GB/T 20385.1-2021 PDF English
US$230.00 · In stock · Download in 9 secondsGB/T 20385.1-2021: Textiles - Determination of organotin compounds - Part 1: Derivatisation method using GC-MS Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB/T 20385.1: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 20385.1-2021 | English | 230 |
Add to Cart
|
0-9 seconds. Auto-delivery
|
Textiles - Determination of organotin compounds - Part 1: Derivatisation method using GC-MS
| Valid |
| GB/T 20385-2006 | English | 359 |
Add to Cart
|
3 days
|
Textiles -- Determination of organotin compounds
| Obsolete |
Excerpted PDFs (Download full copy in 9 seconds upon purchase)PDF Preview: GB/T 20385.1-2021
GB/T 20385.1-2021: Textiles - Determination of organotin compounds - Part 1: Derivatisation method using GC-MS
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT20385.1-2021
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 s1, 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 solution in the refrigerator to reduce the volatilization of the solvent, and the
storage period shall not exceed one year.
8.3.5 Target compound - working solution (the mass concentration of organotin cation is
10 mg/L)
Use the pipette (6.5) to transfer-take an appropriate volume of the target compound - stock
solution (8.3.4) to a volumetric flask of an appropriate volume. Use methanol (5.13) to reach a
constant volume to the scale. Thus, the target compound - working solution with organotin
cation concentration of 10 mg/L is obtained.
Store the target compound - working solution in the refrigerator to reduce the volatilization of
the solvent, and the storage period shall not exceed one month.
8.4 Preparation of Tropolone Solution
Use the analytical balance (6.2) to weigh-take 0.500 g of tropolone (5.12) into a glass beaker;
use about 20 mL of methanol (5.13) to dissolve it, then, transfer it to a 100 mL volumetric flask.
Use methanol to dilute to the scale. Thus, tropolone solution with a concentration of 5 g/L is
obtained.
Store this solution in the refrigerator to reduce the volatilization of the solvent, and the storage
period is one month.
8.5 Preparation of Buffer Solution
Prepare sodium acetate solution with a concentration of 0.2 mol/L. For example, weigh-take
16.4 g of anhydrous sodium acetate (5.14) into 1 L of water (5.1); use glacial acetic acid (5.3)
to adjust the pH value to 4.5.
8.6 Preparation of Standard Curve
8.6.1 Optionally prepare standard solutions with a concentration of 100 g/L, 200 g/L, 300
g/L, 400 g/L and 500 g/L.
8.6.2 Use a micropipette (6.4) to draw 20 L, 40 L, 60 L, 80 L and 100 L of the target
compound - working solution (8.3.5). Respectively add them to containers containing 20 mL
of methanol (5.13) / ethanol (5.2) mixed solvent (volume ratio 80 / 20).
8.6.3 Add an appropriate volume of internal standard substance - working solution (8.3.3).
8.6.4 Add 8 mL of pH 4.5 buffer solution (8.5).
8.6.5 Use the pipette (6.5) to draw 1 mL of tropolone solution (8.4) into the container.
8.6.6 Add 100 L of sodium tetraethyl-borate solution (8.2); use the horizontal mechanical
vibrator (6.9) to vigorously oscillate it for 30 min.
8.6.7 Use the pipette (6.5) to draw 2 mL of n-hexane (5.10) into the container; use the horizontal
mechanical vibrator (6.9) to vigorously oscillate it for 30 min.
8.6.8 After stratification, take the n-hexane phase for analysis by GC-MS.
NOTE: if necessary (to obtain a clear n-hexane layer), the centrifuge (6.8) may be used to perform
centrifugation for 5 min.
8.7 Preparation of Sample Solution
8.7.1 Use the analytical balance (6.2) to weigh-take (1.0 0.1) g of specimen into a 50 mL glass
reaction flask with a screw stopper (6.3); record the mass of the specimen as m1, accurate to 0.1
mg.
8.7.2 Add 20 mL of methanol (5.13) / ethanol (5.2) mixed solvent (volume ratio 80 / 20).
8.7.3 Add an appropriate volume of internal standard substance - working solution (8.3.3).
8.7.4 Use the pipette (6.5) to draw 1 mL of tropolone solution (8.4) and add it to the glass
reaction flask with a screw stopper.
8.7.5 In the temperature-controlled ultrasonic generator (6.7), perform ultrasonic extraction at
(60 5) C for 1 h 5 min. Then, cool it to room temperature.
8.7.6 If necessary, centrifuge it for 5 min, then, transfer the supernatant to another container.
8.7.7 Add 8 mL of pH 4.5 buffer solution (8.5).
8.7.8 Add 100 L of sodium tetraethyl-borate solution (8.2); use the horizontal mechanical
vibrator (6.9) to vigorously oscillate it for 30 min.
8.7.9 Use the pipette (6.5) to draw 2 mL of n-hexane (5.10) into the container; use the horizontal
mechanical vibrator (6.9) to vigorously oscillate it for 30 min.
NOTE: Some sample solutions may generate air bubbles and pressure after adding reagents, so be
careful to release excess air in the sealed container before oscillation, so as to ensure the
safety.
8.7.10 If necessary (to obtain a clear n-hexane layer), perform centrifugation for 5 min.
8.7.11 After stratification, take the n-hexane phase for analysis by GC-MS.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
Tips & Frequently Asked QuestionsQuestion 1: How long will the true-PDF of English version of GB/T 20385.1-2021 be delivered?Answer: The full copy PDF of English version of GB/T 20385.1-2021 can be downloaded in 9 seconds, and it will also be emailed to you in 9 seconds (double mechanisms to ensure the delivery reliably), with PDF-invoice. Question 2: Can I share the purchased PDF of GB/T 20385.1-2021_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 20385.1-2021_English will be deemed to be sold to your employer/organization who actually paid for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. www.ChineseStandard.us -- GB/T 20385.1-2021 -- Click this link and select your country/currency to pay, the exact amount in your currency will be printed on the invoice. Full PDF will also be downloaded/emailed in 9 seconds. Question 5: Should I purchase the latest version GB/T 20385.1-2021?Answer: Yes. Unless special scenarios such as technical constraints or academic study, you should always prioritize to purchase the latest version GB/T 20385.1-2021 even if the enforcement date is in future. Complying with the latest version means that, by default, it also complies with all the earlier versions, technically. How to buy and download a true PDF of English version of GB/T 20385.1-2021?A step-by-step guide to download PDF of GB/T 20385.1-2021_EnglishStep 1: Visit website https://www.ChineseStandard.net (Pay in USD), or https://www.ChineseStandard.us (Pay in any currencies such as Euro, KRW, JPY, AUD).
Step 2: Search keyword "GB/T 20385.1-2021".
Step 3: Click "Add to Cart". If multiple PDFs are required, repeat steps 2 and 3 to add up to 12 PDFs to cart.
Step 4: Select payment option (Via payment agents Stripe or PayPal).
Step 5: Customize Tax Invoice -- Fill up your email etc.
Step 6: Click "Checkout".
Step 7: Make payment by credit card, PayPal, Google Pay etc. After the payment is completed and in 9 seconds, you will receive 2 emails attached with the purchased PDFs and PDF-invoice, respectively.
Step 8: Optional -- Go to download PDF.
Step 9: Optional -- Click Open/Download PDF to download PDFs and invoice.
See screenshots for above steps: Steps 1~3 Steps 4~6 Step 7 Step 8 Step 9
|