JEOL : Simultaneous analysis of TSCA and RoHS by using GC/MS/MS

Product used ： Mass spectrometer(MS)

Introduction

TSCA is an abbreviation for Toxic Substances Control Act. In February 2021, the U.S. Environmental Protection Agency (EPA) regulated the five substances listed in Table 1 and prohibited the use of some of them. For DecaBDE, PIP (3:1), and HCBD, there is not regulation value and they are supposed to be non-detectable (N.D.). Since there is no regulation value, it is necessary to detect even lower concentration. As an analysis method, SIM measurement by GC-QMS that is same as RoHS analysis is considered. However, it has possibility that the SIM measurement is affected by matrix components, because some material sample contain many matrix components. Therefore, there is a concern that quantitative analysis by SIM measurement is difficult. On the other hand, the SRM measurement of GC/MS/MS use a combination of selected precursor ion and generated product ion from its selected precursor ion, so selectivity of detection ion and detection sensitivity will be improved. As a result, the influence of matrix components can be reduced, and it is possible to detect components contained in material sample. In this study, we report on the simultaneous analysis of TSCA and RoHS by using GC/MS/MS.

Method

The measurement was performed using GC triple quadrupole mass spectrometer JMS-TQ4000GC UltraQuad™ TQ (Fig. 1). For the extract, 10 mg of a small fragment scraped from electronic parts was sonicated in 1 mL of THF for 60 minutes. The measurement condition is shown in Table 2 and the SRM transition is shown in Table 3. In this measurement, PIP (3:1) which has a lot of attention as TSCA component, 2,4,6-TTBP and PCTP which have clear regulation value, and phthalates of RoHS were measured as target component. Calibration curves were prepared in the concentration range of 0.001 - 0.05 ppm for PIP (3:1), 2.5 - 125 ppm for 2,4,6-TTBP, 10 - 500 ppm for PCTP, and 0.5 - 25 ppm for phthalates.

Result <_li3d_22_22_>●Calibration curve and SRM chromatogram peak

The calibration curve is shown in Fig. 2 and the SRM chromatogram peaks of the TSCA component are shown in Fig. 3. The calibration curve showed linearity with a correlation coefficient (R) of 0.999 or more for all components of TSCA and RoHS. For the SRM chromatogram peak, peaks of only PCTP showed a tailing peak shape due to the presence of SH group. Although sensitivity and chromatogram peak shape are expected to improve by derivatization, detection was possible without derivatization in this concentration range. Regarding other components, good chromatogram peaks were obtained.

Fig. 2 Calibration curve

Fig. 3 SRM chromatogram peaks of TSCA component

●Result of the extracted sample

The SRM chromatogram peaks of the TSCA components obtained from the extract are shown in Fig. 4, and the quantitative value for each component are shown in Table 4. All target components were detected in the extract. Especially, PIP(3:1) has many isomers and RT confirmation is difficult without a reference component. However, the SRM measurement is confirmed that at least four isomers were observed based on the relationship between precursor ion and product ion.

Fig. 4 SRM chromatogram peaks of TSCA component in the extracted sample

Conclusion

The SRM measurement of GC/MS/MS is an effective measurement method for TSCA and RoHS analysis. The SRM measurement use a combination of selected precursor ion and generated product ion from its selected precursor ion, so selectivity of detection ion and detection sensitivity are improved. As a result, the influence of matrix components can be reduced, and it is possible to detect components contained in trace amounts. Especially for TSCA component with N.D., SRM measurement is suitable for its analysis because it is desirable to detect even lower concentrations.

Solutions by field

Chemistry

Semiconductor

Electrical / Electronic Component

Plastics / Polymer

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JMS-TQ4000GCTriple Quadrupole Mass Spectrometer