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GB/T 24167-2022Determination of chlorinated toluenes in dye products (English PDF)

染料产品中氯化甲苯的测定

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

March 9, 2022

Implementation date

October 1, 2022

Scope

GB/T 24167-2022 is the English-translated version of 染料产品中氯化甲苯的测定.

GB/T 24167-2022 is the Chinese national method for measuring the residues of twelve chlorinated toluenes in dye products by gas chromatography-mass spectrometry.

It gives the principle, the reagents and materials, the apparatus, the preparation and extraction of the sample, the chromatographic and spectrometric conditions, the identification and quantification of each compound, the calculation, the precision and the test report.

It applies to the determination of chlorinated toluenes in dye products of every type, where they are process residues that are restricted. Dye works, textile buyers and testing laboratories use it.

It replaces GB/T 24167-2009, was issued on 9 March 2022 and has applied since 1 October 2022.

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Document preview — GB/T 24167-2022

National Standard of the People's Republic of China

ICS
71.100.01
Classification
G 55
Replacing
GB/T 24167-2009

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword3
  • 1 Scope5
  • 2 Normative Reference5
  • 3 Terms and Definitions5
  • 4 Principle of Method5
  • 5 Reagents or Materials5
  • 6 Apparatus6
  • 7 Preparation of Standard Solutions6
  • 8 Preparation of Sample Solutions7
  • 9 Test Procedures7
  • 10 Calculation of Result8
  • 11 Detection Limits, Precision and Accuracy9
  • 12 Test Report9
  • Appendix A (Normative) Types and Measurement Parameters of Chlorinated Toluene .10
  • Appendix B (Informative) Chromatogram of Chlorinated Toluene Standard Substance .11

1 Scope

This Document specifies a method for the determination of 12 chlorinated toluene residues in dye products by gas chromatography-mass spectrometry (GC/MS).

This Document applies to the determination of chlorinated toluene in various types of dye products.

2 Normative Reference

The provisions in following documents become the essential provisions of this Document through reference in this Document. For the dated documents, only the versions with the dates indicated are applicable to this Document; for the undated documents, only the latest version (including all the amendments) is applicable to this Document.

GB/T 8170-2008 Rules of Rounding off for Numerical Values & Expression and Judgement of Limiting Values

3 Terms and Definitions

This Document does not give the terms and definitions.

4 Principle of Method

In an ultrasonic bath, the chlorinated toluene in the specimen is extracted with dichloromethane, separated and determined by gas chromatography-mass spectrometry (GC/MS), and quantified by the external standard method of peak area.

5 Reagents or Materials

5.1 The types and measurement parameters of chlorinated toluene standard substances shall comply with the provisions of Appendix A.

5.2 Dichloromethane, chromatographically pure.

6 Apparatus

6.1 Gas chromatography-mass spectrometer (GC/MS): with EI source.

6.2 Chromatographic column: 50% silicone oil stationary phase, such as DB-17MS, 30mx0.25mmx0.25µm or equivalent.

6.3 Analytical balance: accuracy 0.01mg.

6.4 Ultrasonic generator.

6.5 Extractor: tube with stopper, 10mL

6.6 Centrifuge: 4000r/min.

6.7 Nitrogen blowing concentrator.

7 Preparation of Standard Solutions

7.1 Chlorinated toluene single standard stock solution

Respectively take 10mg of the standard substances listed in Appendix A, accurate to 0.01mg; dissolve with dichloromethane and make constant volume to a 10mL volumetric flask to prepare a single standard stock solution containing 1000mg/L of chlorinated toluene. The single standard stock solution shall be kept under 4 °C and protected from light, sealed and refrigerated; and the validity period is one month. Also certified standard solutions, such as single- component chlorinated toluene standard solutions or chlorinated toluene mixed standard solutions can be directly purchased.

7.2 Chlorinated toluene mixed standard working solution

Pipette 0.5mL of each single standard stock solutions of chlorinated toluene (see 7.1) to 10mL volumetric flasks; dilute to the mark with dichloromethane; and prepare a standard working solution containing 50mg/L of chlorinated toluene.

7.3 Standard working solutions

Use chlorinated toluene mixed standard working solution (see 7.2) to prepare the standard working solution; and the appropriate concentration can be prepared according to the content of the target substance in the specimen. m - the mass value of the specimen, in g.

The calculation result is rounded-off to two digits after the decimal point.

The calculation results are rounded-off according to the provisions of GB/T 8170-2008.

11 Detection Limits, Precision and Accuracy

11.1 Detection limit

When using the Method-I in Clause 8 to prepare sample solution, the detection limit of 12 chlorinated toluenes shall be 0.5mg/kg. When using the Method-II to prepare the sample solution, the detection limit is 2.5mg/kg.

11.2 Precision

In the same laboratory, the absolute difference between two independent measurement results obtained by the same operator using the same equipment, according to the same measurement method, and independently of each other on the same measured object in a short period of time is no greater than 20% of the arithmetic mean of the two determination results.

11.3 Accuracy

Use the standard addition method, add an appropriate amount of chlorinated toluene standard solution to 1g of dye specimen; and the concentration of the standard addition is 10mg/kg.

Operate according to the provisions of Clause 8; and the measured recovery rate of various chlorinated toluenes shall be 70% ~120%.

12 Test Report

The test report shall at least give the following:

a) description of the specimen;

b) this Document number;

c) test conditions;

d) test results;

e) deviations from the standard; f) Test date.

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 22 pages — is available in the English PDF.

Referenced standards

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Editions of GB/T 24167

EditionTitleRevisionStatus
GB/T 24167-2022Determination of chlorinated toluenes in dye productscurrent editionCurrent
GB/T 24167-2009Determination of chlorinated toluenes in dye productsprevious editionSuperseded

This page sells the current edition, GB/T 24167-2022. Earlier editions are listed for reference only.

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