Stepwise injection photometric determination of mercaptanes in air

An automated procedure is developed for the photometric determination of mercaptanes in air. To achieve the required selectivity of analyte determination, a scheme of sample preparation was elaborated, which includes the liquid absorption separation of interfering components (hydrogen sulfide and sulfur dioxide) and mercaptanes on two consequent chromatography columns with glass wool impregnated with a zinc acetate solution and an alkaline solution of cadmium chloride. Therein, the impurities specified were separated in the first column, while the target materials were gathered on the second one. The materials were detected with high sensitivity by their reaction with an iodine/starch complex under the conditions of step-wise injection analysis. The analytical range for mercaptane sulfur was from 0.5 to 7.5 μg/m³ for a sample volume of 1 m³.     

Direct determination of δ44/42Ca isotope ratio by ion chromatography/low‐resolution multicollector ICPMS

High‐precision on‐line procedure for measurement of calcium isotopic ratio by coupling ion chromatography to multicollector inductively coupled plasma mass spectrometry was developed. Calcium separation from the sample matrix was achieved on an ion chromatography column—IonPac CS16—ID 3 mm connected with CERS 500 2 mm suppressor and followed by multicollector inductively coupled plasma mass spectrometry calcium isotopic ratio determination. Dry plasma mode was used with Aridus II desolvation system. To sustained samples with high level of total dissolved salts as well as account capacity of applied analytical column, the method has been optimized regarding calcium isotope ratio measurements with low‐resolution mass spectrometry. Mass discrimination and instrument drift were corrected by sample‐standard bracketing method using the ⁴⁴Ca/⁴²Ca isotope ratio of SRM 915a as a standard. Good accuracy and reasonable precision of calcium isotope ratio (generally 0.20‰ [2SD]) were achieved, which are comparable to off‐line Ca separation and continuous measurement. The reproducibility of the proposed analytical procedure was verified by measuring the SRM 915a standard as a sample randomly over 3 months (n = 56). Applicability of the protocol was demonstrated for matrix‐rich natural water samples, coral samples, and bone standard reference materials.     

Determination of Alkali and Alkaline-Earth Elements in Table Salt and Sodium Chloride by Sonoluminescence

The application of sonoluminescence to the determination of sodium, calcium, and magnesium in table salt and sodium chloride solutions is studied. It is shown that the analytical performance of the procedure proposed for the determination of sodium in sodium chloride, rock salt, and vacuum-evaporated salt solutions is better than that of the known methods, in particular, atomic absorption spectrometry. This is because the proposed procedure does not require substantial sample dilution. Calcium and magnesium in these samples can be determined with satisfactory analytical performance at concentrations higher than 10 g/L.     

Rapid method for the determination of radiostrontium in milk

A radiochemical procedure comprising ion chromatography for preconcentration, oxalate precipitation for alkali/alkaline earth separation, strontium specific extraction chromatography with a crown ether for calcium/strontium separation, carbonate precipitation for counting on a low background proportional counter, provides a simple, rapid (48 h) and effective method for radiostrontium determination in emergency situation in milk. The separation scheme gives a strontium recovery rate of 62% and an empiric relative standard deviation of 11%. The detection limit for 500 ml milk and 3600-second counting time is 0.090 Bq^.l^-1.     

Isolation of radioactive strontium from natural samples: A semi-automatic procedure

A procedure for semi-automatic isolation and determination of radioactive strontium from natural samples was developed. The method was tested by the determination of⁹⁰Sr in soil samples and the results obtained were compared to those obtained by the standard procedure. The procedure consists of leaching of strontium (and other cations as well) from soil samples with a water suspension of the cation exchanger Amberlite IR-20, the separation of strontium from other cations, e.g., potassium, calcium, sodium, barium by the anion exchangers Amberlite CG-400 or Dowex Ag 1×8 with 0.25M HNO₃ in ethanol-methanol mixture as eluent in the apparatus specially constructed for this purpose. Determination of⁹⁰Sr was done on the low-level gas-flow β-counter and by Cherenkow counting on the liquid-scintillation counter few hours after the separation. It was shown that this procedure might be successfully applied for rapid determination of⁹⁰Sr in soil samples and other natural samples in a timesaving manner.     

Cyclic flow-injection photometric determination of mercaptans in hydrocarbon gases

A procedure for the automated photometric determination of mercaptans in hydrocarbon gases was developed using sodium nitroprusside as a photometric reagent. The analytical range was from 10 to 150 mg/m³ at a sample volume of 0.4 L and preconcentration time of 2 min.     

Natural radioactivity in building materials utilized in the State of Kuwait

A simple radiochemical procedure is described for the determination of⁹⁰Sr in brines, which are very highly concentrated in sodium, calcium, potassium, magnesium, chloride and sulfate ions. The method is based on the different solubility of yttrium as compared to that of strontium, calcium and magnesium in ammonium chloride solutions, and utilizes Eichroms resin TRU·Spec for the purification of the yttrium fraction. The overall time required for the⁹⁰Sr analysis (excluding the counting time) is less than one day. Because the procedure involves only rather simple steps, it is well suited for routine analyses of large sample numbers.     

Rapid determination of 226Ra in environmental samples

A new rapid method for the determination of ²²⁶Ra in environmental samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used for emergency response or routine sample analyses. The need for rapid analyses in the event of a Radiological Dispersive Device or Improvised Nuclear Device event is well-known. In addition, the recent accident at Fukushima Nuclear Power Plant in March, 2011 reinforces the need to have rapid analyses for radionuclides in environmental samples in the event of a nuclear accident. ²²⁶Ra (T1/2?=?1,620?years) is one of the most toxic of the long-lived alpha-emitters present in the environment due to its long life and its tendency to concentrate in bones, which increases the internal radiation dose of individuals. The new method to determine ²²⁶Ra in environmental samples utilizes a rapid sodium hydroxide fusion method for solid samples, calcium carbonate precipitation to preconcentrate Ra, and rapid column separation steps to remove interferences. The column separation process uses cation exchange resin to remove large amounts of calcium, Sr Resin to remove barium and Ln Resin as a final purification step to remove ²²⁵Ac and potential interferences. The purified ²²⁶Ra sample test sources are prepared using barium sulfate microprecipitation in the presence of isopropanol for counting by alpha spectrometry. The method showed good chemical recoveries and effective removal of interferences. The determination of ²²⁶Ra in environmental samples can be performed in less than 16?h for vegetation, concrete, brick, soil, and air filter samples with excellent quality for emergency or routine analyses. The sample preparation work takes less than 6?h. ²²⁵Ra (T1/2?=?14.9?day) tracer is used and the ²²⁵Ra progeny ²¹⁷At is used to determine chemical yield via alpha spectrometry. The rapid fusion technique is a rugged sample digestion method that ensures that any refractory radium particles are effectively digested. The preconcentration and column separation steps can also be applied to aqueous samples with good results.     

Stepwise injection photometric determination of nickel in air aerosols

A procedure is developed for the automated determination of nickel in air aerosols; it involves the adhesive separation of aerosols on a fiberglass column in the on-site mode followed by the photometric determination of analytes with dimethyl glyoxime under the conditions of stepwise injection analysis of aerosol concentrates. The analytical range for nickel is 1.5–38 μg/m³; the detection limit of the method is 0.5 μg/m³ at an air sample volume of 30 L. The duration of sampling to an adhesive column and concentrate analysis were 15 and 10 min, respectively.     

Selective determination of trace arsenic and antimony species in natural waters by gas chromatography with a photoionization detector

Traces amounts of arsenic and antimony in water samples were determined by gas chromatography with a photoionization detector after liquidnitrogen cold trapping of their hydrides. The sample solution was treated with sodium hydroborate (NaBH₄) under weak-acid conditions for arsenic(III) and antimony(III) determination, and under strong-acid conditions for arsenic(III+V) and antimony(III+V) determination. Large amounts of carbon dioxide (CO₂) and water vapor obscured determination of arsine and stibine. Better separation from interference could be achieved by removing CO₂ and water vapor in two tubes containing sodium hydroxide pellets and calcium chloride, respectively. The detection limits of this method were 1.8 ng dm^?3 for arsenic and 9.4 ng dm^?3 for antimony in the case of 100-cm³ sample volumes. Therefore, it is suitable for determination of trace arsenic and antimony in natural waters.     

Use of Extraction Chromatography, Ion Chromatography and Liquid Scintillation Spectrometry for Rapid Determination of Strontium-89 and Strontium-90 in Food in Cases of Increased Release of radionuclides

For rapid determination of ⁸⁹Sr and ⁹⁰Sr in food, isocratic ion chromatography used for Sr isolation and purification is integrated in a complete analytical system comprising sample preparation, incineration, dissolution, phosphate precipitation for alkali/alkaline carth separation, and Sr specific extraction chromatography on crown ether basis for Ca/Sr separation. Strontium-89 and ⁹⁰Sr are determined by liquid scintillation spectrometry after carbonate precipitation. The components of the mixed spectra obtained are calculated by the computerized spectra subtraction method. Two days plus measuring time are required for single, three for double analysis. The limit of detection for ⁸⁹Sr and ⁹⁰Sr is ca. 0.1 Bq·kg^–1, related to the fresh produce.     

Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of cyanide using cadmium carbonate as a new solid-phase reactor

A new and simple flow injection system procedure has been developed for the indirect determination of cyanide. The method is based on insertion of aqueous cyanide solutions into an on-line cadmium carbonate packed column (25% m/m suspended on silica gel beads) and a sodium hydroxide with pH 10 is used as the carrier stream. The eluent containing the analyte as cadmiumcyanide complexes, produced from reaction between cadmium carbonate and cyanide, measured by flame atomic absorption spectrometry. The absorbance is proportional to the concentration of cyanide in the sample. The linear range of the system is up to 15 mg L⁻¹ with a detection limit 0.2 mg L⁻¹ and sampling rate 72 h⁻¹. The method is suitable for determination of cyanide in industrial waste waters with a relative standard deviation better than 1.22%.     

Rapid non-destructive determination of thin films of platinum by particle back-scattering

Rutherford back-scattering of α-particles is used to determine trace amounts of thin films of platinum. The method is sensitive to 0.3 ng of platinum and the response is linear from at least 0.01 to 80 μg Pt cm^-2 of substrate surface area. Calibration with weighed standards reveals good accuracy and precision throughout the linear range. Up to at least 80 μg cm^-2, no matrix effects can be observed for platinum determinations on Mylar, carbon, glass, and glass or quartz coated with up to 0.5 μm thicknesses of tin oxide. Particle-induced x-ray emission spectra are included to show their utility in surface composition analysis. The analytical procedure for the determination of platinum is rapid and non-destructive, and requires minimal sample preparation.     

A novel approach to Ca-Sr separation in the determination of90Sr using inorganic exchangers: An application to environmental samples

A procedure for⁹⁰Sr determination in calcium rich samples is presented. It is based on the precipitation of calcium oxalate in homogeneous solution and under controlled conditions to minimize the coprecipitation of strontium. The latter is subsequently separated as carbonate and radiochemical purification is completed by ion exchange chromatography on two inorganic exchangers: PRTD (partially reduced tin dioxide) and CUCR (copper chromate). The procedure was applied to environmental samples such as ashed sediment, fish and vegetable and results are reported.     

Ion-chromatographic determination of phosphates in castables

A procedure for the determination of orthophosphate and condensed phosphates in castables is proposed. The sample is calcined with sodium carbonate and leached with deionized water. After removing the interfering components from the matrix by cation-exchange, the sample solution is subjected to ion-chromatographic determination with gradient elution and conductivity detection. Recoveries are within 84–89% with a relative standard deviation of less than 3.6%.     

Solid phase extraction of trace amounts of Pb(II) in opium, heroin, lipstick, plants and water samples using modified magnetite nanoparticles prior to its atomic absorption determination

A new, simple, fast and reliable solid-phase extraction method has been developed for separation/preconcentration of trace amounts of Pb(II) using dithizone/sodium dodecyl sulfate-immobilized on alumina-coated magnetite nanoparticles, and its determination by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after eluting with 4.0?mol?L^?1 HNO₃. Optimal experimental conditions including pH, sample volume, eluent concentration and volume, and co-existing ions have been studied and established. Under the optimal experimental conditions, the preconcentration factor, detection limit, linear range and relative standard deviation of Pb(II) using FAAS technique were 280 (for 560?mL of sample solution), 0.28?ng?mL^?1, 1.4?C70?ng?mL^?1 and 4.6% (for 10?ng?mL^?1, n?=?10), respectively. These analytical parameters using GFAAS technique were 300 (for 600?mL of sample solution), 0.002?ng?mL^?1, 0.006?C13.2?ng?mL^?1 and 3.1% (for 5?ng?mL^?1, n?=?10), respectively. The presented procedure was successfully applied for determination of Pb(II) content in opium, heroin, lipstick, plants and water samples.     

Sequential determination of uranium (IV), free acidity and hydrazine in a single aliquot

A simple analytical procedure for the sequential determination of uranium (IV), free acidity and hydrazine in presence of hydrolysable ions is developed and described. In this method, first, uranium (IV) is determined using fiber optic aided spectrophotometry then same solution is used for determination of free acidity and hydrazine. Free acid is titrated with standard sodium carbonate solution after uranium (IV) is masked with EDTA. Once the end point for the free acid is determined at pH 3.0, an aliquot of formaldehyde is added to liberate the acid equivalent to hydrazine which is then titrated with the same standard sodium carbonate solution using an automatic titration system. The described method is simple, accurate and reproducible. The overall recovery of uranium (IV), nitric acid and hydrazine is 98% with 3% relative standard deviation respectively. The major advantage of the method is that it uses sodium carbonate a primary standard as titrant and generation of corrosive analytical wastes containing oxalate or sulphate is avoided. Valuable metals like uranium and plutonium can easily be recovered from analytical waste before final disposal.     

Determination of low-level90Sr in environmental materials: A novel approach to the classical method

A method was developed for the separation of strontium from large amounts of calcium which does not depend on fuming nitric acid. A sample in the form of mixed carbonates or oxides is stirred into concentrated nitric acid in the proportion 17 w/v. Strontium forms insoluble nitrates while calcium remains in the solution. Two re-precipitation steps combined with an acetone wash yield a very pure strontium salt which is suitable for gravimetric determination of recovery. The method, devised originally for⁹⁰Sr assay in sea water, can also be applied to solid samples which present analytical problems due to their high calcium content.     

Separation of Some Herbicides by Two Dimensional Thin Layer Chromatography on Calcium Sulphate

Abstract

Two dimensional thin layer chromatography is being used for the last forty years¹ and now it has became an important tool for the separations of varying complexity. Various coating materials such as alumina, cellulose, kieselgel G, silica gel, silufol and polyamide have been used and studied for the separation of organics such as alkaloids, amino acids, carbohydrates, fatty acids, glycopeptides, glycolipids, lipids, phospholipids, pigments, protiens, peptides, pesticides, steroids and inorganics such as oxy acids of phosphorus, metal ions. Our previous work^{2′3′4′5′6} shows that calcium sulphate coated paper and glass plates have a great separation potential for herbicides containing carboxyl group. Therefore now an attempt is made to test the separation potential of calcium sulphate alone and calcium sulphate containing aluminium oxide active neutral, calcium carbonate and p-dimethylaminobenzaldehyde for some nerbicides by two dimensional thin layer chromatography. The results obtained are discxissed in this paper.     

Determination of Hg in seawater by inductively coupled plasma mass spectrometry after on-line pre-concentration

A method for the determination of Hg in seawater by inductively coupled plasma mass spectrometry, after an on-line separation and pre-concentration, is described. The matrix separation was accomplished by retention of the Hg complex with the ammonium salt of O,O-diethyl dithiophosphoric acid on C₁₈ immobilized on silica in a micro-column. Before pre-concentration, the seawater sample was acidified with HNO₃ to 0.14 mol l⁻¹. Methanol was used as the eluent, which was introduced into the conventional pneumatic nebulizer of the instrument. External calibration with aqueous analytical solutions, submitted to the same procedure, was used. An enhancement factor of 16 was obtained, and the limit of detection was 5 ng l⁻¹. The sample consumption was 2.3 ml per determination, and the sampling frequency was 21 h⁻¹. The accuracy was tested by comparison with vapor generation inductively coupled plasma mass spectrometry. The agreement between the Hg concentrations measured by the two methods in the seawater samples was good.