GB/T 24168-2023 PDF English
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| GB/T 24168-2023 | English | 260 |
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Determination of the content of phthalate in textile dyeing and finishing auxiliaries
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| GB/T 24168-2009 | English | 479 |
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Determination of the content of phthalate in textile dyeing and finishing auxiliaries
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GB/T 24168-2023: Determination of the content of phthalate in textile dyeing and finishing auxiliaries
---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/GBT24168-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
CCS G 70
GB/T 24168-2023
Replacing GB/T 24168-2009
Determination of the content of phthalate in textile dyeing
and finishing auxiliaries
ISSUED ON: NOVEMBER 27, 2023
IMPLEMENTED ON: JUNE 01, 2024
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions ... 5
4 Principle ... 5
5 Determination method ... 6
6 Detection limit, recovery rate and precision ... 10
7 Test report ... 11
Annex A (normative) 24 kinds of phthalate standard substances ... 12
Annex B (informative) Retention time and characteristic ions of 24 kinds of phthalate
standard substances ... 13
Annex C (informative) Gas chromatography-mass spectrometry total ion flow diagrams
of phthalate standard solutions ... 15
Foreword
This document was drafted in accordance with the provisions of GB/T 1.1-2020
“Directives for standardization - Part 1: Rules for the structure and drafting of
standardizing documents”.
This document replaces GB/T 24168-2009 “Determination of the content of phthalate
in textile dyeing and finishing auxiliaries”. Compared with GB/T 24168-2009, in
addition to structural adjustments and editorial changes, the main technical changes are
as follows:
- ADD the type of phthalate (see Clause 1 of this document);
- MODIFY the content of the reagents and materials (see 5.2 of this document, 4.2
of the 2009 edition);
- MODIFY the specifications of the extractor in the instruments and equipment [see
5.3.5 of this document, 4.3d) of the 2009 edition];
- ADD the requirements for analytical balance (see 5.3.4 of this document);
- MODIFY the gas chromatography-mass spectrometry analysis conditions (see 5.4
of this document, 4.4.2 of the 2009 edition);
- MODIFY the method for preparing standard solutions (see 5.5.1, 5.5.2, 5.5.3 of
this document, 4.2 of the 2009 edition);
- MODIFY the method for preparing sample solutions (see 5.5.4 of this document,
4.4.1 of the 2009 edition);
- ADD the provisions for the maximum deviation of the relative ion abundance of
characteristic ions in qualitative determination (see Table 2 of this document);
- MODIFY the detection limit and recovery rate (see 6.1, 6.2 of this document, 5.1,
5.2 of the 2009 edition);
- MODIFY the content of the test report (see Clause 7 of this document, Clause 6 of
the 2009 edition).
Attention is drawn to the possibility that some of the elements of this document may be
the subject of patent rights. The issuing authority of this document shall not be held
responsible for identifying any or all such patent rights.
This document was proposed by China Petroleum and Chemical Industry Federation.
This document shall be under the jurisdiction of National Technical Committee on
Dyestuff of Standardization Administration of China (SAC/TC 134).
Determination of the content of phthalate in textile dyeing
and finishing auxiliaries
WARNING -- People who use this document shall have practical experience in
regular laboratory work. This document does not point out all possible safety
issues. Users are responsible for taking appropriate safety and health measures
and ensuring that the conditions stipulated by relevant national laws and
regulations are met.
1 Scope
This document describes the gas chromatography-mass spectrometry (GC/MS)
determination method for 24 kinds of phthalates in textile dyeing and finishing
auxiliaries.
This document applies to the determination of phthalates in various categories of textile
dyeing and finishing auxiliaries.
NOTE: The names of the 24 kinds of phthalates are shown in Annex A.
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 6682-2008 Water for analytical laboratory use - Specification and test methods
GB/T 8170-2008 Rules of rounding off for numerical values & 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 extraction with n-hexane-acetone mixed solvent or other suitable solvent, the
textile dyeing and finishing auxiliary samples are determined by gas chromatography-
mass spectrometry, the retention time and characteristic ions are used for qualitative
analysis, and the external standard method of the peak area of quantitative ions is used
for quantitative analysis.
5 Determination method
5.1 General provisions
Unless otherwise specified, only reagents confirmed as analytical reagent and grade 3
water specified in GB/T 6682-2008 are used. The test results are determined according
to the rounded value comparison method in 4.3.3 of GB/T 8170-2008.
5.2 Reagents and materials
5.2.1 Phthalate standard substances: meet the requirements of Annex A, and the content
is ≥ 98 % (mass fraction).
5.2.2 n-hexane: chromatographically pure.
5.2.3 Acetone: chromatographically pure.
5.2.4 n-hexane-acetone mixed solvent: the volume ratio of n-hexane to acetone is 1:1.
5.3 Instruments and equipment
5.3.1 Gas chromatograph-mass spectrometer (GC/MS): equipped with electron impact
(EI) ion source.
5.3.2 Chromatographic column: 50 % phenylmethylpolysiloxane stationary phase, such
as 30 m × 0.25 mm × 0.25 μm or equivalent chromatographic column.
5.3.3 Micro-syringe or autosampler.
5.3.4 Analytical balance: accuracy of 0.01 mg.
5.3.5 Extractor: made of hard glass, tubular, with ground mouth and bottle stopper, 25
mL.
5.3.6 Ultrasonic generator: working frequency of 40 kHz.
5.3.7 Polytetrafluoroethylene membrane filter head: 0.45 μm.
5.3.8 Centrifuge tube with ground mouth and stopper: 10 mL.
5.3.9 Centrifuge: 4000 r/min.
5.4 Gas chromatography-mass spectrometry analysis conditions
5.5.2 Phthalate single standard intermediate solution
Pipette 0.1 mL of each phthalate single standard stock solution into a 10 mL volumetric
flask, dilute to the mark with n-hexane or other suitable solvents to prepare a single
standard intermediate solution. The mass concentration of diisononyl phthalate (DINP)
and diisodecyl phthalate (DIDP) solutions is 50 mg/L, and the mass concentration of
the remaining substances is 10 mg/L.
NOTE: The standard intermediate solution is sealed and stored in a refrigerator at 0 ℃ ~ 4 ℃, and
the validity period is 6 months.
5.5.3 Standard working solution
Use the phthalate single standard intermediate solution to prepare a single standard
working solution or a mixed standard working solution. It can prepare the appropriate
concentration according to the content of the target substance in the sample.
NOTE: The standard working solution is sealed and stored in a refrigerator at 0 ℃ ~ 4 ℃, and the
validity period is 1 month.
5.5.4 Sample solution
Weigh 1.0 g of sample (accurate to 0.0001 g), place in an extractor, accurately add 10.0
mL of n-hexane-acetone mixed solution or other suitable extractant, shake well, and
extract in an ultrasonic generator for 20 minutes and ensure complete extraction. Use a
0.45 μm polytetrafluoroethylene membrane filter to inject and filter the extract into a
small sample bottle for chromatographic analysis.
If the sample is water-soluble, when necessary, add 2 mL of water to the sample first,
shake evenly, and then add 10.0 mL of n-hexane-acetone mixed solution or other
suitable extractant; if the sample is turbid after ultrasonic extraction, use a centrifugal
device to centrifuge until the layers are separated and then take the upper clear liquid
for analysis.
Prepare a blank sample at the same time.
5.6 Determination
5.6.1 Qualitative analysis
By comparing the retention time and relative abundance of characteristic ions of the
target compound in the sample and the standard working solution, it requires the signal-
to-noise ratio (S/N) of the chromatographic peak of the tested specific phthalate to be
greater than 3, the retention time of the specific phthalate in the sample is consistent
with the retention time of the target compound in the standard solution, and the
corresponding characteristic ion abundance ratio of the specific phthalate in the tested
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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