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Determination of harmful substances in textile dyeing and finishing auxiliaries - Part 4: Determination of polycyclic aromatic hydrocarbons(PAHs)
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GB/T 29493.4-2023
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GB/T 29493.4-2013 | English | 399 |
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Determination of harmful substances in textile dyeing and finishing auxiliaries -- Part 4: Determination of polycyclic aromatic hydrocarbons -- GC/MS method
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GB/T 29493.4-2013
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Standard ID | GB/T 29493.4-2023 (GB/T29493.4-2023) | Description (Translated English) | Determination of harmful substances in textile dyeing and finishing auxiliaries - Part 4: Determination of polycyclic aromatic hydrocarbons(PAHs) | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | G70 | Classification of International Standard | 71.100.40 | Word Count Estimation | 14,112 | Date of Issue | 2023-09-07 | Date of Implementation | 2024-04-01 | Older Standard (superseded by this standard) | GB/T 29493.4-2013 | Drafting Organization | Shanghai Tianxiang Quality Technical Service Co., Ltd., Zhejiang Chuanhua Functional New Materials Co., Ltd., Chuanhua Zhilian Co., Ltd., Shenghong Group Co., Ltd., Zhangjiagang Debao Chemical Co., Ltd., Fujian Fiber Inspection Center, Hangzhou Chuanhua Fine Chemicals Ltd. | Administrative Organization | National Dyestuff Standardization Technical Committee (SAC/TC 134) | Proposing organization | China Petroleum and Chemical Industry Federation | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Administration | Standard ID | GB/T 29493.4-2013 (GB/T29493.4-2013) | Description (Translated English) | Determination of harmful substances in textile dyeing and finishing auxiliaries. Part 4: Determination of polycyclic aromatic hydrocarbons. GC/MS method | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | G70 | Classification of International Standard | 71.100.40 | Word Count Estimation | 10,132 | Quoted Standard | GB/T 8170-2008 | Drafting Organization | Intertek Testing Services Ltd. Shanghai | Administrative Organization | National Standardization Technical Committee dye auxiliaries Technical Committee | Regulation (derived from) | National Standards Bulletin 2013 No. 2 | Proposing organization | China Petroleum and Chemical Industry Federation | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | Summary | This standard specifies the textile dyeing and finishing auxiliaries polycyclic aromatic compounds by gas chromatography mass spectrometry. This section applies to all types of textile dyeing and finishing auxiliaries in the determination of polycyclic ar |
GB/T 29493.4-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
CCS G 70
Replacing GB/T 29493.4-2013
Determination of harmful materials in textile dyeing and
finishing auxiliaries - Part 4: Determination of polycyclic
aromatic hydrocarbons (PAHs)
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 ... 8
7 Test steps ... 9
8 Test data processing ... 11
9 Lower limit of determination, recovery rate, precision ... 11
10 test report ... 12
Annex A (normative) Basic information on PAH compounds and internal standard
materials tested in this document ... 13
Annex B (informative) Quantitative and qualitative ion information for PAH
compounds and internal standard materials ... 15
Annex C (informative) Gas chromatography-mass spectrometry total ion
chromatogram of polycyclic aromatic hydrocarbon compounds and internal standard
materials ... 17
Determination of harmful materials in textile dyeing and
finishing auxiliaries - Part 4: Determination of polycyclic
aromatic hydrocarbons (PAHs)
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 PAH compounds in textile
dyeing and finishing auxiliaries using gas chromatography-mass spectrometry (GC-
MS).
This document is applicable to the determination of 24 polycyclic aromatic
hydrocarbon 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 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
Toluene is used to conduct ultrasonic extraction of polycyclic aromatic hydrocarbons
in the sample. Determine by gas chromatography-mass spectrometry. Use the internal
standard method to quantify.
5 Reagents or materials
Unless otherwise specified, only use the confirmed analytically-pure reagents.
5.1 Toluene.
5.2 Polycyclic aromatic hydrocarbons standard materials: see Table A.1. No. 9, No. 11,
No. 21~ No. 24 in Table A.1: Purity (mass fraction) ≥ 99%.
5.3 Internal standard material: Purity (mass fraction) ≥99%, see Table A.2.
5.4 Standard stock solutions of 18 kinds of polycyclic aromatic hydrocarbons (see No.
1 to No. 8, No. 10, No. 12 to No. 20 in Table A.1), 1000 mg/L: commercially available
standard products.
NOTE: Refer to the relevant certificates for the storage environment and validity period of
commercially available standard products.
5.5 Single standard stock solutions of 6 polycyclic aromatic hydrocarbons (see No. 9,
No. 11, No. 21 to No. 24 in Table A.1), 1000 mg/L: Accurately weigh 10 mg (accurate
to 0.1mg) of 1-methylpyrene, cyclopentene [c,d] pyrene, dibenzo [a,l] pyrene,
dibenzo [a,e] pyrene, dibenzo [a,i] pyrene and dibenzo [a,h] pyrene.
Dissolve with toluene (5.1) and make the volume to 10 mL. Mix well.
NOTE: The 6 single-standard stock solutions of polycyclic aromatic hydrocarbons are stored in the
dark at 0℃~4℃. Validity period is 12 months.
5.6 PAH primary mixed standard intermediate solution: Accurately pipette 100 μL of
18 polycyclic aromatic hydrocarbons standard stock solutions (see 5.4) and 1-
methylpyrene, cyclopentene [c,d] pyrene single standard stock solutions (see 5.5),
400 μL of dibenzo [a,l] pyrene, dibenzo [a,e] pyrene, dibenzo [a,i] pyrene,
dibenzo [a,h] pyrene single standard stock solution (see 5.5) in a 10 mL volumetric
flask. Set to the volume with toluene (5.1), so as to obtain first-level mixed standard
intermediate solution, in which the mass concentration of dibenzo [a,l] pyrene,
dibenzo [a,e] pyrene, dibenzo [a,i] pyrene and dibenzo [a,h] pyrene is 40
mg/L; the mass concentration of the remaining 20 polycyclic aromatic hydrocarbons is
10 mg/L.
NOTE: The primary mixed standard intermediate solution of polycyclic aromatic hydrocarbons
shall be stored in the dark at 0℃~4℃. Validity period is 3 months.
5.7 Polycyclic aromatic hydrocarbon secondary mixed standard intermediate solution:
Accurately pipet 1 mL of the PAH primary mixed standard intermediate solution (see
5.6) into a 10 mL volumetric flask. Set to the volume with toluene (5.1) and mix evenly,
so as to obtain secondary mixed standard intermediate solution, in which the mass
concentration of dibenzo [a,l] pyrene, dibenzo [a,e] pyrene, dibenzo [a,i]
6.2 Temperature-controlled ultrasonic water bath: operating frequency is 40 kHz,
temperature is controllable at (60±5)℃.
6.3 Analytical balance: sensitivity is 0.1 mg.
6.4 Extractor: stoppered glass test tube, 50mL.
6.5 Volumetric flasks: 10 mL, 100 mL, 500 mL.
6.6 Needle filter head: 0.45 μm, nylon.
7 Test steps
7.1 Extraction
Accurately weigh 0.50 g of specimen (accurate to 0.001 g) and place it in the extractor
(6.4). Accurately add 20 mL of toluene solution containing internal standard (see 5.11).
Seal with plug. Place the extractor in a temperature-controlled ultrasonic water bath
(6.2). After extraction at (60±5)℃ for (60±5) min, cool to room temperature. Use the
needle filter head (6.6) to filter the sample solution into the sample bottle. Perform gas
chromatography-mass spectrometry analysis.
7.2 Analysis method
7.2.1 Analysis conditions
Since test results depend on the instrument used, it is not possible to give universal
parameters for chromatographic analysis. The set parameters shall ensure that the
component being measured can be effectively separated from other components during
chromatographic determination. The parameters listed below prove to be feasible:
a) Chromatographic column: PAH special column, 20 m × 0.18 mm × 0.14 μm, or
equivalent;
b) Inlet temperature: 320℃;
c) Mass spectrometry interface temperature: 320℃;
d) Carrier gas: helium, purity (volume fraction) ≥99.999%;
e) Carrier gas flow rate: 1.0 mL/min;
f) Injection volume: 1.0 μL;
g) Injection method: splitless injection;
h) Column temperature:
8 Test data processing
8.1 Result calculation
The determination results are expressed as the testing results of various polycyclic
aromatic hydrocarbon compounds.
The content of various polycyclic aromatic hydrocarbon compounds in the specimen is
calculated as (Xi). Values are expressed in milligrams per kilogram (mg/kg). Calculate
according to formula (1):
Where,
Ai - The numerical value of the peak area of polycyclic aromatic hydrocarbon
compounds in the specimen solution;
ρis - The value of the mass concentration of polycyclic aromatic hydrocarbon
compounds in the standard working solution, in micrograms per liter (μg/L);
V - The value of the volume of toluene used for ultrasonic extraction, in milliliters (mL);
Aisc - The value of the peak area of the internal standard in the standard working solution;
Ais - The value of the peak area of polycyclic aromatic hydrocarbon compounds in the
standard working solution;
m - The value of the sample mass, in grams (g);
Aiss - The value of the peak area of the internal standard material in the specimen
solution;
f - The dilution factor.
8.2 Result expression
The calculation results are expressed as the arithmetic mean of two parallel
determination results. Round to one decimal place 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 dibenzo [a,l] pyrene, dibenzo [a,e] pyrene, dibenzo
[a,i] pyrene and dibenzo [a,h] pyrene in this document is 0.8 mg/ kg. The lower limit of
determination of the remaining 20 PAHs is 0.2 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.
......
GB/T 29493.4-2013
Determination of harmful substances in textile dyeing and finishing auxiliaries.Part 4. Determination of polycyclic aromatic hydrocarbons.GC/MS method
ICS 71.100.40
G70
National Standards of People's Republic of China
Determination of the textile dyeing and finishing auxiliaries harmful substances
Part 4. polycyclic aromatic compounds (PAHs)
Gas chromatography - mass spectrometry
finishingauxiliaries-Part 4. Determinationofpolycyclic
Issued on. 2013-02-07
2013-09-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
GB/T 29493 "textile dyeing and finishing auxiliaries of harmful substances Determination" is divided into nine sections.
--- Part 1. Determination of polybrominated biphenyls and polybrominated diphenyl ethers by gas chromatography - mass spectrometry;
--- Part 2. perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) High performance liquid chromatography - mass
Spectroscopy;
--- Part 3. organotin compounds by gas chromatography - mass spectrometry;
--- Part 4. polycyclic aromatic compounds (PAHs) by gas chromatography - mass spectrometry;
--- Part 5. Determination of the formaldehyde content of the emulsion polymer free;
--- Part 6. polyurethane prepolymer isocyanate determination of the ester group content;
--- Part 7. polyurethane coating finishing agent diisocyanate determination ester monomer;
--- Part 8. Determination of acrylic products in the residual monomers;
--- Part 9. Determination of acrylamide.
This is Part 4 GB/T 29493 of.
This section drafted in accordance with GB/T 1.1-2009 given rules.
This part is proposed by the China Petroleum and Chemical Industry Association.
This part of the National Standardization Technical Committee of dye auxiliaries Technical Committee (SAC/TC134/SC1) centralized.
This section drafted by. Intertek Testing Services Limited Shanghai, Zhejiang Chuan Co., Ltd., Foshan City, the mass of fine USI
Chemical Co., Ltd.
The main drafters of this part. such as Chen, Wang Jianping, Sheqiong Lei, Zhao Ting, Zhao Mei, Wang Shengpeng, Mo Gang.
Determination of the textile dyeing and finishing auxiliaries harmful substances
Part 4. polycyclic aromatic compounds (PAHs)
Gas chromatography - mass spectrometry
1 Scope
GB/T 29493 provisions of this part of the textile dyeing and finishing auxiliaries polycyclic aromatic compounds by gas chromatography - mass spectrometry method.
This section applies to all types of textile dyeing assay polycyclic aromatic compound additives.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein
Member. For undated references, the latest edition (including any amendments) applies to this document.
GB/T 8170-2008 revised value represents about rules and limit values and judgment
3 Terms and Definitions
The following terms and definitions apply to this document.
3.1
Polycyclic aromatic compound polycyclicaromatichydrocarbons; PAHs
Containing two or more fused aromatic hydrocarbon aromatic ring. The ring may also have a short alkyl or cycloalkyl substituent.
Note. The 16 kinds of polycyclic aromatic compounds in this section measured in 1979 by the US Environmental Protection Agency (EnvironmentalProtectionAgency, EPA)
And set out in regulation.
Principle 4
With toluene sample of polycyclic aromatic compounds ultrasonic extraction, gas chromatography - mass spectrometry separation (GC/MSD)
And testing, internal standard.
5 Reagents and materials
Unless otherwise specified, use only recognized as analytical reagents.
5.1 toluene.
5.2 polycyclic aromatic compounds standards (see Table 1). Commercially mixed standard stock solution of 2000mg/L, the standard stock solution to save environment
See valid and relevant certificates.
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