SN/T 3587-2016_English: PDF (SN/T3587-2016)
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SN/T 3587-2016 | English | 165 |
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Textiles for import and export--Determination of residual admides solvent--Gas chromatography-mass spectrometry method
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SN/T 3587-2016
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SN/T 3587-2013 | English | 279 |
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Determination of N, N-dimethylformamide and N, N-dimethylacetamide in textile for import and export. Gas chromatography-Mass method
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SN/T 3587-2013
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Standard ID | SN/T 3587-2016 (SN/T3587-2016) | Description (Translated English) | Textiles for import and export--Determination of residual admides solvent--Gas chromatography-mass spectrometry method | Sector / Industry | Commodity Inspection Standard (Recommended) | Classification of Chinese Standard | W55 | Classification of International Standard | 59.080.01 | Word Count Estimation | 8,846 | Date of Issue | 2016-06-28 | Date of Implementation | 2017-02-01 | Older Standard (superseded by this standard) | SN/T 3587-2013 | Drafting Organization | Shenzhen Inspection and Quarantine Science Research Institute, the People's Republic of China Shenzhen Entry-Exit Inspection and Quarantine Bureau | Administrative Organization | National Certification and Accreditation Administration Committee | Regulation (derived from) | State-Quality-Inspection-Accredidation [2016] No.318 | Proposing organization | National Certification and Accreditation Administration Committee | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China | Standard ID | SN/T 3587-2013 (SN/T3587-2013) | Description (Translated English) | Determination of N, N-dimethylformamide and N, N-dimethylacetamide in textile for import and export. Gas chromatography-Mass method | Sector / Industry | Commodity Inspection Standard (Recommended) | Classification of Chinese Standard | W55 | Classification of International Standard | 59.080.01 | Word Count Estimation | 7,755 | Drafting Organization | People's Republic of China Putian Entry-Exit Inspection and Quarantine Bureau | Administrative Organization | National Certification and Accreditation Administration | Regulation (derived from) | National quality recognition (2013), No. 464; industry standard filing Notice No. 1 of 2014 (No. 169 overall) | Proposing organization | Certification and Accreditation Administration of the People's Republic of China | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China | Summary | This standard specifies the textile N. N-dimethylformamide and N, N-dimethylacetamide and the residual mass of a latent potential vapor detection colors. This standard applies to the determination of textiles. |
SN/T 3587-2016
SN
ENTRY-EXIT INSPECTION AND QUARANTINE STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
Replacing SN/T 3587-2013
Textiles for import and export - Determination of
residual admides solvent - Gas chromatography-mass
spectrometry method
ISSUED ON: JUNE 28, 2016
IMPLEMENTED ON: FEBRUARY 01, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and materials ... 4
4 Instruments and equipment... 5
5 Analytical procedures ... 5
6 Calculation of results ... 7
7 Low limit of determination ... 7
8 Recovery rate ... 8
9 Precision ... 8
10 Test report ... 8
Appendix A (Informative) Reference qualitative and quantitative ions for amide
compounds ... 9
Appendix B (Informative) Gas chromatography-mass spectrometry
chromatogram of amide standard substances ... 10
Textiles for import and export - Determination of
residual admides solvent - Gas chromatography-mass
spectrometry method
1 Scope
This standard specifies the gas chromatograph-mass spectrometry method, for
the detection of 5 residual amide solvents (see Appendix A) in textiles.
This standard applies to the determination of the 5 residual amide solvents in
various textile materials and their products.
2 Principle
The sample is ultrasonically extracted by methanol, concentrated to a constant
volume. The sample solution is measured by a gas chromatography-mass
spectrometer. It is subject to qualitative determination by full scan detection,
AND quantification by external standard method by the use of selective ion.
3 Reagents and materials
3.1 Methanol: Chromatographically pure.
3.2 The 5 types of amide standard materials: Purity ≥ 95%; please refer to
Appendix A.
3.3 Standard stock solution: Weigh the appropriate amount of amide standard
substance (3.2), respectively. Use methanol (3.1) to prepare standard stock
solution, which has a concentration of 1000 mL. Contain it in a brown bottle.
Note: The standard stock solution is stored in a refrigerator at 0 °C ~ 4 °C in the dark.
The validity period is 3 months.
3.4 Series of standard working solutions: Accurately pipette a certain volume of
standard stock solution (3.3) as needed. Use methanol (3.1) to dilute it into a
series of mixed standard working solutions of appropriate concentration.
Note: The standard working solution is prepared before use. The linear range, which
is measured under different working conditions by different instruments, is different.
The linearity of the concentration range of the standard solution of 5 amide compounds,
b) Column temperature: ;
c) Inlet temperature: 230 °C:
d) Temperature at the interface of mass spectrometer: 280 °C;
e) Temperature of ion source: 220 °C;
f) Quadrupole's temperature: 150 °C;
g) Ionization method: EI;
h) Ionization energy: 70 eV;
i) Injection volume: 1.0 µL;
j) Sampling mode: Pulse-split injection, which has a split ratio of 20:1;
k) Carrier gas: Helium (purity ≥ 99.999%), which has a flow rate 0.8 mL/min;
l) Solvent delay: 3 min;
m) Measurement method: Full scan (SCAN) and selective ion monitoring
(SIM) are performed at the same time. Refer to Appendix A for selective
ions.
5.2.2 Qualitative and quantitative analysis by gas chromatography/mass
spectrometry
According to the content of the analyte in the sample solution, select a standard
working solution, which has a similar concentration. The response values of the
amide compounds in BOTH the standard working solution AND the sample
solution to be tested shall be within the linear range of the instrument detection.
Standard working solution and sample solution are interleaved at equal volume,
for the purposes of determination.
This standard uses the full scan mode for qualitative; it uses selective ion
monitoring mode for quantitative. For the selection of qualitative ions and
quantitative ions, refer to Appendix A. BOTH the standard solution AND the
sample solution are tested according to the conditions specified in 5.2.1. If, in
the sample solution, there appears a peak, at the same retention time as the
standard solution, THEN, the selective ion shall be confirmed. Through
confirmation and analysis, if all of the following conditions are met [Translator
note: the sentences are restructured as follows]:
- The retention time of the chromatographic peak of the analyte is consistent
with that of the standard substance;
8 Recovery rate
Quantitatively add a standard solution, which has an appropriate known
concentration, into the specimen. Perform recovery rate analysis according to
5.2.1. The recovery rate of 5 types of amide compounds is 80% ~ 110%.
9 Precision
In the same laboratory, when the same operator uses the same equipment,
according to the same test method, to test the same tested object independently
in a short time, the absolute value of the two test results obtained is not greater
than 10% of the arithmetic mean of the two measured values, under the premise
of 95% confidence.
10 Test report
The test report shall at least provide the following:
a) Sample source and description;
b) The standards used;
c) The test method used;
d) Test results;
e) Any details that deviate from this standard.
......
SN/T 3587-2013
Determination of N, N-dimethylformamide and N, N-dimethylacetamide in textile for import and export. Gas chromatography-Mass method
People's Republic of China Entry-Exit Inspection and Quarantine Standards
Import and export of textiles in N, N- dimethylformamide and
N, N- dimethylacetamide Determination of GC-MS
DeterminationofN, N-dimethylformamideandN, N-dimethylacetamideintextile
Issued on. 2013-08-30
2014-03-01 implementation
People's Republic of China
The State Administration of Quality Supervision, Inspection and Quarantine released
Foreword
This standard was drafted in accordance with GB/T 1.1-2009 given rules.
This standard is proposed and managed by the National Certification and Accreditation Administration Committee.
This standard was drafted. Exit Inspection and Quarantine People's Republic of China Putian, Quanzhou, People's Republic of China Entry-Exit Inspection and
Quarantine Bureau.
The main drafters of this standard. Cheng group, Tongyu Gui, Lin Bifen, Huang Ping, Fang Guangwei, Liang Ming, forest, Li Yijun, Fu Junyuan, Chen Shaohua,
Zhang Baoxiu.
Import and export of textiles in N, N- dimethylformamide and
N, N- dimethylacetamide Determination of GC-MS
1 Scope
This standard specifies the textiles N, N- dimethylformamide and N, N- dimethylacetamide Residues by Gas Chromatography - Mass Spectrometry
method.
This standard applies to the determination of textiles.
Principle 2
N samples extracted with methylene chloride residues in an ultrasonic bath, of N- dimethylformamide and N, N- dimethylacetamide, and concentrated to volume
After the sample solution by gas chromatography - mass spectrometry to detect the use of qualitative full scan detection, select ion external standard.
3 Reagents and materials
Unless otherwise indicated, the reagents used were of analytical grade or higher purity reagents.
3.1 methylene chloride by gas chromatography - mass spectrometry examination without the presence of interference substances.
3.2 Methanol. chromatographically pure.
3.3 N, N- dimethylformamide (English name. N, N-Dimethylformamide, CAS number. 68-12-2, molecular formula. C3H7NO).
Purity ≥98%.
3.4 N, N- dimethylacetamide (English name. N, N-Dimethylacetamide, CAS number. 127-19-5 molecular formula. C4H9NO).
Purity ≥98%.
3.5 standard stock solution. Accurately weigh an appropriate amount of N, N- dimethylformamide and N, N- dimethylacetamide standards, respectively, with methanol
(3.2) formulated at a concentration of 1000μg/mL standard stock solution, put in a brown bottle.
NOTE. The standard stock solution at 0 ℃ ~ 4 ℃ refrigerator, valid for six months.
3.6 standard solution. diluted with methylene chloride mixed solution of appropriate concentration standard work needed.
NOTE. The standard working solution at 0 ℃ ~ 4 ℃ refrigerator, valid for three months.
3.7 graphite carbon column (250mg, 3mL). dichloromethane with 3mL activated graphite carbon column, and kept moist.
3.8 microporous membrane. nylon filters, 0.2μm.
4 instruments and equipment
4.1 Gas chromatography - mass spectrometry. with EI source.
4.2 Analysis of balance. a sense of the amount of 0.01mg and 0.01g.
4.3 ultrasonic cleaning. the operating frequency of 40kHz.
4.4 rotary evaporator.
4.5 Reactor. a tube with a screw cap (polytetrafluoroethylene gaskets), about 50mL, made of hard glass.
4.6 concentrated bottle. 150mL.
4.7 plug tube. 10mL.
......
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