Abstract
In 2013, the European Union expanded the list of hazardous substances contained in the RoHS Directive. In addition, certain phthalate esters, such as dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP) and diisobutyl phthalate (DIBP), will be categorized as RoHS-prohibited substances starting from July 2019. Although pyrolysis–gas chromatography–mass spectrometry (Py-GC-MS) is a promising analytical method for the screening of phthalate esters, we have developed a novel soft-ionization MS method that is quantitative as well as faster and more convenient for this purpose. The sample was measured three times, after providing the calibration curve using a powdery standard material of SPEX. The data collection time is 5 min, and continuous measurements are completed within 8 min per sample. The mass spectrum was corrected by dividing the intensity by the sample weight. For the coefficient of variation, DBP was 2.9%, BBP was 3.4%, DEHP was 3.6%, and good reproducibility was observed. Precise analyses of phthalate esters using traditional methods can require solvent extraction times of up to 24 h as well as special techniques. Therefore, a screening method that can be easily carried out by anyone within ten minutes is very attractive.
Highlights
For the detailed measurement of polybrominated biphenyls and polybrominated diphenyl ethers, solvent extraction is carried out for more than 8 h as a pretreatment, and the measurement is performed with a gas chromatograph–mass spectrometer (GC-MS)
We developed a new apparatus, in which atmospheric pressure chemical ionization (APCI) excellent in selectivity, was used, and we are applying the apparatus to the present field [17]
We conducted the following evaluations in order to apply our equipment: (i) investigation of the detectability of dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP); (ii) DBP þ diisobutyl phthalate (DIBP), BBP, DEHP þ di-n-octyl phthalate (DNOP) were prepared in each PE matrix, and the effectiveness of the apparatus for analysis of these samples was evaluated; (iii) DBP, BBP, DEHP: we made samples containing 500, 1000, 1500 and 2000 mg g21 each in polyvinyl chloride (PVC) and investigated the correlation between analysis results and concentration values by our equipment; (iv) investigation of the extensibility of our analysis subjects. (Here, because bromodiphenyl ether is subject to regulation in RoHS2, we investigated the detection of these substances.)
Summary
Six hazardous substances (Cd, Pb, Hg, Cr, polybrominated biphenyls and polybrominated diphenyl 2 ethers), was implemented in July 2006 [2]. The RoHS Recast Directive (RoHS2, Directive 2011/65/EC) was issued in the Official Journal of the European Union in July 2011 [3]. According to this directive, the screening measurement of hazardous substances is mainly performed using X-ray fluorescence spectrometer, with which the measurement can be carried out non-destructively in about 10 min. For the detailed measurement of polybrominated biphenyls and polybrominated diphenyl ethers, solvent extraction is carried out for more than 8 h as a pretreatment, and the measurement is performed with a gas chromatograph–mass spectrometer (GC-MS)
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