Ultrasound-assisted extraction of Pb, Cd, Cr, Mn, Fe, Cu, Zn from edible oils with tetramethylammonium hydroxide and EDTA followed by determination using graphite furnace atomic absorption spectrometer.

A new method for extraction and determination of trace and ultratrace impurities from edible oils via an ultrasound-assisted extraction using tetramethylammonium hydroxide (TMAH) and ethylenediaminetetraacetic acid (EDTA) has been described. Method is simple and sensitive. Extraction variables like pH, concentrations of TMAH and EDTA, ultrasonication and centrifugation times were all optimised for analytes using engine-oil. Under optimised conditions, extraction of spiked analytes from all the edible oils into aqueous-medium were investigated and found to be quantitative (89-101%). Using this method, concentrations of impurities in edible-oils were determined by graphite furnace atomic absorption spectrometer (GFAAS) using standard-addition calibration method and validated with microwave-digestion method. The method was successfully applied to edible oils extracted from various seeds such as mustard oil, sun flower oil, sesame oil, ground nut oil, coconut oil, rice bran oil and corn oil containing ultratrace impurities. Accuracy of developed method for edible-oils was checked with corresponding results obtained by microwave digestion method.

Modified matrix volatilization setup for characterization of high purity germanium.

Modified matrix volatilization (MV) method has been described to characterize high purity germanium material of 7 N (99.99999%) purity. Transport of both, the chlorine gas generated in-situ in this method and the argon gas (carrier) is fine controlled by means of a mass flow controller. This enabled both uniform reaction of chlorine gas with the germanium matrix and smooth removal of germanium matrix as its chloride. This resulted in improvement in the reproducibility of the analytical results. The use of quartz reaction vessel has lead to the reduction in the process blank levels. The combined effect of these modifications in the MV setup has resulted in very consistent and low process blanks and hence improved detection limits of this method. Applicability of the method has been expanded to rare earth elements and other elements after examining their recoveries. The quantification is done by using inductively coupled plasma quadrupole mass spectrometer (ICP-QMS) and continuum source graphite furnace atomic absorption spectrometry (CS-GFAAS). In the absence of certified reference materials for high pure germanium, the accuracy of the method is established by spike recovery tests. The precision of the method has been found to vary from 1 to 30% for concentrations between 1 and 30 ng g(-1). The limits of detection (LOD) for the target analytes are found to be between 18 and 0.033 ng g(-1).

Sequential extraction of platinum, cisplatin and carboplatin from environmental samples and pre-concentration/separation using vesicular coacervative extraction and determination by continuum source ETAAS.

A sequential extraction procedure is developed for the separation of trace levels of hexachloroplatinate, cisplatin and carboplatin from soil, which are then, pre-concentrated using a vesicular coacervative cloud point extraction method prior to their determination as platinum by continuum source ETAAS. Sequential extraction of carboplatin, cisplatin and hexachloroplatinate from a specific red soil is achieved by using the 20% HCl, aqua regia at room temperature and by combination of aqua regia and HF with microwave digestion, respectively. The pre-concentration of these species from the extracted solutions is based on the formation of extractable hydrophobic complexes of PtCl6(2-) anionic species with free cationic head groups solubilizing sites of the Triton X-114 co-surfactant stabilized TOMAC (tri-octyl methyl ammonium chloride) vesicles through electrostatic attraction. This process separates the platinum from bulk aqueous solution into a small vesicular rich phase. The parameters affecting the extraction procedures are optimized. Under the optimized conditions, the achieved pre-concentration factor is 20 and detection limit is 0.5 ng g(-1) for soil and 0.02 ng mL(-1) for water samples. The spiked recoveries of hexachloroplatinate, cisplatin and carboplatin in water and soil extracts in the vesicular coacervative extraction are in the range of 96-102% at 0.5-1 ng mL(-1) with relative standard deviation of 1-3%. The accuracy of the method for platinum determination is evaluated by analyzing CCRMP PTC-1a copper-nickel sulfide concentrate and BCR 723 road dust certified reference materials and the obtained results agreed with the certified values with 95% confidence level of student t-test. The results were also compared to mixed-micelle (MM)-CPE method reported in the literature.

Microwave assisted aqua regia extraction of thallium from sediment and coal fly ash samples and interference free determination by continuum source ETAAS after cloud point extraction.

A simple cloud point extraction method is described for the separation and pre-concentration of thallium from the microwave assisted aqua regia extracts of sediment and coal fly ash samples. The method is based on the formation of extractable species of thallium and its interaction with hydrophobic solubilizing sites of Triton X-114 micelles in the presence of aqua regia and electrolyte NaCl. These interactions of micelles are used for extraction of thallium from a bulk aqueous phase into a small micelles-rich phase. The potential chloride interferences are eliminated effectively, which enabled interference free determination of thallium from aqua regia extracts using continuum source ETAAS. The parameters affecting the extraction process are optimized. Under the optimized conditions, pre-concentration factor and limit of detection are 40 and 0.2 ng g(-1), respectively. The recoveries are in the range of 95-102%. A characteristic mass, 13 pg was obtained. The accuracy of the method is verified by analyzing certified reference materials such as NIST 1633b coal fly ash, NIST 1944 marine sediment and GBW 07312 stream sediments. The results obtained are in good agreement with the certified values and method is also applied to real samples.

Cloud point extraction of trace metals from seawater and determination by electrothermal atomic absorption spectrometry with iridium permanent modifier.

A simple method is described for preconcentration and separation of trace metals such as Ag, Co, Cr, Cu, Fe, Mn, Ni and Pb simultaneously from seawater using a cloud point extraction (CPE) procedure. Triton X-114 nonionic surfactant and ammonium pyrrolidine dithiocarbamate (APDC) have been used as an extraction medium and a chelating extractant, respectively. The amounts of Triton X-114 and APDC and the pH value necessary for extraction were carefully optimized. The preconcentration factor of about 200 is achieved for all the studied metals. Electrothermal atomic absorption spectrometry (ETAAS) with an Ir coated graphite tube as permanent chemical modifier has been used for determination. The limits of detection of Ag, Co, Cr, Cu, Fe, Mn, Ni and Pb were 0.003, 0.008, 0.003, 0.006, 0.015, 0.002, 0.009 and 0.01 ng ml-1, respectively. Certified reference materials such as CASS-4 and NASS-5 (seawater) and NIST-1640 (natural water) have been used for validation of the new method. The relative standard deviation (%) obtained for all the metals are in the range 0.8 - 3.6% for natural water and 11-25% for seawater materials, except for Co in NASS-5 for which it was 50%.