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GB/T 24167-2022 English PDF (GBT24167-2022)

GB/T 24167-2022 English PDF (GBT24167-2022)

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GB/T 24167-2022: Determination of chlorinated toluenes in dye products

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.
GB/T 24167-2022
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.100.01; 87.060.10
CCS G 55
Replacing GB/T 24167-2009
Determination of Chlorinated Toluenes in Dye Products
ISSUED ON: MARCH 09, 2022
IMPLEMENTED ON: OCTOBER 01, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of the PEOPLE Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative Reference ... 5
3 Terms and Definitions ... 5
4 Principle of Method ... 5
5 Reagents or Materials ... 5
6 Apparatus ... 6
7 Preparation of Standard Solutions ... 6
8 Preparation of Sample Solutions ... 7
9 Test Procedures ... 7
10 Calculation of Result ... 8
11 Detection Limits, Precision and Accuracy ... 9
12 Test Report ... 9
Appendix A (Normative) Types and Measurement Parameters of Chlorinated Toluene ... 10
Appendix B (Informative) Chromatogram of Chlorinated Toluene Standard Substance ... 11
Determination of Chlorinated Toluenes in Dye Products
WARNING - Persons using this document shall have practical working experience in formal laboratory. This Document does not address all possible security issues. It is the user's responsibility to take appropriate safety and health measures, and to ensure compliance with the conditions stipulated by relevant national regulations. 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 and 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, 30m??0.25mm??0.25??m 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 ??? 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.

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