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