GB/T 23972-2009 PDF English
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GB/T 23972-2009: Determination of alkylphenols and alkylphenol polyethoxylates in textile dyeing and finishing auxiliaries - LC/MS method
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NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.100.40 G 70 Determination of alkylphenols and alkylphenol polyethoxylates in textile dyeing and finishing auxiliaries - LC/MS method Issued on. JUNE 02, 2009 Implemented on. FEBRUARY 01, 2010 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Terms and definitions... 4 4 Determination methods... 5 5 Low detection limit, recovery and precision... 9 6 Test report... 9 Appendix A (Normative) CAS RN of common octylphenol, nonylphenol, octylphenol polyethoxylate and nonylphenol polyethoxylate... 10 Appendix B (Informative) Schematic diagrams... 11Foreword
Appendix A of this Standard is a normative appendix; Appendix B is an informative appendix. This Standard was proposed by China Petroleum and Chemical Industry Federation. This Standard shall be under the jurisdiction of National Technical Committee 134 on Dyestuff of Standardization Administration of China (SAC/TC 134). The drafting organizations of this Standard. Shenyang Research Institute of Chemical Industry, Zhejiang Transfar Co., Ltd., Intertek Testing Services Shanghai Limited. The drafters of this Standard. Pu Aijun, Lu Linguang, Ji Lanqin, Lv Tiehai, Zhao Ting, Shen Rijiong, Chen Ru, Zhao Mei, Ji Hao, Wang Jianping. Determination of alkylphenols and alkylphenol polyethoxylates in textile dyeing and finishing auxiliaries - LC/MS method1 Scope
This Standard specifies the determination methods of alkylphenols and alkylphenol polyethoxylates in textile dyeing and finishing auxiliaries. This Standard applies to the determination of contents of alkylphenols and alkylphenol polyethoxylates in textile dyeing and finishing auxiliaries by LC/MS method.2 Normative references
The terms in the following documents become the terms of this Standard by reference to this Standard. For dated references, all subsequent amendments (not including errata content) or revisions do not apply to this standard. However, parties to agreements that are based on this Standard are encouraged to study whether the latest versions of these documents can be used. For undated references, the latest edition applies to this Standard. GB/T 6682-2008, Water for analytical laboratory use - Specification and test methods (ISO 3696.1987, MOD)3 Terms and definitions
The following terms and definitions are applicable to this Standard. 3.1 Alkylphenols, AP for short The molecular structure of alkylphenols is. R-C6H4-OH. The substances that are commonly used in this category are octylphenol (C8H17-C6H4-OH, OP for short) and nonylphenol (C9H19-C6H4-OH, NP for short).4 Determination methods
4.1 General provisions Unless otherwise specified, use only reagents that are identified as analytical reagents, and grade-3 water that is specified in GB/T 6682-2008.The determination of the test results shall be made according to the rounding comparison method of 4.3.3 in GB/T 8170-2008. 4.2 Method summary For the sample, use methanol as a solvent; use the ultrasonic vibration method to dissolve the alkylphenols and alkylphenol polyethoxylates in the textile dyeing and finishing auxiliaries; filter through a filter membrane; then, use the LC/MS method to select multiple fragment ions from the characteristic ions; 4.3 Instruments and apparatuses a) HPLC-MS. 4.4 Reagents and solutions 4.5 Determination conditions 4.6 Solution preparation 4.6.1 Preparation of standard solutions Accurately weigh appropriate amounts of OP, NP, OPEO, and NPEO standards; use methanol to respectively prepare standard stock solutions whose concentration is 1 mg/mL. 4.7 Determination steps Turn on the liquid chromatography-mass spectrometer to warm up; after the instrument runs stably, first perform a full-scan analysis of the sample; then, compare it with the retention time of the standard sample and the mass spectrum for determination; select a standard test solution of similar concentration; use the selected ions that are specified in Table 2 for measurement. Inject the sample through the autosampler. After the last component had flowed out, use the data processor to process the result. 4.8 Result calculation The content of alkylphenols or alkylphenol polyethoxylates in textile dyeing and finishing auxiliary products is calculated in mass fraction wi; the value is expressed in (mg/kg); it is calculated according to Formula (1).5 Low detection limit, recovery and precision
5.1 Low detection limit The lower detection limits of this method for octylphenol, nonylphenol, octylphenol polyethoxylate and nonylphenol polyethoxylate in the sample are 25 mg/kg, 25 mg/kg, 10 mg/kg, 10 mg/kg. 5.3 Precision The absolute difference between two independent test results, that are gained in the same laboratory, by the same operator, with the same equipment, by the same test method, of which the same test object is tested independently of each other in a short time, is not greater than 20% of the arithmetic mean of the two determination values.6 Test report
The test report shall at least provide the following contents. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
