GB/T 2912.3-2009 English PDF (GBT2912.3-2009)

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GB/T 2912.3-2009: Textiles -- Determination of formaldehyde -- Part 3: High performance liquid chromatography method
GB/T 2912.3-2009
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
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)
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
(GB/T 6682-2008, ISO 3696:1987, MOD)
5.3 High performance liquid chromatograph equipped with UV detector (UVD) or diode
array detector (DAD).
5.4 0.45µm filter membrane.
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.
6.2 Derivatization
Accurately transfer 1.0mL of the above sample solution (6.1) and 2.0mL of the
derivatization test solution (4.3) into 10mL stoppered test tube; after mixing evenly,
stand in (60±2) °C water bath to react for 30min. After such solution is cooled off to the
room temperature, filter by 0.45µm filtered membrane for the HPLC/UVD or
HPLC/DAD analysis.
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.
a) Liquid chromatographic column: C18, 5µm, 4.6mm×250mm or equivalent;
b) Mobile phase: acetonitrile + water (65+35);
c) Flow rate: 1.0mL/min;
d) Column temperature: 30°C;
e) Detection wavelength: 355nm;
f) Sampling injection volume: 20µL.
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