Screening analysis of Dechlorane Plus and UV-328 by PY-GC/MS method [GC-QMS Application]

1. Introduction

2. Experiment

The standard samples for calibration curves of the DP and UV-328 ware prepared in the same way as MSTips No. 290 by using the resin matrix solution and mixed liquid standard samples as described in IEC 62321-8. Acrylonitrile Butadiene Styrene (ABS) was used for resin matrix. Calibration curves were prepared for each compound at concentrations of 100 ppm to 2000 ppm in the resin by varying concentrations of mixed liquid standard samples (addition amount 5 µL) furthermore reproducibility at lower concentration limit (100 ppm) was calculated and Instrument Detection Limit (IDL) was too. Additionally, each compound at concentration of 1000 ppm in Polystyrene (PS) and Polycarbonate (PC) moreover ABS were measured and their recovery rates were calculated by using quantitative value from the calibration curve. Insulating sticky tape and Impact absorption gel sheet ware used for the actual samples. Samples were cut with a knife and measured in put directly in an Eco-cup. The conditions of the instrument used for measuring were shown in Table 1.

Table 1. Measurement Condition

3. Results

3-1. Chromatograms and Calibration curves

SIM chromatograms of DP and UV-328 at concentration of 100 ppm in ABS were shown in Figure 1, Calibration curves of each compound draw by measuring pseudo-standard samples at concentration of 100, 200, 500, 1000, 2000 ppm in ABS were shown Figure 2. Incidentally, the area of 2 isomer peaks (syn-DP, anti-DP) were totaled. About linearity of calibration curves, good results were obtained, with coefficient of determination was more than 0.999.

Figure 1. SIM chromatograms of each compound at 100 ppm

Figure 2. Calibration curve of each compound

3-2. Reproducibility and Instrument Detection Limit

The relative standard deviation (%RSD) of quantitative values obtained by measuring sample in number of trials n=8 at concentration of lower limit in resin (100 ppm) and the calculated IDL were shown in Table 2. At each compound, good results were obtained, with %RSD was less than 5% and IDL was 10 ppm or less. Incidentally, IDL was calculated with t-value of t-test.

Table 2. Relative standard deviation of each compound andInstrument Detection Limit of each compound

3-3. Recovery rates of each compound in each resin matrix

TIC chromatograms of DP and UV-328 at concentration of 1000 ppm in ABS were shown in Figure 3. Recovery rates of each compound were evaluated by quantitative values obtained by measuring sample in number of trials n=8 at concentration in resin 1000 ppm were shown in Table 3. Average recovery rate of DP is 88～102 % and of UV-328 is 87～101 %, the result indicated that a screening analysis was adequate.

Figure 3. TICC chromatograms of each compound at 1000 ppm in ABS matrix sample

Table 3. Recoveryrates in each matrix sample

3-4 Measurement of Actual samples

Actual samples were measured in number of trials n=5 respectively. SIM chromatogram of DP from Insulating sticky tape and UV-328 from Impact absorption gel sheet were shown in Figure 4. %RSD calculated by using calibration curve were shown in Table 4. %RSD was less than 10 % at over a wide concentration range of approximately 85～1.3×10^5 ppm, the result indicates that a screening analysis was adequate.

Figure 4. SIM chromatograms of each compound at real sample

Table 4. Relative standard deviation of each compound

Conclusion

DP and UV-328 regulated by POPs were analyzed by using PY-GCMS method. Good results of linearity of calibration curve and reproducibility at concentration of lower limit were obtained. It was quite possible to screening analysis. Additionally, Good results of recovery rate of each resin matrix were obtained. So, it could be applied to actual samples.

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