Analytical application of DHOA for the determination of trace metallic constituents in U based fuel materials by ICP-AES

DHOA (Di-n-hexyl-octanamide) is one of the alternative extractants to TBP (tri-n-butyl phosphate) known for the extraction of uranium from moderate nitric acid medium without significant extraction of the fission products. Analytical application of DHOA was explored to develop a methodology for determination of trace metallic constituents in uranium based nuclear materials. This involved the separation of uranium matrix by 1.1 M DHOA-dodecane followed by the analysis of the raffinate for trace constituents by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). A systematic study showed that four contacts of 1.1 M DHOA-dodecane were required for quantitative extraction of U from 4 M HNO₃ feed for the sample size of 1 g in 10 mL. The feasibility of using DHOA for extraction of U from trace metallic constituents in U based fuel materials without losing trace quantities of analytes of interest was studied by using synthetic samples after appropriate spiking of common impurities and critical elements at their required specification limits (common elements—5 ppm, critical elements—1 ppm). A systematic study was carried out to compare the analytical performance of DHOA with TBP, which revealed that DHOA could successfully be employed for the determination of 19 trace constituents with lower estimation limits of 5 ppm for common impurities and 1 ppm for critical elements.     

Chiral HPLC Method for the Novel Triazole Antitubercular Compound MSDRT 12

Cyclohex-3-enyl(5-phenyl-4H-1,2,4-triazol-3-yl)methanol (MSDRT 12) is a novel triazole-based antitubercular compound with two chiral centres. Evaluation of the enantio-specific antitubercular activity has established that the stereoisomer 3 of MSDRT12 (Isomer 3) was the most potent isomer with a minimum inhibitory concentration of 0.78 μg/mL. The other stereoisomers show negligible or no activity. A sensitive, simple, specific, precise and accurate chiral chromatographic method for the direct analysis of the four stereoisomers of MSDRT 12 and the active Isomer 3 has been developed and validated. The method has also been validated for analysing the stereoisomeric impurities Isomer 1, Isomer 2 and Isomer 4 in the active Isomer 3. The separation of the four stereoisomers of MSDRT 12 was achieved using an immobilized polysaccharide-based column, Chiralpak ID with amylose tris(3-chlorophenylcarbamate) as the chiral selector. The separation was performed using a mixture of n-hexane, isopropyl alcohol, ethanol and diethylamine (60:35:5:0.1 v/v/v/v) at a flow rate of 1 mL/min. The method offers excellent separation of the four stereoisomers with resolution more than 1.5 and tailing factor <1.5. The standard curves were linear over the concentration range 5–500 μg/mL and 0.40–505 μg/mL for MSDRT 12 and Isomer 3, respectively. Excellent linearity in the range 0.4–5 μg/mL was obtained for Isomer 1, Isomer 2 and Isomer 4 and these stereoisomeric impurities could be accurately and precisely quantified at a level of 0.1 % of the active isomer.     

Zinc–aluminum layered double hydroxide as a nano-sorbent for removal of Reactive Yellow 84 dye from textile wastewater effluents

In this research, the zinc–aluminum layered double hydroxide (Zn–Al LDH) was synthesized and structurally and morphologically characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and N₂ adsorption–desorption techniques. The obtained nano-structured inorganic material was employed as an innovative nano-sorbent for separation of Reactive Yellow 84 (RY84) dye from aqueous solutions, which can be spectrophotometrically monitored at λ = 359 nm. The effect of several parameters such as type of interlayer anion in Zn–Al LDH structure, pH, sample flow rate, elution conditions, amount of nano-sorbent, sample volume and co-existing ions on the retention efficiency was investigated and optimized. The results showed that trace amounts of the RY84 could be retained using a column packed with 300 mg of the Zn–Al(NO₃ ^?) LDH at pH 8 and stripped by 2.5 mL of 3.0 mol L^?1 NaOH. Under the optimum experimental conditions, the limit of detection and the relative standard deviation were 0.04 μg mL^?1 and 1.8 %, respectively. The calibration graph using the presented solid phase extraction system was linear in the range of 0.15–1.5 μg mL^?1 with a correlation coefficient of 0.9982. The method was successfully applied to removal of RY84 from several textile wastewater effluents.     

Direct spectrophotometric determination of ruthenium in aqueous streams of nuclear reprocessing

A fiber optic aided spectrophotometric technique has been developed for determination of ruthenium in nitric acid medium. The developed method is simple, accurate and applicable to aqueous streams of nuclear reprocessing. The system obeys Lambert–Beer’s law at 468 nm in the concentration range of 30–360 μg/mL of ruthenium. The molar absorption coefficient, detection limit and Sandell’s sensitivity are 68.477 L Mol^?1 cm^?1, 31 μg/mL and 0.0124 μg/cm² respectively. Relative standard deviation was less than 2 % and correlation coefficient was 0.9998. The results obtained by the developed procedure are in good agreement with those obtained by the standard ICP-OES method. Fission products like zirconium and strontium are not interfering. Uranium is interfering and needs prior separation by solvent extraction method. The developed method is adaptable for remote operation and on-line monitoring.     

Development and Validation of a New LC Method for Analysis of Brimonidine Tartrate and Related Compounds

A novel liquid chromatographic method for analysis three potential impurities in brimonidine tartrate drug substance has been developed and validated. Efficient chromatographic separation was achieved on a C₈ column (250 mm × 4.6 mm, 5-μm particles) with a simple mobile-phase gradient at a flow rate of 1.0 mL min^?1. Quantification was achieved by use of ultraviolet detection at 248 nm. Resolution between brimonidine tartrate and its three potential impurities was greater than 3.0. Regression analysis showed the r value (correlation coefficient) was >0.999 for brimonidine and its three impurities. The method was capable of detecting all three impurities of brimonidine tartrate at levels below 0.07 μg in a test concentration of brimonidine tartrate of 1.0 mg mL^?1 and for an injection volume of 10 μL. A solution of brimonidine tartrate in acetonitrile–water 2:8 (v/v) was stable for 48 h. The drug was subjected to stress conditions as prescribed by the ICH. Degradation was found to occur slightly under oxidative stress conditions but the drug was stable to aqueous, acidic, and basic hydrolysis, and photolytic and thermal stress. The assay of the stressed samples was calculated relative to a qualified reference standard and the mass balance was found close to 99.8%. The method was validated for linearity, accuracy, precision, and robustness.     

Sorption of uranium using silica gel with benzoylthiourea derivatives

Benzoylthiourea derivatives (N,N-diphenyl-N′-(3-methylbenzoyl)thiourea and diphenyl-N′-(4-methylbenzoyl)thiourea) were impregnated onto silica gel. The preconcentration of uranium(VI) from aqueous solution was investigated. Extraction conditions were optimized in batch method prior to determination by uv–visible absorption spectrometry using arsenazo(III). The optimum pH for quantitative adsorption was found as 3–7. Quantitative recovery of uranium (VI) was achieved by stripping with 0.1 mol L^?1 HCl. Equilibration time was determined as 30 min for 99% sorption of U(VI). Under optimal conditions, dynamic linear range of for U(VI) was found as 0.25–10 μg mL^?1. The relative standard deviation as percentage and detection limit were 5.0% (n = 10) for 10 μg mL^?1 U(VI) solution and 8.7 ng mL^?1, respectively. The method was employed to the preconcentration of U(VI) ions in soil and tap water samples.     

Uranium (VI) recovery from saline environment by a marine unicellular cyanobacterium, Synechococcus elongatus

Sequestration of uranium from simulated sea water and reverse osmosis concentrates by the marine cyanobacterium, Synechococcus elongatus was assessed. Short term experiments established removal of 90–98 % uranium by the strain from simulated sea water containing 13 nM uranyl carbonate at pH 7.8, resulting in a loading of 7–42 μg U g^?1 over a period of 1–5 days respectively. Long term experiments involving repeated exposure of Synechococcus biomass to fresh simulated sea water every third day, showed a loading of 2,960 μg U g^?1 in 4 weeks. Nearly 85–90 % of cell bound uranium could be desorbed using 0.1 N HCl. The organism could sequester uranium (13,306 μg U g^?1 in 24 h) from aqueous solutions supplemented with 0.6 M NaCl and 21 μM [UO₂(CO₃)₂]^2? at pH 7.8. The results demonstrate noteworthy potential of this organism for harnessing uranium from marine environments.     

Stress Degradation Studies on Aripiprazole and Development of a Validated Stability Indicating LC Method

The present paper describes the development of a stability indicating reversed phase column liquid chromatographic method for aripiprazole in the presence of its impurities and degradation products generated from forced decomposition studies. The drug substance was subjected to stress conditions of aqueous hydrolysis, oxidative, photolytic and thermal stress degradation. The degradation of aripiprazole was observed under acid hydrolysis and peroxide. The drug was found to be stable to other stress conditions attempted. Successful separation of the drug from the synthetic impurities and degradation products formed under stress conditions was achieved on an Inertsil phenyl column using a mixture of 0.2% trifluoroacetic acid and acetonitrile (55:45, v/v). The developed LC method was validated with respect to linearity, accuracy, precision, specificity and robustness. The assay method was found linear in the range of 25–200 μg mL^?1 with a correlation coefficient of 0.9999 and the linearity of the impurities were established from LOQ to 0.3%. Recoveries of the assay and impurities were found between 97.2 and 104.6%. The developed LC method for the related substances and assay determination of aripiprazole can be used to evaluate the quality of regular production samples. It can also be used to test the stability samples of aripiprazole. To the best of our knowledge, the validated stability indicating LC method which separates all the impurities disclosed in this investigation was not published elsewhere.     

Estimation of distribution coefficient of uranium around a uranium mining site

Distribution coefficient (K _d) of uranium and its daughter products are very important for migration study around uranium mining sites. Since the distribution coefficient depends very much on the soil and groundwater chemistry, generation of site specific K _d is very important. In the literature there is a large variation of K _d values of uranium. For realistic prediction of contaminant migration, literature K _d value is not very effective. So site specific experimental K _d values are required. The present study emphasizes on the estimation of site specific distribution coefficient for uranium around a uranium mining site. The soil and groundwater parameters which affect the K _d value of uranium have also been estimated. Soil and groundwater samples from nine locations around Turamdih uranium mining site were collected and chemically characterized for various parameters. The distribution coefficient of uranium in top and one meter depth soil samples from above locations were estimated using laboratory batch method. The distribution coefficient of uranium varies from 69 ± 4 to 5524 ± 285 l/kg. No significant difference in uranium K _d values was observed for top and one meter depth soil samples. In the top and one meter depth soil samples uranium K _d values vary from 129 ± 8 to 5524 ± 285 and 69 ± 4 to 3862 ± 195 l/kg respectively. For the estimation of distribution coefficient of uranium different parameters like equilibration time, solid to solution ratio, method of tracer addition to solution, solid-solution separation method etc. have been optimized. The distribution coefficient of uranium determined in the present study will be used for the migration study of uranium around uranium mining sites.     

Selective ion exchange separation of uranium from concomitant impurities in uranium materials and subsequent determination of the impurities by ICP-OES

An ion exchange method has been developed for the separation of uranium from trace level metallic impurities prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES) in uranium materials. Selective separation of uranium from trace level metallic impurities consisting Cr, Co, Cu, Fe, Mn, Cd, Gd, Dy, Ni, and Ca was achieved on anion exchange resin Dowex 1 × 8 in sulphate medium. The resin (100–200 mesh, in chloride form) was packed in a small Teflon column (7.8 cm × 0.8 cm I.D.) and brought into sulphate form by passing 0.2 N ammonium sulphate solution. Optimum experimental conditions including pH and concentration of sulphate in the liquid phase were investigated for the effective uptake of uranium by the column. Uranium was selectively retained on the column as anionic complex with sulphate, while impurities were passed through the column. Post column solution was collected and analyzed by ICP-OES for the determination of metallic impurities. Up to 2,500 μg/mL of uranium was retained with >99% efficiency after passing 25 mL sample through the column at pH 3. Percentage recoveries obtained for most of the metallic impurities were >95% with relative standard deviations <5%. The method established was applied for the determination of gadolinium in urania–gadolinia (UO₂–Gd₂O₃) ceramic nuclear fuel and excellent results were achieved. Solvent extraction method using tributylphosphate (TBP) as extractant was also applied for the separation of uranium in urania–gadolinia nuclear fuel samples prior to the determination of gadolinium by ICP-OES. The results obtained with the present method were found very comparable with those of the solvent extraction method.     

Simultaneous quantification of 28 synthetic cathinones and metabolites in urine by liquid chromatography-high resolution mass spectrometry

Synthetic cathinones are novel stimulants derived from cathinone, with amphetamines or cocaine-like effects, often labeled “not for human consumption” and considered “legal highs”. Emergence of these new designer drugs complicate interpretation of forensic and clinical cases, with introduction of many new analogs designed to circumvent legislation and vary effects and potencies. We developed a method for the simultaneous quantification of 28 synthetic cathinones, including four metabolites, in urine by liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). These cathinones include cathinone, methcathinone, and synthetic cathinones position-3’-substituted, N-alkyl-substituted, ring-substituted, methylenedioxy-substituted, and pyrrolidinyl-substituted. One mL phosphate buffer pH 6 and 25 μL IStd solution were combined with 0.25 mL urine, and subjected to solid phase cation exchange extraction (SOLA SCX). The chromatographic reverse-phase separation was achieved with a gradient mobile phase of 0.1 % formic acid in water and in acetonitrile in 20 min. We employed a Q Exactive high resolution mass spectrometer, with compounds identified and quantified by target-MSMS experiments. The assay was linear from 0.5–1 to 100 μg/L, with limits of detection of 0.25–1 μg/L. Imprecision (n?=?20) was <15.9 % and accuracy (n?=?20) 85.2–118.1 %. Extraction efficiency was 78.9–116.7 % (CV 1.4–16.7 %, n?=?5), process efficiency 57.7–104.9 %, and matrix effects from ?29.5 % to 1.5 % (CV 1.9–13.1 %, n?=?10). Most synthetic cathinones were stable at 4 °C for 72 h (n?=?27) and after 3 freeze-thaw cycles (n?=?26), but many (n?=?19) were not stable at room temperature for 24 h (losses up to ?67.6 %). The method was applied to authentic urine specimens from synthetic cathinone users. This method provides a comprehensive confirmation method for 28 synthetic cathinones in urine, with good selectivity and specificity.     

Qualitative/quantitative strategy for the determination of glufosinate and metabolites in plants

A simple method for the simultaneous determination of glufosinate and its metabolites in plants based on liquid chromatography–ultraviolet (LC–UV) absorption detection after derivatization with fluorenylmethoxycarbonyl chloride (FMOC-Cl) of some analytes to facilitate separation is reported here. Nonavailable standard metabolites were identified by LC–TOF/mass spectrometry (MS), which also confirmed all target analytes. Ultrasound-assisted extraction was used for sample preparation (power of 70 W and duty cycle of 0.7 s/s for 10 min) with subsequent evaporation of the extractant, reconstitution and filtration as the cleanup/concentration step prior to derivatization, and chromatographic separation and detection at 270 nm for underivatized analytes and 340 nm for those that were derivatized. The chromatographic analysis was completed in 40 min using a Luna® column (C18 phase). The analytical characteristics of the method were linear dynamic range of the calibration curves within 0.047–700 μg/mL with a regression coefficient (rc) of 0.999 for glufosinate, 0.077–700 μg/mL with a rc of 0.998 for N-acetyl-glufosinate, and 0.116–600 μg/mL with a rc of 0.998 for 3-(methylphosphinico)propanoic acid. The precision for the determination of glufosinate (studied at two levels, 0.1 and 5 μg/mL) was 2.7 and 6.0 % for repeatability and 4.7 and 7.2 % for within-laboratory reproducibility, respectively. Identification and confirmatory analysis of the presence of glufosinate and metabolites in the extracts from treated plants was carried out by LC–TOF/MS in high-resolution mode for the precursor ion. The method was validated by analyzing wheat (Triticum aestivum) samples (resistant and susceptible biotypes) treated with 300 g of glufosinate/ha following conventional agronomical practices.     

A Stability Indicating LC Method for Deferasirox in Bulk Drugs and Pharmaceutical Dosage Forms

A novel, sensitive, stability indicating RP-LC method has been developed for the quantitative determination of deferasirox, its related impurities in both bulk drugs and pharmaceutical dosage forms. Efficient chromatographic separation was achieved on a C18 stationary phase with simple mobile phase combination delivered in an isocratic mode and quantitation was by ultraviolet detection at 245 nm. The mobile phase consisted of buffer, acetonitrile and methanol (50:45:5, v/v) delivered at a flow rate of 1.0 mL min^?1. Buffer consisted of 10 mM potassium dihydrogen orthophosphate monohydrate, pH adjusted to 3.0 by using orthophosphoric acid. In the developed LC method the resolution (R _s ) between deferasirox and its four potential impurities was found to be greater than 2.0. Regression analysis showed an r value (correlation coefficient) greater than 0.999 for deferasirox and its four impurities. This method was capable to detect all four impurities of deferasirox at a level of 0.002% with respect to test concentration of 0.5 mg mL^?1 for a 10 μL injection volume. The inter- and intra-day precision values for all four impurities and for deferasirox was found to be within 2.0% RSD. The method showed good and consistent recoveries for deferasirox in bulk drugs (98.3–101.1%), pharmaceutical dosage forms (100.2–103.1%) and for its all the four impurities (99.7–102.1%). The test solution was found to be stable in methanol for 48 h. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in acid stress hydrolysis. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.95%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.     

Stability-Indicating LC Method for Analysis of Lornoxicam in the Dosage Form

A simple, rapid, and precise method has been developed for quantitative analysis of lornoxicam (Lxm) in pharmaceutical dosage forms. Chromatographic separation of Lxm and its degradation products was achieved on a C₁₈ analytical column with 0.05% (v/v) aqueous trifluoroacetic acid–acetonitrile, 70:30 (v/v), as mobile phase. The flow rate was 1.0 mL min^?1, the column temperature 30 °C, and detection was by absorption at 295 nm using a photodiode-array detector. The number of theoretical plates and tailing factor for Lxm were 6,577 and 1.03, respectively. Lxm was exposed to thermal, photolytic, hydrolytic, and oxidative stress, and the stressed samples were analysed by use of the proposed method. Peak homogeneity data for Lxm in the chromatograms from the stressed samples, obtained by use of the photodiode-array detector, demonstrated the specificity of the method for analysis of Lxm in the presence of the degradation products. The linearity of the method was excellent over the range 10–200 μg mL^?1 Lxm. The correlation coefficient was 0.9999. Relative standard deviations of peak areas from six measurements were always less than 2%. The proposed method was found to be suitable and accurate for quantitative analysis of Lxm and study of its stability.     

Preconcentration and spectrophotometric determination of trace amount of formaldehyde using hollow fiber liquid-phase microextraction based on derivatization by Hantzsch reaction

Formaldehyde is known as a highly toxic compound to humans and identified as a carcinogenic substance. In this study, Hantzsch reaction was utilized for the derivatization of trace amounts of formaldehyde in aqueous samples with acetylacetone in the presence of ammonia to form an extractable colored product named 3,5-diacetyl 1,4-dihydrolutidine (DDL) and its further extraction using two-phase hollow fiber liquid-phase microextraction. The main experimental variables affecting the extraction performance were investigated and optimized. Under the optimum conditions (sample volume 12 mL; reaction temperature 70 °C; ammonium acetate buffer solution 4 mL 0.1 mol L^?1; acetylacetone 5 mL 0.15 mol L^?1; solvent octanol, salt concentration 20% (w/v) NaCl; pH of donor phase 7.0; stirring speed 400 rpm and extraction time 30 min), the linear dynamic range, limit of detection (LOD as 3S _b/m) and relative standard deviation (RSD %) of the proposed method were obtained as 5–250 μg L^?1 (r ² = 0.9979), 3.6 μg L^?1 and 2.5%, respectively. Finally, the applicability of the proposed method was examined, and very good results were obtained. The results confirmed the applicability of the proposed method as a versatile, low-cost and sensitive preconcentration method for determination of low concentrations of formaldehyde in aqueous solutions.     

Stress Degradation Behavior of Entacapone and Development of LC Stability-Indicating Related Substances and Assay Method

A new, sensitive, stability indicating gradient RP-LC related substances and assay method has been developed for the quantitative determination of entacapone in bulk drugs. Efficient chromatographic separation was achieved on a C18 stationary phase with simple mobile phase combination of buffer and acetonitrile. Buffer consisted of 0.1% orthophosphoric acid, delivered in a gradient mode and quantitation was carried out using ultraviolet detection at 220 nm with a flow rate of 1.5 mL min^?1. In the developed LC method the resolution (R _s ) between entacapone and its three potential process impurities were found to be >2.0. Regression analysis showed an r ² value (correlation coefficient) >0.99 for entacapone and its three potential impurities. This method was capable to detect all three process impurities of entacapone at a level of 0.003% with respect to test concentration of 0.5 mg mL^?1 for a 20 μL injection volume. The inter- and intra-day precision values for all three impurities and for entacapone was found to be within 2.0% RSD. The method has shown good and consistent recoveries for entacapone in bulk drugs (99.2–101.5%) and its three impurities (99.5–102.2%). The test solution was found to be stable in diluent for 48 h. The drug substances were subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in acid stress, base stress and oxidative conditions. The stressed test solutions were assayed against the qualified working standard of entacapone and the mass balance in each case was close to 99.7% indicating that the developed method was stability-indicating. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.     

Detection of uranium with a wireless sensing method by using salophen as receptor and magnetic nanoparticles as signal-amplifying tags

A new wireless sensing method for the detection of uranium in water samples has been reported in this paper. The method is based on a sandwich-type detection strategy. Salophen, a tetradentate ligand of uranyl ion, was immobilized on the surface of the polyurethane-protected magnetoelastic sensor as receptor for the capture of uranyl ion. The phosphorylated polyvinyl alcohol coated magnetic Fe₃O₄ nanoparticles were used as signal-amplifying tags of uranyl ion. In a procedure of determining uranium, firstly uranyl ion in sample solution was captured on the sensor surface. Then the captured uranyl bound the nanoparticle through its coordination with the phosphate group. The amount of uranium was detected through the measure of the resonance frequency shift caused by the enhanced mass loading on the sensor surface. A linear range was found to be 0.2–20.0 μg/L under optimal conditions with a detection limit of 0.11 μg/L. The method has been applied to determine uranium in environmental water samples with the relative standard deviations of 2.1–3.6 % and the recoveries of 98.0–101.5 %. The present technique is one of the most suitable techniques for assay of uranium at trace level in environmental water samples collected from different sources.     

Synergistic solvent extraction of copper, cobalt, rhodium and iridium into 1, 2-Dichloroethane at trace level by newly synthesized 25, 26, 27, 28-tetrahydroxy-5, 11, 17, 23-tetra-[4-(N-hydroxyl-3-phenylprop-2-enimidamido) phenylazo] calix[4]arene

A spectrophotometric method for determination of copper, cobalt, rhodium and iridium ions from nitric acid media after extraction of these ions by 25, 26, 27, 28-tetrahydroxy-5, 11, 17, 23-tetra-[4-(N-hydroxyl-3-phenylprop-2-enimidamido) phenylazo] calix [4] arene (THPAC) has been developed and possible synergistic effect has been investigated. The maximum enhancement was obtained in the presence of 30% 1, 2-dichloroethane in DMF and 3M nitric acid. The trace amounts of the metal were determined spectrophotometrically. Beer’s law was obeyed in concentration range 5.0–10.0 μg, 6.0–120.0 μg, 12.0–100.0 μg, and 10.0–130.0 μg/10 mL of the final solution of copper, cobalt, rhodium and iridium, respectively. The molar absorptivities (l mol^?1 cm^?1) and Sandell’s sensitivities (μg cm^?1) were calculated: Cu (II) = 0.96 × 10^4, 0.0066; Co (II) = 1.13 × 10⁴, 0.0052; Rh (III) = 0.98 × 10⁴, 0.012; and Ir (III) = 2.03 × 10⁴, 0.0095, respectively. Seven replicate analyses containing of 20.0 μg of Cu (II), 24.0 μg of Co (II), 36.0 μg of Rh (III) and 25.0 μg of Ir (III) gave mean absorbance 0.302, 0.462, 0.344, 0.264; and relative standard deviation 0.65, 0.85, 1.10, 1.08%, respectively. The interference of various ions was studied and optimum conditions were developed for determination of metals in certain alloys, environmental, pharmaceutical and synthetic samples.     

Determination of analytes at trace level in uranium matrix by ICP-AES without chemical/physical separation

Determination of trace metallic constituents in nuclear materials e.g. U, Pu, Am, Zr etc. by Atomic Emission Spectroscopy requires the separation of the major matrix without the loss of analytes at trace level. For DC Arc carrier distillation technique, carrier is used to separate the matrix physically according to the volatility of the analytes while appropriate extractant in suitable diluent is used for chemical separation in inductively coupled plasma atomic emission spectroscopy (ICP-AES). In the present study an attempt was made to develop a methodology for the determination of B, Cd, Mg, Zn, Al, Sr and Sc at trace level (up to 0.1 μg/mL) in uranium matrix without any chemical or physical separation. It involves identification of suitable analytical lines of uranium for its ICP-AES determination; study the spectral interference of uranium to choose interference free analytical lines, optimization of instrumental and experimental parameters etc. The method was validated using synthetic samples.