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Separation and Isolation of Volatile Organic Compounds Using  Vacuum Distillation with GC/MS Determination

Table 1.   Yields and precision errors for vacuum distilled compounds
COMPOUND Oila Waterb Soilc Fishd
Chloromethane N/Ad 93±18 66±32 N/A
Bromomethane N/A 105± 9 63±33 N/A
Vinyl Chloride N/A 105± 9 60±25 N/A
Chloroethane N/A 88±10 52±21 N/A
Methylene Chloride 63±34 72±13 66±15 CONTe
Acetone CONT 70±23 CONT CONT
Carbon Disulfide 98±40 110± 8 50±23 79±36
1,1-Dichloroethene 100±25 84± 6 53±20 122±39
1,1-Dichloroethane 98±21 96±11 67±19 126±35
trans-1,2-Trichloroethene 89±22 84± 6 59±19 109±46
Cis-1,2-Dichloroethene 102±12 85± 8 66±16 106±22
Chloroform 96±12 91±14 114±28 111±32
1,2-Dichloroethane 110±19 93±15 99±14 117±27
2-Butanone INTf INT INT INT
1,1,1-Trichloroethane 91±12 96±13 137±23 106±30
Carbon Tetrachloride 91±40 91±14 82±59 83±34
Vinyl Acetate INT 72±13 84±12 INT
Bromodichloromethane 84± 7 92±11 49±12 97±22
1,1,2,2-Tetrachloroethane 62±10 78±20 75±22 67±20
1,2-Dichloropropane 68±34 89±14 56±17 117±23
trans-1,3-Dichloropropene 78± 9 94±15 70±18 92±22
Trichloroethene 81± 7 86± 8 52±16 98±31
Dibromochloromethane 81±19 90±12 74±18 71±19
1,1,2-trichloroethane 75± 8 87±14 66±20 92±20
Benzene 115± 6 86± 9 54±12 129±35
Cis-1,3-Dichloropropene 78± 8 94±12 64±20 102±24
Bromoform 48± 6 81±21 58±19 58±19
2-Hexanone INT 54±17 99±20 INT
4-Methyl -2-pentanone INT 69±20 79±24 113±37
Tetrachlorethene 58± 8 91±11 56±16 66±20
Toluene 85±10 89±11 50±13 CONT
Chlorobenzene 50± 6 88±12 61±18 65±19
Ethylbenzene 48± 6 90±12 70±23 74±19
Styrene 55± 7 89± 9 66±19 57±14
Para-xylene 25±10 86± 8 60±19 46±13
Ortho-xylene 45± 7 86±10 66±20 83±20
Bromofluorobenzene 38± 4 94±11 73±19 52±15


a 1 g cod liver oil emulsified with lecithin and 5 ml water. Concentration is 250 ppb.
b 5 g of soil mixed with 5 ml water. Concentration is 50 ppb.
c 10 g fish tissue mixed with 5 ml water. Concentration is 25 ppb.
d No analyses.
e Excessive concentration of analyte in sample prior to spiking.
f Spectral interferences due to concentration of co-eluting hydrocarbons present in sample

 

Table 2.   Method detection limits using standardized vacuum distillation following Resource Conservation and Recovery Act guidelines with GC/MS quantitation

Compound

 Watera (ppb) Soilb (ppb) Tissuec (ppb) Oild (ppb)
Chloromethane 3.1 8.6 7.8 N/Ae
Bromomethane 2.5 4.9 9.7 N/A
Vinyl Chloride 4.0 7.1 9.5 N/A
Chloroethane 6.1 7.5 9.2 N/A
Methylene Chloride 3.1 3.3 CONTf 0.08
Acetone 33.0 CONT CONT 0.12
Carbon Disulfide 2.5 3.2 5.4 0.19
1,1-Dichloroethene 3.4 3.8 4.0 0.19
1,1-Dichloroethane 2.3 1.7 4.0 0.13
trans-2,3-Dichloroethene 3.0 3.2 4.4 0.09
cis-1,2-Dichloroethene 2.4 2.7 4.7 0.08
Chloroform 2.7 2.6 5.6 0.06
1,2-Dichloroethane 1.6 1.7 3.3 0.06
2-Butanone 57.0 INTg INT INT
1,1,1-Trichloroethane 1.6 2.4 1.1 0.08
Carbon Tetrachloride 1.5 1.7 3.2 0.15
Vinyl Acetate 23.0 INT INT INT
Bromodichloromethane 2.0 2.3 3.2 0.05
1,1,2,2-Tetrachloroethane 3.6 3.2 4.4 0.09
1,2-Dichloropropane 2.9 3.7 3.8 0.12
trans-1,3-Dichloropropane 2.3 2.4 3.8 0.08
Trichloroethene 2.5 3.0 3.1 0.06
Dibromochloromethane 2.1 2.9 3.5 0.04
1,1,2-Trichloroethene 2.7 2.8 4.4 0.07
Benzene 1.7 2.9 3.6 0.03
cis-1,3-Dichloropropene 2.1 2.5 3.5 0.06
Bromoform 2.3 2.5 4.9 0.10
2-Hexanone 4.6 4.6 7.7 INT
4-Methyl-2-pentanone 3.8 3.9 7.5 INT
Tetrachloroethene 1.8 2.6 4.3 0.12
Toluene 1.8 4.4 3.0 0.09
Chlorobenzene 2.4 2.6 3.3 0.07
Ethylbenzene 2.4 4.1 3.6 0.09
Styrene 2.0 2.5 3.5 0.16
para-Xylene 2.3 3.9 3.7 0.18
ortho-Xylene 2.4 4.1 3.3 0.08

a 5 ml water.
b 5 g soil.
c 10 g tissue.
d 1 g cod liver oil.
e No analyses
f Excessive concentration of analyte in sample prior to spiking.
g Spectral interferences due to elevated concentration of co-eluting hydrocarbons present in sample.

 

 

 


 

National Exposure Research Laboratory
Author:  Mike Hiatt / Email:  Hiatt.Mike@epa.gov
Send questions or comments to the Information Desk
ESD Info Desk (contractor operated)
(Library-lv@epa.gov)

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