GB/T 29493.3-2013 in English

《GB/T 29493.3-2013纺织染整助剂中有害物质的测定 第3部分：有机锡化合物的测定 气相色谱-质谱法》由TC134（全国染料标准化技术委员会）归口，TC134SC1（全国染料标准化技术委员会印染助剂分会）执行，主管部门为中国石油和化学工业联合会。

1 Scope

This part of GB/T 29493 specifies the method for determining organotins in textile dyeing and finishing auxiliaries by gas chromatograph-mass spectrometer (GC/MS).

This part is applicable to the determination of organotins in textile dyeing and finishing auxiliaries.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the normative document (including any amendments) applies.

GB/T 6682-2008 Water for analytical laboratory use - specification and test methods
GB/T 8170-2008 Rules of rounding off for numerical values & expression and judgment of limiting values

3 Principle

The sample is ultrasonically extracted with ethanol, and the derivatized extract is directly extracted by using sodium tetraethylborate as a derivatizing reagent and n-hexane as an extractant. The extract is determined by gas chromatography-mass spectrometry (GC/MS) and quantified by internal standard method.

4 Reagents and solutions

Unless otherwise specified, only recognized analytical reagent and Class 2 water (specified in GB/T 6682-2008) shall be used.

4.1 Normal hexane.

4.2 Glacial acetic acid

4.3 Ethanol

4.4 Sodium diethyldithioformate solution: weigh 2 g of sodium diethyldithioformate and dissolve it in ethanol to a constant volume of 25 mL.

4.5 Acetate buffer solution: weigh 136.08 g of sodium acetate trihydrate, dissolve it with 800 mL of Class 2 water, adjust the pH to 4.5 with glacial acetic acid (about 100 mL), dilute to a constant volume of 1 L with Class 2 water and then shake well.

4.6 Anhydrous sodium sulfate.

4.7 Tetrahydrofuran.

Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and solutions
5 Apparatus
6 Analytical procedures
7 Calculation of results
8 Lower determination limit, recovery rate and precision
9 Test report
Annex A (Informative) Total ion chromatogram and standard mass spectrogram of standard derivatized organotin