A method based on pressurized fluid extraction (PFE) was developed for measuring microplastics in environmental samples. This method can address some limitations of the current microplastic methods and provide laboratories with a simple analytical method for quantifying common microplastics in a range of environmental samples. The method was initially developed by recovering 101% to 111% of spiked plastics on glass beads and was then applied to a composted municipal waste sample with spike recoveries ranging from 85% to 94%. The results from municipal waste samples and soil samples collected from an industrial area demonstrated that the method is a promising alternative for determining the concentration and identity of microplastics in environmental samples.
Matching spectra is necessary for database searches, assessing the source of an unknown sample, structure elucidation, and classification of spectra. A direct method of matching is to compare, point by point, two digitized spectra, the outcome being a parameter which quantifies the degree of similarity or dissimilarity between the spectra. Examples studied here are correlation coefficient squared, and Euclidean cosine squared, both applied to the raw spectra and first difference values of absorbance. It is shown that spectra do not fulfill the requirements for a normal statistical interpretation of the correlation coefficient; in particular they are not normally distributed variables. It is therefore not correct to use a Student-t test to calculate the probability of the null hypothesis that two spectra are not correlated on the basis of a correlation coefficient between them. We have investigated the effect on the similarity indices, of systematically changing the mean and standard deviation of a single Gaussian peak relative to a reference Gaussian peak; and of changing one peak, and of changing many peaks, in a simulated ten-peak spectrum. Squared Euclidean cosine is least sensitive to changes and the first difference methods are most sensitive to changes in mean and standard deviation of peaks. A shift of the center of a peak has a greater effect on the indices than increases in peak width, but a decrease in peak width does lead to significant changes in the indices. We recommend that if these indices are to be used to match spectra, appropriate windows should be chosen to avoid dilution by regions with no significant change.
Four comparison statistics ('similarity indices') for the identification of the source of a petroleum oil spill based on the ASTM standard test method D3414 were investigated. Namely, (1) first difference correlation coefficient squared and (2) correlation coefficient squared, (3) first difference Euclidean cosine squared and (4) Euclidean cosine squared. For numerical comparison, an FTIR spectrum is divided into three regions, described as: fingerprint (900-700 cm(-1)), generic (1350-900 cm(-1)) and supplementary (1770-1685 cm(-1)), which are the same as the three major regions recommended by the ASTM standard. For fresh oil samples, each similarity index was able to distinguish between replicate independent spectra of the same sample and between different samples. In general, the two first difference-based indices worked better than their parent indices. To provide samples to reveal relationships between weathered and fresh oils, a simple artificial weathering procedure was carried out. Euclidean cosine and correlation coefficients both worked well to maintain identification of a match in the fingerprint region and the two first difference indices were better in the generic region. Receiver operating characteristic curves (true positive rate versus false positive rate) for decisions on matching using the fingerprint region showed two samples could be matched when the difference in weathering time was up to 7 days. Beyond this time the true positive rate falls and samples cannot be reliably matched. However, artificial weathering of a fresh source sample can aid the matching of a weathered sample to its real source from a pool of very similar candidates.
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