GB/T 2912.3-2009 PDF English
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Textiles -- Determination of formaldehyde -- Part 3: High performance liquid chromatography method
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GB/T 2912.3-2009: Textiles -- Determination of formaldehyde -- Part 3: High performance liquid chromatography method
---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/GBT2912.3-2009
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
W 04
Textiles - Determination of Formaldehyde - Part 3.
High Performance Liquid Chromatography Method
Issued on. JUNE 19, 2009
Implemented on. FEBRUARY 01, 2010
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Principle... 5
4 Reagents and Materials... 5
5 Apparatus... 5
6 Analytical Procedures... 6
7 Calculation Results... 7
8 Detection Limit and Recovery Rate... 8
9 Test Report... 8
Appendix A (Informative) 2,4-dinitrophenylhydrazone Liquid Chromatography
Retention Time and Chromatogram... 9
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.
This Part was proposed by China National Textile and Apparel Council.
This Part shall be under the jurisdiction of Basic Standard Division of National
Technical Committee for Standardization of Textile (SAC/TC 209/SC 1).
Drafting organizations of this Part. Zhejiang Academy of Science and Technology for
Inspection and Quarantine; Entry-Exit Inspection and Quarantine Bureau of Huzhou;
Zhejiang Sci-Tech University; Shandong Entry-Exit Inspection and Quarantine Bureau.
Chief drafting staffs of this Part. Zhao Shanhong, Jiang Yongxiang, Chen Haixiang,
Pan Jianjun, Tan Jinhui, Wang Dong and Wu Gang.
Textiles - Determination of Formaldehyde - Part 3.
High Performance Liquid Chromatography Method
Warning. Personnel using this Part of GB/T 2912 shall have the hands-on
experience working in formal laboratory. This Part does not address all possible
security issues. The user is responsible to take appropriate safety and health
measures, and ensures the conditions specified by the relevant national
regulations.
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
6.1 Sample pretreatment
Determine the free and hydrolyzed formaldehyde. perform as per the provisions of
Clause 7 in GB/T 2912.1-2009.
Determine the released formaldehyde. perform as per the provisions of Clause 7 and
8.1 in GB/T 2912.2-2009.
6.3 Determination
6.3.1 Liquid chromatography analytical conditions
Since the test results depend on the used instrument, the general parameter of the
chromatographic analysis can’t be given; the following parameters have proven to be
suitable for the test.
6.3.2 Standard operating curve
6.3.2.1 separately transfer 1.0, 2.0, 5.0, 10.0, 20.0 and 50.0mL of formaldehyde
standard working solution (4.5) into 100mL volumetric flasks; dilute with water to the
scale (formaldehyde concentrations are 0.15, 0.30, 0.75, 1.5, 3.0 and 7.5µg/mL,
respectively). The diluted formaldehyde standard serial solutions shall be derivatized
as per the requirements of 6.2.
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.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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