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GB/T 29493.3-2023 English PDF (GBT29493.3-2023)

GB/T 29493.3-2023 English PDF (GBT29493.3-2023)

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GB/T 29493.3-2023: Determination of harmful substances in textile dyeing and finishing auxiliaries - Part 3: Determination of organotins

This document describes a method for the determination of organotin compounds in textile dyeing and finishing auxiliaries using gas chromatography-mass spectrometry (GC-MS). This document is applicable to the determination of 18 organotin compounds (see Annex A) in textile dyeing and finishing auxiliaries.
GB/T 29493.3-2023
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.100.40
CCS G 70
Replacing GB/T 29493.3-2013
Determination of harmful materials in textile dyeing and
finishing auxiliaries - Part 3: Determination of organotins
ISSUED ON: SEPTEMBER 07, 2023
IMPLEMENTED ON: APRIL 01, 2024
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 or materials ... 7
6 Instruments and equipment ... 9
7 Test steps ... 9
8 Test data processing ... 11
9 Lower limit of determination, recovery rate, precision ... 13
10 test report ... 13
Annex A (normative) Basic information on organotin compounds, internal standard materials and standard stock solution preparation information tested in this document ... 14
Annex B (informative) Quantitative and qualitative ion information of target organotins and internal standard materials ... 17
Annex C (informative) Gas chromatography-mass spectrometry total ion current chromatogram of organic tin and internal standard ethylated derivatives ... 18 Determination of harmful materials in textile dyeing and
finishing auxiliaries - Part 3: Determination of organotins
WARNING -- Personnel using this document shall have practical experience in formal laboratory work. This document does not identify all possible security issues. Users are responsible for taking appropriate safety and health measures and ensuring compliance with relevant national regulations.
1 Scope
This document describes a method for the determination of organotin compounds in textile dyeing and finishing auxiliaries using gas chromatography-mass spectrometry (GC-MS).
This document is applicable to the determination of 18 organotin compounds (see Annex A) 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 referenced document (including any amendments) applies. GB/T 6682, Water for analytical laboratory use -- Specification and test methods GB/T 8170-2008, Rules of rounding off for numerical values and expression and judgement of limiting values
3 Terms and definitions
There are no terms or definitions to be defined in this document.
4 Principle
After the specimen is extracted with a methanol-ethanol mixed solvent added with sodium diethyldithiocarbamate. Under the conditions of pH=4.5, the organotin compounds are converted into the corresponding volatile ethylated derivatives by reacting with sodium tetraethylborate. Extract with n-hexane. Determine by gas chromatography-mass spectrometry. Use the internal standard method to quantify. Continuously fill a screw-capped sample bottle with an inert gas (such as nitrogen, argon). Pipette 10 mL of tetrahydrofuran into a screw-capped sample bottle. Open the 2 g package of sodium tetraethylborate. Quickly add to sample bottle. Seal. Dissolve. If sodium tetraethylborate is packaged in 5 g, increase the volume of tetrahydrofuran added accordingly. Ensure that the mass concentration of sodium tetraethylborate is 0.2 g/mL.
5.16 Organotin standard stock solution, 1000 ??g/mL: Weigh each organotin standard material (5.10) according to Table A.1 (accurate to 0.1 mg). Dissolve in methanol (5.3) respectively and set the volume to 25 mL.
NOTE: Organotin standard stock solution is stored in the dark at 0???~4???. Validity period is 1 year. 5.17 Organotin intermediate concentration mixed solution, 10 ??g/mL: Pipette 1 mL of organotin standard stock solution (5.16) into a 100 mL volumetric flask. Set the volume to the scale with methanol (5.3).
NOTE: The mixed solution of organotin with intermediate concentration shall be stored in the dark at 0???~4???. Validity period is 1 month.
5.18 Organotin standard mixed solution, 1 ??g/mL: Pipette 10 mL of organotin intermediate concentration mixed solution (5.17) with a mass concentration of 10 ??g/mL into a 100 mL volumetric flask. Set the volume to the scale with methanol (5.3). NOTE: Organotin standard mixed solution shall be stored in the dark at 0???~4???. Validity period is 2 weeks.
5.19 Internal standard stock solution, 1000 ??g/mL: Weigh (accurate to 0.1 mg) each internal standard material (5.11) according to Table A.2. Dissolve in methanol (5.3) and set the volume to 25 mL.
NOTE: The internal standard stock solution is stored in the dark at 0???~4???. Validity period is 1 year.
5.20 Internal standard intermediate concentration mixed solution, 10 ??g/mL: Pipette 1 mL of internal standard stock solution (5.19) into a 100 mL volumetric flask. Set the volume to the scale with methanol (5.3).
NOTE: The internal standard intermediate concentration mixed solution is stored in the dark at 0???~4???. Validity period is 1 month.
5.21 Internal standard mixed solution, 1 ??g/mL: Pipette 10 mL of the internal standard intermediate concentration mixed solution (5.20) with a mass concentration of 10 ??g/mL into a 100 mL volumetric flask. Set the volume to the scale with methanol (5.3). NOTE: The internal standard mixed solution is stored in the dark at 0???~4???. Validity period is 2 weeks. 6 Instruments and equipment
6.1 Gas chromatography-mass spectrometer.
6.2 Analytical balance: sensitivity is 0.1 mg.
6.3 Screw cap test tubes: 50 mL, 70 mL.
6.4 Shaker: speed is controllable at 300 r/min.
6.5 Ultrasonic generator: working frequency is (40??5) kHz, with temperature controllable.
6.6 pH meter: Equipped with glass composite electrode; measuring range (pH value) is 0~14, accurate to 0.01 pH unit.
6.7 Pipette gun: According to the needs of use, select an appropriate measuring range; equipped with a disposable tip.
7 Test steps
7.1 Extraction
Take representative samples. Mix thoroughly. Accurately weigh 2.0 g of specimen (accurate to 0.001 g) and place it in a 50 mL screw-capped test tube (6.3). Add 20 mL of sodium diethyldithiocarbamate solution (5.13) and 200 ??L of internal standard mixed solution (5.21) to the test tube. Tighten the test tube cap. Shake vigorously to immerse all specimens in the liquid. Place in an ultrasonic generator for extraction at room temperature for 1 h. Let sit. If the sample is not completely dissolved, transfer the extraction solution to another 50 mL screw-cap test tube (6.3). Then use 20 mL of sodium diethyldithiocarbamate solution (5.13) and 200 ??L of internal standard mixed solution (5.21) to treat the residue once in the same way. Combine the extracts. 7.2 Derivatization
Accurately transfer 10 mL of the extract treated in 7.1 into a 70 mL screw-capped test tube (6.3). Add 10 mL of acetate buffer solution (5.14). Adjust pH to 4.5 with acetic acid (5.2). Add 300 ??L of derivatization reagent (5.15) and 5 mL of n-hexane (5.1) in sequence. Tighten the test tube cap. Shake vigorously to mix. Shake on a shaker at 300 r/min for 30 min. Add appropriate amount of anhydrous sodium sulfate (5.6). Let it stand until the n-hexane in the upper layer becomes clear. Take the n-hexane layer for gas chromatography-mass spectrometry analysis.
NOTE 1: Tetra-substituted organotins are processed simultaneously with other organotins, but do not participate in the derivatization reaction process.
The determination results are expressed as the detection results of various organotin cations/organotins, respectively.
The content of various organotin cations/organotin in the specimen is calculated as Xi. Values are expressed in milligrams per kilogram (mg/kg). Calculate according to formula (1):
Where,
Ai - The value of the peak area of the target organotin ethylated derivative/organotin in the specimen solution;
??is - The value of the target organotin cation/organotin mass concentration in the standard working solution, in micrograms per liter (??g/L);
V - The value of the volume of n-hexane extraction solution, in milliliters (mL); Aisc - The value of the peak area of the internal standard ethylated derivative/organotin in the standard working solution;
Ais - The value of the peak area of the target organotin ethylated derivative/organotin in the standard working solution;
m - The value of the specimen mass, in grams (g);
Aiss - The value of the peak area of the internal standard ethylated derivative/organotin in the specimen solution;
V0 - The value of the volume of sodium diethyldithiocarbamate solution used for ultrasonic extraction, in milliliters (mL);
V1 - The value of the volume of the extract used for derivatization, in milliliters (mL); f - The dilution factor.
8.2 Result expression
The calculation results are expressed as the arithmetic mean of two parallel determination results. Round to two decimal places according to 4.3.3 Rounding value comparison method in GB/T 8170-2008.
9 Lower limit of determination, recovery rate, precision
9.1 Lower limit of determination
The lower limit of determination of various organotin compounds in this document is 0.05 mg/kg.
9.2 Recovery rate
The sample spike recovery rate is 70%~120%.
9.3 Precision
In the same laboratory, the same operator uses the same equipment and follows the same testing method to independently test the same tested object in a short period of time. The absolute difference between the two independent test results obtained is not greater than 20% of the arithmetic mean of the two measured values.
10 test report
The test report shall at least provide the following content:
a) Sample source and description;
b) Reference to this document;
c) Deviations from this document;
d) Abnormal situations occurred during the test;
e) Test results;
f) Test date.

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