GB/T 2912.3-2009Textiles - Determination of formaldehyde - Part 3: High performance liquid chromatography method (English PDF)

Foreword

GB/T 2912 Textiles - Determination of Formaldehyde consists of the following parts.

--- Part 1: Free and Hydrolyzed Formaldehyde (Water Extraction Method);

--- Part 2: Released Formaldehyde (Vapor Absorption Method);

--- Part 3: High Performance Liquid Chromatography Method. This Part belongs to Part 3 of GB/T 2912. The Appendix A of this Part is informative.

1 Scope

This Part of GB/T 2912 specifies the method using the high-performance liquid chromatography - ultraviolet detector (HPLC/UVD) or diode array detector (HPLC/DAD) to determine the contents of free and hydrolyzed formaldehyde or released formaldehyde in the textile.

This Part is applicable to any types of textiles.

This Part is applicable to the textiles with formaldehyde content between 5mg/kg and 1000mg/kg; especially the samples of dark extract liquid.

2 Normative References

The provisions in following documents become the provisions of this Part through reference in this Part of GB/T 2912. For dated references, the subsequent amendments (excluding corrigendum) or revisions do not apply to this Part, however, parties who reach an agreement based on this Part are encouraged to study if the latest versions of these documents are applicable. For undated references, the latest edition of the referenced document applies.

GB/T 2912.1-2009 Textiles - Determination of Formaldehyde - Part 1: Free and Hydrolyzed Formaldehyde (Water Extraction Method) (ISO 14184-1:1998, MOD)

GB/T 2912.2009 Textiles - Determination of Formaldehyde - Part 2: Released Formaldehyde (Vapor Absorption Method) (ISO 14184-2:1998, MOD)

3 Principle

After the specimen is subjected to water extraction or vapor absorption treatment, take 2,4-dinitrophenylhydrazine as a derivatization reagent to generate 2,4-dinitrophenylhydrazone; determine by high performance liquid chromatography-ultraviolet detector (HPLC/UVD) or diode array detector (HPLC/DAD);

4 Reagents and Materials

Unless otherwise is specified, all the used reagents are analytical reagents. The test water shall conform to the provision of Class-II water specified in GB/T 6682.

4.1 Acetonitrile. chromatographically pure.

4.2 Formaldehyde solution. concentration is about 37% (mass fraction).

4.3 Derivatization test solution. take 0.05g of 2,4-dinitrophenylhydrazine; dissolve it in.

4.4 Formaldehyde standard stock solution. pipette 3.8mL of formaldehyde solution (4.2) into 1000mL brown volumetric flask; dilute with water to the scale (formaldehyde content is about 1500µg/mL); calibrate its exact concentration according to the method specified in Appendix A in GB/T 2912.1-2009.

5 Apparatus

5.1 Balance, weighing accuracy is 0.001g.

5.2 Constant temperature water bath, (60±2) °C.

5.3 High performance liquid chromatograph equipped with UV detector (UVD) or diode array detector (DAD).

6 Analytical Procedures

7 Calculation Results

Use the peak area of 2,4-dinitrophenylhydrazone determined by 6.3.3, according to the standard operating curve (6.3.2) to check out the formaldehyde concentration, expressed in µg/mL. Calculate the free and hydrolyzed formaldehyde content in sample by Formula (1); and calculate the released formaldehyde content in the sample by Formula (2).

8 Detection Limit and Recovery Rate

The detection limit of this method is 5.0mg/kg. Under the formaldehyde addition concentration of 7.5mg/kg~75mg/kg, the recovery rate is 85%~105%.

9 Test Report

The test report shall contain the following contents. […]