) 160°C 1 min
10°C/min
20°C/min
1. 2. 3. 4.
5. 6. 7. 8.
Hold up time to Methanol Acetaldehyde Ethanol
Acetone Iso-Propanol N-Propanol (ISTD) N-Butanol
165°C 0.5 min 15°C/min
120°C 1 min
1 2 3 5 6 4
7 4
5
2
8
6
3
1
20 min
0
Column: Carrier: Column: Injection: Oven: Detector:
Helium, 25 psi Ultra 1 (Cross-Linked Methyl Silicone), 25 m x 0.2 mm x 0.33 m (Part No. 19091A-102) Split, 1 l Temperature program listed above FID
Oven: Inlet: Detector:
Flumethasone
1
0.5
1.5 2 Time (min)
2.5
HP-Blood Alcohol Column 7.5 m x 0.32 mm (Part No. 19091-S510) Temperature program listed above 270°C, constant flow, 68 cm/sec Helium FID 250°C
Solvents in Blood by Headspace 280°C
Constant Flow 50°C
Pressure Programming
AB C
20°C/min
Back Pressure Regulated On-Col umn
1. 2. 3. 4. 5. 6.
Methyl ethyl ketone Benzene Methyl isobutyl ketone Toluene Methyl n-butyl ketone Ethylbenzene
7. 8. 9. 10. 11.
p-Xylene m-Xylene 1-Butanol o-Xylene Styrene
110°C 40°C 10 min
7 1
Column: Injection: Oven: Detector:
420
30 min A. Pressure program: 2 psi to 7 psi at 0.3 psi/min B. Constant flow: 2 psi at 50°C C. Constant pressure: 2 psi HP-1 (Cross-Linked Methyl Silicone), 5 m x 0.53 mm x 2.65 m (Part No. 19095S-100) On column, 2 l, inlet temperature program: 50°C for 1 min, 150°C/min to 300°C Temperature program listed above ECD Pub No.: 5952-6975
0
Sample: Carrier: Column: Injection: Oven: Detector:
5
5°C/min
9
2
Carrier:
3
3
10
4
5
15 Time (min)
6
8 10
11
20
1 ml blood and 100 l IS (1-butanol) Helium, 25 cm/sec 3.4 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.53 mm x 1.0 m (Part No. 19095N-123) Split (2:1), 1 ml, inlet 180°C Temperature program listed above FID 220°C
Consumer/Foods/Flavors/Fragrances
Consumer/Foods/Flavors/Fragrances Saturated Triglycerides C2 to C22 Separated on Short HP-1 column 7. 8. 9. 10. 11.
Triacetin (2:0) Tributyrin (4:0) Tricaproin (6:0) Tricaprylin (8:0) Tricaprin (10:0) Trilaurin (12:0)
Trimyristin (14:0) Tripalmitin (16:0) Tristearin (18:0) Triarachidin (20:0) Tribehenin (22:0)
1
325°C 5 min 80°C 1 min
4
Pseudomonas Aeruginosa Methyl Ester: 6. C16:1 CIS 9 1. C10:0 30H 7. C16:1 2. C12:0 8. C16:0 3. C12:0 20H 9. C18:1 4. C12:0 30H 10. C18:0 5. C14:0
15°C/min
5°C/min
170°C 5
6
7
8
9
6
10
GC: Carrier: Column: Inlet: Oven: Detector:
5
10 Time (min)
15
1
20
2 34
8
Carrier: Column:
GC: Carrier: Column: Inlet: Oven: Detector:
10
6
89
20 min
Hydrogen Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.2 mm x 0.33 m (Part No. 19091B-102) Split (100:1) Temperature program listed above FID Pub No.: 5953-1857
Injection: Oven: Detector:
1. 2. 3. 4. 5. 6. 7. 8. 9.
C16:0 C16:1 C18:0 C18:1 C18:2 C18:3 C20:0 C22:0 C24:0
1. 2. 3. 4.
5. 6. 7. 8.
C16:0 C16:1n9 cis C18:0 C18:1n9 cis
C18:1n11cis C18:2n9, 12ncis C18:3n9, 12ncis, n15 cis C20:0
4
5
0
1 2 5
Derivatized Greek Olive Oil (FAMEs) Cis/Trans FAMEs Column
4
3
10
20 min
Greek Olive Oil (Methyl Ester)
2
7
3 4
9
5
6890 Hydrogen, constant flow 138 cm/sec, 1.1 psi (10 ml/min) HP-1, 5 m x 0.53 mm x 0.15 m (Part No. 19091Z-220) EPC cool on-column Temperature program listed above FID 360°C
1
5°C/min
170°C
7
11 0
270°C (2 min)
270°C (2 min)
2
3
Pseudomonas Cepa Methyl Ester: 6. C16:0 30H 1. C14:0 7. C18:1 Trans 9 2. C14:0 30H 8. C18:0 3. C16:1 CIS 9 9. C19:0 Cyclo 4. C16:0 5. C17:0 Cyclo
Applications
1. 2. 3. 4. 5. 6.
Fatty Acid Profile of Pseudomonas
1
6 7
9
8
15 20 Time (min)
25
6890 Helium, constant flow 46.6 psi HP-INNOWax, 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) 1.5 l, 260°C, deactivated liner with glass wool 150°C (1 min), 2.9°C/min 230°C (1 min) FID 260°C
2
30
0
Sample: Carrier: Column: Injection: Oven: Detector:
2
4
3 5 6 Time (min)
6 7 8
8 10
Olive Oil Hydrogen at 40 cm/sec HP-23, 30 m x 0.32 mm x 0.25 m (Part No. 19091H-113) Split (100:1), 1 ml, 250°C Isothermal at 175°C FID 300°C, Nitrogen make up gas at 30 ml/min
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421
Applications
Consumer/Foods/Flavors/Fragrances
GC and GC/MS Applications
Fatty Acid Profile of Salmonella Choleraesuis Methyl Ester: 1. C12:0 2. C14:0 3. DD 4. C14:0 30H 5. C16:1 CIS 9
6. 7. 8. 9.
270°C
C16:0 C17:0 Cyclo C18:1 C19:0 Cyclo
170°C
4 56
2
Trichloroesters of Fatty Acids Straight Chain
5°C/min
1. 2. 3. 4. 5. 6. 7.
8. 9. 10. 11. 12. 13.
Acetic acid Propanoic Butyric Valeric Caproic Heptanoic Octanoic
Nonanoic Decanoic Undecanoic Lauric Tridecanoic Myristic
14. 15. 16. 17. 18. 19.
Pentadecanoic Palmitic Heptadecanoic Stearic Nonadecanoic Arachidic
8
7
85°C
265°C (10 min) 7°C/min
5 min
1 1
2
3 4
15
11
5 6
9 10
7 8
12
9
17
13 14
16
18 19
3 46 min 20 min Carrier: Column:
Hydrogen Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.2 mm x 0.33 µm (Part No. 19091B-102) Split (100:1) Temperature program listed above FID Pub No.: 5953-1857
Injection: Oven: Detector:
Vegetable Oil Fatty Acid Methyl Esters 1. 2. 3. 4. 5. 6.
7. 8. 9. 10. 11.
C14:0 C16:0 C18:0 C18:1 C18:2 C18:3
225°C 150°C 1 min
Hydrogen, 4 ml/min HP-5 (Cross-Linked 5% Phenyl Methyl Silicone), 30 m x 0.53 mm x 0.88 m (Part No. 19095J-023) Split (10:1), 1 l Temperature program listed above ECD
Injection: Oven: Detector:
Fatty Acid Methyl Esters 260°C (7 min)
C20:0 C20:1 C22:0 C22:1 C24:0
Carrier: Column:
5°C/min
15°C/min
1. 2. 3. 4. 5.
6. 7. 8. 9.
C9:0 C10:0 C11:0 C10:20H C10:30H
6
2
10. 11. 12. 13.
C12:0 C13:0 C14:0 C15:0
8
4
14. 15. 16. 17.
C14:20H C14:30H C16:0 C17:0
C16:20H C18:0 C19:0 C20:0
12 15
2 1
3
10
3
7
9
7
13
16
11
5
4
1
17
9
10
5
8
14
11
6
0 Sample: Carrier: Column: Injection: Oven: Detector:
422
2
4
6
8 10 Time (min)
12
14
16
25 g/l in methylene chloride Helium, 40 cm/sec, 14 psi (150°C), 2.1 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.32 mm x 0.5 m (Part No. 19091N-213) Split (45:1), 1 l, inlet 220°C Temperature program listed above FID 275°C
3 GC: Sample: Carrier: Column: Injection: Oven: Detector:
3.5
4
4.5 5 Time (min)
5.5
6
6890 FAME Standards Helium 68.4 (64 cm/sec), constant flow HP-1MS, 20 m x 0.10 mm x 0.40 mm (Part No. 19091S-942) 1 ml 50:1, split 275°C 70°C (1 min), to 180°C at 80°C/min, to 300°C at 40°C/min, 300°C (1 min) Pub No.: 5965-7874 FID 300°C
Consumer/Foods/Flavors/Fragrances
Polyunsaturated Fatty Acid Methyl Esters 1. 2. 3. 4. 5. 6. 7. 8.
C14:0 C16:0 C16:1w7 C18:0 C18:1w9 C18:1w7 C18:2w6 C18:3w3 4
9. 10. 11. 12. 13. 14. 15. 16. 5
C20:1w9 C20:2w6 C20:3w6 C20:4w6 C20:5w3 C22:4w6 C22:5w3 C22:6w3
150°C 1 min
6
12
FAMEs C14-C24 250°C (5 min)
200°C
2°C/min
15°C/min
1. 2. 3. 4. 5.
6. 7. 8. 9.
Myristoleate Palmitate Palmitoleate Stearate Arachidate 1 2
Eicosenoate-cis-11 Behenate Erucate 180°C Nervonate 1 min
10°C/min
3 4
5
14
2
250°C (8 min)
8 6
7
7 8
11 9 10
1
0
10
Sample: Carrier: Column:
15 Time (min)
13
16 15
20
25
9
0
50 g/l in methylene chloride Helium, 30 cm/sec, 10.7 psi (150°C), 1.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.32 mm x 0.5 m (Part No. 19091N-213) Split (60:1), 0.5 l, inlet 220°C Temperature program listed above FID 275°C
Injection: Oven: Detector:
Fatty Acid Methyl Esters 1. 2. 3. 4. 5.
C3 C4 C5 C6 C7
6. 7. 8. 9. 10.
11. 12. 13. 14. 15.
C8 C9 C10 C11 C12
2
4
Sample: Carrier : Column:
6
8 10 Time (min)
12
14
16
0.1-0.2% in methyl formate Helium, 45 cm/sec, 16.8 psi (180°C), 2.3 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.32 mm x 0.5 m (Part No. 19091N-213) Split (20:1), 0.5 l, inlet 250°C Temperature program listed above FID 275°C
Injection: Oven: Detector:
Free Fatty Acids
C14 C16 C18 C20 C22
250°C (5 min) 10°C/min
50°C 3 min
5
1. 2. 3. 4. 5. 6.
7. 8. 9. 10. 11. 12.
C2 C3 C4 C5 C5-Iso C6
13. 14. 15. 16. 17. 18.
C7 C8 C10 C12 C14 C14:1
C16 C16:1 C18 C18:1 C18:2 C18:3
250°C (5 min) 120°C 1 min
10°C/min
Applications
3
12 1
13 14 4 8 6 3
7
10
15
1 1
9 2
34 5
67 8
10
11 12 13
9
14 16
15 17 18
12
0 Sample : Carrier : Column : Injection : Oven : Detector :
5
10
15 Time (min)
20
25
0
0.1-0.2% in methyl formate Helium, 40 cm/sec, 11.8 psi (50°C), 2.6 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.32 mm x 0.5 m (Part No. 19091N-213) Split (100:1), 0.5 l ml, inlet 220°C Temperature program listed above FID 275°C
Sample: Carrier: Column: Injection: Oven: Detector:
Time (min)
15
0.05 to 0.11% each in methylene chloride Helium 42 cm/sec, 24 psi (120°C) 1.8 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (40:1), 1 l, inlet 250°C Temperature program listed above Pub No.: 5091-6687E FID 280°C
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423
Applications
Consumer/Foods/Flavors/Fragrances
GC and GC/MS Applications
Purgeable Organics in Beer 1. 2. 3. 4. 5.
6. 7. 8. 9.
Ethanol n-propanol Ethyl acetate iso-amyl alcohol Ethyl butyrate
23
1
iso-Amyl acetate Ethyl caproate Ethyl caprylate Ethyl caprate -20°C 2 min
6
4
Alcohol Beverage Standard
7
180°C 6°C/min
1. 2. 3. 4. 5. 6.
7. 8. 9. 10. 11. 12.
Acetaldehyde Acetone Ethyl formate Ethyl acetate Acetal Methanol Ethanol
8
Diacetyl 13. n-amyl alcohol sec-butanol 14. Acetic acid 15. Propionic acid n-propanol iso-butanol n-butanol 200°C (2 min) iso-amyl alcohol 60°C 4 min
6
1
6°C/min
9 5 9
10
11
12
5 13
8
4 23
14
7
15
40 min 20 min Carrier: Column:
Helium, 25 cm/sec Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.32 mm x 0.52 m (Part No. 19091B-112) Split (100:1), 1 l Temperature program listed above Pub No.: 5953-1581 FID
Injection: Oven: Detector:
Brandy 1. 2. 3. 4. 5.
Carrier: Column:
Hydrogen HP-FFAP (Cross-Linked PEG-TPA), 50 m x 0.2 mm x 0.33 m (Part No. 19091F-105) Split (100:1), 1 l Temperature program listed above FID
Injection: Oven: Detector:
Bourbon 6. iso-Butanol 7. 2-Methyl-1-butanol or 3-Methyl-1-Butanol 8. Acetic acid 250°C (2 min)
Acetaldehyde Ethyl acetate Methanol Ethanol n-Propanol
150°C
250°C (2 min)
4
5
Sample: Carrier: Column: Injection: Oven: Detector:
424
8 5
8
23
1 10
7
6
Time (min)
20
20°C/min
5°C/min
35°C 5 min
2
6
0
Acetic acid n-Propanol iso-Butanol 2-Methyl-1-butanol or 3-Methyl-1-Butanol 150°C
7
1
5. 6. 7. 8.
Acetaldehyde Ethyl acetate Methanol Ethanol
5°C/min
35°C 5 min
4
20°C/min
1. 2. 3. 4.
3
30
Neat Helium, 33 cm/sec, 15.5 psi (35°C), 1.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (25:1), 1 l, inlet 220°C Temperature program listed above FID 280°C
0 Sample: Carrier: Column: Injection: Oven: Detector:
10
Time (min)
20
30
Neat Helium, 33 cm/sec, 15.5 psi (35°C), 1.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (25:1), 1 l, inlet 220°C Temperature program listed above FID 280°C Pub No.: 5962-0031E
Consumer/Foods/Flavors/Fragrances
Wine, Cabernet 1. 2. 3. 4. 5.
Whiskey
Acetaldehyde Ethyl acetate Methanol Ethanol n-Propanol
6. iso-Butanol 7. 2-Methyl-1-butanol or 3-Methyl-1-Butanol 8. Acetic acid 250°C (2 min) 150°C
n-Propanol Acetic acid Ethyl acetate iso-butanol
5. 6. 7. 8.
Acetaldehyde/diethylacetal 9. Ethyl octanoate Iso-amyl alcohol 10. C-10 A cid n-Amyl alcohol 11. Ethyl decanoate C-8 acid 12. C-12 Acid 13. Ethyl dodecanoate
5°C/min
35°C 5 min 4
20°C/min
1. 2. 3. 4.
1
4 6 7
8
240°C (16 min) 40°C 8 min
3 7
10°C/min
3 2 1
5
0
Injection: Oven: Detector:
2
10
Time (min)
20
30
1 1
1 13 2
40 min
Neat Helium, 33 cm/sec, 15.5 psi (35°C), 1.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (25:1), 1 l, inlet 220°C Temperature program listed above FID 280°C Pub No.: 5962-0031E, 5091-9464E
Scotch 1. 2. 3. 4.
9 1 8 0
Carrier: Column:
Helium, 5 psi Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 50 m x 0.32 mm x 0.52 m (Part No. 19091B-115) Split (30:1), 1 l Temperature program listed above MSD
Injection: Oven: Detector:
Perfume
Acetaldehyde Ethanol n-Propanol Ethylacetate
1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
5. Isobutanol 6. Acetal 7. 3-Methyl-1-butanol 8. 2-Methyl-1-butanol 5
2 3
Limonene Linalool Linalyl acetate Benzyl acetate Citronellol Benzene ethanol a-Methyl Ionone Carvocrol and geraniol iso-Amyl salicylate n-Amyl salicylate
11. 12. 13. 14. 15. 16. 17. 18. 19.
Commamyl acetate Acetylcedrene Diethyl phthalate 80°C Tonalid 1 min Coumarin Musk xylene Benzyl benzoate Benzyl salicylate 13 Musk ketone
8
4
10
7 3
1
1
Injection: Oven: Detector:
5
7
15
12 11
16 17
14
19
6 12 min
Carrier: Column:
9
2 8
5°C/min
18 6
4
250°C (2 min)
Applications
Sample: Carrier: Column:
5
6
0
Helium, 28 cm/sec HP-101 (Methyl Silicone Fluid), 50 m x 0.32 mm x 0.3 m (Part No. 19091Y-015) Split, 1 l 32°C isothermal FID Pub No.: 5963-7017E
Sample: Carrier : Column: Injection: Oven: Detector:
5
10
15 20 Time (min)
25
30
Neat Helium, 30 cm/sec, 0.9 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (10:1), 1 l, inlet 250°C Temperature program listed above MSD 280°C
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425
Applications
Consumer/Foods/Flavors/Fragrances
GC and GC/MS Applications
Fragrance Standard Sample 250°C (5 min) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.
Carrier: Column: Injection: Oven: Detector:
Ethyl acetate Diacetyl cis-3-Hexanol trans-2-Hexanal Prenyl acetate Benzaldehyde Limonene Maltol Octanol cis-3-Hexenylacetate p-Methyl cresol p-Cresol Nonanal Linalool Rose oxide Camphor Benzyl acetate Menthol alpha-Terpineol
20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.
Decanal Citronellol Cinnamic aldehyde Geraniol Indole Heliotropine Phenylpropyl acetate Eugenol Citronellyl acetate Vanillin Dimethyl anthranilate Cyclamen aldehyde Lilial Musk xylol Helional Methyl naphthyl ketone Hedione Isopropyl myristate Ethylene brassylate
11
50°C
5°C/min
1 min 17 35
38
29 5 14
16
28
15
1
36 27 20 21 19 30 18 31
6 7 12
Helium, 1 ml/min constant flow HP-1 (Cross-Linked Methyl Silicone), 30 m x 0.25 mm x 0.25 m (Part No. 19091Z-133) 1 l, Agilent 7673 with 250 m nanoliter adapter on-column injection; syringe (Part No. 5181-3321) Temperature program listed above MSD 280°C
22
23
5.00
10.00
15.00 20.00 Time (min)
37
25.00
30.00
Fragrance Standard Mix 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.
1-Limonene cis-3-Hexenal Prenyl acetate cis-3-Hexenyl acetate Rose oxide Hexenol Nonanal p-Methyl cresol Decanal Camphor Benzyl aldehyde Linalool Octanol Menthol Citronellyl acetate alpha-Terpineol Benzyl acetate Citronellol Geraniol
20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37.
Phenyl propyl acetate Maltol Cyclamen aldehyde Cinnamic aldehyde Isopropyl myristate Unknown Dimethyl anthranilate p-Cresol Eugenol Heliotropine Helional Indole Methyl naphthyl ketone Musk xylol Vanillin Ethylene brassylate Lilial Hidione
250°C (2 min) 80°C
9
33
18 25 26 20
5
4
13 11
5
35
21
31
24 7 10
14 15 12 17
34
29
19 22 23
27 28 30
8
Injection: Oven: Detector:
426
500 ppm in ethanol Helium, 30 cm/sec, 0.9 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 0.00 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) 0.2 l, Agilent 7673 with, nanoliter adapter, on-column Temperature program listed above MSD 280°C
5.00
36
16
6
3
2
Sample: Carrier: Column:
5°C/min
1 min
32
10.00
15.00 20.00 Time (min)
25.00
30.00
Consumer/Foods/Flavors/Fragrances
Man's Cologne 1. 2. 3. 4. 5. 6.
L-Limonene Unknown Linalool Linalyl acetate 1,2-Pronanediol Menthol
7. 8. 9. 10. 11. 12.
1-Octanol, 2,7-dimethyl alpha-Terpineol Benzyl acetate Geranyl acetate beta-Citronellol Geraniol 3
5
38. 39. 40. 41. 42. 43.
Benzyl alcohol Phenyl ethyl alcohol Anis aldehyde iso-Amyl salicylate Amyl salicylate Patchouli alcohol
6
13. 14. 15. 16. 17. 18.
11
Heliotropine OTMS Diethyl phthalate Coumarin Vanillin Musk ambrette
19. 20. 21. 22.
Benzyl benzoate Musk T Musk ketone Benzoic acid
250°C 2 min 80°C 1 min
5°C/min
25
19 23
1
9
27
22 12
4
7
8
10
15 13 14
16
18
24
20
28
5.00 10.00 15.00 20.00 25.00 30.00 Time (min) Neat Helium, 30 cm/sec, 0.9 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.25 mm x 0.25 m (Part No. 19091N-133) Split (10:1), 1 l, inlet 250°C Temperature program listed above MSD 280°C
Flavor Mixture Fenchone Thujone Benzaldehyde trans-Carveol Farnesol cis-Carveol trans-Geraniol
35.00
Cosmetics by Headspace 8. 9. 10. 11. 12. 13.
210°C 2 min
Citral Eugenol Vanillan trans-Isoeugenol trans-Citronellyl tiglate cis-Citronellyl tiglate
80°C 1 min
8°C/min
1. 2. 3. 4. 5. 6.
Cineole Limonene Menthone Menthol Carvone Anethole
200°C (5 min) 40°C 5 min 2
13
9
2
3 3
Carrier: Column: Injection: Oven: Detector:
5
5
8
Time (min)
6
10
7 46
4
1
5
1
0
8°C/min
Applications
Sample: Carrier : Column: Injection: Oven: Detector:
1. 2. 3. 4. 5. 6. 7.
26
21
17
12 11
10
15
Helium, 90 kPa., 2.2 ml/min constant flow Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.32 mm x 0.52 m (Part No. 19091B-112) Split (20:1), 1 l, inlet 250°C Temperature program listed above IRD, 280°C, Wide Band MCT, 550 to 4000 cm-1
25 min Carrier: Column: Injection: Oven: Detector:
Helium, 20 cm/sec PONA (Cross-Linked Methyl Silicone), 50 m x 0.2 mm x 0.5 m (Part No. 19091S-001) Split (20:1), headspace, 1 l Temperature program listed above Pub No.: 5953-8063 MSD
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427
Applications
Consumer/Foods/Flavors/Fragrances
GC and GC/MS Applications
Strawberry Syrup 1. 2. 3. 4. 5. 6.
Peppermint Oil
7. Ethyl benzoate Ethyl acetate 8. Citronellol Ethyl butyrate iso-Amyl acetate 9. Geraniol 10. Ethyl-3-phenyl oxiran carboxylate Amyl acetate 250°C (2 min) iso-Amyl butyrate 11. Strawberry aldehyde 12. Benzyl benzoate Amyl butyrate 60°C 10°C/min 1 min 2 34 1
1. 2. 3. 4.
5. 6. 7. 8.
Limonene Cineole Menthone Menthofuran
d-iso-Menthone Menthyl acetate Menthol Germacrene
250°C 10°C/min
60°C 1 min 7
3 2
11
4
5
6
10
6
1
5
7
8
12 89
0
Sample: Carrier: Column: Injection: Oven: Detector:
5
10 Time (min)
15
0
20
Neat syrup Helium, 40 cm/sec, 11.7 psi (60°C), 2.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.32 mm x 0.5 m (Part No. 19091N-213) Split (60:1), 0.2 l, inlet 220°C Temperature program listed above FID 275°C
Sample: Carrier: Column: Injection: Oven: Detector:
2
4
6
8 10 Time (min)
12
14
Neat Helium, 40 cm/sec, 11.7 psi (60°C), 2.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.32 mm x 0.5 m (Part No. 19091N-213) Split (60:1), 0.5 l, inlet 220°C Temperature program listed above FID 275°C
Analysis of Resoloids
Beeswax Absolute
360°C 90°C 40°C 1 min
Styrex Resin
Benzoin Siam
Carrier: Column: Injection: Inlet: Oven: Detector:
428
Helium 37 cm/sec (40°C), 1.8 ml/min constant flow HP-1 (Cross-Linked Methyl Silicone), 30 m x 0.25 mm x 0.25 m (Part No. 19091Z-433) On-column,1 l 50°C (0.1 min) to 370°C (5 min) at 50°C/min Temperature program listed above FID 375°C
16
25°C/min
10 min
Consumer/Foods/Flavors/Fragrances
SFE of Conifer Species 1. 2. 3. 4.
Tricyclene a-Pinene Camphene Bromononane (ISTD)
SFE of Fragrance in Liquid Detergent 275°C
5. Bornyl acetate 6. Diterpene 7. Diterpene
250°C 280°C (5 min)
220°C 50°C
20°C/min
10°C/min
3°C/min
35°C 1 min
trans-geraniol
4°C/min
-citronellol
1
benzyl iso-amyl ether
linalool 2
Carbon = 496 nm
5
4
Orange R
7
6
-myrcene
3
0
Carrier: Column: Injection: Oven: Detector:
10
20
30 Time (min)
40
50
Helium HP-1 (Cross-Linked Methyl Silicone), 25 m x 0.32 mm x 0.17 m (Part No. 19091Z-012) 1 l, inlet 280°C (0.80/ml extract density) Temperature program listed above AED
Beeswax
10 Carrier: Column: Injection: Oven: Detector:
20
30
40 50 Time (min)
60
70
Helium 28 cm/sec, 28.5 psi (35°C), 1.0 ml/min constant flow PONA, 50 m x 0.2 mm x 0.5 m (Part No. 19091S-001) 1 m x 0.53 mm retention gap (Part No. 19095-60610) On-column,1 l, oven track mode Temperature program listed above MSD 280°C
TMS Derivatives of Monosaccharide 230°C (10 min)
350°C (10 min) 130°C
10°C/min
5°C/min
0.5 min
Applications
150°C
15 min Carrier: Column: Injection: Oven: Detector:
20 min
Helium, 8 psi Ultra 1 (Cross-Linked Methyl Silicone), 25 m x 0.2 mm x 0.11 m (use 6 m only), (Part No. 19091A-002) Split, 1 l Temperature program listed above FID
Carrier: Column: Injection: Oven: Detector:
Helium, 16 psi Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.2 mm x 0.33 m (Part No. 19091A-102) Split, 1 l Temperature program listed above MSD
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429
Applications
Consumer/Foods/Flavors/Fragrances
GC and GC/MS Applications
Sulfur and Selenium in Garlic by Headspace 1. 2. 3. 4. 5. 6. 7. 7a.
8. 9. 10. 11. 12. 13. 14.
CH3-Se-CH3 C3H5-S-CH3 C3H5-Se-CH3 CH3-S-S-CH3 C3H5-S-C3H5 CH3-S-Se-CH3 C3H5-S-S-CH3 CH3-Se-Se-CH3
CH3-Se-S-C3H5 CH3-S-S-S-CH3 C3H5-S-S-C3H5 CH3-S-Se-S-CH3 CH3-S-S-S-C3H5 C3H5-S-S-S-C3H5 C3H5-S-S-S-C3H5
230°C 5 min 35°C 3 min
(B)
5°C/min
2
(A)
10
AED
2
4
S
10
7
5
12
1
13
3
9.00 10.00
11
7a
0
10
Time (min)
9
6
8 1
3 4
9 6
Carrier:
20
30
8
11
15.00 20.00 Time (min)
25.00
(A): Helium, 28 cm/sec, 18 psi (35°C), 1.2 ml/min constant flow (B): Helium, 28 cm/sec, 5.6 psi (35°C), 1.2 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 60 m x 0.32 mm x 0.25 m (Part No. 19091N-116) Splitless, SI inlet (140°C), Temperature program listed above AED 190°C and MSD 230°C
Column: Injection: Oven: Detector:
SFE of Hops
13
12
7
C
Se
MSD
5
Food Label by Headspace 250°C
1. Myrcene 2. b-Caryophyllene 3. Humulene
50°C
210°C (5 min) 40°C
5°C/min
3 min 1
2
6°C/min
3
0
10
Time (min)
20
30
35 min Carrier: Column: Injection: Oven: Detector:
430
Helium, 10 psi HP-5 (Cross-Linked 5% Phenyl Methyl Silicone), 30 m x 0.53 mm x 0.88 m (Part No. 19095J-023) On-column, 1 l Temperature program listed above FID 300°C Pub No.: 5952-2342
Sample: Carrier: Column: Injection: Oven: Detector:
One 1 x 2 inch label Helium, 35 cm/sec 4 psi (40°C), 5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 30 m x 0.53 mm x 1.0 m (Part No. 19095N-123) Split (10:1), 1 ml Headspace, inlet 220°C Temperature program listed above FID 300°C
Environmental
Environmental EPA 624 Volatile Organics 1. 2. 3. 4. 5.
Chloromethane vinyl chloride Bromoethane chloroethane Trichlorofluoromethane 1,1-Dichloroethylene Methylene chloride
6. 7. 8. 9. 10.
18. 19. 20. 21. 22.
trans-1,2-Dichloroethylene 1,1-Dichloroethane(IS) Bromochloromethane Chloroform 1,1,1-trichloroethane Carbon tetrachloride
Benzene 1,2-dichloroethane 1,4-Difluorobenzene(IS) Trichloroethene 1,2-Dichloropropane Bromodichloromethane
cis-1,3-Dichloropropene Toluene trans-1,2-Dichloropropene 1,1,2-Trichloroethane tetrachloroethene 27. Dibromochloromethane 28. Chlorobenzene
23. 24. 25. 26.
11. 12. 13. 14. 15. 16. 17.
140°C (5 min)
21 35°C
11
3 4 1 2
0
2
12 13 15 14
16
7
4
6
27
19
26
8
10
28
22
20
9 8 10
6 5
5°C/min
1 min
24 17
Ethyl benzene Bromoform Bromofluorobenzene(SS) 1,1,2,2-Tetrachloroethane 1,3 Dichlorobenzene 1,4-Dichlorobenzene 1,2-Dichlorobenzene
23
18
Carrier: Column:
25
Hydrogen, 39 psi, 5.3 ml/min (35°C) HP-624, 30 m x 0.32 mm x 1.8 m (Part No. 19091V-413) Split (20:1), 1 l, inlet 200°C 35°C (1 min) to 140°C (5 min) at 5°C/min FID 2505C
Injection: Oven: Detector:
12 14 Time (min)
16
18
20
22
Purgeable Halocarbons Chloromethane Vinyl chloride Bromoethane Chloroethane 1,1-Dichloroethylene Methylene chloride
7. 8. 9. 10. 11. 12.
trans-1,2 Dichloroethylene 1,1-Dichloroethane Bromochloromethane Chloroform 1,1,1-Trichloroethane Carbon tetrachloride 1
3 45
1,2-Dichloroethane Trichloroethylene 1,2-Dichloropropane Bromodichloromethane cis-1,3-Dichloropropene
12
7 2
13. 14. 15. 16. 17.
15
16 17
18. 19. 20. 21. 22.
18 22
trans-1,3-Dichloropropene 1,1,2-trichloroethane Tetrachloroethylene Dibromochloromethane Chlorobenzene
25
26
23. 24. 25. 26. 27.
Bromoform 1,1,2,2-tetrachloroethane 1,3 Dichlorobenzene(m) 1,4-Dichlorobenzene(p) 1,2-Dichlorobenzene(o)
Applications
1. 2. 3. 4. 5. 6.
27
8 6
14
19
140°C (5 min)
24
20
10
35°C
5°C/min
1 min 9
21
11
23
13 0
10 Carrier: Column: Injection: Oven: Detector:
20 Time (min) Hydrogen, 39 psi, 5.3 ml/min (35°C) HP-624, 30 m x 0.32 mm x 1.8 m (Part No. 19091V-413) Split (20:1), 1 l, inlet 200°C Temperature program listed above FID 250°C
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30
431
Applications
Environmental
GC and GC/MS Applications
Purgeable Organic Compounds 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.
14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26.
Dichlorodifluoromethane Chloromethane Vinyl chloride Bromomethane Chloroethane Trichlorofluoromethane 1,1-Dichloroethene Methylene chloride trans-1,2-Dichloroethene 1,1-Dichloroethane 2,2-Dichloropropane cis-1,2-Dichloroethene Bromochloromethane
Chloroform 1,1,1-Trichloroethane 1,1-Dichloropropene Carbon tetrachloride Benzene 1,2-Dichloroethane Fluorobenzene ISTD Trichloroethene Bromodichloromethane cis-1,3-Dichloropropene Toluene trans-1,3-Dichloropropene 1,1,2-Trichloroethane
27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39.
40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52.
Tetrachloroethene 1,3-Dichloropropene Dibromochloromethane 1,2-Dibromomethane Chlorobenzene 1,1,1,2-Tetrachloroethane Ethylbenzene m-Xylene 1,2-Dichloropropane Dibromomethane p-Xylene o-Xylene Styrene
Bromoform Isopropylbenzene 4-Bromofluorobenzene SURR Bromobenzene 1,1,2,2-Tetrachloroethane 1,2,3-Trichloropropane n-Propylbenzene 2-Chlorotoluene 4-Chlorotoluene 1,3,5-Triethylbenzene tert-Butylbenzene 1,2,4-Trimethylbenzene sec-Butylbenzene
53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63.
By Purge and Trap (EPA Method 524.2/6234/8260) Extracted ion chromatogram
7
1
2 3 45
6
8
9 10
5.00 Carrier: Column: Injection: Oven: Detector:
18, 19 21 20
16, 17 11, 12
220°C
10.00
20°C/min
160°C
26 25
1,3-Dichlorobenzene 4-Isopropyltoluene 1,4-Dichlorobenzene 1,2-Dichlorobenzene-d4 SURR 1,2-Dichlorobenzene n-Butylbenzene 1,2-Dibromo-3-chloropropane 1,2,4-Trichlorobenzene Hexachlorobutadiene Naphthalene 1,2,3-Trichlorobenzene
38, 39
34, 35 29, 30
44, 45 43
5 min
54, 55
42
28 27
15.00
50
60
40
61, 62 63
59 25.00
20.00
Time (min)
6 min 6°C/min
35°C
56, 57, 58
36, 37
Helium, 8.5 ml/min HP-624, 30 m x 0.53 mm x 3 m (Part No. 19095V-423) Use jet separator (Part No. 59913A, #007) Temperature program listed above MSD
30.00
Pub No.: 5091-0677, 5091-2477E, 5091-5909
Purgeable Halocarbons and Aromatics 1. 2. 3. 4. 5.
Chloroethane 1,1-Dichloroethane Methylene chloride trans-1,2-Dichloreoethene 1,1-Dichloreoethane
6. 7. 8. 9. 10.
Bromochloromethane Chloroform 1,1,1-Trichloroethane Carbon tetrachloride 1,2-Dichloroethane
11. 12. 13. 14. 15.
Trichlooethene 1,2-Dichloropropane Bromodichloromethane trans-1,3-Dichloropropene cis-1,3-Dichloropropene
22
18 PID
11 14 2
23 5
ELCD 1
4
8
24
15
18
35°C
23 24 21 22
5 min
5°C/min
19
0
432
1,1,2,2-Tetrachloroethane 1,3-Dichlorobenzene 1,4-Dichlorobenzene 1,2-Dichlorobenzene
140°C 5 min
9
Carrier: Column: Injection: Oven: Detector:
21. 22. 23. 24.
15
7 10 12 1314 16 17 11 6
1,1,2-Trichloroethane Tetrachloroethene Dibromochloromethane Chlorobenzene Bromoform
23
16
4
16. 17. 18. 19. 20.
Helium, 8.5 ml/min HP-624, 30 m x 0.53 mm x 3 m (Part No. 19095V-423) Tekmar LSC-2 Purge & Trap System, Tenax Trap, Packed injection port (250°C) Temperature program listed above ELCD; PID
20
30 min
Pub No.: 5954-7613
Environmental
Purgeable Halocarbons and Aromatics 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.
Dichlorodifluoromethane 13. Chloroform 25. Toluene 37. o-Xylene 49. 1,2,4-Trimethylbenzene 38. Styrene 50. sec-Butylbenzene Chloromethane 14. Bromochloromethane 26. trans-1,3-Dichloropropene 39. Isopropyl benzene Vinyl chloride 15. 1,1,1-Trichloroethane 27. 1,1,2-Trichloroethane 51. p-Isopropyltoluene 40. Bromoform Bromomethane 16. 1,1-Dichloropropene 28. 1,3-Dichloropropane 52. 1,3-Dichlorobenzene 41. 1,1,2,2-Tetrachloroethane Chloroethane 17. Carbon tetrachloride 29. Tetrachloroethene 53. 1,4-Dichlorobenzene Trichlorofluoromethane 18. 1,2-Dichloroethane 30. Dibromochloromethane 42. 1,2,3-Trichloropropane 54. n-Butylbenzene 1,1-Dichloroethene 31. 1,2-Dibromoethane 19. Benzene 43. n-Propyl benzene 55. 1,2-Dichlorobenzene 20. Trichloroethene Methylene chloride 32. Chlorobenzene 44. Bromobenzene 56. 1,2-Dibromo-3-chloropropane 21. 1,2-Dichloropropane 57. 1,2,4-Trichlorobenzene trans-1,2-dichloroethene 33. 1,1,1,2-Tetrachloroethane 45. 1,3,5-Trimethylbenzene 1,1-Dichloroethane 22. Bromodichloromethane 34. Ethyl benzene 46. 2-Chlorotoluene 58. Hexachlorobutadiene 23. Dibromomethane 35. m-Xylene 59. Naphthalene 2,2-Dichloropropane 47. 4-Chlorotoluene 24. cis-1,3-Dichloropropene 60. 1,2,3-Trichlorobenzene cis-1,2-Dichloroethene 36. p-Xylene 48. tert-Butylbenzene By Purge and Trap (EPA Method 502.2/8020/8021) 35, 36 44 200°C 10, 11 RT=48.5 min ELCD PID RT=48.6 13 45, 46 27 32, 34 20 14 52 47, 48 32 33 35°C 21 58 3°C/min 29 18 49 53 59 10 min 40 22 28 15 55 37,38 8 53 57 60 16 55 54 10 43 41 52 12 20 57 60 31 39 50 23 7 9 9 47 29 58 24 16 46 42 7 26 24 56 1 44 5, 6 3 26 234 1 10 Carrier: Column: Injection:
10 30 40 50 Time (min) Helium, 30 cm/sec, 10 ml/min constant flow HP-VOC, 105 m x 0.53 mm x 3 m (Part No. 19095R-420) O.I. 4460 Purge/Trap, 5 ml water sample
20
20
30 40 50 Time (min) Oven: Temperature program listed above Detector: ELCD 900°C and PID 250°C
Purgeable Halocarbons and Aromatics
150°C 55°C -70°C 4 min
19
9
25 +26 35 +36 53 50 52 54 51 59 44 49 46 32 43 57 60 38 39
230°C 20°C/min
34
3°C/min
7
20°C/min
20
16
6
3
29 24
20
10
30 Time (min)
2
Sample: Carrier: Column: Oven: Detector: Peak ID:
1
0
10
58
4
PID 0
12
20
Time (min)
30
37
Applications
By Purge and Trap with Cryo Focusing
40
40
50
16 ppb each component in 5 ml water Helium, 3 ml/min constant flow HP-VOC, 90 m x 0.32 mm x 1.8 m (Part No. 19091R-319) Temperature program listed above PID 250°C and ELCD 850°C See above
50
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433
Applications
Environmental
GC and GC/MS Applications
Chlorinated Pesticides 1
EPA - 608 Targeted Compounds 2
5
9
6
20 11
7 10
4
1A. Splitless Injection
12
15 14 18 13 1617
3
a 6
10
8 1 2
12
14
16
18
20
5 6
7 10
4
1. 2. 3. 4. 5. 6. 7. 10. 11. 12. 13. 14. 15. 16. 17. 18.
-BHC -BHC -BHC Heptachlor -BHC Aldrin Heptachlor epoxide Endosulfan I 4,4'-DDE Dieldrin Endrin 4,4'-DDD Endosulfan II 4,4'-DDT Endrin aldehyde Endosulfan sulfate
12
14 15 18 13 16 17
Carrier: Column :
Helium, 20 cm/sec, 2.2 psi (80 ), 2.4 ml/min constant flow HP-608, 30 m x 0.53 mm x 0.5 m (Part No. 19095S-023) Splitless, 1 l, inlet 250°C on column, 1 l, oven-track mode Temperature program listed above ECD 330°C Pub No.: 5963-2003
Injection: a 10
8
12
14
16
18
Oven: Detector: 20
Volatile Halocarbons by Headspace 1. 2. 3. 4. 5.
Chloroform 1,1,1-Trichloroethane Carbon tetrachloride Bromodichloromethane 1,1,2-Trichloroethane
6. 7. 8. 9. 10.
30°C/min 85°C
1B. On-Column Injection
11
3
6
250°C 5°C/min
195°C
Purgeable Aromatics (BTX) by Headspace
Dibromochloromethane Tetrachloroethylene Bromoform o-dichlorobenzene 2,4-Trichlorobenzene
1. 2. 3. 4.
Benzene Toluene m-+p-Xylene o-Xylene
130°C (2 min) 40°C
3
10°C/min
3 min 100°C (8 min)
7 40°C
4
10°C/min
4 min 3
1
1
6
2
4
2 8 5
10 9
14 min
20 min Carrier: Column: Injection: Oven: Detector:
434
Helium, 49 cm/sec HP-1, 25 m x 0.32 mm x 0.52 m (Part No. 19091J-112) Split (64:1), headspace 10 ppb/component Temperature program listed above ECD
Carrier: Column: Injection: Oven: Detector:
Helium, 24 cm/sec HP-1 (Cross-Linked Methyl Silicone), 25 m x 0.32 mm x 0.52 m (Part No. 19091Z-112) Headspace (Agilent 19395A) split (50:1), 1 l Temperature program listed above FID Pub. No.: 5953-1820
Environmental
Analysis of Volatile Organics 1. 2. 3. 4. 5.
Trihalomethanes (THMS)
trans-1,2-Dichloroethene Carbon tetrachloride Benzene Tetrachloroethene Ethylbenzene
140°C 35°C
3
150°C 1
50°C
2
10°C/min
3
H
1
1
5
23
Chloroform Dichlorobromoform Chlorodibromoform Bromoform
15°C/min
4 min
5
1. 2. 3. 4.
2
4 CI
C
4
8 min 1
4 8 min 8 min Helium, 0.134 ml/min (29 cm/sec) HP-5 (Cross-Linked 5% Phenyl Methyl Silicone), 10 m x 0.10 mm x 0.34 m (Part No. 19091S-003) Split (1200:1), 1 l Temperature program listed above Pub. No.: 5954-8711 AED
Injection: Oven: Detector:
Fast Chromatography 60 VOC Compounds 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
Trichlorofluoromethane 1,1-Dichloroethene 1,1-Dichloroethene Benzene 1,2-Dichloropropane Toluene 1,2-Dibromoethane o-Xylene 1,4-Dichlorobenzene Naphthalene
Pollutants in a Chemical Dump Site 220°C
35°C
15°C/min
4 min
Injection: Oven: Detector:
10 min Hydrogen, 10 kPa HP-1 (Cross-Linked Methyl Silicone), 30 m x 0.53 mm x 2.65 m (HP Part No. 19095Z-123) Retention Gap: 1.5 m x 0.53 mm (Part No. 19095-22010) 1 l, on-column, oven track mode Temperature program listed above ECD Pub No.: 5091-1657
5. 6. 7. 8. 9. 10.
1. Chlorotoluene 2. Benzaldehyde 3. A. 1,4-Dichlorobenzene 4. B. Nitrobenzene
1 ppb
2 GC: Sample: Carrier: Column: Injection: Oven:
4 3
4
35°C 5 min
8°C/min
B 8
2
6
A 3
1
3
235°C
1
9
1
Chlorobenzaldehyde Benzyl chloride Dichlorotoluene Bornyl chloride Trichlorobenzene Chlorobenzyl chloride
Applications
Carrier: Column:
Carrier: Column:
6
6
8 Time (min)
5973 GCD 10 ml split (ratio 40:1) Helium, 0.65 ml/min constant flow HP-624, 25 m x 200 m x 1.12 m, (Part No. 19091V-402) HP 7695 Purge & Trap Temperature program shown above
12
14
(nm) Carbon 495.7
8
7 5 6 3 8 4
7 10
5 7
A
10 5
4
16
5
15
Time (min)
Chlorine 479.5
20
25
Carrier: Column:
Pub No.: 5965-6692
Helium, 0.75 ml/min Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.2 mm x 0.11 µm (Part No. 19091B-002) Injection: Split (40:1), 1 µl Oven: Temperature program listed above Pub No.: 5959-8709 Detector: AED
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435
Applications
Environmental
GC and GC/MS Applications
Semivolatile Organics: EPA Method 525 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.
Acenaphthene-d10 Hexachlorocyclopentadiene Dimethylphthalate Acenaphthalate 2-Chlorobiphenyl Fluorene Diethylphthalate 2,3-Dichlorobiphenyl Hexachlorobenzene Simazine Atrazine Phenathrene-d10
13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24.
Pentachlorophenol Lindane Phenanthrene Anthacene 2,4,5-trichlorobiphenyl Heptachlor Alachlor Di-n-butylphthalate 2,2',4,4'-tatrachlorobiphenyl Aldrin Heptachlor epoxide 2,2',3',4,6-pentachlorobiphenyl
1
25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35.
300°C (5 min) 6°C/min
160°C 30°C
45°C 1 min
12
4
5.00
15.00
10.00
45 46 44
25.00
20.00
2,2',3,3',4,4',6'-heptachlorobiphenyl Methoxychlor 2,2',3,3',4,5',6,6'-octachlorobiphenyl Di(2-ethylhexyl)phthalate Benzo[b]fluoranthene Benzo (k) fluoranthene Benzo[a]pyrene Perylene-d12 Indeno{1,2,3,c,d}pyrene Dibenz[a,h]anthracene Benzo[g,h,i]perylene
GC: Column:
32 43 5 6 15 16 3 18 9 26 35 7 33 13 1719 20 25 39 41 9 24 22 29 31 34 38 2 42 11 37 40 23 28 30
36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46.
Gamma-chlordane Pyrene Alpha-chlordane Trans nonachlor 2,2',4,4',5,6'-hexachlorobiphenyl Endrin Butylbenzylphthalate Chrysene -d12 Di(2-ethylhexyl)adipate Benz (a) anthracene Chrysene
30.00
Time (min)
6890 HP-5MS, 30 m x 0.25 mm x 0.25 µm (Part No. 19091S-433) Temp: 250°C Carrier gas: Helium Inj. port: Splitless, 6 µl Inj. technique: Agilent 7673B automated sampler, fast injection Volume injected: Splitless, 1µl Inlet press. Prog: 35 psi (0.2 min) at 40 psi/min to 7.4 psi (1 ml/min constant flow) Purge on: 1 min Initial temp: 45°C (1 min) Oven: Temperature program listed above Transfer line: 280°C capillary direct Solvent delay: 3.5 min Mass range: 5-450 Detector: MSD Pub No.: 5963-2003
Semivolatiles Water Analysis, GC/MS 1. 2. 3. 4. 5. 6. 7. 8. 9.
10. 11. 12. 13. 14. 15. 16. 17. 18.
Bis (2-chloroethyl) ether Dichlorobenzene, 1,3Dichlorobenzene, 1,4Dichlorobenzene, 1,2Bis (2-chloroisopropyl) ether N-nitroso di-n-propylamine Hexachloroethanene Nitrobenzene Isophorone
Bis (2-chloroethoxy) methane Trichlorobenzene, 1,2,4Naphthalene Hexachlorobutadiene Hexachlorocyclopentadiene 2-Chloronaphthalene Acenaphthylene Dimethyl phthalate Dinitrotoluene, 2,6-
310°C (5 min)
15
11, 12
1
10 13
14
7 23 8 4
16
34
28
19
9 6
31
7°C/min
80°C
21
27
24
17
25
18
26
Acenaphthene Dinitrotoluene, 2,4Fluorene Diethyl phthalate 4-Chlorophenyl phenyl ether N-Nitrosodiphenylamine Azobenzene 4-Bromophenyl phenyl ether Hexachlorobenzene
28. 29. 30. 31. 32. 33. 34. 35. 36.
29
30
33
36
38 35 37 39
40 41
20
436
10.00
15.00
Time (min)
44 43 42
5
5.00
Phenanthrene Anthracene Di-n-butylphthalate Fluoranthene Pyrene Butylbenzyl phthalate Benz (a) anthracene Chrysene Dichlorobenzidine, 3,3'-
32
22, 23
4 min
19. 20. 21. 22. 23. 24. 25. 26. 27.
20.00
25.00
30.00
37. 38. 39. 40. 41. 42. 43. 44.
Bis-(2-ethylhexyl) phthalate Di-n-octyl phthalate Benzo (b) fluoranthene Benzo (k) fluoranthene Benzo (a) fluoranthene ndeno (1,2,3-c,d) pyrene Dibenz (a,h) anthracene Benzo (g,h,i) perylene
Temperature: 83°C, 50°C/min to 315°C (5 min) Volume injected: 1 ml Column: HP-5MS, 30 m x 0.25 mm x 0.25 m (Part No. 19091S-433) Carrier gas: Helium, 33 cm/sec (1 ml/min) constant flow Oven: Temp. Program listed above Initial temperature: 80C for 4 min Detector: MSD, 280°C
Environmental
Polynuclear Aromatic Hydrocarbons 1. 2. 3. 4. 5. 6.
7. 8. 9. 10. 11.
Naphthalene Acenaphthylene Acenapthene Fluorene Phenanthrene Anthracene
Fluoranthene Pyrene Benzo(a)anthracene Chrysene Benzo(b)fluoranthene
Polynuclear Aromatic Hydrocarbons 12. 13. 14. 15. 16.
Benzo(k)fluoranthene Benzo(e)pyrene Indeno(1,2,3)pyrene Dibenzoanthracene Benzo(g,h,i)perylene
1. 2. 3. 4. 5. 6.
300°C 3°C min
160°C
Naphthalene Acenaphthylene Acenaphthene Fluorene Phenanthrene Anthracene
1 234 7 8
7. 8. 9. 10. 11.
Fluoranthene Pyrene Benzo(a)anthracene Chrysene Benzo(b)fluoranthene
56
10
5 GC: Carrier: Column: Inlet: Oven: Detector:
7
8
15
910
9 10
20
25
11 12 1112
35
30
Time (min) 6890 Hydrogen, constant flow, 10.2 psi, flow 1.5 ml/min HP-5, 30 m x 0.25 mm x 0.25 µm HP-5MS (Part No. 19091S-433) 1 µl 0.01 mg each/ml, split 25/1, 325°C Temperature program listed above FID 325°C
300°C 3°C min
80°C 25°C/min 1.5 min
13
15 14 16
13
Benzo(k)fluoranthene Benzo(e)pyrene Indeno(1,2,3)pyrene Dibenzoanthracene Benzo(g,h,i)perylene 160°C
80°C 25°C/min 1 min
1 23 4
12. 13. 14. 15. 16.
15 14 16
40 GC: Sample: Carrier: Column: Injection: Oven: Detector:
Pub No.: 5965-7874
10
20
30
40
Time (min) 6890 PAH Standards Hydrogen (40 cm/sec), Constant Flow, initial pressure-9 psi HP-5TA, 30 m x 0.25 mm x 0.25 µm (Part No 19091M-433) 1 µl, 100:1 split Temperature program listed above Pub No.: 5965-7874 FID 325°C
Pesticides, Standard Mix Tetrachloro-m-xylene (SS1) alpha-BHC Lindane beta-BHC Heptachlor delta-BHC Aldrin Heptachlor epoxide Endosulfan I 4,4'-DDE
11. 12. 13. 14. 15. 16. 17. 18. 19. 20.
Dieldrin Endrin 4,4'-DDD Endosulfan II 4,4'-DDT Endrin aldehyde Endosulfan sulfate Methoxychlor Endrin ketone Decachlorobiphenyl (SS2) 1
280°C 160°C 10°C/min 1 min
3 20
2 6
7 8
45
0 GC: Column: Detector: Carrier gas: Injection: Oven:
2
300°C 2 min 25°C/min
Applications
1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
4
9
6
11 10
Time (min)
18 14 16 17 13 12 15
8
19
10
12
5890 Series II with EPC HP-35, 30 m x 0.53 mm x 1.0 m ECD Pressure program: 8.6 psi (1 min) at 0.5 psi/min to 12 psi and at 3.0 psi/min to 25 psi (0 min) Splitless, 1 l, purge delay, 0.75 min, inlet temperature of 250C Temperature program listed above
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437
Applications
Environmental
GC and GC/MS Applications
Organochlorine Pesticides (Dual Column Analysis) EPA - 608 Targeted Compounds 9. Dialdrin 1. alpha-BHC 10. 4,4'-DDE 2. beta-BHC 11. Endrin 3. gamma-BHC 12. Endosulfan II 4. delta-BHC 13. 4,4'-DDD 5. Heptachlor 14. Endrinaldehyde 6. Aldrin 7. Aeptachlorepoxide 15. Endosulfan sulfate 16. 4.4'-DDT 8. Endosulfan 1
205°C 180°C 80°C 1 min
4 min
250°C
290°C 2 min 20°C/min
5°C/min
195°C 30°C/min 85°C
30°C/min
9
6
3 10
1
7 2
1 9 10 11 12 13 16 14
6 5
11
8
4
3
2
8
4
15
Carrier: Column:
Helium, 12.4 psi PAS-1701 25 m x 0.32 mm x 0.25 µm (Part No. 19091S-011) Splitless, 200 ppb (main components), 1 ml Temperature program listed above ECD
Injection: Oven: Detector:
Etridiazole Chloroneb Propachlor Trifluralin a-BHC Hexachlorobenzene ß-BHC O-BHC Y-BHC Chlorothalonil 6 5 Heptachlor Aldrin DCPA
14. 15. 16. 17. 18. 19. 20. 21.
15
10 13
8
1
14 11
180°C
5 GC: Carrier: Column: Injection:
438
5890 EPC Helium, 45 cm/sec (80°C) constant flow HP-5MS (Part No. 19091S-433) Splitless, 1 µl
290°C 2 min 20°C/min
8. 9. 10. 11. 12. 13. 14. 15. 16.
1
21 23 24 22
Time (min) 15
25 26
Endosulfan 1 Dieldrin 4,4′-DDE Endrin Endosulfan II 4,4′-DDD Endrin aldehyde Endosulfan sulfate 110°C 4,4′-DDT 1 min 13
3 5
2°C/min 16
9 10
7
11
27 29
15
160°C 3°C/min
133°C
14
6
18 19
20
10
alpha-BHC beta-BHC Lindane delta-BHC Heptachlor Aldrin Heptachlor epoxide
16
2 3
30°C/min
4 min 3°/ min
1. 2. 3. 4. 5. 6. 7.
4
12
7
Chlorobenzilate 4,4'-DDD Endrin aldehyde Endosulfan sulfate 4,4'-DDT Methoxychlor cis-Permethrin trans-Permethrin 205°C
17 80°C 1 min
9
4
Chlorinated Pesticides 22. 23. 24. 25. 26. 27. 28. 29.
Heptachlor epoxide Y-Chlordane Endosulfan I a-Chlordane Dieldrin 4,4'-DDE Endrin Endosulfan II
Helium, 15.7 psi PAS-5 25 m x 0.32 mm x 0.52 µm (Part No. 19091S-010) Splitless, 200 ppb (main components), 1 µl Temperature program listed above ECD Pub. No.: 5952-2341
Injection: Oven: Detector:
Chlorinated Pesticides: EPA Method 508 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.
16 13 12 15 14
25 min
25 min Carrier: Column:
7
5
8
12
28
20
Purge delay: 1 min Head pressure:24 psi Oven: Temperature program above Makeup gas: Nitrogen, 60 ml/min Anode purge: 3 ml/min Detector: ECD 320°C
0 Carrier: Column: Injection: Oven: Detector:
23 min Helium, 30 psi Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone) 25 m x 0.2 mm x 0.11 µm (Part No. 19091B-002) Splitless, 0.5 µl Temperature program listed above Pub No.: 5952-0209 ECD
Environmental
Organochlorine Pesticides and PCBs: CLP Pesticides Tetachloro-m-xylene 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.
a-BHC Y-BHC ß-BHC Heptachlor O-BHC Aldrin Heptachlor epoxide Y-Chlordane a-Chlordane Endosulfan I 4,4′-DDE
190°C
12. Dieldrin 13. Endrin 14. 4,4′-DDE 15. Endosulfan II 16. 4,4′-DDT 17. Edrin aldehyde 18. Endosulfan sulfate 19. Methoxychlor 20. Endrin ketone SS2.Decachlorobiphenyl
80°C 30°C/min 1 min
SS2
SS1
11
1 GC: Carrier: Column: Vol. inj.: Pneumatics: Purge delay: Void time: Temp: Makeup gas: Anode purge: Detector: Oven:
300°C 2 min 6°C/min
5890 Series II Helium, 20 cm/sec, 2.2 psi (80°C), 2.4 ml/min, constant flow HP-608, 30 m x 0.53 x 0.5 (Part No. 19095S-023) 1 µl Splitless mode 1 min 2.75 min 250°C Nitrogen, 65 ml/min 6 ml/min ECD, 320°C Temperature program listed above
2
10 5
3
5
6
7
4
89
10
19
12
15
20
14 13 16 18 17
15 Time (min)
20
Pub No.: 5963-2003
Nitrogen/Phosphorus Containing Pesticides: EPA Method 507
2
5 7 36 8
16. 17. 18. 19. 20. 21. 22.
Propazine Terbufos Pronamide Diazinon Disulfoton Terbacil Metribuzin
23. 24. 25. 26. 27. 28. 29.
Simetryn Alachlor Ametryn Prometryn Terbutryn Bromacil Metolachlor
Tricyclazole Merphos Carboxin Norflurazon Hexazinone Fenarimol Fluridone
20 19
40
27
30
37 36 35
11 21
28 29
15
10 Time (min)
42
38
22
18
205°C 178°C 4 min 30°C/min
310°C 4 min 30°C/min
2°C/min
GC: Column:
23
1
5
37. 38. 39. 40. 41. 42. 43.
80°C
24 25, 26 17
0
Triademefon MGK-264 Diphenamid Stirofos Butachlor Fenamiphos Napropamide
41
9 13 14 12 15 16
10
4
30. 31. 32. 33. 34. 35. 36.
Applications
EPA - 507 Targeted Compounds 9. Ethoprop 1. Dichlorvos 10. Cycloate 2. EPTC 11. Chlorpropham 3. Butylate 12. Atraton 4. Mevinphos 13. Simazine 5. Vernolate 14. Prometon 6. Pebulate 15. Atrazine 7. Tebuthiuron 8. Molinate
32 31
34 33
43 39
20
25
5890 Series II HP-5MS, 30 m x 0.25 mm x 0.25 µm (Part No. 19091S-433) Temperature: 260°C Volume injected: 1 µl Pneumatics: Splitless mode Purge delay: 1 min Carrier gas: Helium, 30 cm/sec (13.6 psi) pressure program Oven: Temperature program listed 1st ramp: 0.5 psi/min to 21 psi 2nd ramp: 1 psi/min to 31 psi Final temperature: 310°C for 4 min Detector: NPD, 290°C Makeup gas: Helium, 30 ml/min Hydrogen: 4.0 ml/min Pub No.: 5963-2003
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439
Applications
Environmental
GC and GC/MS Applications
Chlordane and Toxaphene 300°C (1 min) 20°C/min
280°C (1 min) 190°C 80°C 1 min
Chlordane
0
10
3°C/min
30°C/min
15 Time (min)
Toxaphene
20
Carrier: Column:
25
0
10
Injection: Oven: Detector:
Helium, 20 cm/sec 2.2 psi (80°C), 2.4 ml/min constant flow HP-608, 30 m x 0.53 mm x 0.5 µm (Part No. 19095S-023) Splitless, 1 µl, inlet 250°C Temperature program listed above ECD 330°C
Organo Chlorine Pesticides
Phenols
1. 2. 3. 4. 5. 6.
7. 8. 9. 10. 11.
Tetrachloro m-xylene a-BHC Lindane Heptachlor Endosulfan Dieldrin
275°C
150°C
20
EPA-625 Acid Extract 1. Phenol 2. 2-Chlorophenol 3. 2-Nitrophenol 4. 2,4-Dimethylphenol 5. 2,4-Dichlorophenol 6. 4-Chloro-m-cresol
7. 8. 9. 10. 11.
2,4,6-Trichlorophenol 2,4-Dinitrophenol 4-Nitrophenol 4,6-Dinitro-o-cresol Pentachlorophenol
40°C
1 78 9
5
4
Sample: Carrier: Column: Inlet: Oven: Detector:
440
1.5
2 Time (min)
5 ppb CLP A in iso-octane Helium 0.6 ml/min, constant flow HP-5, 10 m x 0.1 mm x 0.17 µm (Part No. 19091S-002) Split 10:1, 0.5 µl Temperature program listed above Micro ECD
2.5
3
9
3 5
1
30°C/min
11
2
0.5
200°C (2 min) 20°C/min
70°C (1 min)
6 4
25
Pub No.: 5091-7567
45°C/min
0.015 min
3 1 2
Endrin DDD DDT Methoxychlor Decachlorobiphenyl 10
15 Time (min)
10
7 8
3.5
Carrier: Column: Injection: Oven: Detector:
8 min Helium Ultra 2 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.32 mm x 0.52 µm (Part No. 19091B-112) On-column, 1 µl Temperature program listed above FID
11
Environmental
Fungicides 1. 2. 3. 4. 5. 6. 7.
Organotin Compounds
Dihcloro metabolite of terrazole Terrazole Pentachlorobenzene Hexachlorobenzene Pentachloronitrobenzene Pentachloroaniline Pentachlorothioanisole
1. 2. 3. 4. 5. 6. 7.
260°C 5°C/min
35°C 1 min
7 6
4
Dimethylpentyltin Tetrabutyltin Methtyltripentyltin Tributylpentyltin Dibutylpentyltin Butlypentyltin Tetrapentyltin
260°C 50°C 1 min
5
Sn (303 nm)
3
2 3
1
5
15°C/min
4
6 7
2 1 8
7
Injection: Oven: Detector:
12 min Hydrogen, 66 cm/sec HP-101 (Methyl Silicone Fluid), 25 m x 0.2 mm x 0.2 µm (Part No. 19091Y-102) 10 30 pg/component, 1 µl Temperature program listed above ECD Pub No.: 5953-1470
Organomercury Compounds
Carrier: Column: Injection: Oven: Detector:
80°C 4 min
Helium, 100 kPa HP-1 (Cross-Linked Methyl Silicone), 25 m x 0.32 mm x 0.17 µm (Part No. 19091Z-012) Splitless, 1 µl Temperature program listed above AED 330°C Pub No.: 5091-1551E
60°C
5°C/min
Ph2Hg 38 pg
0
5°C/min
Bu4Sn Bu2SnPh Bu2SnPh2 BuSnPh2
Solvent Vent
MeHgPh 40 pg
10
20
Me2SnPh 10 pg 35 Time (min)
40
45
Injection: Oven: Detector:
Helium, 0.75 ml/min constant flow HP-5 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.2 mm x 0.11 µm (Part No. 19091J-002) Splitless, inlet 300°C, 1 µl Temperature program listed above AED 300°C, Tin selective at 303.4 µm Pub No.: 43-5091-6499E
Carrier: Column : Injection: Oven: Detector:
10
40
50
BuSnPh2 78 pg Ph4Sn Oct2SnPh 35 pg
Bu4Sn 14 pg Bu2SnPh 17 pg
Solvent Vent 0
Carrier: Column :
30 BuSnPh2 35 pg
Harbor Sediment
30
Oct2SnPh
360°C
Standard Solution
254 µm
25
12
Organotin Compounds 300°C
20
11
20
Time (min)
30
40
Helium, 0.75 ml/min constant flow HP-5 (Cross-Linked 5% Phenyl Methyl Silicone), 25 m x 0.2 mm x 0.11 µm (Part No. 19091J-002) Splitless, 1 µl, inlet 300°C Temperature program listed above AED 300°C, Hg selective at 254 µm Pub No.: 5091-6500E
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441
Applications
Carrier: Column:
10 9 Time (min)
Applications
Environmental
GC and GC/MS Applications
Volatiles Waste and Soil Analysis, GC/MS 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
Pentafluorobenzene Dichlorodifluoromethane Chloromethane Vinyl chloride Bromomethane Chloroethane Trichlorofluoromethane 1,1-Dichloroethene Methylene chloride trans-1,2-Dichloroethene
11. 12. 13. 14. 15. 16. 17. 18. 19. 20.
1,1-Dichloroethane 2,2-Dichloropropane cis-1,2-Dichloroethene Bromochloromethane Chloroform Dibromofluoromethane 1,1,1-Trichloroethane 1,4-Difluorobenzene Carbon tetrachloride 1,1-Dichloropropene 40
21. Benzene 22. 1,2-Dichloroethane 23. Trichloroethene 24. 1,2-Dichloropropane 25. Dibromomethane 26. Bromodichloromethane 27. cis-1,3-Dichloropropene 28. Toluene-d8 29. Toluene 30. trans-1,3-Dichloropropene 52, 49, 41, 53 60, 42 58, 61 59 48 56 21, 45 39 55 57 12, 19, 22 29 44 47 16, 37 46 7 13 20 54 30 33, 31 25 63 65 5 1 23 34 14 17 32 64 66 4 8 9 10 15 35 18 24 2628 11 43 36 23 27 62
31. 32. 33. 34. 35. 36. 37. 38. 39. 40.
1,1,2-Trichloroethane 2-Bromo-1-chloropropane Tetrachloroethene 1,3-Dichloropropane Dibromochloromethane 1,2-Dibromoethane Chlorobenzene 1,1,1,2-Tetrachloroethane Ethylbenzene m,p-Xylene
Purge/trap parameters Line temperature: 120C Valve temperature: 120C MCS temperature: 120C Purge temperature/time: 30C (11 min) Dry purge time: 3 min MCS desorb temperature: 45C Desorb pre-heat:250C 8.00 24.00 Desorb 4.00 6.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 2.00 Time (min) temperature/time: 255C (2 min) Oven parameters Bake Sample 5 ml, 100 ppb calibration standard mix Initial temperature: 35C (4 min) temperature/time: 260C (8 min) Injection parameters Ramps 1st ramp: 8C/min to 180C MCS bake Temperature: 220C Final temperature: 180C (2.87 min) temperature: 310C Injection: P/T, split mode (split ratio 40:1) Detector parameters TPC pressure: 8.0 psi Carrier: Helium, 0.5 ml/min constant flow, 9.3 psi Transfer line: 280C capillary direct (35C) vacuum compensated Solvent delay: 0.9 min Column: HP-VOC, 30 m x 0.2 mm x 1.11 m (Part No. 19091R-303) Mass range: 45-450
57. o-Xylene 58. Styrene 59. Bromoform 60. 1,4-Dichlorobenzene-d4 61. Isopropylbenzene 62. 4-Bromofluorobenzene 63. Bromobenzene 64. 1,1,2,2-Tetrachloroethane 65. 1,2,3-Trichloropropane 66. n-Propylbenzene 41. 2-Chlorotoluene 42. 4-Chlorotoluene 43. 1,3,5-Trimethylbenzene 44. tert-Butylbenzene 45. 1,2,4-Trimethylbenzene 46. sec-Butylbenzene 47. 1,3-Dichlorobenzene 48. 4-Isopropyltoluene 49. 1,4-Dichlorobenzene 50. 1,2-Dichlorobenzene 51. n-Butylbenzene 52. 1,2-Dibromo-3-chloropropane 53. 1,2,4-Trichlorobenzene 54. Hexachlorobutadiene 55. Naphthalene 56. 1,2,3-Trichlorobenzene
Volatiles in Water (EPA Method 524.2) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.
Dichlorodifluoromethane Chloromethane Vinyl chloride Bromomethane Chloroethane Trichlorofluoromethane 1, 1-Dichloroethane Methylene chloride 1-1, 2-Dichloroethene 1, 1-Dichloroethane 2, 2-Dichloropropane c-1, 2-Dichloroethene Bromochloromethane Chloroform 1, 1, 1-Trichloroethane 1, 1-Dichloropropene
Column: Oven: Carrier: Injector: Detector: Vocarb 3000 Purge Flow:
17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32.
25 m x 0.2 mm x 1.12 m HP-624 (Part No. 19091V-402) 35 (4 min), 8°C/min to 180°C Helium, 7.3 psi, Constant Flow P&T, Split 30/1 MSD, 2505C Trap 6 40 ml/min 3 2 1 45 2
442
33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48.
Carbon Tetrachloride Benzene 1, 2-Dichloroethane Fluorobenzene Trichloroethene 1, 1-Dichloropropane Dibromomethane Bromodichloromethane c-1, 3-Dichloropropene Toluene t-1, 3-Dichloropropene 1, 1, 2-Trichloroethane Tetrachloroethen 1, 3-Dichloropropane Dibromochloromethane 1, 2-Dibromoethane
Chlorobenzene 1, 1, 1, 2-Tetrachloroethane Ethylbenzene m-Xylene p-Xylene o-Xylene Styrene Bromoform Isopropylbenzene 4-Bromofluorobenzene Bromobenzene 1, 1, 2, 2-Tetrachloroethane 1, 2, 3-Trichloropropane n-Proplybenzene 2-Chlorotoluene 4-Chlorotoluene
49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63.
1, 3, 5-Trimethylbenzene t-Butylbenzene 1, 2, 4-Trimethylbenzene s-Butylbenzene 1, 3-Dichlorobenzene 4-Isopropyltoluene 1, 4-Dichlorobenzene 1, 2-Dichlorobenzene-d4 1, 2-Dichlorobenzene n-Butylbenzene 1, 2-Dibromo-3-chloropropane 1, 2, 4-Trichlorobenzene Hexachlorobutadiene Naphthalene 1, 2, 3-Trichlorobenzene
36,37
11,12 7
9 8
4
10 6
16,17 18,19 14
33
26 29,30
21
15
35
34
13
20 8
22 24 28 25 27 31 23 32 10
12 14 Time (min)
47,48,49
P&T Parameters Line Temp: 120°C Valve Temp: 120°C MCS Temp: 100°C Purge Temp: 30°C (11 min) Dry Purge Time: 2 min MCS Desorb Temp: 40°C Desorb Preheat: 250°C Desorb Temp: 255°C (2 min) Bake Temp: 260°C (8 min) MCS Bake Temp: 180°C
52,53,54,55 41 46 51 43 50 44 45 56,57,58
38,39
61,62 60
59
40 42 16
18
20
22
63
Environmental
Pharmaceutical Solvents Extended List 1. 2. 3. 4. 5.
Methane Methanol (solvent) Acetonitrile (50 mg/ml) Methylene Chloride (500 mg/ml) Chloroform (50 mg/ml)
6. 7. 8. 9. 10.
Benzene (100 g/ml) 1,2-Dichloroethane (100 mg/ml) Trichloroethene (100 mg/ml) 1,4 Dioxane (100 mg/ml) Pyridine (100 mg/ml)
120°C 30°C 20 min
1
2
15°C/min 10
4 9 6 8
3
7 5
0
15
10
5
20
25
Time (min.)
GC: Sample: Column:
Carrier: Oven: Injector: Detector:
6890 50-500 ppm each component 60 m x 0.25 mm x 1.4 mm HP-624 (Part No. 19091V-436)
Hydrogen, 2.0 ml/min, Constant Flow 30°C (20 min), 15°C/min 120°C 200°C, 1 ml, 50/1Split 280°C, FID
Column: Carrier: Oven: Injector: Detector:
HP-624 25 m x 0.2 mm x 1.12 mm (Part No. 19091V-402) Helium, 32 cm/sec, constant flow Temperature listed above 1 ml, PTV, 220°C MSD, 250°C
Applications
Pharmaceutical Solvents
220°C 5 min 10°C/min 40°C 25°C/min 1 min 100°C
9
3
10
8
5 6
12
7
13
18
14
4 19
20
1 2 11 1
1. 2. 3. 4. 5.
2
3
Iso Octane Cyclohexane Benzene Pyridine Toluene
4
5
11. 12. 13. 14. 15.
6
7
2-methyl Pyridine Chlorobenzene Ethyl benzene Xylene(s) Styrene
8
16 15 17 10 9
33
34
35
36
37
38
39
40
41
Time (min.) 16. 17. 18. 19. 20.
Benzaldehyde 1,3-dichloro Benzene 1,4-dichloro 1,2-dichloro Benzene Phenyl Ethanol
www.agilent.com/chem
21. 22. 23. 24. 25.
Thioanisole Dimethoxy Toluene Dimethylformamide Anisole Ethylene Glycol
443
Applications
Environmental
GC and GC/MS Applications
Semivolatiles Solid Waste Analysis, GC/MS 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.
23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43.
1,4-Dichlorobenzene-d4 Pyridine N-Nitrosodimethylamine 2-Picoline Methyl methanesulfonate 2-Fluorophenol Ethyl methanesulfonate Phenol-d5 Phenol Aniline bis(2-Chloroethyl)ether 2-Chlorophenol 1,3-Dichlorobenzene 1,4-Dichlorobenzene Benzyl alcohol 1,2-Dichlorobenzene 2-Methylphenol bis(2-chloro-isopropyl)ether 4-Methylphenol Acetophenone n-Nitroso-di-n-propylamine Hexachloroethane
Nitrobenzene-d5 Nitrobenzene Naphthalene-d8 N-Nitrosopiperidine Isophorone 2-Nitrophenol 2,4-Dimethylphenol bis(2-Chloroethoxy)methane 2,4-Dichlorophenol Benzoic acid 1,2,4-Trichlorobenzene a-,a-Dimethylphenethylamine Naphthalene 4-Chloroaniline 2,6-Dichlorophenol Hexachlorobutadiene N-Nitroso-di-n-butylamine 4-Chloro-3-methylphenol 2-Methylnaphthalene 1,2,4,5-Tetrachlorobenzene Hexachlorocyclopentadiene
44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64.
Acenaphthene-d10 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol 2-Fluorobiphenyl 2-Chloronaphthalene 1-Chloronaphthalene 2-Nitroaniline Dimethylphthalate Acenaphthylene 2,6-Dinitrotoluene 3-Nitroaniline Acenaphthene 2,4-Dinitrophenol Dibenzofuran Pentachlorobenzene 4-Nitrophenol 2,4-Dinitrotoluene 1-Napthylamine 2-Napthylamine 2,3,4,6-Tetrachlorophenol Fluorene
65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85.
68 64, 66 34, 35 23, 24 21 25
19, 20 13, 14 8, 9 12 6
29 16
27
30
36, 41 37
33
42 43
58, 60 81 78, 80 82 83
51
74, 75
90
87 84
89
76
39 79
67 81
96 82
88
50
Chrysene-d12 Pyrene Terphenyl-d14 p-Dimethylaminoazobenzene Butylbenzyl phthalate Benzo[a]anthracene 3,3'-Dichlorobenzidine Chyrsene bis(2-Ethylhexyl)phthalate Perylene-d12 Di-n-octylphthalate Benzo[b]fluoranthene 7,12-Dimethylbenz(a) anthracene 99. Benzo (k) fluoranthene 100. Benzo[a]pyrene 101. 3-Methylcholanthrene 102. Dibenzo(a,j)acridine 103. Dibenz[a,h]anthracene 104. Indeno (1,2,3-cd) pyrene 105. Benzo[g,h,i]perylene
93, 94
52, 53 55
11
86. 87. 88. 89. 90. 91. 92. 93. 94. 95. 96. 97. 98.
65
62, 63 47
Diethylphthalate 4-Chlorophenyl-phenylether 4-Nitroaniline Diphenylamine n-Nitrosodiphenylamine Diphenylhydrazine 4,6-Dinitro-2-methylphenol Phenanthrene-d10 2,4,6-Tribromophenol 4-Bromophenyl-phenyl ether Phenacetin Hexachlorobenzene 4-Aminobiphenyl Pentachlorophenol Pentachloronitrobenzene Pronamide Phenanthrene Anthracene Di-n-butylphthalate Fluoranthene Benzidine
86
98, 99
91 92
85
100
102
72
7
3
95 2
4
5 4.00
6.00
8.00
12.00
10.00
14.00
Time (min.)
280°C 45°C 1 min
444
104
101
97
73
24°C/min
310°C 1 min 5°C/min
Conditions: Column: Carrier: Injection: Oven: Detector:
HP-5MS, 30 m x 0.25 mm x 0.25 m (Part No. 14091S-433) Helium, pressure program 0.1 psi (0.1 min) at 99 psi/min to 7.4 psi 0.1 l, 250°C Termperature program listed above MSD, 280°C
1600
103 105
Environmental
Organohalide Pesticides in Water, EPA Method 505 1. 2. 3. 4. 5. 6. 7. 8.
9. 10. 11. 12. 13. 14. 15. 16.
Hexachlorocyclopentadiene Hexachlorobenzene Simazine Atrazine Lindane Heptachlor Alachlor Adrin
Heptachlor epoxide δ-Chlordane α-Chlordane trans-Nonachlor Dieldrin Endrin cis-Nonachlor Methoxychlor
2 4 15 3
Injection parameters Temperature 250°C Volume Injected: 1 µl splitless Purge delay: 1 min Carrier gas: Helium, 2.0 m./min, constant flow, 42 cm/sec (22.4 psi at 80°C) Oven parameters Initial temperature Ramps 1st ramp: 2nd ramp: 3rd ramp: Final Temperature:
5
6
5
10
Column: Carrier: Injection: Detector:
Detector parameters ECD: 300°C Makeup gas: N2, 60 m./min Anode purge 6 ml/min
8 9
1
80°C (1 min) 30°C/min to 175°C (4 min) 6°C/min to 215°C (2 min) 15°C/min to 290°C 290°C (5 min)
10
7
Time (min.)
80°C 1 min
16
11 12 14 13
215°C 2 min 6°C/min
175°C 4 min 30°C/min
290°C 5 min 15°C/min
20
15
HP-5MS, 30 m x 0.25 mm x 0.25 m (Part No. 19091S-433) Helium, 42 cm/sec, constant flow 1 l splitless (1 min), 250°C ECD, 300°C
Sample 16 components EPA-505 targeted pesticides and 14 ppb Aroclor 1260 in hexane. Concentration of pesticides: 50 ppb each except 1.25 ppm for atrazine and simazine.
Pub No.: 5963-2003
EPA Method 625 Semivolatiles bis(2-chloroethyl)ether Dichlorobenzene, 1,3Dichlorobenzene 1,4Dichlorobenzene 1,2bis(2-chloroisopropyl) ether N-nitroso-di-n-propylamine Hexachloroethanene Nitrobenzene Isophorone
10. bis(2-chloroethoxy)methane 11. Trichlorobenzene 1,2,412. Napthalene 13. Hexachlorobutadiene 14. Hexachlorocyclopentadiene 15. 2-Chloronaphthalene 16. Dimethyl phthalate 17. Acenaphthylene 18. Dinitrotoluene 2, 617,18
19. 20. 21. 22. 23. 24. 25. 26. 27.
Acenaphthene Dinitrotoluene 2,4 diethyl phthalate Fluorene 4-chlorophenyl phenyl ether N-Nitrosodiphenylamine Azobenzene 4-Bromophenyl phenyl ether Hexachlorobenzene
12
2
4 5
1
11
7
3
8
23
15 19
22
14
9 10
80°C 4 min
26
21 25 24
28,45 29 27
30
6
35 36
31 32
Bis -2-ethylhexyl)phthalate Di-n-octyl phthalate Di-n-octyl phthalate Benzo (k) fluoranthene Benzo (a) fluoranthene Indeno (1,2,3-c,d) pyrene Dibenz (a,h) anthracene Benzo (g,h,i) perylene
Helium, 1ml/min constant flow HP-5 Trace Analysis 30 m x 0.25 mm x 0.25 µm (Part No. 19091M-443) Split/splitless Temperature program listed MS, 280°C
Injection: Oven: Detector:
38 40
34
20
37. 38. 39. 40. 41. 42. 43. 44.
Column:
37
7°C/min 33
16
Anthracene Phenanthrene Di-n- butylphthalate Fluoranthene Pyrene ButylBenzyl phthalate Benz (a) anthracene Chrysene Dichlorobenzidine, 3,3Carrier:
310°C 5 min
13
28. 29. 30. 31. 32. 33. 34. 35. 36.
Applications
1. 2. 3. 4. 5. 6. 7. 8. 9.
39
41
42
43
44
0 12.00
14.00
16.00
18.00
20.00
22.00
Time (min.)
24.00
26.00
www.agilent.com/chem
28.00
30.00 Pub No.: 5963-2003
445
Applications
Environmental
GC and GC/MS Applications
Nitrogen/Phosphorus Containing Pesticides, EPA Method 507 1. 2. 3. 4.
3
1
EPA Method 504
4
1. 1,2 Dibromoethane (EDB) 2. 1,2-Dibromo-3-chloropropane (DBCP)
Prometon Atrazine Prometryne Ametryn
200°C 1 min
40°C 4 min
2
1
10°C/min
2 0
10
30
20 Time (min)
40
Oven parameters Initial temperature 80°C Ramps 1st ramp: 30°C/min to 178°C (4 min) 2nd ramp: 2°C/min to 205°C 3rd ramp: 30°C/min to 310°C Final Temperature: 310°C for 4 min
Injection parameters Temperature 260°C Volume Injected: 1 µl Pneumatics: Splitless mode Purge delay: 1 min Carrier gas: Helium, 30 cm/sec measured at 80°C Pressure programming Initial head pressure: 13.6 psi 1st ramp: 0.5 psi/min to 21 psi 2nd ramp: 1 psi/min to 31 psi Void time: 1.63 min
0
2
GC: Sample: Carrier: Column:
Detector parameters Temperature: 290°C Makeup gas: Helium, 30 m./min Hydrogen: 4 ml/min
4
6
8
10 12 Time (min)
14
6890 10 ppb in hexane Helium 0.9 ml/min, constant flow HP-1MS, 30 m x 0.25 mm x 1.0 µm (Part No. 19091S-733) Splitless, 250°C, 1l, purge time 1 min Temperature program listed above ECD 300°C
Injection: Oven: Detector:
16
18
Pub No.: 5965-7874
Pub No.: 5963-2003
Semivolatiles, EPA Method 624 1. 2. 3. 4. 5. 6. 7. 8. 9.
Bis (2-chloroethyl) ether Dichlorobenzene, 1,3Dichlorobenzene, 1,4Dichlorobenzene, 1,2Bis (2-chloroisopropyl) ether N-nitroso di-n-propylamine Hexachloroethanene Nitrobenzene Isophorone
10. 11. 12. 13. 14. 15. 16. 17. 18.
Bis (2-chloroethoxy) methane Trichlorobenzene, 1,2,4Naphthalene Hexachlorobutadiene Hexachlorocyclopentadiene 2-Chloronaphthalene Acenaphthylene 1Dimethyl phthalate Dinitroluene, 2,6-
19. 20. 21. 22. 23. 24. 25. 26. 27.
Acenaphthene Dinitrotoluene, 2,4Fluorene Diethyl phthalate 4-Chlorophenyl phenyl ether N-Nitrosodiphenylamine 2Azobenzene 4-Bromophenyl phenyl ether Hexachlorobenzene
28. 29. 30. 31. 32. 33. 34. 35. 36.
Phenanthrene Anthracene Di-n-butylphthalate Floranthene Pyrene Butylbenzyl phthalate Benz (a) anthracene Chrysene Dichlorobenzidine, 3,3'-
32 31
22 23 19
9
1112
6 10
13
15 16 21 24 27 14
5.00
446
34 30
33 36
35
38 40 41 37 39
25
17
80°C 4 min
44
GC: Carrier: Column: Injection:
20
Oven: Detector: 10.00
15.00 20.00 Time (min)
25.00
30.00
Bis(2-ethylhexyl) phthalate Di-n-octyl phthalate Benzo (b) fluoranthene Benzo (k) fluoranthene Benzo (a) fluoranthene Indeno (1,2,3-c,d) pyrene Dibenz (a,h) anthracene Benzo (g,h,i) perylene
310°C 5 min 7°C/min
43 42
26
18
3 7 2 48 1 5
28 29
37. 38. 39. 40. 41. 42. 43. 44.
6890 Helium, 33 cm/sec (1 ml/min) constant flow HP-5MS, 30 m x 0.25 mm x 0.25 µm (Part No. 19091S-433) On-column, 1 µl, inlet=83°C to 315°C (5 min) at 50°C/min Temperature program listed above MSD 280°C
Pub No.: 5963-2003
Environmental
Polychlorinated Biphenyls (PCBs) heptahexa-
octa-
penta-
tri-
320°C 5 min 10°C/min 80°C 30°C/min 2 min 200°C
tetranonadeca-
di-
tri-
8
10
12
GC: Sample: Carrier: Column: Inlet: Oven: Detector:
14
Time (min) 16
18
20
22
6890/microECD HP 7673, 10 µl syringe, 1 µl injection Helium, 16.8 psi, flow 1.4 ml/min HP-5MS, 30 m x 0.25 mm x 0.25 µm (Part No. 19091S-433) Splitless Temperature program listed above 330°C makeup gas: nitrogen, constant column and makeup flow
EPA Method 8061 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
11. 12. 13. 14. 15. 16. 17. 18. 19. 20.
Dimethyl phthalate Diethyl phthalate Di-isobutyl phthalate Di-n-butyl phthalate bis (4-Methyl-2-pentyl) phthalate bis (methoxyethyl) phthalate Di-amyl phthalate bis (2-Ethoxyexyl) phthalate Hexyl-2-ethylhexyl phthalate Di-n-hexyl phthalate
HP-608
17
3
Injection: Oven: Detector:
6890 Helium, 20 cm/sec 2.1 psi constant flow HP-5 30 m x 0.53 mm x 0.5 µm 30 m x 0.53 mm x 0.88 µm (Part No. 19091J-023) HP-608 (Part No. 19095S-023) 260°C, 2 µl splitless pressure pulse split/less 1 min at 20 psi 60°C Dual ECD, 300°C
18
4 6
7
9 8
3
11 14 10
5°C/min
60°C 35°C/min 6.5 min
13
15
16 1
15 Time (min)
20
25
5
20
4 6
19 10
280°C 200°C
12
17
20
2
5
GC: Carrier: Columns:
HP-5
12
5
1
bis (2-Ethylhexyl) phthalate Butylbenzyl phthalate bis (2-n-Butoxyethyl) phthalate Dicyclohexyl methyl phthalate Di-n-octyl phthalate Di-nonyl phthalate Benzyl benzoate (IS) Di-phenyl phthalate (SS1) Di-phenyl isophthalate (SS2) Dibenzyl phthalate (SS3)
Applications
Semivolatiles Phthalate Esters
5
7 8
9
11
1013
2
10
www.agilent.com/chem
14
15 Time (min)
18
15 19
20
16
25 Pub No.: 5963-2003
447
Applications
Petrochemical/Hydrocarbon Processing
GC and GC/MS Applications
Petrochemical/Hydrocarbon Processing C1-C5 Hydrocarbons 1. 2. 3. 4. 5. 6.
7. 8. 9. 10. 11. 12.
Methane Ethane Ethylene Propane Cyclopropane Propylene 2 6 7 1 4
Fast C1 to C10 hydrocarbon separation
iso-Butane n-Butane Propadiene Acetylene trans-2-Butene 1-Butene
13. 14. 15. 16. 17. 18.
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.
Isobutylene cis-2-Butene iso-Pentane n-Pentane 1,3-Butadiene Propyne
8
3
12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.
Methane Ethane Ethylene Propane Cyclopropane Propylene iso-Butane n-Butane Propadiene Acetylene trans-2-Butene
Butene-1 isobutylene cis-2-Butene iso-Pentane n-Pentane 1,3-Butadiene Propyne trans-Pentene Pentene-1 iso-Pentane cis-2-Pentene
23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33.
Hexane Benzene Heptane i-Octane n-Octane Cyclohexene Toluene Nonane Ethylbenzene p-Xylene Decane 250°C 2 min
12
5
11
23
16
14
15
10 9
Injection: Oven: Detector:
10 15 Time (min.) Helium, 50 cm/sec (100°C), 7 ml/min, constant flow HP-PLOT/Al2O3s" 50 m x 0.32 mm x 8 µm (Part No. 19095P-S15) Split (65:1) 5 µl, Inlet 250°C 100°C isothermal FID 250°C
20
Methane Ethane Ethylene Propane Cycloproprane Propylene iso-Butane n-Butane
9. 10. 11. 12. 13. 14. 15.
12 3 4
8
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.
1.5 min 17 11 12 1416
9 10 5
Injection: Oven: Detector:
448
32
5
3
4 Time (min)
5
6
7
HP-PLOT Al2O3 S", 30 m x 0.25 mm x 5 m (Part No. 19091P-S33) Temperature program listed above Hydrogen, 28psi @120C 250C, Split flow 120 ml/min FID 250C 5 l headspace gases
Methane Ethane Ethylene Propane Cyclopropane Propylene iso-Butane n-Butane Propadiene Acetylene trans-2-Butene Butene-1 4 7 8 17 2 1 15 16 11
13
Carrier: Column:
28-31
Extended Analysis (C1 to C10) n-Pentane 1,3-Butadiene trans-2-Pentene 2-Methyl-2-butene 1-Pentene cis-2-Pentene 180°C n-Hexane 2 min 100°C 10°C/min 5°C/min 35°C
6
0
26-27
33
2
Oven: Carrier: Inlet: Detector: Sample:
16. 17. 18. 19. 20. 21. 22.
Propadiene Acetylene trans-2-Butene 1-Butene Isobutylene cis-2-Butene iso-Pentane
7
1
Column:
Light Hydrocarbons 1. 2. 3. 4. 5. 6. 7. 8.
25
25°C/min
18
5
Carrier: Column:
24
11-16 17-22
17 0
0
120°C 1 min
1-10
13
10
15 Time (min)
6
20 21 19 18 20
Helium, 50 cm/sec (35°C), 7 ml/min, constant flow HP-PLOT/Al2O3 30 m x 0.53 mm x 15 µm (Part No. 19095P-M23) Split (65:1) 5 µl, Inlet 250°C Temperature program listed above FID 250°C
13
26 18 25 24
12
10 5 9
20 0 Carrier: Column: Injection: Oven: Detector:
10
Isolbutylene cis-2-Butene Cyclopentane iso-Pentane n-Pentane 1,3-Butadiene trans-2-Pentane 2-Methyl-2-butene 1-Pentene cis-2-Pentene TDB Cyclohexane
25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36.
2-Methyl-pentane n-Hexane Heptane Benzene iso-Octane n-Octane Toluene Nonpane Ethylbenzene p- and m-Xylene o-Xylene Decane 225°C
14
3
25
13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24.
180°C 100°C 5 min 40°C 7.5°C/min 2.5 min 23 30 31 22 28 29 34 21 27 20 35 33 19 32
20 min 15°C/min
10 min 12.5°C/min
36
30 50 40 Time (min) Helium, 50 cm/sec, (35°C), 7 ml/min constant flow HP-PLOT/Al2O3 50 m x 0.53 mm x 15 µm (Part No. 19095P-S25) Splitless, 5 µl, inlet temp at 250°C Temperature program listed above FID 250°C 20
Petrochemical/Hydrocarbon Processing
Oxygenates in Hydrocarbon Sample 1. 2. 3. 4.
Ethanol 2-Propanone Dichloromethane Acetic acid, methyl ester
5. 6. 7. 8.
Aromatics in Benzene Calibration Mix of Aromatics in Benzne ASTM Method 4494
Diethyl ether Pentane Acetic acid, ethyl ester Hexane 250°C
1
1. 2. 3. 4. 5. 6.
8
15°C/min
150°C 2 min
Cyclohexane Nonane Benzene Toluene Undecane Ethylbenzene 1
7. 8. 9. 10. 11.
p-Xylene m-Xylene Cumene o-Xylene n-Propylbenzene 92°C (4.5 min)
3 60°C
4°C/min
1 min
5 2
220°C (5 mins) 20°C/min
11
6 4
2
5
6 78
9 10
7
4 3
GC: Column: Oven: Carrier: Detector: Butadiene concentration:
4 Time (min)
5
6
Injection: Oven: Detector:
1000 ppm in methanol
Hydrocarbons C1-C5 Using an HP-PLOT Q Column 180°C 7.5°C/min
60°C 8 min C4s C3s C2s
6
10
12
14
0.1% in benzene Helium, 32 cm/sec, 19.9 psi (60°C), 2.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 60 m x 0.32 mm x 0.5 µm (Part No. 19091N-216) Split (100:1), 0.5 µl, inlet temp at 220°C Temperature program listed above FID 270°C
Purity of o-Xylene ASTM Method 3797 1. Hydrocarbon 2. Ethylbenzene 3. p-Xylene 4. Cumene 5. o-Xylene
isobutane n-butane Cyclopropane
8
Time (min) Sample: Carrier: Column:
6890 HP-PLOT Q (Part No. 19095P-QO4) Temperature program listed above Helium, 25 psig FID
C1
4
7
92°C (4.5 min) 60°C
220°C (1 min) 20°C/min
4°C/min
1 min 3
Applications
3
2
1
5
C5s 4 1
0
5
10
15
20
Time (min) 2 GC: Sample: Carrier: Column: Injection: Oven: Detector:
6890 17 HC, 5µl (C1-20%, C2 to C5-1% to 14%) Hydrogen, 8 ml/min @ 60°C HP-PLOT Q, 0.53 mm x 30 m x 40 µm (Part No. 19095P-Q04) 250°C Split ratio 12:1 Temperature program listed above FID 250°C
0 Sample: Carrier: Column: Pub No.: 5965-7872
Injection: Oven: Detector:
5 10 15 20 Time (min) Neat, 98%+ Helium, 32 cm/sec, 19.9 psi (60°C), 2.5 ml/min constant flow HP-INNOWax (Cross-Linked PEG), 60 m x 0.32 mm x 0.5 µm (Part No. 19091N-216) Split (100:1), 0.5 µl, inlet 220°C Temperature program listed above FID 270°C
www.agilent.com/chem
449
Applications
Petrochemical/Hydrocarbon Processing
GC and GC/MS Applications
Impurities in Styrene: ASTM D5135 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.
Nonaromatics Ethylbenzene p-Xylene m-Xylene Isopropylbenzene o-Xylene n-Propylbenzene p/m-Ethyltoluene Styrene a-Methylstyrene (366 ppm) Phenylacetylene (58 ppm) 2 -Methylstyrene Benzaldehyde 4
Transformer Oil Gas 150°C
5 min
Injection: Oven: Detector:
7
6 11
7
13
12
8 5
Methane Ethane Ethylene Propane Propylene Acetylene 1-Butene
1
1
GC: Carrier: Column:
2 3 6
3
2.5
5
10
5
0
2 min 10°C/min
80°C
9
1. 2. 3. 4. 5. 6. 7.
4
7.5 Time (min)
0
10
12.5
5890 Series II GC Helium 8.6 psi (28 cm/sec), constant flow, 1.5 ml/min HP-INNOWax 30 m x 0.32 mm x 0.5 µm (Part No. 19091N-213) Split (40:1), 0.5 µl Temperature program listed above Pub No.: 5964-2129 FID 270°C
Natural Gas
2
Sample:
4 Time (min)
6
8
Qualitative Test Sample Transformer Oil Gas (Part No. 5080-8750) Helium, 50 cm/sec, 100°C HP PLOT Al2O3s" 50 m x 0.53 mm x 15 µm (Part No. 19095P-S25) Splitless, 5 µl, 250°C 100°C, isothermal FID 250°C
Carrier: Column: Injection: Oven: Detector:
Natural Gas (Hydrocarbon)
Ethane
Methane
60°C 2 min
1 min 30°C/min 23 1
Water
Air/CO
1. 2. 3. 4. 5. 6. 7. 8.
240°C
5 4
C3
Methane Ethane Propane iso-Butane n-Butane iso-Pentane n-Pentane n-Hexane 180°C
i-C4/n-C4 100°C 67
i-C5/n-C5 neo-C5
70th Run
C6
30°C/min
1.5 min
C7
8
1st Run 0
2
4 Time (min)
6
8
0
1
2
3 Time (min)
GC: Sample: Carrier: Column: Injection: Oven: Detector:
450
6890 0.25 cc natural gas sample Helium (8.6 ml/min @ 60°C) HP-PLOT Q, 30 m x 0.53 mm x 40 µm (Part No. 19095P-Q04) Split mode (100 ml/min) Temperature program listed above TCD 250°C Publication No.: 5965-7872
Sample: Carrier: Column: Injection: Oven: Detector:
Natural gas (Part No. 5080-8756) Helium, 50 cm/sec (100°C), 6 ml/min HP-PLOT/Al2O3 15 m x 0.53 mm x 15 µm (Part No. 19095P-S21) Split (50:1), 5 µl, Inlet 250°C Temperature program listed above FID 250°C
4
5
Petrochemical/Hydrocarbon Processing
Baseline Resolution of Air/CO, CO2, and Methane in a Natural Gas Sample Methane 240°C
CO2
Ethane
Air/CO
1 min 30°C/min
60°C 2 min
Natural Gas (Hydrocarbon) 1. 2. 3. 4. 5.
6. 7. 8. 9.
C1 C2 C3 IC4 NC4
IC5 NC5 C6 C7
123 45
180°C 100°C
30°C/min
1.5 min 6 7
Water C3
i-C4/n-C4 i-C5/n-C5 neo-C5
2
GC: Sample: Carrier: Column:
4 Time (min)
C6
6
C7 9
8
0
6890 0.25 cc natural gas sample, Methane, 80%+ Helium (8.6 ml/min @ 60°C) HP-PLOT Q, 30 m x 0.53 mm x 40 µm (Part No. 19095P-Q04) Split mode (12:1) Temperature program listed above TCD 250°C
Injection: Oven: Detector:
Carrier: Column:
Publication No.: 5965-7872
Separation of Refinery Gas Sample
1
1. 2. 3. 4. 5. 6. 7. 8. 9.
2 3 5
10. 11. 12. 13. 14. 15. 16. 17.
Air/CO C1 CO2 Ethylene C2 H2O COS H2O Propylene
2
4
6 Time (min)
8
10
12
Helium, 1 ml/min PONA (Cross-Linked Methyl Silicone), 50 m x 0.2 mm x 0.5 µm (Part No. 19091S-001) Split (200 400:1) Temperature program listed above FID 250°C Pub No.: 5091-0691E
Injection: Oven: Detector:
Refinery Gas
C3 MeOH i-C4 t-C4 n-C4 cis-C4 i-C5 n-C5
200°C 1 min
60°C
20°C/min
1. 2. 3. 4. 5. 6.
7. 8. 9. 10. 11. 12.
Methane Ethane Ethylene Propane Propylene iso-Butane 2
5 min
n-Butane trans-2-Butene 1-Butene cis-2 Butene iso-Pentane n-Pentane
Applications
H2S
0
8
6
13
4 14
11
7 12
4 6
10 7
8
9
GC: Sample: Carrier: Column: Inlet: Oven: Split flow: Detector:
2
4
6 Time (min)
8
6890 Refinery gas and others Helium p=9.0 psi @ 60°C HP-PLOT Q, 0.53 mm x 30 m x 40 µm (Part No. 19095P-Q04) 250°C Split mode 0.25 cc valve Temperature program listed above 100 ml/min TCD 250°C
10
8 3
16 17 0
0
9
1
10
5
2
11 4
12
6
8
12 10
12
Time (min) GC: Carrier: Column: Injection: Oven: Split: Detector:
6890 Helium 7 ml/min HP-PLOT/AI203 50 m x 0.53 mm x 15 µm (Part No. 19095P-S25) Split (100:1), inlet 250°C, 5 µl 100°C Isothermal 100 ml/min FID 250°C
Pub No.: 5965-7872
www.agilent.com/chem
Pub No.: 5964-2129
451
Applications
Petrochemical/Hydrocarbon Processing
GC and GC/MS Applications
Refinery Gas (Hydrocarbon) 1. 2. 3. 4. 5.
6. 7. 8. 9. 10.
C1 C2, C2= C3= C3 IC4 2
3
Oxygenates in Gasoline
NC4 1-Butene/t-2-butene cis-2-Butene 35°C IC5 3 min NC5 4
1. 2. 3. 4.
100°C 5 min 10°C/min
8
12
0
5
10 Time (min)
Column: 5
6
Time (min) Helium, 1 ml/min PONA (Cross-Linked Methyl Silicone), 50 m x 0.2 mm x 0.5 µm (Part No. 19091S-001) Split (200 400:1), 2 cc loop Temperature program listed above Pub No.: 5091-0691E FID 250°C
Carrier: Column: Injection: Oven: Detector:
BTEX in Gasoline 1. 2. 3. 4. 5. 6. 7.
Pre-column: Injection: Oven: Detector:
5 7
4 6
20
Carrier: Column: Injection: Oven: Detector:
452
10 15 Time (min)
20
Helium (A) 10.7 psi (60°C) constant flow (B) Pressure program: 9 psi (9.5 min) to 30 psi (4 min) at 99 psi/min HP-1 (Cross-Linked Methyl Silicone), 30 m x 0.53 mm x 2.65 µm (Part No. 19095Z-123) 20% TCEP on Chromosorb PAW 80/100 56 cm x 1.6 mm x 0.32 mm Split (20:1), 3 µl 60°C isothermal Pub No.: 5091-4701E TCD 200°C
30
40
325°C 40°C/min
40°C 1.5 min
C9 5
1 2
4
C21 7
6
1
Time (min)
5
0
Reformate Gasoline
3
10
20
Methylene chloride
80°C 35 min 2°C/min
60°C
3
0
15
6
3 min
92 Octane Commercial Gasoline
2
7
Total Recoverable Petroleum Hydrocarbons (TPHs) Diesel Range
Benzene MIK (ISTD) Toluene Ethyl benzene p/m-Xylene o-Xylene C9, C10 plus nonaromatics
1
45
6 Valve Off
Carrier:
4
3 7 12
Valve On 1
Ethylene glycol dimethyl ether Benzene/1-methylcyclopentene TAME Heavy hydrocarbons (B) Pressure program 8
(A) Constant Flow
567 8 3 4 5
3
5. 6. 7. 8.
Ethanol MTBE Methanol ETBE
0
10
20
30
2
3
4
5
6
7
8
Time (min)
40
Time (min)
Helium, 10.7 psi constant flow HP-1 (Cross-Linked Methyl Silicone), 30 m x 0.53 mm x 2.65 µm (Part No. 19095Z-123) Split (17:1), 1 µl Temperature program listed above TCD 200°C Pub No.: 5091-5608E
GC: Carrier: Column: Injection: Oven:
6890 Helium 0.6 ml/min HP-5, 10 m x 100 mm x 0.17 µm (Part No. 19091S-002) Splitless, 0.1 µl Temperature program listed above Pub No.: 5965-6692
Petrochemical/Hydrocarbon Processing
BTEX
Olefins to C5 1. 2. 3. 4. 5.
1
Methanol Benzene Toluene Ethyl benzene Xylenes
1. 2. 3. 4. 5.
250°C 15°C/min
150°C 2 min
Ethylene Propylene 1-Butene 1-Pentene 1-Hexene
250°C 50°C 2 min 5
1
4 3
2
2
15°C/min
3 4
5
20 0 1
2
3
GC: Carrier: Column:
4
5
6 7 Time (min)
8
9
10
10 12 Time (min)
6890 Helium, 25 psig HP-PLOT Q, 30 m x 0.53 mm 40 µm (Part No. 19095P-Q04) Oven: Temperature program listed above Detector: FID Analyte concentration:100 ppm v/v
Pub No.: 5965-7872
14
16
18 20
Pub No.: 5965-7872
Sulfur Compounds in Naphtha
1. Ethylene oxide 2. 2-Chloropropene
1. 2. 3. 4.
250°C 2
8
12
Ethylene Oxide Synthetic Standard
1
6
GC: Carrier: Column:
6890 Helium, 25 psig HP-PLOT Q, 30 m x 0.53 mm x 40 µm (Part No. 19095P-Q04) Temperature program listed above FID
Oven: Detector:
11
4
50°C
15°C/min
2 min
Thiophene Methyl thiophenes Ethyl and dimethyl thiophenes Benzothiophene
1
130°C 70°C 35°C (15 min)
2
3
15°C/min
8°C/min
Applications
0
2
4
20
0
2
4
6
8
10 12 Time (min)
14
16
18
42 min
20
GC: 6890 Carrier: Helium, 25 psi Column: HP-PLOT Q, 30 m x 0.53 mm x 40 µm (Part No. 19095P-Q04) Injection: Split (40:1), 1 µl liquid injection, Oven: Temperature program listed above Detector: FID Pub No.: 5965-7872 Analyte concentration: 2000 ppm v/v
Carrier: Column: Injection: Oven: Detector:
www.agilent.com/chem
Helium, 26 cm/sec PONA (Cross-Linked Methyl Silicone), 50 m x 0.2 mm x 0.5 µm (Part No. 19091S-001) Split (400:1), 3 µl Temperature program listed above Pub No.: 5954-7615 FPD
453
Applications
Petrochemical/Hydrocarbon Processing
GC and GC/MS Applications
Sulfur Gases 1. 2. 3. 4. 5. 6.
Sulfur Compounds in Natural GasSynthetic Mixture
COS + SO Methyl mercaptan Ethyl mercaptan Isopropyl mercaptan n-Propyl mercaptan sec-Butyl mercaptan
1
1. 2. 3. 4. 5. 6. 7. 8. 9.
4
Hydrogen sulfide Methyl mercaptan Ethyl mercaptan Dimethyl sulfide Isopropyl mercaptan tert-Butyl mercaptan n-Propyl mercaptan Thiophene and sec-Butyl mercaptan Isobutyl mercaptan 1 234
11 5 7 8 9 12 10
10. 11. 12. 13. 14. 15. 16.
n-Butyl mercaptan tert-Amyl mercaptan iso-Amyl mercaptan n-Amyl mercaptan n-Hexyl mercaptan tert-Dibutyl disulfide n-Octyl mercaptan 300°C 7°C/min
35°C 10 min 16
13
5 3 14
2 6
Carrier: Column: Injection: Oven: Detector:
5 min Helium, 26 cm/sec HP-1 (Cross-Linked Methyl Silicone), 10 m x 0.53 mm x 2.65 µm (Part No. 19095Z-121) Splitless, 0.5 ml (capillary injection port) 35°C FPD
C20 C22 C24 C26 C28
6. 7. 8. 9. 10.
30 min Helium HP-1 (Cross-Linked Methyl Silicone), 50 m x 0.2 mm x 0.5 µm (Part No. 19091Z-205) Split (100:1) 0.5 ml Temperature program listed above FPD Pub No.: 5953-1662
Carrier: Column: Injection: Oven: Detector:
Petroleum Wax 1. 2. 3. 4. 5.
15
6
Polywax 500 320°C 10 min
C30 C32 C34 C36 C38
65°C
1. 2. 3. 4. 5. 6.
6°C/min
34 5 6 7 8
350°C 15 min
C20 C30 C40 C50 C60 C69
50°C
2
10°C/min
3
2 9 4
10
1
1 10
Carrier: Column: Injection: Inlet: Oven: Detector:
454
20
Time (min)
30
40
Helium, 22 psi at 65°C, constant flow mode HP-5 (Cross-Linked 5% Phenyl Methyl Silicone), 50 m x 0.32 mm x 0.17 µm (Part No. 19091J-015) On-column injection, 1 µl 68°C to 250°C at 15°C/min Temperature program listed above Pub No.: 5091-4209E FID
5 6 0 Carrier: Column: Injection: Oven: Detector:
45 min Helium, pressure program: 7 psi (1 min) to 18 psi (16 min) at 0.5 psi/min HP-1 (Cross-Linked Methyl Silicone), 15 m x 0.53 mm x 0.88 µm (Part No. 19095Z-023) 1 µl, on-column injection, oven track mode Temperature program listed above Pub No.: 5952-6971 FID 390°C
Petrochemical/Hydrocarbon Processing
Sulfur Compounds in Hexane
SFE of Diesel Oil in Soil
1. Propyl mercaptan 2. Dimethyl disulfide 3. Diethyl disulfide
280°C
250°C
20°C/min
50°C 2 min
15°C/min
10°C 2 min
1 2
2
GC: Carrier: Column: Oven: Detector: Analyte concentration:
4
6
8 10 Time (min)
12
14
16
18
20
6890 10 psi Helium head pressure HP PLOT Q, 0.53 x 30 m x 40 µm (Part No. 19095P-Q04) Temperature program listed above FID
0
2
Carrier: Column:
50 ppm
Pub No.: 5965-7872
Reference Gas Oil
4
Helium 45 cm/sec (70°C), 6 ml/min constant flow HP-50+ (Cross-Linked 50% Phenyl Methyl Silicone), 30 m x 0.53 mm x 1.0 µm (Part No. 19095L-023) Splitless, 1 µl, inlet 280°C Temperature program listed above FID 300°C
Injection: Oven: Detector:
35°C
NIST 1-K Kerosene, SRM 16160.0152 wt% Sulfur
S 0
15
20
15°C/min
C
S channel
10
335°C 10 min 40°C
10°C/min
C channel
5
12
SimDis of Kerosene 335°C 10 min
ASTM 2887
0
10
6 8 Time (min)
Applications
0
3
2
4
6 Time (min)
8
10
25
Time (min) Carrier: Column: Injection: Oven: Detector:
Helium, 5 psi, constant pressure mode with EPC HP-1 (Cross-Linked Methyl Silicone), 15 m x 0.53 mm x 0.88 µm (Part No. 19095Z-023) On-column injection, 0.2 µl neat, oven-track mode Temperature program listed above AED 350°C Pub No.: 5091-5303E
Carrier: Column: Injection: Oven: Detector:
Helium, 22 psi HP-1 (Cross-Linked Methyl Silicone), 25 m x 0.32 mm x 0.17 µm (Part No. 19091Z-012) Split (36:1), 0.2 µl neat Temperature program listed above Pub No.: 5091-5303E AED 350°C
www.agilent.com/chem
455
Applications
Petrochemical/Hydrocarbon Processing
GC and GC/MS Applications
SimDis of Diesel Fuel
Natural Gas 335°C 10 min
0.010 wt % Sulfur XRF 40°C
15°C/min
1. 2. 3. 4. 5. 6. 7.
Methane Ethylene Propane Isobutane Butane Isopentane Pentane 2
1
C
3
S
4 5
0
2
8 10 Time (min)
6
4
12
14
6
16 0
2
4
7
8
6
10
12
14
Time (min) Carrier: Column:
Helium, 22 psi HP-1 (Cross-Linked Methyl Silicone), 25 m x 0.32 mm x 0.17 µm (Part No. 19091Z-012) Split (36:1), 0.2 µl neat Temperature program listed above AED 350°C Pub No.: 5091-5303E
Injection: Oven: Detector:
Refinery Gas 1. 2. 3. 4. 5. 6. 7.
GC: Carrier: Column:
6890 Helium 23 cm/sec, constant pressure HP-1 60 m x 0.53 mm x 5 µm (Part No. 19095Z-626) 35 Isothermal Split (250:1), 0.5 cc FID
Oven: Injection: Detector:
Pub No.: 5964-2129E
Refinery Gas 8. 9. 10. 11. 12. 13.
Methane Ethylene Acetylene Ethane Propylene Propane Propadiene
iso-Pentane 1-Pentene n-Pentene trans-2-Pentene cis-2-Pentene 2-Methyl2-Butene
14. 15. 16. 17. 18. 19. 20.
1. 2. 3. 4. 5. 6.
Cyclopropane Isobutane Isobulylene 1,3-Butadiene n-Butane trans-2-Butene cis-2-Butene
7. 8. 9. 10. 11. 12.
Methane Ethane Ethylene Propane Propylene iso-Butane
9
n-Butane trans-2-Butene 1-Butene cis-2 Butene iso-Pentane n-Pentane
2
6
6
12 4 11 13 10
5 34 2 1
7
14
1 15
7
17 16
8
3 18
19
GC: Carrier: Column: Injection: Oven: Detector:
456
8
9
11 Time (min)
6890 Helium 23 cm/sec HP-1 100 m x 0.25 mm x 0.5 µm (Part No. 19091Z-530) Split (250:1), 500 µl 35°C isothermal FID
8 5
10 11
12
20 0
7
9
12
13 GC: Carrier: Column:
Pub No.: 5964-2129E
Injection: Oven: Detector:
2
4
6 Time (min)
8
6890 Helium 7 ml/min HP-PLOT/AI203 50 m x 0.53 mm x 15 µm (Part No. 19095P-S25) Split (100:1), inlet 250°C, 5 µl 100°C FID 250°C
10
12
Pub No.: 5964-2129E
Petrochemical/Hydrocarbon Processing
Butadiene and Aromatics 1. 2. 3. 4.
1,3-Butadiene Cyclopentene 1 Benzene Toluene
1,3-Butadiene 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
250°C
2 150°C 2 min
15°C/min
11. 12. 13. 14. 15. 16. 17. 18. 19.
Methane Ethane Ethylene Propane Cyclopropane Propylene iso-Butane n-Butane Propadiene Acetylene
trans-2-Butene 20. 2-Methyl-2-butene 1-Butene 21. Pentene-1 Iso-Butylene 22. cis-2-Pentene 180°C cis-2-Butene 23. n-Hexane Iso-Pentane 100°C 10°C/min n-Pentane 1, 3-Butadiene 35°C 5°C/min Propyne 2.5 min trans-2-Penten 13 17 7 8 e 4 12
4
2
3 1
0
1
2
3
4
5 6 Time (min)
7
8
9
6
14 16
3
10
10
9
5
GC: Carrier: Column:
6890 Helium, 25 psig HP-PLOT Q, 30 m x 0.53 mm x 40 µm (Part No. 19095P-Q04) Oven: Temperature program listed above Detector: FID Concentration: 200 ppm (v/v) Pub No.: 5964-2129E, 5965-7872
5
0 GC: Carrier: Column: Injection: Oven: Detector:
11
10
15 Time (min)
15
18 19 20 21 22 23 20
25
6890 Helium, 30 cm/sec (35°C), 4.6 ml/min constant flow HP-PLOT Al2O3, 50 m x 0.53 mm x 15 µm (Part No. 19095P-S25) Splitless, 5 µl; Inlet 250°C Temperature program listed above FID 250°C Pub No.: 5964-2129E
Propylene 180°C Methane
Ethane Ethylene Propane Cyclopropane Propylene iso-Butane n-Butane
9. 10. 11. 12. 13. 14. 15.
Propadiene Acetylene trans-2-Butene Butene-1 Iso-Butylene cis-2-Butene Iso-Pentane
16. 17. 18. 19. 20. 21. 22. 23.
n-Pentane 1, 3-Butadiene Propyne trans-2-Pentene 2-Methyl-2-butene Pentene-1 cis-2-Pentene n-Hexane
100°C 35°C 2.5 min 6
4
Injection: Oven: Detector:
6890 Propylene 90% Helium, 28 cm/ sec (35°C), 4.0 ml/ min constant flow HP- PLOT/Al2O3, 50 m x 0. 53 mm x 15 µm (Part No. 19095P-S25) Splitless, 5 µl; inlet 250°C Temperature program listed above FID 250°C
5°C/min
7 17
8
GC: Sample: Carrier: Column:
10°C/min
Applications
1. 2. 3. 4. 5. 6. 7. 8.
11
12 14
2
16
13 15 1 10 5 0
5
10
9 15 Time (min)
20
19
20 21 22
18
23 25
30
Pub No.: 5964-2129E
www.agilent.com/chem
457
Applications
Petrochemical/Hydrocarbon Processing
GC and GC/MS Applications
Ethylene 1. 2. 3. 4. 5. 6. 7. 8.
9. 10. 11. 12. 13. 14. 15. 16.
Methane Ethane Ethylene Propane Cyclopropane Propylene iso-Butane n-Butane
17. 18. 19. 20. 21. 22. 23.
Propadiene Acetylene trans-2-Butene Butene-1 Iso-Butylene cis-2-Butene Iso-Pentane n-Pentane 1, 1 2
3
3-Butadiene Propyne trans-2-Pentene 2-Methyl-2-butene Pentene-1 cis-2-Pentene n-Hexane
GC: Sample: Carrier:
6890 Ethylene 98.4% Helium, 50 cm/ sec (35°C), 7 ml/ min constant flow HP- PLOT/Al2O3, 50 m x 0. 53 mm x 15 µm (Part No. 19095P-S25) Split (65:1), 5 µl; inlet 250°C Temperature program listed above FID 250°C
Column: Injection: Oven: Detector:
4
6
100°C
7 8 35°C 2 min
11
5°C/min
17
12 14 16
13 18 19
15
20 9
10
22
5 0
23
10
5
21
15
20
25
Time (min)
Permanent Gases
Pub No.: 5964-2129E
Noble Gases 1. 2. 3. 4. 5. 6.
4
Neon Argon Oxygen Nitrogen Methane Carbon monoxide
1. 2. 3. 4. 5. 6.
Neon Argon Oxygen Nitrogen Krypton Xenon
35°C 3 min
120°C 5 min 25°C/min
4 2
3
5 6 6
5 1 2
1 3
2 GC: Sample: Carrier: Column: Oven: Detector:
4 Time (min)
6
6890 250 ml, split (75:1) Helium, 2 µl/min HP-PLOT/MoleSieve, 30 m x 0.32 mm x 12 µm (Part No. 19091P-MS4) 40°C Isothermal TCD Pub No.: 5964-2129E
458
2 GC: Sample: Carrier: Column: Oven: Detector:
Time (min)
6
6890 250 µl, split (50:1) Helium, 4 ml/min HP-PLOT/MoleSieve, 30 m x 0.53 mm x 50 µm (Part No. 19095P-MS0) Temperature program listed above TCD Pub No.: 5964-2129E
Petrochemical/Hydrocarbon Processing
Odor Additives Separation of Mercaptans and Other Sulfur Compounds on HP-Plot Q 1. 2. 3. 4. 5. 6.
Hydrogen Sulfide Carbonyl Sulfide Ethanelthiol iso-propyl mercaptan n-propyl mercaptan n-butyl mercaptan
1. 2. 3. 4.
240°C 2 min
105°C 1 min
Sulfur Odorants in Natural Gas
15°C/min
Hydrogen sulfide COS t-butyl mercaptan Methyl ethyl sulfide
250°C 30°C 1 min
10°C/min
1
5
3 4
3
2
4
6
1
2
6 Time (min)
4
8
10
6890 Hydrogen p=3.8 psi @ 60°C HP-PLOT Q, 0.53 mm x 30 m x 40 µm (Part No. 19095P-Q04) Inlet: 250°C Split mode 0.25 cc injection Oven: Temperature program listed above Split flow: 100 ml/min Detector: FID 250°C Concentrations: H2, COS: