GB/T 25011-2010Test method and determination for DDT content of marine antifouling paints (English PDF)

1 Scope

This standard specifies the determination of DDT (including DDT, including isomers and their derivatives) in marine antifouling paints by gas chromatography

Reagents, equipment, sampling, test procedures, the results of the decision and test reports.

This standard applies to the determination of DDT in ship antifouling paint, and it is also applicable to the ship antifouling paint which recognizes DDT as biocide.

2 normative reference documents

The terms of the following documents are hereby incorporated by reference into this standard. Whichever is the date of the reference file, which is followed by all (Excluding corrigenda) or revisions do not apply to this standard, however, encourage the parties to reach an agreement under this standard

Whether you can use the latest version of these files. For undated references, the latest edition applies to this standard.

GB/T 3186 Sampling of raw materials for paints, varnishes and varnishes and varnishes (GB/T 3186-2006, ISO 15528..2000, IDT)

Basic principles

The test method is mainly based on a gas chromatograph with an electron capture detector for determination.

Electron capture detector is a selective detector, the halogen, S, P, N, O negative negative elements of the material, a great response, and the

Non-electronegative substances, the response is very small. DDT with a strong negative charge of chlorine, the use of electronic capture detector this feature can be detected

A small amount of DDT (including four forms, p, p'-DDE, o, p'-DDT, p, p'-DDD and p, p'-DDT).

In this standard, samples were extracted with pure n-hexane, and 14% propyl cyanonitrile and 86% dimethylpolysiloxane were mixed

Fixed liquid separation, electronic capture detector for testing, external standard method for quantitative.

4 reagent

Organic solvents should be re-steamed and chromatographed to verify the presence of non-interfering substances. The test reagents include.

a) n-hexane. chromatographic purity;

b) chromatographic standard sample. p, p'-DDE, o, p'-DDT, p, p'-DDD, p, p'-DDT, content 98% ~ 99% c) anhydrous sodium sulfate. analytical grade;

d) Carrier gas. nitrogen, purity 99.999%, filtered by deoxidizing tube, oxygen content less than 0.0005%, hydrogen content less than 0.0001%;

e) standard stock solution. accurately weighed p, p'-DDE, o, p'-DDT, p, p'-DDD, p, p'-DDT 10mg, respectively

100mL brown volumetric flask, diluted with n-hexane to the mark, mix and store at 4 ° C (sample storage period is

2 months);

f) mixed standard working fluid. According to the electronic capture detector sensitivity and linear requirements, respectively, to measure a certain amount of four standard stock solution

In the same volumetric flask, diluted with n-hexane to the mark, prepared into several concentrations of standard working fluid, stored at 4 °C

Product storage period of 2 months).

5 equipment

The main equipment of the test include.

a) a gas chromatograph with an electron capture detector;

b) Column. phi0.32mm × 30m capillary column, coated with 14% propyl cyanide and 86% dimethylpolysiloxane mixed fixative;

c) Oscillator;

d) microinjector. 5 [mu] L, 10 [mu] L;