SN/T 4670-2016 in English

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This standard is developed in accordance with the rules given in GB/T 1.1-2009.

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This standard was proposed by and is under the jurisdiction of the Certification and Accreditation Administration of the People's Republic of China.
Textiles for import and export—Determination of glyoxal, formaldehyde and glutaraldehyde—
High performance liquid chromatography

1 Scope

This standard specifies high performance liquid chromatography (HPLC) for determination of free and hydrolyzed glyoxal, formaldehyde and glutaraldehyde in textiles.

This standard is applicable to the determination of free and hydrolyzed glyoxal, formaldehyde and glutaraldehyde content in various textile materials and their products.

2 Normative reference

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

The specimen is extracted with water, and the aldehyde compounds in the extraction solution act with 2,4-dinitrophenylhydrazine under acidic conditions to produce 2,4-dinitrophenylhydrazone accordingly, which then is separated by using reversed-phase liquid chromatography column, and determined by high performance liquid chromatography equipped with secondary array tube detector or ultraviolet detector, and finally be quantified with external standard method.

4 Reagents and materials

Unless otherwise specified, the reagents used are analytical grade, and the water used is Grade I water conforming to GB/T 6682.

4.1 Acetonitrile: chromatographically pure.

4.2 Glacial acetic acid.

4.3 2,4-dinitrophenylhydrazine (DNPH)

4.4 2,4-dinitrophenylhydrazine solution: weigh 0.07 g of 2,4-dinitrophenylhydrazine (4.3) into a 100 mL beaker, add about 80 mL of acetonitrile and 0.5 mL of glacial acetic acid, and stir until dinitrophenylhydrazine is completely dissolved, then immediately transfer it to a 100 mL brown volumetric flask, dilute to the scale with acetonitrile, and shake well.

4.5 Formaldehyde standard aqueous solution: with a concentration of 1,000 mg/L.

4.6 Glyoxal standard aqueous solution: with a concentration of 1,000 mg/L.

4.7 Glutaraldehyde standard aqueous solution: with a concentration of 1,000 mg/L.

4.8 Mixed standard solution: with water as the solvent, pipette 10 mL of formaldehyde standard aqueous solution (4.5), 10 ml of glyoxal standard aqueous solution (4.6) and 10 ml of glutaraldehyde standard aqueous solution (4.7) respectively into a 100 mL volumetric flask, and dilute to 100 mL to prepare a mixed standard solution of three aldehydes with a concentration of 100 mg/L.

4.9 Mixed standard working solution: with water as the dilution solvent, dilute the mixed standard solution of three aldehydes (4.8) step by step to prepare standard working solutions with concentrations of 0.2 mg/L, 0.5 mg/L, 1.0 mg/L, 2.0 mg/L, 4.0 mg/L and 5.0 mg/L respectively. The standard working solution is prepared immediately before use.

5 Apparatus

5.1 High performance liquid chromatograph (HPLC): with diode array detector (DAD) or ultraviolet detector (UVD).

5.2 Vortex mixer: an ultrasonic water bath with controllable temperature.

5.3 Thermostatic oscillator: (40±2)°C and (60±2)°C.

5.4 Analytical balance: with a minimum division of 0.1 mg.

5.5 Organic phase filter membrane: with a pore diameter of 0.45 μm.

5.6 Volumetric flask: 100 mL.

5.7 Colorimetric tube with stopper: 10 mL.

5.8 Pipette: 5 mL.

5.9 Triangular flask with stopper: 150 mL.

5.10 Glass sand core funnel.

6 Analysis procedure

6.1 Specimens

6.1.1 Basic requirements

Samples shall be sealed and packed with aluminum film or other materials that do not release organic substances, and test specimens shall be prepared for determination as soon as possible after the sample is unpacked.

6.1.2 Preparation of specimens

Cut two specimens at the center of the sample or 5 cm away from the edge of the sample, with a mass of not less than 10 g, all of which shall be cut to less than 5 mm × 5 mm, and sealed in a wide-mouth bottle for determination.

6.2 Extraction of aldehyde compounds

Accurately weigh 1.0 g of specimen (6.1.2) (accurate to 0.1 mg), place it in a 150 mL triangular flask (5.9), add 80 mL of water, seal it with a stopper, and then place it in a (40±2)°C thermostatic oscillator (5.3) to assist extraction for (60±5) min; filter it with the sand core funnel (5.10), wash the specimen on the triangular flask and funnel with a small amount of water, combine the filtrate into a 100 mL volumetric flask, and dilute with water to the scale, shake well, which is used as the extraction solution for later use.

Foreword i
1 Scope
2 Normative reference
3 Principle
4 Reagents and materials
5 Apparatus
6 Analysis procedure
7 Calculation of result
8 Determination of low limit and limit of quantitation
9 Precision
Annex A (Informative) Liquid chromatogram of glyoxal, formaldehyde and glutaraldehyde derivatives
Annex B (Informative) UV absorption spectrograms of glyoxal, formaldehyde and glutaraldehyde derivatives by liquid chromatography