67 research outputs found

    Biopolymer Test Kit for Colorimetric Detection of Chlorine in Water

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    The objective of the study was to fabricate the colorimetric sensor of biodegradable material for free chlorine determination. The colorimetric reagent of N,N-diethyl-p-phenylenediamine sulfate (DPD) was entrapped in the hybrid biopolymer film of agar (AG) and tapioca starch (TAS) and it was coated on the plastic micro-PCR tube. The pink product obtained from the reaction between DPD reagent and chlorine could indicate the presence of residual chlorine in the water.  The condition for the sensor film synthesis was optimized by the digital image analytical technique with mobile phone application. The results were showed that Red-Green-Blue (RGB) intensity of reaction product was not changed, even through the DPD reagent was added over 0.2 g/mL. The addition of 16 g/L EDTA in the buffer solution could reduce the interference effect from some metals, especially Fe3+, contaminated in water sample. The water pH could be maintained for best analysis at the volume ratio between buffer and DPD solution of 0.5:1. The incubation of colorimetric film at 60 °C and 60 minutes provided the best sensor performance with fast analysis of 1 min reaction time. In conjunction with the digital image colorimetry (DIC), the developed test kit did not provided only the qualitative information, but the rapid quantitative analysis could be also fulfilled. A wide linear range of 0.3 to 15 mg/L chlorine concentration with good linearity (R2 > 0.99) was achieved by this coupled technique. The application of biopolymer film to various kind of real water samples showed the good performances, which were comparable with the standard spectrophotometry (no significantly different results at 95% confidence level). These could promote the use of biopolymer test kit as the environmentally-friendly analytical method for chlorine in water

    Microcrystalline testing used in combination with Raman micro-spectroscopy for absolute identification of novel psychoactive substances

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    Two new psychoactive substances, namely 4-methylmethcathinone (mephedrone) and 5,6-methylenedioxy-2-aminoindane (MDAI) were analysed with a novel combination of microcrystalline tests followed by Raman micro-spectroscopy to facilitate their absolute identification. The discrimination power of the proposed combination was successfully demonstrated through the analysis of the positional isomers 2- and 3-methylmethcathinone. The addition of mercury dichloride as a microcrystalline test reagent produced specific microcrystals of each tested analyte. The robustness of the method was evaluated in the presence of common cutting agents (caffeine and benzocaine) as well as on street samples. The crystal lattice structures of mephedrone, 2-methylmethcathinone and MDAI mercury dichloride microcrystals were determined by single crystal X-ray diffraction. This confirmed the presence of both drug and reagent together in the lattice and accounts for the distinct habit of the observed microcrystals. Raman spectra of the formed microcrystals differed from those obtained from their standard salt form by loss and/or gain of some vibrational modes. Particularly important was the appearance of the mercury chloride link to each tested drug molecule which showed as strong bands at low wavenumbers. Its presence was corroborated by its detection in the crystal lattice. It was therefore concluded that microcrystalline testing followed by Raman micro-spectroscopy satisfies the technique combination requirement for psychoactive substances recommended by the Scientific Working Group for the Analysis of Seized Drugs (SWGDRUG) and provides a rapid and cheap analysis route. The proposed technique combination also aids the development of new microcrystalline tests as it allows for confirmation of the uniqueness of the developed microcrystals almost in-situ rather than growing single crystals for often long periods of time needed for single crystal X-ray diffraction analysis

    Chromogenic and Fluorogenic Probes for the Detection of Illicit Drugs

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    [EN] The consumption of illicit drugs has increased exponentially in recent years and has become a problem that worries both governments and international institutions. The rapid emergence of new compounds, their easy access, the low levels at which these substances are able to produce an effect, and their short time of permanence in the organism make it necessary to develop highly rapid, easy, sensitive, and selective methods for their detection. Currently, the most widely used methods for drug detection are based on techniques that require large measurement times, the use of sophisticated equipment, and qualified personnel. Chromo- and fluorogenic methods are an alternative to those classical procedures.We thank the Spanish Government [projects MAT2015-64139-C4-1-R and AGL2015-70235-C2-2-R (MINECO/FEDER)] and the Generalitat Valenciana (project PROMETEOII/2014/047) for support. S.E.S thanks the Ministerio de Economia y Competitividad for his Juan de la Cierva contract. 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    Evaluating the performance of three GC columns commonly used for the analysis of ignitable liquid mixtures encountered in fire debris

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    The analysis of debris recovered from fire scenes for the presence of ignitable liquids is of increasing importance for fire scene investigation. Increasingly this is carried out using Gas chromatography-mass spectroscopy (GCMS) using a standard dimethylpolysiloxane capillary column. Various publications in the available literature and survey data from forensic science laboratories favour HP-1 or HP-5 columns or their equivalent but no direct comparison of the sensitivity, selectivity or resolution of these columns for test mixtures relevant to ignitable liquid matrices have been published. This present work addresses this by analysing a matrix matched test mixture and an ignitable liquid test mixture using three different commercially available dimethylpolysiloxane columns currently referenced in the literature for ignitable liquid analysis. The ASTM standard method for analysis of ignitable liquids using GCMS was adopted and systematically modified for each column to afford maximum separation of the analytes and the results are presented
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