ISO-6468-1996.pdf
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1、INTERNATIONAL STANDARD IS0 6468 First edition 1996-12-15 Water quality - Determination of certain organochlorine insecticides, polychlorinated biphenyls and chlorobenzenes - Gas chromatographic method after liquid-liquid extraction Qua/it6 de I eau - Dosage de certains insecticides organochlorks, de
2、s polychlorobiphknyles et des chlorobenz below concen- trations of 10 rig/l, special care is necessary. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editi
3、ons indicated were valid. All standards are subject to revision, and parties to agreements based on the International Standard are encouraged to in- vestigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently
4、 valid Inter- national Standards. IS0 5667-i :1980, Water quality- Sampling - Part 1: Guidance on the design on sampling programmes. IS0 5667-2:1991, Water quality - Sampling - Part 2: Guidance on sampling techniques. 3 Principle Liquid-liquid extraction of organochlorine insecticides, chlorobenzene
5、s and PCBs by an extraction solvent. After the concentration of the components with low volatility and after any clean-up steps which may be necessary, the sample extracts are analysed by gas chromatography, using an electron-capture detector. 1 Copyright International Organization for Standardizati
6、on Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/18/2007 19:40:39 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 6466: 1996(E) Table 1 - Detection limits Acronyms Chemical names (IUPAC) Detection limits Organoc
7、hlorine insecticides: HCH 1, 2, 3, 4, 5. 6-hexachlorocyclohexane, five stereoisomers: alpha-HCH beta-HCH Lindane gamma-HCH defta-HCH epsilon-HCH o,p -DDE 1 ,l -dichloro-2-(2-chlorophenyl l )-2-(4-chlorophenyl)ethylene n,p -DDE 1 ,l-dichloro-2,2-bis(4-chlorophenyl)ethylene 1 rig/l ,p -TDE 1 ,l-dichlo
8、ro-2-(2-chlorophenyl)-2-(4-chlorophenyl)ethane (= o,p -DDD) to up -TDE 1 ,l -dichloro-2, 2-bis(4-chlorophenyl)ethane (= p,p -DDD) 10 rig/l Y,P -DDT 1 ,l ,l-trichloro-2-(2-chlorophenyl)-2-(4-chlorophenyI)ethane depending YQ -DDT 1 ,l ,l -trichloro-2,2-bis(4-chlorophenyl)ethane on the Methoxychlor 1 ,
9、l ,l -trichloro-2,2-bis(4-methoxyphenyl)ethane compound Ndrin (1 R, 4S, 4a.X 5S, 8R, 8aR)-1, 2, 3, 4, 10, lo-hexachloro-l , 4, 4a, 5, 8, 8a-hexahydro-l , 4: 5.8-dimethanonaphthalene Dleldrln (lR, 4S, 4aS, 5R, 8R, 7S, 8S, 8aR)-1,2,3,4,10,10-hexachloro-1,4,4a, 5, 6,7,8,8a-octahydrod, 7-epoxy-1,4: 5,8-
10、dimethanonaphthalene Endrtn (lR, 4S, 4aS, 5S, 6S, 7R, 8R, 8aR)-1,2,3,4.10,10-hexachloro-1,4,4a, 5, 6,7,8,8a-octahydro-6,7-epoxy-1,4: 5,8-dimethanonaphthalene Heptachlorl) 1,4,5.6,7.8,8-heptachloro-3a, 4,7,7a-tetrahydro-4,7-methanoindenel) Heptachlor-epoxide 1, 4, 5, 6, 7, 8, 8-heptachloro-2.3-epoxy-
11、3a,4,7,7a-tetrahydro-4,7 -methanoindane Endosulfanl) 2) lf4,5,6,7,7,7-hexachloro-8,9.l0-trinorborn-5-en-2, 3-ylene-dimethyl- enesulfite: alpha-Endosulfan beta-Endosulfan Chlorobenzenes: TrCB trichlorobenzene 1 n TeCB tetrachlorobenzene to PeCB pentachlorobenzene lOngA HCB hexachlorobenzene depending
12、 on PCNB (Quintozene) pentachloronitrobenzene the compound Polychlorlnated biphenyls: PCB 28 2,4,4 -trichlorobiphenyl PCB 52 2,2 , 5,5 -tetrachlorobiphenyl 1 n PCB 101 2,2 , 4,5,5 -pentachlorobiphenyl to PCB 138 2,2 , 3,4,4 , 5 -hexachlorobiphenyl 50 rig/l PCB 153 2,2 , 4,4 , 5, S-hexachlorobiphenyl
13、 depending on PCB 180 2,2 , 3,4,4 , 5,5 -heptachlorobiphenyl the compound PCB 194 2,2 , 3,3 , 4,4 , 5, S-octachlorobiphenyl 1) The analysis of a and /3 - endosulfan as well as heptachlor requires special care due to its low stability. 2) The name endosulfan” is not acceptable for use in Italy, as it
14、 is in conflict with a trade mark registered there. 2 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/18/2007 19:40:39 MDTNo reproduction or networking permitted without license from IHS
15、 -,-,- (23 IS0 IS0 6468: 1996(E) Any substance capable of producing a response on the electron-capture detector, at a retention time indis- tinguishable from any compound of interest, will interfere. In practice, many potentially interfering sub- stances will be removed during the extraction and cle
16、an-up procedures. NOTE 1 In general, the use of two capillary columns of different polarity is sufficient for the organochlorine com- pounds analysed according to this International Standard. The results so calculated should be considered as the maximum concentrations, possibly still influenced by c
17、oelut- ing substances. It is possible that there will be cases where a more definite identification is required. 4 Reagents and materials All reagents shall be sufficiently pure to not give rise to significant interfering peaks in the gas chromatograms of the blanks. The purity of reagents used in t
18、he pro- cedure shall be checked by blank determinations (7.6). NOTE 2 Commercial “pesticide grade” solvents are avail- able. The use of these products is recommended only after verifying their quality. The quality of a solvent is checked by evaporation of about 200 ml down to 1 ml and analysis of th
19、e concentrate to determine the compounds subsequently analysed. The solvent should be considered acceptable if it does not give any detectable interfering peaks in the chro- matogram for the substance of interest. 4.1 Water purified, for example, using ion-exchange or carbon-column adsorption. 4.2 E
20、xtraction solvent. Hexane, petroleum ether or heptane are suitable. NOTE 3 Any other solvents meeting the requirements of 8.3 (recovery rate 2 60 %) may be used. muffle furnace. Cool to about 200 “C in the furnace and then to ambient temperature in a desiccator. Store in a sealed glass container. 4.
21、6 Deactivated alumina. Weigh a portion of dry alumina (4.5) into a sealable all- glass container and add 7 % C 0,2 % (m/m) of water (4.1). Seal and agitate for at least 2 h to ensure uni- formity. Store in a sealed glass container. Once the seal has been broken, storage time is nor- mally about one
22、week. After the maximum storage time, reprocess batches as described in 4.5 and this subclause. 4.7 Alumina/silver nitrate. Dissolve 0,75 g k 0,Ol g of silver nitrate in 0,75 ml f 0,Ol ml of water (4.1) using a microburette. Add 4,0 ml + 0,2 ml of acetone followed by 10 g * 0,2 g of deactivated alum
23、ina (4.6). Mix thoroughly by shaking in an open-topped conical flask, protected from light. Allow the acetone to evaporate at room temperature and prevent condensation, for example by warming with the hand. Store in the dark and use within 4 h after preparation. 4.8 Silica gel, of particle size 63 p
24、m to 200 pm, heated at 500 “C f 30 “C in batches not larger than 500 g, for about 14 h. Cool to about 200 “C in the fur- nace and then to ambient temperature in a sealed flask which is placed in a desiccator without desiccant. Use this material within one week. Deactivate the sil- ica gel by weighin
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