GB/T 47489-2026Test method for synthetic leather - Determination of short chain and medium chain chlorinated paraffins (English PDF)

5.3 Short-chain chlorinated paraffin standard solution

5.3.1 Short-chain chlorinated paraffin standard solution with a chlorine content of 55.5%. 100 µg/mL, solvent is n-hexane.

5.3.2 Short-chain chlorinated paraffin standard solution with a chlorine content of 63.0%. 100 µg/mL, solvent is n-hexane.

5.4 Medium-chain chlorinated paraffin standard solution

5.4.1 Medium-chain chlorinated paraffin standard solution with a chlorine content of 52.0%. 100 µg/mL, solvent is n-hexane.

5.4.2 Medium-chain chlorinated paraffin standard solution with a chlorine content of 57.0%. 100 µg/mL, solvent is n-hexane.

8.1.1 Sample Preparation and Analysis

8.1.1.1 Prepare a calibration working solution (50 µg/mL) of short-chain chlorinated paraffin with a chlorine content of 59.0%. Take 533 µL of a short-chain chlorinated paraffin standard solution (5.3.1) with a chlorine content of 55.5% and 467 µL of a short-chain chlorinated paraffin standard solution (5.3.1) with a chlorine content of 63.0%, respectively. Pour the chlorinated paraffin standard solution (5.3.2) into a 2 mL volumetric flask, add 20 µL of internal standard solution (5.2), and n-hexane (5.1). Set the appearance.

8.1.1.2 Sample Extraction Weigh (0.500±0.001) g of sample into a glass sample vial using an analytical balance (6.1), and add

9.9 mL of n-hexane (5.1) and Add 100 µL of internal standard solution (5.2), seal the glass sample vial, and shake until the sample is completely wetted. Place in an ultrasonic water bath at (50±5)°C. Extract (60±2) min in (6.3) and then cool to room temperature.

8.1.1.3 Measurement The calibration working solution and... were analyzed using a gas chromatography-mass spectrometry (GC-ECNI-MS) equipped with an electron capture negative chemical ion source (6.4). The extract was tested. Because test results depend on the instrument used, it is impossible to provide universal parameters for instrumental analysis. The parameters set should ensure that the measured... The components were effectively separated and tested. The parameters given in Table 1 have been proven feasible; adjustments can be made to the parameters for different instrument models to obtain the desired results. Optimal results.

8.1.2 Qualitative and Quantitative Analysis

8.1.2.1 Qualitative Analysis By comparing the retention time, peak shape, and... Qualitative analysis was performed using the ratio of ion abundance to qualitative and quantitative ion abundance. Appendix A provides a reference example for evaluating the peak shape of short-chain chlorinated paraffins. After confirming the presence of short-chain chlorinated paraffins in the sample, quantification was performed using the internal standard method.

8.1.2.2 Quantitative Analysis The sum of the quantitative ion peak areas in the calibration working solution of short-chain chlorinated paraffin with a chlorine content of 59.0% was used to establish a calibration method with respect to the mass concentration. The curve was used to perform quantitative calculations on the sample extraction solution using the internal standard method. The total ion chromatogram (TIC chromatogram) of the sample extraction solution should be obtained from the abundance of the calibrated working solution containing short-chain chlorinated paraffin with a chlorine content of 59.0%. If the sample is outside the specified range, the sample extraction solution should be diluted and the test repeated. The quantitative ion abundance ratio of the sample and the quantitative ion abundance ratio of the calibration working solution of short-chain chlorinated paraffin with a chlorine content of 59.0% should be controlled. The deviation is within ±30%. A short-chain chlorinated paraffin calibration working solution with a chlorine content of 59.0% was added at the end of the sequence or after up to 10 samples as a quality control. For sample preparation and quality control, the test results deviation should be within ±20%. If it exceeds this range, the calibration curve should be re-established and the test should be repeated. The new batch of samples was tested.

8.1.2.3 Interference When the content of medium-chain chlorinated paraffins is high, it can interfere with the quantitative determination of C12Cl7 ions (m/z 375). In this case, interchangeable determination methods can be used. The quantitative and qualitative ions should be identified and noted in the test report.

8.1.2.4 Calculation A linear regression function is established using the ratios (ASCCP-S/Aint.Std-S) and (rhoSCCP-S/rhoint.Std-S), as shown in formula (1).

8.2.1 Sample Preparation and Analysis

8.2.1.1 Prepare a calibration working solution (50 µg/mL) of medium-chain chlorinated paraffin with a chlorine content of 55.0%. Take 400 µL of a medium-chain chlorinated paraffin standard solution with a chlorine content of 52.0% (5.4.1) and 600 µL of a medium-chain chlorinated paraffin standard solution with a chlorine content of 57.0%, respectively. Pour the chlorinated paraffin standard solution (5.4.2) into a 2 mL volumetric flask, add 20 µL of internal standard solution (5.2), and n-hexane (5.1). Set the appearance.

8.2.1.2 Extraction Weigh (0.500±0.001) g of sample into a glass sample vial using an analytical balance (6.1), and add

9.9 mL of n-hexane (5.1) and Add 100 µL of internal standard solution (5.2), seal the glass sample vial, and shake until the sample is completely wetted. Place in an ultrasonic water bath at (50±5)°C. Extract (60±2) min in (6.3) and then cool to room temperature.

8.2.1.3 Measurement The calibration working solution and... were analyzed using a gas chromatography-mass spectrometry (GC-ECNI-MS) equipped with an electron capture negative chemical ion source (6.4). The extract was tested. Because test results depend on the instrument used, it is impossible to provide universal parameters for instrumental analysis. The parameters set should ensure that the measured... The components were effectively separated and tested. The parameters given in Table 1 have been proven feasible; adjustments can be made to the parameters for different instrument models to obtain the desired results. Optimal results.

8.2.2 Qualitative and Quantitative Analysis

8.2.2.1 Qualitative Analysis By comparing the retention time, peak shape, and... Qualitative analysis was performed using the ratio of ion abundance to qualitative and quantitative ion abundance. Appendix B provides a reference example for the peak shape evaluation of medium-chain chlorinated paraffins. After confirming the presence of medium-chain chlorinated paraffins in the sample, quantification was performed using the internal standard method.

8.2.2.2 Quantitative Analysis The sum of the quantitative ion peak areas in the calibration working solution of medium-chain chlorinated paraffin with a chlorine content of 55.0% was used to establish a calibration method with respect to the mass concentration. The curve was used to perform quantitative calculations on the sample extraction solution using the internal standard method. The total ion chromatogram (TIC chromatogram) of the sample extraction solution should be obtained by calibrating the abundance of the working solution in medium-chain chlorinated paraffin with a chlorine content of 55.0%. If the sample is outside the specified range, the sample extraction solution should be diluted and the test repeated. The quantitative ion abundance ratio of the sample and the quantitative ion abundance ratio of the calibration working solution of medium-chain chlorinated paraffin with a chlorine content of 55.0% should be controlled. The deviation is within ±30%. Only when the peak areas of the quantitative ions (m/z 431) and (m/z 445) are greater than the peak areas of the quantitative ions (m/z 403) or (m/z 417) Quantitative analysis should only be performed when the peak shape of a sample is 10% and there is no significant difference compared to the standard spectrum. The response values of the quantitative ions (m/z 445) and (m/z 447) were very low and the peak shapes were not significant enough. If other quantitative ions had typical... If the peak shape can be determined for detection, then the retention time ranges of the quantitative ion (m/z 445) and the quantitative ion (m/z 447) in the standard peak diagram should be considered. Integrate the chromatogram. Add a 55.0% chlorinated paraffin calibration working solution as a quality control at the end of the sequence or after up to 10 samples. For sample preparation and quality control, the test results deviation should be within ±20%. If it exceeds this range, the calibration curve should be re-established and the test should be repeated. The new batch of samples was tested.

8.2.2.3 Interference 8.2.2.3.1 The quantitative ion (m/z 445) response value of C17Cl7 is very low, and its retention time is similar to that of short-chain paraffin chloride ions. If interference from short-chain chlorinated paraffins is detected, quantitative analysis of the C17Cl7 ion (m/z 445) should not be performed. 8.2.2.3.2 When the content of short-chain chlorinated paraffins exceeds 1%, it will seriously interfere with the determination of the content of medium-chain chlorinated paraffins. In this case... The following should be reported. the content of short-chain chlorinated paraffins, with a note stating. "The content of medium-chain chlorinated paraffins is affected by short-chain chlorinated paraffins exceeding 1%." "Unable to determine".

8.2.2.4 Calculation A linear regression function is established using the ratios (AMCCP-S/Aint.Std-S) and (rhoMCCP-S/rhoint.Std-S), as shown in formula (4).

9.Detection Limit The detection limit for this test method is 100 mg/kg.

10 Test Report The test report should include at least the following.

a) This document number;

b) Sample source and description;

c) Test results;

d) Any deviation from this document;

e) Anomalies observed during testing;

g) Other matters that need to be explained.