GB/T 24166-2021 PDF in English
GB/T 24166-2021 (GB/T24166-2021, GBT 24166-2021, GBT24166-2021)
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| GB/T 24166-2021 | English | 170 |
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Determination of the content of chlorinated phenols in dye products
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| GB/T 24166-2009 | English | 125 |
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Determination of the content of chlorinated phenols in dye products
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Standards related to (historical): GB/T 24166-2021
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GB/T 24166-2021: PDF in English (GBT 24166-2021) GB/T 24166-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.01; 87.060.10
CCS G 55
Replacing GB/T 24166-2009
Determination of the Content of Chlorinated Phenols in Dye
Products
ISSUED ON: DECEMBER 31, 2021
IMPLEMENTED ON: JULY 1, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative References ... 5
3 Terms and Definitions ... 5
4 Method Principle ... 5
5 Reagents or Materials ... 6
6 Instruments and Equipment ... 6
7 Preparation of Standard Solutions ... 7
8 Preparation of Sample Solution ... 7
9 Preparation of Standard Working Solution ... 8
10 Test Procedures ... 8
11 Result Calculation ... 9
12 Detection Limit, Precision and Accuracy ... 9
13 Test Report ... 10
Appendix A (normative) Types and Determination Parameters of Chlorinated Phenols
... 11
Appendix B (informative) Schematic Diagram of Total Ion Chromatogram of
Chlorinated Phenols Standard Substance ... 12
Determination of the Content of Chlorinated Phenols in Dye
Products
WARNING: personnel using this document shall have practical experience in formal
laboratory work. This document does not identify all possible safety issues. Users are
responsible for taking appropriate safety and health measures and ensuring compliance
with the conditions specified in relevant national regulations.
1 Scope
This document specifies the method for the determination of 19 chlorinated phenols residues in
dye products using gas chromatography-mass spectrometry (GC/MS).
This document is applicable to the determination of chlorinated phenols in various categories
of dye products.
NOTE: see Appendix A for the types of chlorinated phenols and reference parameters for
determination.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in the text. In terms of references with a specified date, only
versions with a specified date are applicable to this document. In terms of references without a
specified date, the latest version (including all the modifications) is applicable to this document.
GB/T 6682-2008 Water for Analytical Laboratory Use - Specification and Test Methods
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 have terms or definitions that need to be defined.
4 Method Principle
In an ultrasonic bath, use potassium carbonate solution to extract the chlorinated phenols in the
specimen, which is acetylated with acetic anhydride to generate chlorinated phenols acetate.
Though liquid-liquid extraction, extract the chlorinated phenols acetate into n-hexane, then,
adopt the gas chromatograph-mass spectrometer (GC/MS) for analysis and qualitative
determination. Adopt the peak area internal standard method for quantitative determination.
5 Reagents or Materials
5.1 Unless otherwise specified, only reagents confirmed to be analytically pure and Grade-3
water specified in GB/T 6682-2008 are used.
5.2 The types of chlorinated phenols in the standard substance and the determination parameters
shall comply with the stipulations of Appendix A.
5.3 n-Hexane, chromatographically pure.
5.4 Methanol, chromatographically pure.
5.5 Anhydrous potassium carbonate.
5.6 Acetic anhydride.
5.7 Triethylamine.
5.8 Anhydrous sodium sulfate: at 650 C, dry it for 4 hours, take out and place in a desiccator
for later use.
5.9 Potassium carbonate solution: 0.1 mol/L aqueous solution, weigh-take 13.8 g of anhydrous
potassium carbonate, dissolve it in water, and reach a constant volume of 1,000 mL.
6 Instruments and Equipment
6.1 Gas chromatograph-mass spectrometer (GC/MS): equipped with EI source.
6.2 Chromatographic column: 50% phenyl methyl polysiloxane stationary phase, for example,
DB-17MS, 30 m 0.25 mm 0.25 m or equivalent.
6.3 Analytical balance: with an accuracy of 0.01 mg.
6.4 Ultrasonic generator.
6.5 Extractor: tube with a stopper, 10 mL.
6.6 Centrifuge: 4,000 r/min.
6.7 Separating funnel: 150 mL.
6.8 Separating funnel oscillator: with an oscillation frequency above 200 times/min.
7 Preparation of Standard Solutions
7.1 Chlorinated Phenols Single Standard Stock Solution
Respectively weigh-take 10 mg of the standard substance listed in Appendix A, accurate to 0.01
mg. Use methanol to dissolve it and reach a constant volume in a 100 mL volumetric flask.
Prepare it into a single standard stock solution of 100 mg/L chlorinated phenols. The single
standard stock solution shall be stored in a sealed and refrigerated place and in the dark below
4 C. The shelf life is 1 month. Alternatively, certified standard solutions can be directly
purchased, either single-component chlorinated phenols standard solution or chlorinated
phenols mixed standard solution.
7.2 Chlorinated Phenols Mixed Standard Working Solution
Respectively draw 1.0 mL of the chlorinated phenols single standard stock solution (see 7.1)
into a 10 mL volumetric flask, use methanol to dilute to the scale and prepare it into a mixed
standard working solution of 10 mg/L chlorinated phenols.
7.3 Tetrachloroguaiacol (TCG) Internal Standard Stock Solution
Weigh-take 10 mg of the internal standard substance tetrachloroguaiacol (TCG), accurate to
0.01 mg. Use methanol to dissolve it and reach a constant volume in a 100 mL volumetric flask.
Prepare it into an internal standard stock solution of 100 mg/L tetrachloroguaiacol (TCG). The
standard stock solution shall be stored in a sealed and refrigerated place and in the dark below
4 C. The shelf life is 1 month. Alternatively, certified standard solutions can be directly
purchased.
7.4 Tetrachloroguaiacol (TCG) Internal Standard Working Solution
Draw 1.0 mL of the tetrachloroguaiacol (TCG) internal standard stock solution (see 7.3) into a
10 mL volumetric flask, use methanol to dilute it to the scale, and prepare it into an internal
standard working solution of 10 mg/L tetrachloroguaiacol (TCG).
8 Preparation of Sample Solution
8.1 Extraction
Weigh-take 1.0 g of specimen, accurate to 0.0001 g, place it in a 150 mL stoppered conical
flask. Add 20 mL of potassium carbonate solution, thoroughly shake and mix it, and use an
ultrasonic generator to perform ultrasonic extraction for 10 minutes to obtain the extracting
solution.
8.2 Acetylation
Transfer the extracting solution to a 150 mL separating funnel, use a small amount of potassium
carbonate solution to clean the conical flask, and transfer all the washing liquid to the separating
solution (Chapter 8) and standard working solution (Chapter 9). Through retention time and
characteristic ions (see Appendix A), conduct qualitative determination on the target compound,
and use the peak area internal standard method for quantitative determination. In accordance
with this step, analyze and determine the blank specimen. See Appendix B for the
chromatographic diagram.
11 Result Calculation
The content of various chlorinated phenols in the specimen, expressed in wi, is calculated in
accordance with Formula (1):
Where,
wi---the content of the target substance in the specimen, expressed in (mg/kg);
ri---the ratio of peak area response values of chlorinated phenols in the sample solution and the
internal standard substance;
ms---the mass value of the standard sample in the mixed standard solution, expressed in (g);
rs---the ratio of peak area response values of chlorinated phenols in the mixed standard solution
and the internal standard substance;
m---the mass of the specimen, expressed in (g).
The calculation results shall retain two decimal places.
The calculation results shall be rounded-off in accordance with the stipulations of GB/T 8170-
2008.
12 Detection Limit, Precision and Accuracy
12.1 Detection Limit
The detection limit of 19 chlorinated phenols is 0.05 mg/kg.
12.2 Precision
The absolute difference between two independent determination results obtained through
mutually independent determinations carried out in the same laboratory, by the same operator
using the same equipment and the same determination method on the same object within a short
period of time is not greater than 20% of the arithmetic mean of the two determinations.
12.3 Accuracy
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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