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ICS 71.100.01; 87.060.10

CCS G 55

National Standard of the People’s Republic of China

GB/T 24167-2022
Replaces GB/T 24167-2009

Determination of Chlorinated Toluenes

in Dye Products
染料产品中氯化甲苯的测定

(English translation)

Issue date: 2022-03-09 Implementation date: 2022-10-01

Issued by the State Administration for Market Regulation of the
People's Republic of China
the Standardization Administration of the People's Republic
of China

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Contents

Foreword .............................................................................................................................. II
1 Scope ............................................................................................................................. 1
2 Normative References ................................................................................................... 1
3 Terms and Definitions..................................................................................................... 1
4 Principle.......................................................................................................................... 1
5 Reagents or Materials .................................................................................................... 1
6 Apparatus ....................................................................................................................... 2
7 Preparation of Standard Solutions ................................................................................. 2
8 Preparation of Sample Solution ..................................................................................... 2
9 Test Procedures ............................................................................................................. 3
10 Calculation of Results .................................................................................................. 4
11 Detection Limit, Precision and Accuracy ...................................................................... 5
12 Test Report ................................................................................................................... 5
Annex A (Nominative) Types and Determination Parameters of Chlorinated Toluenes ...... 6
Annex B (Informative) Chromatogram of Chlorinated Toluene Standard Substances ....... 7

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Foreword

ChinaStandards.net is in charge of this English translation. In case of any doubt about

the English translation, the Chinese original shall be considered authoritative.

This document is developed in accordance with the rules given in GB/T 1.1-2020
Directives for Standardization — Part 1: Rules for the Structure and Drafting of
Standardizing Documents.

This document replaces GB/T 24167-2009 Determination of the Content of

Polychloriznated Toluenes in Dye Products. In addition to a number of structural
adjustments and editorial changes, the following technical deviations have been made
with respect to GB/T 24167-2009:

— the application scope of the standard is modified (see Clause 1 hereof; Clause 1 of
Edition 2009);

— the determination method of gas chromatography-electron capture detector

(GC-ECD) is deleted (see Clause 4 of Edition 2009);

— the principle is modified (see Clause 4 hereof; Clause 3 of Edition 2009);

— the preparation method of standard solution is modified (see Clause 7 hereof; 4.3 of
Edition 2009);

— the preparation method of sample solution is modified (see Clause 8 hereof; 4.5.1 of
Edition 2009);

— the chromatographic analysis conditions are modified (see 9.1 hereof; 4.5.2 of Edition
2009);

——The detection limit of the method is modified (see 11.1 hereof; 5.1 of Edition 2009);

— the requirements for accuracy determination of the method are modified (see 11.3
hereof; 5.2 of Edition 2009);

— the types of chlorinated toluenes are modified (see Annex A hereof; Annex A of
Edition 2009).

Attention is drawn to the possibility that some of the elements of this document may be the
subject of patent rights. The issuing body of this document shall not be held responsible
for identifying any or all such patent rights.

II

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This document was proposed by China Petroleum and Chemical Industry Association.

This document is under the jurisdiction of the National Technical Committee 134 on
Dyestuff of Standardization Administration of China (SAC/TC 134).

This document was issued in 2009 as first edition, and this is the first revised edition.

III

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Determination of Chlorinated Toluenes in Dye

Products

WARNING——Persons using this document should be familiar with normal laboratory

practice. This document does not purport to address all of the safety concerns, if any,
associated with its use. It is the responsibility of the user to establish appropriate
safety and health practices and to ensure compliance with any national regulatory
conditions.

1 Scope

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

This standard is applicable to determination of chlorinated toluenes in various dye

products.

2 Normative References

The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.

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

3 Terms and Definitions

No terms and definitions are listed in this document.

4 Principle

In ultrasonic bath, chlorinated toluenes are extracted with dichloromethane from samples,
separated and measured by gas chromatography-mass spectrometry (GC/MS), and
quantified by peak area external standard method.

5 Reagents or Materials

5.1 The types and determination parameters of chlorinated toluene standard substances
shall meet the requirements of Annex A.

5.2 Dichloromethane, chromatographic grade.

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6 Apparatus

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

6.2 Chromatographic column: 50% phenylmethyl polysiloxane stationary phase, e.g.,

DB-17MS, 30 m × 0.25mm × 0.25 μm or equivalent.

6.3 Analytical balance: with an accuracy of 0.01mg.

6.4 Ultrasonic generator.

6.5 Extractor: tube with a stopper, 10 mL.

6.6 Centrifuge: 4000 r/min.

6.7 Nitrogen blowing concentrator.

7 Preparation of Standard Solutions

7.1 Single-component standard stock solutions of chlorinated toluene

Weigh 10 mg (to the nearest 0.01 mg) of standard substances listed in Annex A; dissolve
them with dichloromethane and dilute them to a 10 mL volumetric flask to prepare a
single-component standard stock solution with chlorinated toluene of 1000 mg/L, which
shall be stored under 4°C, sealed and refrigerated in a dark place, with a useful life of one
month. Alternatively, certified standard solutions, single-component standard solutions of
chlorinated toluenes or mixed standard solutions of chlorinated toluenes can also be
purchased directly.

7.2 Mixed standard working solution of chlorinated toluenes

Pipette 0.5 mL of single-component standard stock solution of chlorinated toluenes (see

7.1) into a 10 mL volumetric flask, dilute it with dichloromethane to the scale to prepare a
mixed standard working solution with chlorinated toluenes of 50mg/L.

7.3 Standard working solution

The standard working solution is prepared with the mixed standard working solution of
chlorinated toluenes (see 7.2), with concentration dependent on the content of the target
substance in the sample.

8 Preparation of Sample Solution

In general, Method 1 is used to prepare the sample solution for general dye products. If

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