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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 23322-2009 Textiles—Determination of surfactant—Alkylphenol ethoxylates, and the following main technical changes have been made with respect to GB/T 23322-2009:
——the standard is renamed as "Textiles—Determination of surfactant—Alkylphenols and alkylphenol ethoxylates";
——the CAS Nos of standard substances are added (see 4.9, 4.10, 4.11 and 4.12);
——the analytical method of alkylphenol is added;
——the liquid chromatography-mass spectrometry (LC-MS) method is added;
——the method for calculation and expression of results is modified;
——the hydrophilic interaction liquid chromatography (HILIC) method is added in the annex;
——the reversed phase high-performance liquid chromatography (RP-HPLC) method and normal phase high-performance liquid chromatography (NP-HPLC) method are moved from the text to Annex A and Annex B.
This standard was proposed by China National Textile and Apparel Council.
This standard is under the jurisdiction of the National Technical Committee on Textiles of Standardization Administration of China (SAC/TC 209).
The previous edition of this standard is as follows:
——GB/T 23322-2009.
Textiles—Determination of surfactant—
Alkylphenols and alkylphenol ethoxylates
Warning: Persons using this standard shall be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies the detection of alkylphenol (AP) and alkylphenol ethoxylates (APnEO, n = 2–16) in textiles by liquid chromatography-mass spectrometry (LC-MS) method.
This standard is applicable to various textiles.
Note 1: The general molecular structural formula of AP is R—C6H4—OH. In this standard, AP refers to common octylphenol [OP, C8H17—C6H4—OH] and nonylphenol [NP, C9H19—C6H4—OH]. The general molecular structural formula of APnEO is R—C6H4—(OC2H4)nOH. In this standard, APnEO refers to common octylphenol ethoxylates [OPnEO, C8H17—C6H4—(OC2H4)nOH] and nonylphenol ethoxylates [NPnEO, C9H19—C6H4—(OC2H4)nOH].
Note 2: See Annex A, Annex B and Annex C for the determination of AP and APnEO by reversed phase high-performance liquid chromatography (RP-HPLC) method, normal phase high-performance liquid chromatography (NP-HPLC) method and hydrophilic interaction liquid chromatography (HILIC) method, respectively.
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
3 Principle
Perform ultrasonic extraction of AP and APnEO from samples using methanol, carry out determination of the extracts using liquid chromatography-mass spectrometer after concentration and purification, and quantify the extracts by external standard method.
4 Reagents or materials
4.1 Unless otherwise specified, all reagents used in this method are analytically pure, and the water is Grade I water as specified in GB/T 6682.
4.2 Methanol (Grade HPLC).
4.3 Acetonitrile (Grade HPLC).
4.4 n-hexane (Grade HPLC).
4.5 Isopropanol (Grade HPLC).
4.6 Dichloromethane (Grade HPLC).
4.7 Methanol-water solution (3+2): accurately measure 300 mL of methanol (4.2) and 200 mL of water, and mix them evenly for later use.
4.8 Methanol-dichloromethane solution (1+4): accurately measure 100 mL of methanol (4.2) and 400 mL of dichloromethane (4.6), and mix them evenly for later use.
4.9 Octylphenol standard (OP, CAS No. 140-66-9, purity ≥ 97%).
4.10 Nonylphenol standard (NP, CAS No. 25154-52-3, guaranteed reagent).
4.11 Octylphenol ethoxylates standard (OPnEO, CAS No. 9002-93-1, average degree of polymerization n = 9, guaranteed reagent).
4.12 Nonylphenol ethoxylates standard (NPnEO, CAS No. 9016-45-9, average degree of polymerization n = 9, purity ≥ 99%).
4.13 Standard stock solution: accurately weigh an appropriate amount of OP (4.9), NP (4.10), OPnEP (4.11) and NPnEO (4.12) respectively, and prepare single-component standard stock solutions with a concentration of 10 mg/mL with methanol.
4.14 Standard working solution: take appropriate amount of OP, NP, OPnEO and NPnEO standard stock solutions (4.13) respectively, put them in the same volumetric flask, and dilute them with methanol to prepare a mixed standard working solution with the required concentration.
4.15 Solid phase extraction column: filled with lipophilic divinylbenzene and hydrophilic N-vinylpyrrolidone copolymer, 60 mg, 3 mL, which is activated with 2 mL of methanol and 4 mL of water in turn before use.
4.16 Organic filter membrane: 0.22 μm.
5 Apparatus
5.1 Liquid chromatography-mass spectrometer, equipped with electrospray ion source (ESI).
5.2 Analytical balance, with a sensitivity of 0.0001 g.
5.3 Analytical balance, with a sensitivity of 0.01 g.
5.4 Ultrasonic cleaner, with temperature controllable at (70±2)°C.
5.5 Rotary evaporator.
5.6 Solid phase extraction unit.
5.7 Nitrogen blowing instrument.
6 Determination procedures
6.1 Extraction and purification of sample
Take representative samples, cut them into pieces about 5 mm×5 mm, and mix them evenly. Weigh 1 g of the cut sample (to the nearest of 0.01 g), put it in a 50 mL centrifuge tube, add 30 mL of methanol, and perform ultrasonic extraction at (70±2)°C for (60±5) min. Concentrate the extract to be nearly dry below 40°C with rotary evaporator, accurately add 2 mL of methanol to dissolve the residue, and filter it through a 0.22 μm filter membrane (4.16) for determination by LC-MS method.
When impurities in samples (e.g., silk) interfere with detection, the following purification method is adopted. Dissolve the residue in the concentration bottle with 10 mL of methanol-water solution (4.7), and transfer it totally to the solid phase extraction column (4.15), and control the flow rate at 1 mL/min to 2 mL/min. Discard the effluent, dry it under reduced pressure for 10 min, elute with 5 mL of methanol-dichloromethane solution (4.8), and collect the eluate. Dry the eluate with nitrogen below 40°C, accurately add 2 mL of methanol to dissolve the residue, and filter it through a 0.22 μm filter membrane (4.16) for determination by LC-MS method.
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents or materials
5 Apparatus
6 Determination procedures
7 Calculation and expression of results
8 Lower determination limit, recovery rate and precision of the methods
9 Test report
Annex A (Informative) Determination of AP and APnEO by RP-HPLC method
Annex B (Informative) Determination of AP and APnEO by NP-HPLC method
Annex C (Informative) Determination of AP and APnEO by HILIC method
Annex D (Informative) Selective ion monitoring chromatograms of AP and APEO determined by LC-MS method
Annex E (Informative) Mass spectrometry reference conditions
