GB/T 29493.4-2023 PDF in English
GB/T 29493.4-2023 (GB/T29493.4-2023, GBT 29493.4-2023, GBT29493.4-2023)
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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 29493.4-2013 | 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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Standards related to (historical): GB/T 29493.4-2023
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GB/T 29493.4-2023: PDF in English (GBT 29493.4-2023) 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.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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