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GB/T 29493.3-2023 PDF in English


GB/T 29493.3-2023 (GB/T29493.3-2023, GBT 29493.3-2023, GBT29493.3-2023)
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GB/T 29493.3-2023: PDF in English (GBT 29493.3-2023)

GB/T 29493.3-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S 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 μg/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 μg/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 μg/mL: Pipette 10 mL of organotin
intermediate concentration mixed solution (5.17) with a mass concentration of 10
μg/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 μg/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 μg/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 μg/mL: Pipette 10 mL of the internal standard
intermediate concentration mixed solution (5.20) with a mass concentration of 10
μg/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 μL 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 μL 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 μL 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;
ρis - The value of the target organotin cation/organotin mass concentration in the
standard working solution, in micrograms per liter (μg/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.
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.