SN/T 5244-2020Import and export textile processing detergents. Determination of alkyl phenol and alkyl phenol polyoxyethylene ether. High performance liquid chromatography (English PDF)

7.1 Sample preparation

Mix the sample thoroughly before sampling, and take out 5.0 g~10.0 g sample.

Note. viscous samples should be shaken sufficiently to ensure uniform mixing.

7.2 Extraction

Weigh 1.0 g of the above sample, accurate to 0.01 g, add it to the centrifuge tube (6.3), add 10 mL directly to the weighed sample Methanol (5.1), seal and shake and mix, ultrasonically extract at (60 ± 1) °C for 30 min, centrifuge and transfer the supernatant extract to 25 mL Volumetric flask (6.5), add 10 mL of methanol (5.1) to the centrifuge tube (6.3) and shake well to wash, after centrifugation, transfer the supernatant for extraction Fill it to the volumetric flask (6.5), and use methanol (5.1) to make the volume constant. Dilute the sample solution 4 times and transfer it to a sample bottle for liquid chromatography measurement.

7.3 Determination

7.3.1 Liquid chromatography conditions

Since the test results depend on the instrument used, it is impossible to give general parameters for liquid chromatography analysis. The set parameters shall be guaranteed SN/T 5244-2020 to prove that the measured component can be effectively separated from other components during chromatographic determination, the following parameters prove to be feasible.

a) Chromatographic column. C18 reverse phase column, Diamonsil C18 (2), 3.0 mm × 150 mm, 3 µm or equivalent 1).

b) Column temperature. 35 °C.

c) Mobile phase A. methanol; mobile phase B. acetonitrile; mobile phase C. water. See Table 1 for gradient elution.

d) Fluorescence detector. excitation wavelength 230 nm, emission wavelength 296 nm.

e) Flow rate. 0.50 mL/min.

f) Injection volume. 10 µL.

7.3.2 Liquid chromatography determination

The standard solution (5.9) and the sample solution are interspersed with equal volumes, and the standard solution and the sample solution to be tested contain alkylphenol and alkylphenol polyoxyethylene the response value of the enether should be within the linear range of the standard solution, otherwise it needs to be diluted to a suitable concentration before measurement. The color of the sample to be tested the deviation between the retention time of the peak and the retention time of the corresponding chromatographic peak of the standard solution is within ±2.5%, and the external standard method is used according to the area of the chromatographic peak Quantitative.

Analyze the standard solution (5.9) according to the above analysis conditions (7.3.1), and the obtained alkylphenol and alkylphenol polyoxyethylene See Appendix A for the liquid chromatogram of ether.

7.4 Confirmation of results

7.4.1 Confirmation conditions

The sample solution and standard solution with a positive result detected in 7.3.2 are carried out by the following two or one of the following liquid chromatographic separation and analysis methods Confirmation of the retention time comparison of the detected substance, the deviation of the retention time between the chromatographic peak of the detected substance and the chromatographic peak of the corresponding standard solution Within ±2.5%, it can be regarded as the same substance.

Since the test results depend on the instrument used, it is impossible to give general parameters for liquid chromatography analysis. The set parameters shall be guaranteed Prove that the measured component can be effectively separated from other components during chromatographic determination. The parameters given below prove to be feasible.

7.4.2 Confirmation method of C8 column

C8 column analysis conditions include.

a) Chromatographic column. C8 reverse phase column, Diamonsil C8 (2), 3.0 mm × 150 mm, 3 µm or equivalent

b) Chromatographic column temperature. 35 °C.

c) Mobile phase A. methanol; mobile phase B. acetonitrile; mobile phase C. water. See Table 2 for gradient elution.

1) It is an example of a suitable commercially available product. This information is given for the convenience of users of this standard, and does not mean approval of this product. If other equivalent products have with the same effect, these equivalent products can be used.

SN/T 5244-2020

d) Fluorescence detector. excitation wavelength. 230 nm; emission wavelength. 296 nm.

e) Flow rate. 0.45 mL/min.

f) Injection volume. 10 µL.

7.4.3 Confirmation method of phenyl chromatographic column

The analysis conditions of phenyl chromatographic column include.

a) Chromatographic column. phenyl column, Inertsil Ph-3, 3.0 mm × 150 mm, 3 µm or equivalent 2).

b) Chromatographic column temperature. 35 °C.

c) Mobile phase A. methanol; mobile phase B. acetonitrile; mobile phase C. water. See Table 3 for gradient elution.

d) Fluorescence detector. excitation wavelength. 230 nm; emission wavelength. 296 nm.

e) Flow rate. 0.50 mL/min.

f) Injection volume. 10 µL.

7.5 Blank test

Except that no sample is added, the above determination steps (7.2-7.3) are carried out.

7.6 Result calculation

Calculate the content of alkylphenol and alkylphenol polyoxyethylene ether in the sample according to formula (1).

2) It is an example of a suitable commercially available product. This information is given for the convenience of users of this standard, and does not mean approval of this product. If other equivalent products have with the same effect, these equivalent products can be used.

X--The content of alkyl phenol or alkyl phenol polyoxyethylene ether in the sample, in milligrams per kilogram (mg/kg);

Ai--the chromatographic peak area value of alkyl phenol or alkyl phenol polyoxyethylene ether in the sample extract;

A0--the chromatographic peak area value of alkyl phenol or alkyl phenol polyoxyethylene ether in blank sample;

cs--The concentration of alkyl phenol or alkyl phenol polyoxyethylene ether in the standard working solution, in milligrams per liter (mg/L);

V--The final constant volume of the sample solution, in milliliters (mL);

As--the chromatographic peak area value of alkyl phenol or alkyl phenol polyoxyethylene ether in standard working solution;

m--The sample volume represented by the final sample solution, in grams (g).

7.7 Presentation of results

The calculation of the test result is accurate to one decimal place, and the rounding of the value shall be carried out in accordance with the provisions of GB/T 8170.

8.1 Lower limit of determination

Methods The detection limit of octylphenol, nonylphenol, octylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether in samples 10 mg/kg.

8.2 Recovery rate

The method recovery rate is 80% ~ 120%.