Foreword
This document is drafted in accordance with the provisions of GB/T 1.1-2020 "Guidelines for standardization work Part 1: Structure and drafting rules of standardization documents".
Please note that some of the contents of this document may involve patents. The issuer of this document does not assume responsibility for identifying patents. This document is proposed by the China Textile Industry Federation.
This document is categorized by the National Technical Committee for Textile Standardization, Basic Standards Branch (SAC/TC 209/SC 1).
1 Scope
This document specifies the use of inductively coupled plasma mass spectrometry (ICP-MS) to determine the screening method for organotin compounds in textile products. This document applies to all types of textile products.
2 Normative reference documents
The following documents constitute the essential provisions of this document through the normative references in the text. Among them, note the date of the reference document, only the date of the corresponding version applies to this document; do not note the date of the reference document, its latest version (including all the revision of the list) applies to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 20385.1 Textiles, the determination of organotin compounds Part 1: derivatization gas chromatography-mass spectrometry
3 Terminology and definitions
There are no terms and definitions that need to be defined in this document.
4 Principle
The sample is diluted and capacitated by concentrated nitric acid digestion, and the total tin content in the sample is tested and calculated by inductively coupled plasma mass spectrometer (ICP-MS). The total tin content is converted to the organotin cation content to determine whether the sample contains organotin compounds.
5 Reagents
Unless otherwise specified, all reagents are analytically pure.
5.1 water: GB/T 6682 in line with the provisions of the first-class water. 5.2 concentrated nitric acid: superior purity.
5.3 Nitric acid solution: take 20 mL of concentrated nitric acid (5.2), water (5.1) volume to 100 mL.
5.4 Methanol.
5.5 Ethanol.
5.6 Methanol-ethanol mixture: methanol (5.4) and ethanol (5.5) mixed at a volume ratio of 4:1.
6 Apparatus and materials
5.7 Tin standard solution: 1000 mg/L commercially available certified standard substance, CAS No. 7440-31-5.
6.1 Inductively coupled plasma mass spectrometer (ICP-MS).
6.2 Microwave digestion apparatus: with temperature program control function.
6.3 Analytical balance: the division value of 0.000 1 go
6.4 Pipette: capacity of 5 mL, 20 mLo6.5 Volumetric flask: capacity of 25 mL.
6.6 Aqueous filtration membrane: pore size 0.45 um.
7 Analysis steps
7.1 Specimen preparation
Take a representative sample and cut it up (size not larger than 5 mm×5 mm).
8 Calculation of results and judgment
8.1 Calculation of results
9 Recovery, method limit of quantification and precision
9.1 Recovery
Prepare 17 organotin cation standard working solutions with methanol-ethanol mixture (5.6) to appropriate concentrations, respectively. Take 0.5 g of the blank sample in the microwave digestion tube, add 0.1 mL of the prepared single standard solution to the blank sample, add 5 mL of concentrated nitric acid (5.2) accurately, seal the digestion tube and place it in the microwave digestion apparatus, increase the temperature to 160 ℃ within 10 min, hold for 5 min, cool to room temperature, transfer the digestion solution to a 25 ml volumetric flask, fix the volume with water to the scale, and filter through the aqueous phase. The digestion solution was filtered through an aqueous filtration membrane (6.6) and analyzed instrumentally with reference to the conditions in Appendix A. The recovery should be between 70% and 120% after each organotin cation is tested separately and calculated according to equation (2).
10 Test report
Foreword
1 Scope
2 Normative reference documents
3 Terminology and definitions
4 Principle
5 Reagents
6 Apparatus and materials
7 Analysis steps
8 Calculation of results and judgment
9 Recovery, method limit of quantification and precision
10 Test report
