GB/T 23322-2018 PDF English
US$435.00 · In stock · Download in 9 secondsGB/T 23322-2018: Textiles - Determination of surfactant - Alkylphenols and Alkylphenol ethoxylates Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB/T 23322: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 23322-2018 | English | 435 |
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Textiles - Determination of surfactant - Alkylphenols and Alkylphenol ethoxylates
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| GB/T 23322-2009 | English | 559 |
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Textiles -- Determination of surfactant -- Alkylphenol ethoxylates
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GB/T 23322-2018: Textiles - Determination of surfactant - Alkylphenols and Alkylphenol ethoxylates
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT23322-2018
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... 31
1 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 methods
3 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.
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