GB/T 20385.1-2021 English PDF (GBT20385.1-2021)

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GB/T 20385.1-2021: Textiles -- Determination of organotin compounds -- Part 1: Derivatisation method using GC-MS
GB/T 20385.1-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
CCS W 04
Replacing GB/T 20385-2006
Textiles - Determination of Organotin Compounds - Part 1:
Derivatisation Method Using GC-MS
(ISO 22744-1:2020, Textiles and Textile Products - Determination of Organotin
Compounds - Part 1: Derivatisation Method Using Gas Chromatography, MOD)
ISSUED ON: MARCH 9, 2021
IMPLEMENTED ON: OCTOBER 1, 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 ... 9 
7 Sample ... 9 
8 Test Procedures ... 9 
9 Result Calculation ... 16 
10 Test Report ... 18 
Appendix A (informative) Gas Chromatography - Mass Spectrometry (GC-MS)
Reference Test Parameters ... 19 
Appendix B (informative) Feasibility of the Method ... 20 
Textiles - Determination of Organotin Compounds - Part 1:
Derivatisation Method Using GC-MS
WARNING: the personnel adopting this Standard shall have practical experience in
formal laboratory work. This document does not address all possible safety issues. It is
the user’s responsibility to take appropriate safety and health measures, and to ensure the
compliance with the conditions stipulated by relevant national regulations.
1 Scope
This document specifies the test method of determining organotin compounds (see Table 1) in
textile products through the derivatisation method using GC-MS.
This document is applicable to the various types of textile products.
2 Normative References
Through the normative references in this text, the contents of the following documents
constitute indispensable clauses of this document. In terms of references with a specified date,
only versions with a specified date are applicable to this document. In terms of references
without a specified date, the latest version (including all the modifications) is applicable to this
document.
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods (GB/T 6682-
2008, ISO 3696:1987, MOD)
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 Principle
Take tropolone solution as the complexing agent and use methanol - ethanol mixed solvent to
extract organotin compounds in the textiles.
Through the reaction with sodium tetraethyl-boride, convert the polar and high-boiling
organotin into the corresponding volatile alkyl derivatives. Use gas chromatograph - mass
spectrometer (GC-MS) for determination and adopt the internal standard method for
quantitative determination.
5 Reagents
Unless it is otherwise specified, all reagents are analytically pure.
5.1 Water, which complies with Grade-3 water specified in GB/T 6682.
5.2 Ethanol, chromatographically pure, CAS No.: 64-17-5.
5.3 Glacial acetic acid, CAS No.: 64-19-7.
5.4 Sodium tetraethyl-borate, CAS No.: 15523-24-7.
5.5 Tetrahydrofuran, CAS No.: 109-99-9.
5.6 n-heptyltin trichloride, CAS No.: 59344-47-7 (internal standard substance).
5.7 Di-n-heptyltin dichloride, CAS No: 74340-12-8 (internal standard substance).
5.8 Tri-n-pentyltin chloride, CAS No: 3342-67-4 (internal standard substance).
5.9 Tetra-n-propyltin, CAS No.: 2176-98-9 (internal standard substance).
NOTE: if the recovery rate of the internal standard substances (5.6, 5.7, 5.8 and 5.9) is relatively
low, other internal standard substances (for example, deuterated compounds) may be
selected (see also 9.1).
5.10 N-hexane, CAS No.: 110-54-3.
5.11 Inert gas, for example, nitrogen or argon, with a purity of 99.9%.
5.12 Tropolone, CAS No.: 533-75-5.
5.13 Methanol, CAS No.: 67-56-1.
5.14 Anhydrous sodium acetate, CAS No.: 127-09-3.
5.15 Organotin compounds, see Table 1.
6 Instruments and Materials
6.1 Gas chromatograph - mass spectrometer (GC-MS).
6.2 Analytical balance, with a division value of 0.1 mg.
6.3 Glass reaction flask with a screw stopper, 50 mL.
6.4 Micropipette, 10 L ~ 500 L, disposable tip.
6.5 Pipette, with a measuring range of 1 mL ~ 10 mL.
6.6 pH meter, equipped with a glass composite electrode, with a measuring range of 0 ~ 14 and
the measurement accuracy accurate to 0.1.
6.7 Ultrasonic generator, with a working frequency of (40  5) kHz and the temperature
controllable.
6.8 Centrifuge.
6.9 Horizontal mechanical vibrator.
NOTE: the minimum frequency of the horizontal vibrator is 5 s1, and the amplitude is 2 cm ~ 5
cm.
6.10 Volumetric flask, with a volume of 10 mL ~ 500 mL.
NOTE: before use, all glassware shall be soaked in nitric acid (volume fraction: 5%) for 24 h, and
rinsed with water.
7 Sample
The specimen is taken from a single texture of the textile product, for example, fabric, coating
material, polymer or other textures. The specimen preparation process includes separating a
single texture from the product and preparing it into small pieces with a maximum dimension
not exceeding 4 mm.
NOTE: in consideration of the detection limit and quantification limit, for samples of the same
texture, a maximum of three samples can be mixed in testing, and the three samples shall
be of equal mass.
8 Test Procedures
8.1 General
SAFETY WARNING: since sodium tetraethyl-borate is air-sensitive and will
spontaneously ignite in air, sodium tetraethyl-borate solution shall be prepared in a large-
volume fume hood. Organotin is toxic and endocrine disruptor, so special care shall be
taken.
NOTE: before use, all reagents stored below room temperature should be taken out and placed to
reach room temperature.
8.2 Preparation of Sodium Tetraethyl-borate Solution
In an inert environment, weigh-take 2 g of sodium tetraethyl-borate (5.4); add 10 mL of
tetrahydrofuran (5.5) to dissolve it.
Store this solution in an inert gas (5.11) environment. The validity period is 3 months.
NOTE: sodium tetraethyl-borate or its solution can be purchased in fixed weights. An example of
preparation: transfer-take 10 mL of tetrahydrofuran into a 40 mL sample bottle with a
screw cap; open the 2 g package of sodium tetraethyl-borate; add it to the sample bottle
and dissolve it. If the sodium tetraethyl-borate is in 5 g package, accordingly increase the
volume of the added tetrahydrofuran to ensure a concentration of approximately 0.2 g/mL.
8.3 Preparation of Standard Solution
8.3.1 Conversion of organotin cation
The standard substance of organotin chloride is available on the market, but the mass
concentration of the standard curve and the expression of results are all expressed in terms of
organotin cation, and the unit is mg/kg.
Example 1: the corresponding cation of Bu2SnCl2 is Bu2Sn2+.
Table 2 provides the amount of organotin chloride and the weighting factor for re-calculation
of cation (assuming that the chloride purity is 100%).
The target compound solution can be directly purchased with a certificated standard solution,
or prepared by the user.
Each substance is separately prepared: use the analytical balance (6.2) to weigh-take an
appropriate amount of the target compound (see Table 1); select a volumetric flask with an
appropriate volume; use methanol (5.13) to dissolve it and reach a constant volume to the scale.
The concentration of the organotin cation is 1,000 mg/L.
Store the standard ...