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This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 22808-2008 Leather and fur - Chemical tests - Determination of pentachlorophenol content, and the following main technical changes have been made with respect to GB/T 22808-2008:
——The range of chlorinated phenols applicable is expanded (see Clause 1 of this standard; Clause 1 of Edition 2008);
——The clause “3 Abbreviations” is added (see Clause 3);
——The requirement for test water is added; the pentachlorophenol acetate standard stock solution and standard solution are deleted (see 5.1 of this standard; 4.1.2 and 4.1.3 of Edition 2008);
——"Pentachlorophenol standard solution” is revised to "mixed standard solution of chlorinated phenols (CPs)", and test procedures are modified accordingly (see 5.2 of this standard; 4.1.1 of Edition 2008);
——The requirements for shaking frequency of shakers are added (see 6.4);
——The requirements for specimen size are added (see 7.2);
——The requirements for the shaking frequency during extraction are modified (see 8.2 of this standard; 7.2.2 of Edition 2008);
——Calculation formulae are modified (see Clause 9 of this standard; 8.1 of Edition 2008);
——The annex "CAS No. of chlorinated phenols” is added (see Annex C);
——The conditions for chromatographic analysis are moved to Annex D, and the GC-MSD analysis conditions are add (see Annex D of this standard; 7.4 of Edition 2008).
This standard has been redrafted and modified in relation to ISO 17070:2015 Leather - Chemical tests - Determination of tetrachlorophenol-, trichlorophenol-, dichlorophenol-, monochlorophenol-isomers and pentachlorophenol content.
This standard is changed largely from ISO 17070:2015 in terms of structure; the comparison between this standard and ISO 17070:2015 in clause/subclause number is listed in Annex A.
Technical differences have been made in this standard with respect to ISO 17070:2015, and relevant technical differences and their causes have been listed in Annex B.
The following editorial changes are made in this standard:
——The standard name is revised to Leather and fur - Chemical tests - Determination of chlorinated phenols content;
——The footnote to CAS No. is deleted (see footnote 1 of ISO 17070:2015);
——Descriptions of letter symbols in Formula (2) is added (see Clause 9);
——The number of formula related to the factor for conversion D is added (see Clause 9);
——The description in 10 b) is modified (see Clause 10).
This standard was proposed by China National Light Industry Council.
This Standard is under the jurisdiction of the National Technical Committee 252 on Leather of Standardization Administration of China (SAC/TC 252).
The previous edition of this standard is as follows:
——GB/T 22808-2008.
Leather and fur - Chemical tests - Determination of chlorinated phenols content
1 Scope
This standard specifies a method for determining the content of chlorinated phenols (including tetrachlorophenol-, trichlorophenol-, dichlorophenol-, monochlorophenol-isomers, and pentachlorophenol), their salts, and esters in leather and fur.
This standard is applicable to the determination of chlorinated phenols in various types of leather and fur. Bromophenol isomers can also be determined using this method.
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 6682 Water for analytical laboratory use - Specification and test methods (GB/T 6682-2008, ISO 3696:1987, MOD)
GB/T 39364 Leather - Chemical, physical, mechanical and fastness tests - Sampling location (GB/T 39364-2020, ISO 2418:2017, MOD)
QB/T 1267 Fur - Chemical, physical and mechanical and fastness tests - Sampling location (QB/T 1267-2012, ISO 2418:2002, MOD)
QB/T 1272 Fur - Preparation of chemical test samples (QB/T 1272-2012, ISO 4044:2008, MOD)
QB/T 1273 Fur - Chemical tests - Determination of volatile matter (QB/T 1273-2012, ISO 4684-1:2005, MOD)
QB/T 2716 Leather - Preparation of chemical test samples (QB/T 2716-2018, ISO 4044:2008, MOD)
QB/T 2717 Leather - Chemical tests - Determination of volatile matter (QB/T 2717-2018, ISO 4684:2005, MOD)
3 Abbreviations
For the purposes of this document, the following abbreviations apply.
CP chlorinated phenols
DiCP dichlorophenol
MoCP monochlorophenol
PCP pentachlorophenol
TCG tetrachloro-o-methoxyphenol
TeCP tetrachlorophenol
TriCP trichlorophenol
4 Principle
First of all, the specimen is submitted to steam-distillation. After extraction into n-hexane, the chlorinated phenols (CPs) are acetylated by acetic anhydride and the chlorinated phenyl acetates are analysed by gas-chromatography (GC) with an electron capture detector (ECD) or mass selective detector (MSD). Quantification is performed with external standard method and a correction made with internal standard method.
5 Reagents and materials
5.1 General requirements: Unless otherwise specified, analytical grade chemicals shall be used. Test water shall be distilled or deionized, Grade 3 in accordance with GB/T 6682.
5.2 A mixed standard solution of the chlorinated phenols (CPs) which contains the following isomers at a concentration of 100 μg/mL in acetone (5.10).
Note 1: See Annex C for the CAS No. of CPs.
Note 2: Commercial mixed standard solution of chlorinated phenols (CPs) may be used.
5.3 Standard solution of Tetrachloroguaiacol (TCG, CAS No.: 2539-17-5) (tetrachloro-o-methoxyphenol), at a concentration of 100 μg/mL in acetone (internal standard), melting point 118 ℃ to 119 ℃.
5.4 Sulfuric acid solution, 1 mol/L.
5.5 n-hexane.
5.6 Potassium carbonate, K2CO3.
5.7 Acetic anhydride, C4H6O3.
5.8 Anhydrous sodium sulfate.
5.9 Triethyiamine.
5.10 Acetone.
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6 Apparatus
6.1 Gas chromatography (GC), with ECD or MSD detector.
6.2 Analytical balance, weighing to an accuracy of 0.0001 g.
6.3 Steam distillation apparatus.
6.4 Shaker, capable of at least 200 cycles per minute.
6.5 Volumetric flasks, 50 mL and 500 mL.
6.6 Conical flasks, 100 mL and 500 mL.
6.7 Separating funnel, 250 mL, or suitable vessel that allows separation of organic and aqueous phases, that can be sealed for vigorous shaking.
6.8 Pasteur-pipettes, graduated pipettes, or suitable auto-pipettes.
6.9 Strainer with paper filter, diameter 125 mm.
Foreword i
1 Scope
2 Normative references
3 Abbreviations
4 Principle
5 Reagents and materials
6 Apparatus
7 Sampling and preparation of specimens
8 Test procedures
9 Expression of results
10 Test report
Annex A (Informative) Structural changes of this standard with respect to ISO 17070:
Annex B (Informative) Technical differences between this standard and ISO 17070:2015 and their causes
Annex C (Informative) CAS No. of chlorinated phenols (CPs)
Annex D (Informative) Chromatographic analyses
Annex E (Informative) Reliability of the method
