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

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°C~4°C. 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°C~4°C. 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 Instruments and equipment

6.2 Temperature-controlled ultrasonic water bath: operating frequency is 40 kHz, temperature is controllable at (60±5)°C.

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

8 Test data processing

9 Lower limit of determination, recovery rate, precision

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. […]