Contaminants and levels of occurrence in washed and shredded poly(ethylene terephthalate) from curbside collection. II: Validation of extraction procedures, particle size sampling and crystallinity

Abstract

Part I of this study showed that washed and dried, shredded poly(ethylene terephthalate) (PET) (flake) obtained from curbside collection when Soxhlet extracted contained 26 semivolatile contaminants below the US FDA threshold of 215 ppb and six above this level. This paper reports the validation of the Soxhlet extraction technique by comparison with total dissolution with trifluoroacetic acid (TFA). The work was carried out for two of the three particle size ranges obtained by grinding the PET flake (300–425 and 425–700 μm) and for the unground flake. Further validation was undertaken by comparison of contaminant levels determined by total dissolution with TFA and sonication with dichloromethane (DCM) using flake ground to the 0–300 μm size range. The levels of contaminants increased with decreasing particle size range, but X-ray diffraction measurements of degrees of crystallinity were similar for each PET particle size range, thus showing that the differences in contaminant levels were not due to variable percentages of the amorphous material from the tops and bottoms of shredded bottles, relative to the amounts of crystalline PET from the mid-sections of the bottles. Hence, it was postulated that the variations in contaminant levels were due to selective grinding of the more highly contaminated surfaces, whilst the larger particles incorporated the less contaminated interior material. The grinding was also strongly selective with respect to the amorphous flake. Analysis of the segregated amorphous and crystalline flake phases indicated that many contaminants were similarly absorbed into both phases, whilst some were preferred by the amorphous PET and others were preferred by the crystalline PET.