APPLICATION NOTE
Quantitative Method for EPA 8260B Compounds
Using the HAPSITE® ER Portable GC/MS Chemical
Identification System with Headspace Sampling
SystemINTRODUCTION

EXPERIMENTAL

EPA standard method 8260B describes a set ofprocedures and conditions for collection and analysis
of volatile organic compounds (VOCs) for solid wastes.
Several sample collection techniques, including
headspace sampling, are permitted. Gas
chromatographic separation followed by mass spectral(MS) detection and identification of the collected VOCs
is required to characterize the matrix analytes. The
HAPSITE ER Gas Chromatograph/Mass Spectrometer(GC/MS), along with the Headspace Sampling System(HSS) in portable mode, allows for the EPA 8260B
method to be performed on site, eliminating the risk ofsample contamination. After the sample has beencollected, the VOCs are purged from the sample andare collected into the headspace created above theliquid sample.

Five concentrations in the low to mid µg/L (low to midppb) range were prepared for this calibration. Various
volumes of Restek 8260B MegaMix® standard, alongwith the INFICON HSS Internal Standard Mix (IPN 071478), were manually injected into five 40 mL vials
containing 20 mL VOC-free water. The samples werethen allowed to equilibrate in the HSS at 60ºC for about
20 minutes.

INFICON has developed a quantitative method for theHAPSITE ER utilizing the HSS accessory formonitoring analytes listed in the 8260B method. The
method contains a calibration library of 58 analytes
listed in the 8260B method at detection limits in the low
to mid µg/L (low to mid ppb) range. Using the HAPSITE
ER-HSS configuration along with the quantitative
method allows the user to analyze data on-site.

The calibration library included in the methods for theHAPSITE ER with the HSS is in compliance with the8260B method, and quantitative results can beobtained quickly when this method is utilized. Concerns
about sample contamination are also minimized as aresult of on-site sample collection.

Following the analysis of the calibration standards, a58-compound calibration library was built and stored in
the method file. Figure 1 displays a chromatogram
labelled with the method parameters. Table 1 contains
the 58 compounds including quantitation ions (Q. Ion),
retention times, and RSD of average Rf.
CONCLUSION

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Quantitative Method for EPA 8260B Compounds Using the HAPSITE® ER Portable GC/MS Chemical Identification System with

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Headspace Sampling System

Figure 1: Example Chromatogram of the Analytes in the Restek 8260B MegaMix Standard

Naphthalene
Tetrachloroethylene
Trichloroethylene

Column: HP-1MS, 15 m, 0.25 mm id, 1.0 µm df
Temperature Profile: 60°C (hold 2 min, 30 sec.) to 100°C at 10°C/min., to 180°C at 26°C/min. (hold 26 sec)
Table 1: Q. Ion, Retention Time, and RSD of Average Rf of the 8260B MegaMix Standard
Compound

Q. Ion(AMU)

Retention Time(min:sec)

RSD of Average Rf(%)

Vinyl Chloride

6200:38.3

34.04

Bromomethane

9400:40.9

29.63

Chloroethane

6400:41.3

29.27

Trichloromonofluoromethane

10100:45.5

29.88

1,1-Dichloroethene61

00:49.1

24.15

Methylene Chloride

84

00:49.6

33.75

trans-1,2-Dichloroethene96

00:55.7

23.00

1,1-Dichloroethane63

00:57.3

28.90

MTBE

73

00:57.8

21.55

cis-1,2-Dichloroethene96

01:03.9

23.46

Bromochloromethane

130

01:05.6

32.01

Trichloromethane (Chloroform)

85

01:06.616.24

2,2-Dichloropropane

77

01:07.4

27.94

1,2-Dichloroethane62

01:14.5

22.35

1,1,1-Trichloroethane97

01:18.0

27.22

Quantitative Method for EPA 8260B Compounds Using the HAPSITE® ER Portable GC/MS Chemical Identification System with

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Headspace Sampling System

Table 1: Q. Ion, Retention Time, and RSD of Average Rf of the 8260B MegaMix Standard (Continued)
Compound

Q. Ion(AMU)

Retention Time(min:sec)

RSD of Average Rf(%)

1,1-Dichloropropene75

01:23.7

29.53

Benzene78

01:23.9

29.06

Carbon Tetrachloride

117

01:26.2

25.11

Dibromomethane93

01:36.1

27.47

1,2-Dichloropropane

63

01:36.8

23.37

Bromodichloromethane83

01:40.0

28.24

Trichloroethylene

95

01:40.7

28.93

cis-1,3-Dichloropropene

75

01:59.8

23.11

trans-1,3-Dichloropropene75

02:14.6

20.41

1,1,2-Trichloroethane97

02:20.2

27.61

Toluene91

02:29.8

26.83

1,3-Dichloropropane

76

02:30.9

20.36

Dibromochloromethane129

02:45.0

26.39

1,2-Dibromoethane107

02:54.7

29.46

Tetrachloroethylene

166

03:15.2

25.16

1,1,1,2-Tetrachloroethane131

03:47.5

23.41

Chlorobenzene

112

03:47.8

21.64

Ethylbenzene

91

04:09.4

23.72

Bromoform

173

04:18.7

24.18

m-and p-Xylene

91

04:20.2

31.44

Styrene104

04:39.3

28.14

1,1,2,2-Tetrachloroethane83

04:45.0

20.99

o-Xylene91

04:45.0

29.26

1,2,3-Trichloropropane

75

04:52.4

18.86

Bromobenzene

77

05:21.7

27.72

Isopropylbenzene

105

05:21.7

28.61

2-Chlorotoluene

91

05:48.7

28.45

4-Chlorotoluene

126

05:54.6

27.93

n-Propylbenzene

120

05:54.8

30.77

1,3,5-Trimethylbenzene

105

06:12.1

24.78

t-Butyl benzene

119

06:39.1

26.71

1,2,4-Trimethylbenzene

120

06:39.4

28.21

1,3-Dichlorobenzene

146

06:43.5

20.69

1,4-Dichlorobenzene

146

06:49.4

28.45

Quantitative Method for EPA 8260B Compounds Using the HAPSITE® ER Portable GC/MS Chemical Identification System with

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Table 1: Q. Ion, Retention Time, and RSD of Average Rf of the 8260B MegaMix Standard (Continued)
Compound

Q. Ion(AMU)

Retention Time(min:sec)

RSD of Average Rf(%)

sec-Butyl benzene

105

06:55.9

27.16

p-Isopropyltoluene

119

07:07.7

30.06

1,2-Dichlorobenzene

146

07:10.1

18.45

n-Butyl benzene

91

07:32.8

28.68

1,2-Dibromo-3-chloropropane

157

07:36.7

29.82

1,2,4-Trichlorobenzene

180

08:45.0

25.47

Naphthalene

128

08:48.6

28.07

1,2,3-Trichlorobenzene

180

09:02.0

28.62

Hexachlorobutadiene

225

09:10.2

24.05

TM

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