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GB/T 29493.4-2023 English PDF (GBT29493.4-2023)

GB/T 29493.4-2023 English PDF (GBT29493.4-2023)

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GB/T 29493.4-2023: Determination of harmful substances in textile dyeing and finishing auxiliaries - Part 4: Determination of polycyclic aromatic hydrocarbons(PAHs)

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.
GB/T 29493.4-2023
GB
NATIONAL STANDARD OF THE
PEOPLE 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 ??L 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 ??L 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 ??m, 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 ??m, 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 ??L;
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;
??is - The value of the mass concentration of polycyclic aromatic hydrocarbon compounds in the standard working solution, in micrograms per liter (??g/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.

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