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GB/T 24279.2-2021 PDF in English


GB/T 24279.2-2021 (GB/T24279.2-2021, GBT 24279.2-2021, GBT24279.2-2021)
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GB/T 24279.2-2021: PDF in English (GBT 24279.2-2021)

GB/T 24279.2-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
CCS W 04
Textiles - Determination of certain flame retardants -
Part 2: Phosphorus flame retardants
(ISO 17881-2:2016, MOD)
ISSUED ON: MAY 21, 2021
IMPLEMENTED ON: DECEMBER 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
Introduction ... 5 
1 Scope ... 6 
2 Normative references ... 6 
3 Terms and definitions ... 6 
4 Principle ... 6 
5 Reagents ... 7 
6 Instruments and materials ... 7 
7 Test steps ... 7 
8 Result calculation ... 9 
9 Precision ... 9 
10 Test report ... 9 
Annex A (informative) HPLC-MS/MS detection parameters ... 11 
Foreword
This Part was drafted in accordance with the rules given in GB/T 1.1-2020
“Directives for standardization - Part 1: Rules for the structure and drafting of
standardizing documents”.
This Part is Part 2 of GB/T 24279 “Textiles - Determination of certain flame
retardants”. The following parts of GB/T 24279 have been issued:
- Part 1: Brominated flame retardants;
- Part 2: Phosphorus flame retardants.
This Part uses redrafting method to modify and adopt ISO 17881-2:2016
“Textiles - Determination of certain flame retardants - Part 2: Phosphorus flame
retardants”.
The structural differences between this Part and ISO 17881-2:2016 are as
follows:
- added “Normative references” as Clause 2;
- added “Terms and definitions” as Clause 3;
- added “Precision” as Clause 9.
The technical differences between this Part and ISO 17881-2:2016 are as
follows:
- In Clause 5, changed analytically pure to chromatographically pure, added
the purity of the tested standard substance for liquid chromatography
analysis; according to the relevant requirements of prohibited flame
retardants, added the test substance "Di-(2,3-dibromopropyl) phosphate";
- in 5.8, added GB/T 6682 as a reference; specified the requirements for
water used;
- in 6.7, added the balance with a division of 0.01g for weighing textile
specimen;
- in Clause 8, added the provisions that dilution factors and calculation results
are kept to one decimal place, so as to make the calculation and
expression of results clearer;
- in Clause 9, according to relevant domestic standards, added relevant
description on precision.
This Part made the following editorial modifications:
Textiles - Determination of certain flame retardants -
Part 2: Phosphorus flame retardants
WARNING - Personnel using this document should have practical
experience in formal laboratory work. This document does not indicate all
possible security issues. The user is responsible for taking appropriate
safety and health measures and ensuring compliance with the conditions
stipulated by relevant national laws and regulations.
1 Scope
This Part specifies the test method that uses the high-performance liquid
chromatography-tandem mass spectrometer (HPLC-MS/MS) to determine
certain phosphorus flame retardants in textiles.
This Part is applicable to various textiles.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) is applicable to this standard.
GB/T 6682, Water for analytical laboratory use - Specification and test
methods (GB/T 6682-2008, ISO 3696:1987, MOD)
3 Terms and definitions
There are no terms and definitions that need to be defined in this document.
4 Principle
Use acetone as extractant. Extract flame retardant from textile specimens in
ultrasonic generator. Use HPLC-MS/MS to determine flame retardant. Use
external standard method to quantify.
Use acetonitrile (5.6) as solvent to respectively prepare standard stock solution
of each flame retardant (5.1~5.4). The concentration is 1000μg/mL.
7.1.2 Standard working solution
Use acetonitrile to prepare the mixed standard solution. According to the needs,
use acetonitrile to dilute step by step into a series of mixed standard working
solutions of suitable concentration. Choose at least five standard dilution
solutions of appropriate concentration to establish the standard working curve.
Conduct HPLC-MS/MS analysis.
NOTE: Store the standard stock solution in the dark at 0°C~4°C. The validity is 6 months.
Store the standard working solution in the dark at 0°C~4°C. The validity is 3 months.
7.2 Specimen preparation
Take respective specimen from the sample. After cutting and mixing well, use
the balance (6.7) to weigh (1.00±0.01)g of specimen.
7.3 Ultrasonic extraction
Place the specimen in a stoppered glass reaction flask (6.4). Add 20mL of
acetone (5.5). Extract in 40°C ultrasonic generator (6.2) for 40min. Collect the
extract in a 100mL concentrating bottle (6.5). Add another 20mL of acetone to
the reaction flask. Extract 20min at about 40°C. Combine and collect the
extracts in a 100mL concentrating flask (6.5).
Use a rotary evaporator (6.3) to concentrate until the residue is nearly dry. Take
2mL of acetonitrile (5.6) to dissolve the residue. Filter through organic filter
membrane (6.6). The resulting filtrate is used for the determination of flame
retardants.
7.4 Determination
Use HPLC-MS/MS(6.1) to determine the flame retardant in the filtrate obtained
in 7.3. Annex A gives examples of detection parameters for HPLC-MS/MS
determination of flame retardants. Carry out a blank test. Subtract the blank
value.
When the flame retardant concentration is too low, appropriately increase the
specimen mass so that the detection concentration is within the linear range of
the instrument's response value.
When the flame retardant concentration is higher than the linear range of the
instrument response value, the solution is appropriately diluted.
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.