GB/T 23322-2018 PDF English
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GB/T 23322: Historical versions
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| GB/T 23322-2018 | 435 | Add to Cart | Auto, 9 seconds. | Textiles - Determination of surfactant - Alkylphenols and Alkylphenol ethoxylates | Valid |
| GB/T 23322-2009 | 559 | Add to Cart | 4 days | Textiles -- Determination of surfactant -- Alkylphenol ethoxylates | Obsolete |
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GB/T 23322-2018: Textiles - Determination of surfactant - Alkylphenols and Alkylphenol ethoxylates
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NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 59.080.01 W 04 Replacing GB/T 23322-2009 Textiles - Determination of surfactant - Alkylphenols and alkylphenol ethoxylates Issued on. DECEMBER 28, 2018 Implemented on. JULY 01, 2019 Issued by. State Administration for Market Regulation; Standardization Administration of PRC.
Table of Contents
Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Principles... 4 4 Reagents or materials... 5 5 Instruments and equipment... 6 6 Measurement steps... 6 7 Calculation and presentation of results... 9 8 Lower limit of determination, recovery, precision of the method... 12 9 Test report... 12 Appendix A (Informative) Determination method of alkylphenol and alkylphenol ethoxylates by reversed-phase high performance liquid chromatography... 13 Appendix B (Informative) Determination method of alkylphenol and alkylphenol ethoxylates by normal phase high performance liquid chromatography... 17 Appendix C (Informative) Hydrophilic interaction chromatography (HILIC) determination of alkylphenol and alkylphenol ethoxylates... 23 Appendix D (Informative) Selected ion monitoring chromatograms for the determination of AP and APEO by LC-MS... 29 Appendix E (Informative) MS reference conditions... 311 Scope
This standard specifies the liquid chromatography-mass spectrometry detection method of alkylphenol (AP) and alkylphenol ethoxylates (APnEO, n = 2 ~ 16), in textiles. This standard applies to all types of textile products. Note 1.The general molecular structure of AP is. R-C6H4-OH. AP in this standard refers to the common octylphenol [OP, C8H17-C6H4-OH] and nonylphenol [NP, C9H19-C6H4-OH]. The general molecular structure of APnEO is. R-C6H4-(OC2H4)nOH. APnEO in this standard refers to the commonly used octylphenol ethoxylates [OPnEO, C8H17-C6H4-(OC2H4)nOH] and nonylphenol ethoxylates [NPnEO, C9H19-C6H4-(OC2H4)nOH]. Note 2.For the determination method of reversed-phase high-performance liquid chromatography, normal-phase high-performance liquid chromatography, hydrophilic interaction chromatography, of the alkylphenol and alkylphenol ethoxylate, refer to Appendix A, Appendix B, Appendix C, respectively.2 Normative references
The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) is applicable to this standard. GB/T 6682 Water for analytical laboratory use - Specification and test methods3 Principles
The AP and APnEO in the specimen are extracted by methanol ultrasonically. After the extract is concentrated and purified, it was determined by liquid chromatography-mass spectrometer, quantified by external standard method.4 Reagents or materials
4.1 Unless otherwise specified, the reagents used in this method are all analytically pure; the water is the grade-1 water, which is specified in GB/T 6682. 4.2 Methanol (HPLC grade). 4.3 Acetonitrile (HPLC grade). 4.4 n-hexane (HPLC grade). 4.5 Isopropanol (HPLC grade). 4.6 Dichloromethane (HPLC grade). 4.7 Methanol-aqueous solution (3 + 2). Accurately take 300 mL of methanol (4.2) and 200 mL of water. Mix well. Prepare for later use. 4.8 Methanol-dichloromethane solution (1 + 4). Accurately take 100 mL of methanol (4.2) and 400 mL of dichloromethane (4.6). Mix well. Prepare for later use. 4.9 Standard octylphenol (OP, CAS No.140-66-9, purity ≥ 97%). 4.10 Nonylphenol standard (NP, CAS No.25154-52-3, excellent grade pure). 4.15 Solid phase extraction column. The filler is lipophilic divinylbenzene and hydrophilic N-vinylpyrrolidone copolymer, 60 mg, 3 mL. Use 2 mL of methanol and 4 mL of water, to activate it in sequence, before use. 4.16 Organic filter membrane. 0.22 μm.5 Instruments and equipment
5.1 Liquid chromatography-mass spectrometer. Equipped with an electrospray ionization source (ESI). 5.2 Analytical balance. Sensitivity is 0.0001 g. 5.3 Analytical balance. Sensitivity is 0.01 g. 5.4 Ultrasonic cleaner. The temperature can be controlled at (70 ± 2) °C.6 Measurement steps
6.1 Extraction and purification of specimens Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well. Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube. Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min. 6.2 Determination 6.2.1 Reference chromatographic and mass spectrometry conditions for liquid chromatography-mass spectrometry (LC-MS) Since the test results depend on the instrument used, it is impossible to give general parameters for chromatographic analysis. The following parameters have been shown to be suitable for testing. 6.2.2 Reference chromatographic and mass spectrometry conditions for liquid chromatography-tandem mass spectrometry (LC-MS/MS) Since the test results depend on the instrument used, it is impossible to give general parameters for chromatographic analysis. The following parameters have been shown to be suitable for testing. 6.2.4 Quantitative determination Under the best working conditions of the instrument, determine the standard working solution. Take the concentration of the analyte as the abscissa AND the peak area of the analyte as the ordinate, to draw the standard working curve. Use the standard working curve, to make quantitative determination of the sample to be tested, according to the external standard method. The response value of the analyte, in the sample solution, shall be within the linear range, which is determined by the instrument. 6.3 Blank test Follow all of the above steps, except that no specimen is added.7 Calculation and presentation of results
7.1 Calculation formula of LC-MS method Calculate the content of alkylphenols and alkylphenol ethoxylates in the specimen, according to formula (1). 7.2 Calculation formula of LC-MS/MS method 7.2.1 Calculation of APnEO concentration with degree of polymerization n in standard working solution Calculate the mass fraction of each component, in APnEO, according to formula (2). 7.2.2 Calculation of AP and APnEO content Calculate the content of AP in the specimen, according to formula (4).8 Lower limit of determination, recovery, precision of the method
8.1 Lower limit of determination The lower limit of determination of octylphenol, nonylphenol, octylphenol ethoxylates, nonylphenol ethoxylates, in specimen, by LC-MS method, are 0.25 mg/kg, 0.5 mg/kg, 0.5 mg/kg, 0.5 mg/kg, respectively. 8.2 Recovery rate The range of recovery rate of the method is 80% ~ 110%. 8.3 Precision In the same laboratory, when the same operator uses the same equipment and the same test method, to independently test the same tested object, in a short period of time, the absolute difference, between the two independent test results, is not greater than 10% of the arithmetic mean of the two measured values.9 Test report
The test report shall at least give the following.Appendix A
(Informative) Determination method of alkylphenol and alkylphenol ethoxylates by reversed- phase high performance liquid chromatography A.1 Overview This Appendix gives the method for the determination of alkylphenol (AP) and alkylphenol ethoxylates (APnEO, n = 2 ~ 16) in textiles, by reversed-phase high performance liquid chromatography. A.2 Principle The AP and APnEO in the specimen are extracted ultrasonically by methanol. After the extract is concentrated and purified, it is determined by a high performance liquid chromatograph, which is equipped with a fluorescence detector; then quantified by the external standard method. A.3 Reagents or materials Same as Chapter 4. A.4 Instruments and equipment A.4.1 High performance liquid chromatograph, which is equipped with fluorescence detector. A.4.2 Analytical balance. The sensitivity is 0.0001 g. A.4.3 Analytical balance. The sensitivity is 0.01 g. A.4.4 Ultrasonic cleaner. The controllable temperature is (70 ± 2) °C. A.4.5 Rotary evaporator. A.4.6 Solid phase extraction device. A.4.7 Nitrogen blower. A.5 Determination steps A.5.2 Determination A.5.2.1 Reference chromatographic conditions Since the test results depend on the instrument used, it is impossible to give general parameters for chromatographic analysis. The following parameters have been shown to be suitable for testing. A.5.2.2 Chromatographic determination According to the content of AP and APnEO in the sample solution, select the standard working solution, which has similar concentration (4.14). Equal volumes of standard working solution and sample solution are injected alternatively, for determination. The response values of AP and APnEO, in the standard working solution and sample solution, shall be within the linear range, which is detected by the instrument. Under the above chromatographic conditions, the retention time of AP and APnEO is as shown in Table A.1; the liquid chromatogram is as shown in Figure A.1.When the retention time of the chromatographic peak of the sample solution is consistent with that of the standard working solution, LC-MS/MS method can be used, for further analysis and confirmation. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
