GB/T 5750.8-2006 in English

《GB/T 5750.8-2006生活饮用水标准检验方法 有机物指标》由628（国家疾病预防控制局）归口，主管部门为国家疾病预防控制局。
本标准规定了用填充柱气相色谱法测定生活饮用水及其水源中三氯甲烷、四氯化碳、三氯乙烯、二氯一溴甲烷、四氯乙烯、一氯二溴甲烷和三溴甲烷。
本方法适用于生活饮用水及其水源水中三氯甲烷、四氯化碳、三氯乙烯、二氯一溴甲烷、四氯乙烯、一氯二溴甲烷和三溴甲烷的测定。
本法的最低检测质量浓度分别为:三氯甲烷0.6μg/L；四氯化碳0.3μg/L；三氯乙烯3μg/L；二氯一溴甲烷1μg/L；四氯乙烯1.2μg/L；一氯二溴甲烷0.3μg/L；三溴甲烷6μg/L。

1 Carbon Tetroxide

1.1 Packed column gas chromatography
1.1.1 Scope
This Standard specifies the packed column gas chromatography for the determination of trichloromethane, carbon tetrachloride, trichloroethylene, dichloromonobromomethane, tetrachloroethylene, chlorodibromomethane and bromoform in drinking water and its source water.
This method is applicable to determination of trichloromethane, carbon tetrachloride, trichloroethylene, dichloromonobromomethane, tetrachloroethylene, chlorodibromomethane and bromoform in drinking water and its source water.
The minimum detectable mass concentrations in this method are respectively: trichloromethane, 0.6μg/L; carbon tetrachloride, 0.3μg/L; trichloro ethylene, 3μg/L; Bromodichloromethane, 1μ/L;tetrachloroethylene, 1.2μg/L; Chlorodibromomethane, 0.3μg/L; bromoform, 6μg/L.
1.1.2 Principles
Put the to-be-tested water sample in a sealed headspace bottle; after certain time of balance under certain temperature, halohydrocarbon in water escape to the headspace and reaches dynamic balance in gas-liquid phase. On this occasion, concentration of halohydrocarbon in gas phase is proportional to that in liquid phase. By determining the concentration of halohydrocarbon in gas phase, the content of halohydrocarbon in water sample may be calculated.
1.1.3 Reagents and materials
1.1.3.1 Gas carrier
High purity nitrogen (99.999%).
1.1.3.2 Reagents and materials used in preparation of standard sample and sample pretreatment
1.1.3.2.1 Pure water: fresh deionized water, no determined component in the chromatogram examination.
1.1.3.2.2 Ascorbic acid.
1.1.3.2.3 Methanol: top grade pure, no determined component in the chromatogram examination.
1.1.3.2.4 Chromatogram reference materials: trichloromethane (99.92%), Bromodichloromethane (97.3%), chlorodibromomethane (98.1%), bromoform (99.73%), carbon tetrachloride (99.92%), Chlorodibromomethane (99.73%), trichloroethylene (99.53%) are all chromatographically pure.
1.1.3.3 Reagents and materials used in preparation of chromatographic column
1.1.3.3.1 Chromatographic columns and fillers: see the relevant content in 1.1.4.1.3.
1.1.3.3.2 Solvent used in coating stationary liquid: acetone.
1.1.4 Apparatuses
1.1.4.1 Gas chromatograph.
1.1.4.1.1 Electron capture detector.
1.1.4.1.2 Recorder or workstation.
1.1.4.1.3 Chromatographic column
A Type of chromatographic column: U-shaped or spired glass column. Length: 2m; inner diameter: 2 or 3mm.
B Filler:
a Carrier: Chromosorb AW or DMCS 60 meshes ~ 80meshes or 80 ~100meshes. Sieved prior to use and then baked for 2h at 120℃.
b Stationary liquid and its content: 15% DC -550(polymethyl siloxane with 25% of phenyl)
c Coating stationary liquid method: calculate chromatographic column volume, measure off carrier slightly more than the calculated volume and measure its mass. Accurately weigh a given amount of stationary liquid accordingto the mass of carrier, dissolve it in the acetone solvent, after fully dissolved, add it into carrier, and by this time liquid level shall totally immerse the carrier.At room temperature, naturally volatilize the solvent to dry (never by means of stirring with glass rod), packing may be conducted after the solvent is totally volatilized to dry and without acetone odor.
d Packing method: connect column outlet end to the vacuum pump (note : the cotton shall be plugged in the column tube), Terminate small funnel at column inlet, put in the stationary phase therefrom, carry out the column filling by air exhaust while uniform column knocking.
e Aging of chromatographic column: terminate the column inlet to the chromatographic system, empty the end at the column outlet, fill in nitrogen (flow rate: 30mL /min).Age 16h after column temperature ascends to 150℃ at the heating speed of 10℃/30min from 60℃.

Foreword I
1 Carbon Tetroxide
2 1, 2-Dichloroethylene
3 1,1,1- Trichloroethane
4 Vinyl Chloride
5 1,1-Dichloroethene
6 1,2-Dichloroethene
7 Trichloroethylene
8 Tetrachloroethylene
9 Benzapyrene
10 Acrylamide
11 Caprolactam
12 Bis(2-Ethylhexyl)Phthalate
13 Microcystin
14 Acetonitrile
15 Acrylonitrile
16 Acrolein
17 Epoxy Chloropropane
18 Benzene
19 Toluene
20 Dimethylbenzene
21 Ethylbenzene
22 Isopropyl Benzene
23 Chlorobenzene
24 Dichlorobenzene
25 1,2-Dichlorobenzene
26 1,4-Dichlorobenzene
27 Trichlorobenzene
28 Tetrachlorobenzene
29 Nitrobenzene
30 Trinitrotoluene
31 Dinitrobenzene
32 Nitrochlorobenzene
33 Dinitrochlorobenzene
34 Chloroprene
35 Styrene
36 Triethylamine
37 Aniline
38 Carbon disulfide
39 Hydrazine hydrate
40 Turpentine
41 Pyridine
42 Picric Acid
43 N-butyl xanthate
44 Hexachlorobutadiene
Appendix A (Informative) Purge-and-trap/Gas Chromatography - Mass Spectrometry for Determination of Volatile Organic Compound
Appendix B (Informative) Solid-Phase Extraction/Gas Chromatography - Mass Spectrometry for Determination of Half-Volatile Organic Compound
Appendix C (Normative) Normative References