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This document is drafted 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 standard replaces GB/T 24166-2009 Determination of the content of chlorinated phenols in dye products. In addition to structural adjustment and editorial changes, the following main technical changes have been made with respect to GB/T 24166-2009:
——The scope of this 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 quantitative method 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 10.1 hereof; 4.5.4.1 of Edition 2009);
——The detection limit of the method is modified (see 12.1 hereof; 5.1 of Edition 2009);
——The requirements for accuracy determination of the method are modified (see 12.3 hereof; 5.2 of Edition 2009);
——The types of chlorinated phenol target are added (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 on Dyestuff of Standardization Administration of China (SAC/TC 134).
The previous editions of this document are as follows:
This document was firstly issued in 2009, and this edition is the first revision.
Determination of the content of chlorinated phenols in dye products
WARNING——Persons using this document shall be familiar with normal laboratory practice. This document does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of users of this standard to take appropriate measures to ensure the safety and health of personnel, and fulfill statutory and regulatory requirements for this purpose.
1 Scope
This document specifies the method for determination of 19 kinds of chlorinated phenol residues in dye products by gas chromatography-mass spectrometry (GC/MS).
This document is applicable to determination of chlorinated phenols in various dye products.
Note: The types of chlorinated phenols and the reference parameters for their determination are given in Annex A.
2 Normative references
The following documents contain provisions which, through reference in this text, constitute provisions 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 6682-2008 Water for analytical laboratory use—Specification and test methods
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
Chlorinated phenols in the specimen are extracted with potassium carbonate solution in ultrasonic bath, then acetylated with acetic anhydride to produce chlorophenol acetate, which is extracted into hexane by liquid-liquid extraction, and then analyzed and qualitatively by gas chromatography-mass spectrometry (GC/MS), and quantified by peak area internal standard method.
5 Reagents or materials
5.1 Unless otherwise specified, only recognized analytical reagent and Grade 3 water (specified in GB/T 6682-2008) shall be used.
5.2 The types of chlorinated phenols in the standard product and the parameters for their determination are given in Annex A.
5.3 N-hexane: Chromatographically pure.
5.4 Methanol: Chromatographic grade.
5.5 Anhydrous potassium carbonate.
5.6 Acetic anhydride.
5.7 Triethyiamine.
5.8 Anhydrous sodium sulfate: dry at 650°C for 4h, remove and put it in the dryer for further use.
5.9 Potassium carbonate solution: 0.1 mol/L aqueous solution, weigh 13.8g of anhydrous potassium carbonate, dissolve in water, dilute it to the scale to 1,000 mL.
Foreword i
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 Preparation of standard working solutions
10 Test procedures
11 Result calculation
12 Detection limit, precision and accuracy
13 Test report
Annex A (Normative) Types of chlorinated phenols and the parameters for determination
Annex B (Informative) Total ion chromatogram of standard chlorinated phenol substance
