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GB/T 24166-2009 English PDF (GBT24166-2009)

GB/T 24166-2009 English PDF (GBT24166-2009)

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GB/T 24166-2009: Determination of the content of chlorinated phenols in dye products

This Standard specifies the method for the determination of chlorinated phenols (2,3,5,6-tetrachlorophenol and pentachlorophenol) in dye products. This Standard applies to the determination of chlorinated phenols (2,3,5,6-tetrachlorophenol and pentachlorophenol) using gas chromatography-mass selective detector (GC-MSD) and gas chromatography-electron capture detector (GC-ECD) for commercial dyes, dye products, dye intermediates and textile printing and dyeing additives.
GB/T 24166-2009
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.100.01; 87.060.10
G 55
Determination of the content of chlorinated phenols in
dye products
ISSUED ON: JUNE 25, 2009
IMPLEMENTED ON: APRIL 01, 2010
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle ... 5
4 Test method ... 5
5 Lower limit, recovery and precision of determination ... 9
6 Test report ... 10
Annex A (normative) Types of chlorinated phenols ... 11
Annex B (informative) Diagrams of chlorinated phenol acetate standards ... 12 Determination of the content of chlorinated phenols in
dye products
Warning -- Personnel using this Standard shall have practical experience in regular laboratory work. This Standard does not point out all possible safety issues. Users are responsible for taking appropriate safety and
health measures and ensuring compliance with conditions specified in
relevant national regulations.
1 Scope
This Standard specifies the method for the determination of chlorinated phenols (2,3,5,6-tetrachlorophenol and pentachlorophenol) in dye products.
This Standard applies to the determination of chlorinated phenols (2,3,5,6- tetrachlorophenol and pentachlorophenol) using gas chromatography-mass
selective detector (GC-MSD) and gas chromatography-electron capture
detector (GC-ECD) for commercial dyes, dye products, dye intermediates and textile printing and dyeing additives.
2 Normative references
The following documents contain the provisions which, through reference in this Standard, become the provisions of this Standard. For dated references, their subsequent amendments (excluding corrigendum) or revisions do not apply to this Standard. However, the parties who enter into agreement based on this Standard are encouraged to investigate whether the latest versions of these documents are applicable. For undated reference documents, the latest
versions apply to this Standard.
GB/T 6682-2008 Water for analytical laboratory use - Specification and test methods (ISO 3696:1987, MOD)
GB/T 8170-2008 Rules of rounding off for numerical values and expression and judgement of limiting values
3 Principle
Chlorinated phenols are extracted from the sample with potassium carbonate solution. The extract is acetylated with acetic anhydride, and the chlorophenol acetate is extracted with n-hexane. Then the extract is determined using gas chromatography-mass selective detector (GC-MSD) and gas chromatography- electron capture detector (GC-ECD), and quantified by external standard method.
4 Test method
4.1 General
Unless otherwise specified, use only reagents identified as analytically pure and tertiary water as specified in GB/T 6682-2008. The determination of test results shall be carried out in accordance with 4.3.3 round-off comparison method in GB/T 8170-2008.
4.2 Reagents and solutions
a) anhydrous potassium carbonate;
b) acetic anhydride;
c) n-hexane;
d) anhydrous sodium sulfate: dried at 650 ??C for 4 h, and then taken out and placed in a desiccator for use;
e) potassium carbonate solution: 0.1 mol/L aqueous solution; WEIGH 13.8 g of anhydrous potassium carbonate and dissolve in water, and DILUTE to
1000 mL;
f) sodium sulfate solution: 20 g/L;
g) chlorinated phenols standards in Annex A: with content (mass fraction) ??? 99 %.
4.3 Preparation of chlorinated phenols standard solutions
4.3.1 Single stock standard solution
WEIGH 0.01 g (accurate to 0.0001 g) of chlorinated phenols standards listed in Annex A, DISSOLVE with potassium carbonate solution, and DILUTE to
constant volume in a 25 mL volumetric flask, to prepare a single stock standard solution;
??i - the value equivalent to the concentration of chlorinated phenols i in the standard solution, in micrograms per milliliter (??g/mL);
V - the value of the final constant volume of the sample solution, in milliliters (mL);
Ais - the peak area value of the chlorinated phenols i target ion in the standard solution;
m - the value of sample mass, in grams (g).
The calculation result is expressed to two decimal places.
4.5.5.2 Gas chromatography
The content of chlorinated phenols in the sample is calculated as mass fraction wi, and the value is in (mg/kg). It is calculated according to formula (2): where:
hi - the peak height value of chlorophenol acetate i in the sample solution; ??i - the value equivalent to the concentration of chlorinated phenols i in the standard solution, in micrograms per milliliter (??g/mL);
V - the value of the final constant volume of the sample solution, in milliliters (mL);
his - the peak height value of chlorophenol acetate i in the standard solution; m - the value of sample mass, in grams (g).
The calculation result is expressed to two decimal places.
5 Lower limit, recovery and precision of determination
5.1 Lower limit of determination
In this method, the lower limit of determination by gas chromatography-mass spectrometry is 0.1 mg/kg, and the lower limit of determination by gas
chromatography is 0.01 mg/kg.

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