SN/T 5236-2020Import and export textiles Determination of harmful dyes Liquid chromatography-high resolution mass spectrometry (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

1 Scope

This standard specifies the use of liquid chromatography-high resolution mass spectrometry (LC-HRMS) for the simultaneous determination of 46 hazardous dyes in textile products.

method.

This standard applies to the determination of 46 harmful dyes in textile products processed by printing and dyeing.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.

GB/T 6682 Analytical laboratory water specifications and test methods

3 Principle

The sample was heated and extracted with pyridine-aqueous solution as the extraction solvent, the supernatant was diluted, and then liquid chromatography-high resolution mass spectrometry (LC-HRMS) determination, external standard method quantification.

4 Reagents and materials

Unless otherwise stated, all reagents used are of analytical grade. The water is the first grade water that meets the requirements of GB/T 6682.

4.1 Acetonitrile. chromatographically pure.

4.2 Methanol. chromatographically pure.

4.3 Pyridine. excellent grade pure.

4.4 Ammonium acetate. chromatographically pure.

4.5 Formic acid. chromatographically pure.

4.6 Aqueous solution of ammonium acetate (0.385 g/L). accurately weigh 0.385 g of ammonium acetate (4.4) and dissolve in water, and transfer to a 1000 mL volumetric flask.

Constant volume with water.

4.7 Ammonium acetate aqueous solution (0.385 g/L, containing 0.01% formic acid). accurately weigh 0.385 g of ammonium acetate (4.4) and dissolve in water, and add 100 µL Formic acid (4.5), transfer to a 1000 mL volumetric flask, and dilute to volume with water.

4.8 Pyridine-aqueous solution (11, volume ratio). equal volume of pyridine (4.3) is mutually soluble in water and stored in a brown glass bottle.

4.9 Methanol-aqueous solution (11, volume ratio). equal volume of methanol (4.2) and water are mutually soluble.

4.10 46 kinds of dye standards. see Appendix A.

4.11 Standard stock solution. accurately weigh an appropriate amount of dye standard and dissolve it with the solvent listed in Appendix A to make an effective concentration of 100 mg/L Standard stock solution. The validity period of the standard stock solution is 12 months when stored in a refrigerator at -18 °C and protected from light.

4.12 Mixed standard working solution. accurately pipette an appropriate amount of standard stock solution and use methanol-aqueous solution (4.9) to prepare a concentration of 1 mg/L the mixed standard working solution of, or the standard working solution of other concentration can be prepared as needed. Stored in the refrigerator at -18 °C and protected from light, the validity period of the standard working solution is 1 month.

5 Apparatus and equipment

5.1 Liquid Chromatography-High Resolution Mass Spectrometer (LC-HRMS). Distributed Spray Ion Source (ESI).

5.2 Heating source. equipment that can generate a heat source of (100±2)°C, such as a water bath placed on an electric hot plate and heated to boiling.

5.3 Glass sample bottle. 40 mL with screw cap (with PTFE gasket).

5.4 Electronic balance. Sensitivity 0.01 g and 0.1 mg.

5.5 Microporous membrane. 0.22 µm, polytetrafluoroethylene.

6 Analysis steps

7 Result calculation

The harmful dye content in the sample is calculated according to formula (1). The calculation result needs to deduct the blank value.

8 Low limit of determination, recovery and precision

9 Test report

The test report should at least give the following contents.

a) Sample source and description;

b) Instruments and standards used;

c) Test results;

d) Any details that deviate from this standard;

e) Test date.

Appendix A

(Informative appendix) 46 harmful dyes

Table A.1 Information about 46 dye compounds

Appendix B

(Informative appendix) 46 dyes LC-HRMS conditions 1) B.1 Primary scan resolution. R=70 000 (FWHM at m/z.200).

B.2 Secondary scanning resolution. R=17 500 (FWHM at m/z.200).

B.3 First-level scanning range. m/z 150~1 000.

B.4 Spray voltage. 3.5 kV for positive ion mode and -2.9 kV for negative ion mode.

B.5 S-lens RF level. 50 V for positive ion mode and -50 V for negative ion mode.

B.6 Capillary temperature. 320 °C.

B.7 Sheath gas (N2) pressure. 2.76 × 10

5 Pa (ie 40 arb).

B.8 Auxiliary gas (N2) flow rate. 3.33 L/min (that is, 10 arb).

B.9 Atomizing gas temperature. 300 °C.

B.10 Collision mode...