Determination of the total calcium concentration of serum by ICAP-AES

Summary The determination of nitrate, nitrite, phosphate, chloride and sulphate in aqueous extracts of salads and vegetables by ion chromatography is described. The method is reliable and fast, and needs no derivatisation nor clean-up besides filtration. Without using a preconcentration column, the detection limits are 0.1 ppm for nitrate, nitrite and sulphate, 0.04 ppm for chloride and 0.4 ppm for phosphate. Calibration curves with reference to peak heights are linear within the concentration range usually obtained.

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Bestimmung von Nitrat und anderen anorganischen Anionen (NO ₂ ^– , PO ₄ ^3– , Cl^–, SO ₄ ^2– ) in Salat und Gemüse durch Ionen-Chromatographie

Zusammenfassung Es wird die Bestimmung von Nitrat, Nitrit, Phosphat, Clorid und Sulfat in wässrigen Extrakten von Salat und Gemüse durch Ionen-Chromatographie beschrieben. Die Methode ist zuverlässig und schnell und bedarf neben der Filtration keiner weiteren Derivatisierungsoder Reinigungsschritte. Die Nachweisgrenze liegt für Nitrat, Nitrit und Sulfat bei 0,1 ppm, für Chlorid bei 0,04 ppm und für Phosphat bei 0,4 ppm, dies ohne Vorkonzentrierung. Im üblicherweise verwendeten Konzentrationsbereich sind alle Eichkurven linear.

     

Preparation of quaternized dimethylaminoethylmethacrylate grafted nonwoven fabric for the removal of phosphate

Dimethylaminoethylmethacrylate (DMAEMA) grafted polyethylene/polypropylene (PE/PP) nonwoven fabric was prepared by radiation-induced graft polymerization. Grafting conditions were optimized and about 150% DMAEMA grafted samples were used for further experiments. DMAEMA graft chains were later quaternized with dimethyl sulphate for the removal of phosphate ions. Adsorption experiments were conducted with quaternized DMAEMA grafted fabric for phosphate removal at low (0.5–25 ppm) and high phosphate concentrations (50–1000 ppm). Adsorbed phosphate amounts at pH 7 were found to be 63 mg phosphate/g polymer and 512 mg phosphate/g polymer for low (25 ppm) and high phosphate concentrations (1000 ppm) respectively showing the efficiency of the adsorbent material in removing phosphate. The pH effect on phosphate adsorption showed that the quaternized DMAEMA grafted nonwoven fabric can adsorb phosphate over a wide pH range (5.00–9.00) indicating that adsorbent material can effectively remove different forms of phosphate ions, namely H₂PO₄^?, HPO₄^2? and PO₄^3? in aqueous solution at this pH range where the species exist. Competitive adsorption experiments were also carried out with two concentration levels at pH 7 to investigate the effect of competing ions. Phosphate adsorption on quaternized DMAEMA grafted nonwoven fabric was found to be higher than the other competing ions at two concentration levels. At high concentration level, the adsorption order was phosphate>nitrite>bromide>sulphate>nitrate whereas at low concentration level, the order was phosphate?sulphate>bromide>nitrite>nitrate.     

An improved turbidimetric procedure for the determination of sulphate in plants and soils

A rapid turbidimetric procedure for the determination of sulphate in soils and plants has been developed with sorbitol as stabilizing agent. When used in a concentration of 20% in the final volume, the sorbitol regulates the size of the BaSO(4) particles formed and stabilizes them against sedimentation, growth and aggregation for long periods of time. The conditions of precipitation are not rigorous, as they are in similar procedures. Linearity of the calibration curve up to 50 ppm of sulphate and good reproducibility are special attributes of the procedure.     

Studies in atomic-fluorescence spectroscopy-V The fluorescence characteristics and determination of antimony

Atomic-fluorescence of antimony may be generated in an air-propane flame by nebulizing aqueous solutions of antimony salts whilst irradiating the flame by means of a microwave-excited electrode-less discharge tube operating at 30 W. The strongest fluorescence is exhibited by the (4)S(11 2 ) --> (4)P(1 3 ) 2311 A resonance line and weaker signals are observed at the 2068 and 2176 A resonance lines and at four intercombination lines, at 2598, 2671, 2770 and 2878 A. A process of thermally assisted direct-line fluorescence is postulated to account for the otherwise inexplicable intensity of the 2598 A line emission. Atomic-fluorescence spectroscopy at 2176 A permits the determination of antimony in the range 0.1-120 ppm with a detection limit of 0.05 ppm. With the same equipment and source, the range of measurement for atomic-absorption was 6-120 ppm and the detection limit was 1 ppm. No interferences were observed from 100-fold molar amounts of Cd, Co, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, NH(4), Pb and Zn or from arsenate, chloride, nitrate, phosphate and sulphate.     

Determination of trace amounts of sulphur in selenium

Determination of trace amounts of sulphur as Methylene Blue after reduction of sulphate to sulphide by hydriodic and hypophosphorous acids in acetic acid solution is applied to the determination of trace amounts of sulphur in selenium after removal of the selenium by evaporation with hydrobromic acid. Samples of 100 mg or less of selenium are chosen if the sulphur content is greater than 5-10 ppm; the time required for the separation is about 1.5 hr; 100 ppm of sulphur has been determined with a coeffident of variation of 5.2%. If the sulphur content is less than 5 ppm, 1-g samples must be taken and the time required is then about 3 hr; 0.4 ppm of sulphur has been determined with a standard deviation of 0.13 ppm. The accuracy of the method seems to be well within the random error.     

Über basische Aluminiumsalze und ihre Lösungen. XI. Vergleichende 27Al-NMR-Untersuchungen am Mineral Zunyit und basischen Aluminium-Salzen mit tridekameren Al-oxo-hydroxo-aquo-Kationen

Basic Aluminium Salts and their Solutions. XI. ²⁷Al-NMR Studies Comparing the Mineral Zunyite and Basic Aluminium Salts of Tridecameric Al-oxo-hydroxo-aquo-Cations Solid-state high resolution ²⁷Al NMR studies of basic aluminum sulphate and the mineral zunyite, both containing tridecameric Al-oxo-hydroxo groups, show different ²⁷Al spectra. While for zunyite both AlO₆ octahedra (0 ppm) and the central AlO₄ tetrahedron (69 ppm) are observed in the spectrum, in the case of the basic aluminum sulphate only the tetrahedrally coordinated Al (59 ppm) is detected by NMR. This behaviour is explained by structural data, which indicate stronger distortions of the AlO₆ octahedra in the case of the basic aluminum sulphate. The increased shielding of the fourcoordinated Al of the basic sulphate is attributed to an increased ionic character of the Al? O bond in this compound.     

Extraction - Spectrophotometric Determination of Phosphate Using N-Phenylbenzohydroxamic Acid

Abstract

A simple solvent extraction and spectrophotometric method for the determination of micro amount of phosphate (PO₄) is described. Phosphate is selectively separated from associated elements by reacting it with calcium and extracting excess calcium with N-phenylbenzohydroxamic acid (PBHA) at pH 11.3. The excess calcium was determined in ultra-violet and visible region and hence the phosphate content was calculated. The Beer's law is obeyed in the range 0.5 ? 10.0 ppm at 340 nm and 0.25 - 8.0 ppm at 560 nm of phosphate for a fixed amount of calcium (20.0 ppm). These results are also compared with those obtained by atomic absorption spectrophotometry. The method has been applied for the determination of phosphate in pharmaceutical and other samples.     

Removal of sulphate and phosphate from aqueous solutions using a food grade polysaccharide as flocculant

The mucilage extracted from the seeds of Tamarindus indica pods, a food grade natural polysaccharide, is used as a flocculant for removal of sulphate and phosphate ions in aqueous medium. The maximum removal obtained was 73.71% for sulphate ions and 75.71% for phosphate ions after 30 min. The optimum mucilage dose was 50 mg/L for both sulphate and phosphate ions. The maximum removal was obtained at acidic pH for both the ions. A series of contact time experiments were conducted to assess the system variables such as concentrations of mucilage and ions and pH. The conductivity measurements were also done and correlated with the percent removal. This eco-friendly food grade polysaccharide was proved to be a very good flocculant for the removal of sulphate and phosphate ions.     

Spectrophotometric determination of calcium with a flow injection system

The indirect spectrophotometric determination of 0.8–7.2 ppm calcium in the presence of magnesium, phosphate and sulphate by flow injection analysis (f.i.a.) is described. The method is based on the exchange reaction between the calcium and the zinc complex of ethylene glycol-bis(2-aminoethylether)tetraacetic acid (EGTA) in the presence of 4-(2-pyridylazo)resorcinol (PAR): Ca + Zn(EGTA) + 2 PAR ? Zn(PAR)₂ + Ca(EGTA). A home-made and a commercial flow injection system with a sampling rate of 80 h^?1, are compared. Results for water samples are in good agreement with those obtained by atomic absorption spectrometry.     

The indirect spectrophotometric determination of sulphate with 2-aminoperimidine hydrochloride

Summary A method is described for the indirect determination of sulphate after precipitation of 2-aminoperimidine sulphate. Beer's law is obeyed over the range 0–30 ppm. Interferences have been investigated. The application of the method to rainwater is discussed.

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Zusammenfassung Ein Verfahren zur indirekten Bestimmung von Sulfat nach Fällung als 2-Aminoperimidinsulfat wurde beschrieben. Zwischen null und 30 ppm ist das Beersche Gesetz erfüllt. In Betracht kommende Störungen wurden geprüft. Die Anwendung der Methode auf Regenwasser wurde erörtert.

     

Turbidimetric determination of sulphate in plant digests and natural waters by flow injection analysis with alternating streams

An improved flow injection system with alternating streams of reagents is described for the turbidimetric determination of sulphate. Samples are injected into an inert carrier stream which is mixed with barium chloride to form a barium sulphate suspension. The range of the method can be extended to low concentrations by continuously adding sulphate to the sample carrier stream. System performance is improved by automatic alternate pumping of the reagent stream and an alkaline EDTA solution at high flow rate. All operations are controlled by an electronically-operated proportional injector-commutator. Even after routine analysis of 3000 samples of natural waters and plant digests, baseline drift was not observed. The proposed method is suitable for 120 samples per hour with a relative standard deviation less than 1% for sulphate concentrations in the range 1–30 ppm (waters) or 5–200 ppm (plant digests). The results compare well with those obtained by standard manual procedures.     

A Raman and infrared spectroscopic study of the mineral delvauxite CaFe4(3+)(PO4,SO4)2(OH)8·4-6H2O--a 'colloidal' mineral

The mineral delvauxite CaFe(4)(3+)(PO(4),SO(4))(2)(OH)(8)·4-6H(2)O has been characterised by Raman spectroscopy and infrared spectroscopy. The mineral is associated with the minerals diadochite and destinezite. Delvauxite appears to vary in crystallinity from amorphous to semi-crystalline. The mineral is often X-ray non-diffracting. The minerals are found in soils and may be described as 'colloidal' minerals. Vibrational spectroscopy enables determination of the molecular structure of delvauxite. Bands are assigned to phosphate and sulphate stretching and bending modes. Two symmetric stretching modes for both the phosphate and sulphate symmetric stretching modes support the concept of non-equivalent phosphate and sulphate units in the mineral structure. Multiple water bending and stretching modes imply that non-equivalent water molecules in the structure exist with different hydrogen bond strengths.     

Determination of radioactive bulk and surface concentration by beta-detection

Electrolytes of alkaline zincate, acidified zinc sulphate, zinc-ammonia, zinc-ammonia-EDTA, zinc-EDTA/NaOH have been examined in order to verify their applicability for electrodeposition (ED) of zinc on stainless steel (SS) disc at ppm level. Operating parameters suitable for ED of zinc at 90% deposition (amount of zinc removed from plating solution) on SS disc using a total 1 ppm zinc in a 5 cm³ bath volume were determined. It helped to prepare radioactive source (⁶⁵Zn) using inactive Zn as carrier. Speciation of zinc in a Zn-oxalate-EDTA-ammonia bath has been computed.     

31P-Kernresonanzspektrometrische Untersuchungen an Phosphato-Cobalt(III)- und Rhodium(III)-Komplexen

³¹P N.M.R. Spectroscopic Investigations of Phosphato Complexes of Cobalt(III) and Rhodium(III) ³¹P n.m.r. spectra of phosphato complexes of cobalt and rhodium(III) are recorded. The coordination shift of monodentate phosphate is 8–9 ppm, of bidentate phosphate 18 ppm, of phosphite 10–11 ppm, of fluorophosphate 6–7 ppm. Monophosphato and pentaamminaquacobalt complexes condense with the elimination of water to a m?-complex. The ability of the phosphato complexes of cobalt(III) to condense phosphate to diphosphate was investigated. After heating [CoPO₄en₂] · 2 H₂O with an excess of dihydrogenphosphate only small amounts of the expected diphosphate complex could be detected. The analogous reaction with fluorophosphate results in an appreciably higher yield of the diphosphate complex.     

Determination of barium in sulphide ores, concentrates and other geological samples by flame atomic-absorption spectrometry

A rapid, precise and selective analytical method has been developed for estimation of barium in geological samples by flame atomic-absorption spectrometry. The method consists of precipitation of barium sulphate with ammonium sulphate, followed by dissolution of the sulphates in EDTA at pH 10. The barium in this solution is measured by AAS with a nitrous oxide-acetylene flame. Appreciable amounts of lead, calcium and strontium can be tolerated in the method, which has been applied for estimation of barium in sulphide ores and concentrates of lead, zinc and copper, and is feasible for estimation of barium from 20.0 ppm to the per cent level in such geological samples.     

Response Surface Optimization of the Critical Medium Components for Pullulan Production by <Emphasis Type="Italic">Aureobasidium pullulans</Emphasis> FB-1

Culture conditions for pullulan production by Aureobasidium pullulans were optimized using response surface methodology at shake flask level without pH control. In the present investigation, a five-level with five-factor central composite rotatable design of experiments was employed to optimize the levels of five factors significantly affecting the pullulan production, biomass production, and sugar utilization in submerged cultivation. The selected factors included concentration of sucrose, ammonium sulphate, yeast extract, dipotassium hydrogen phosphate, and sodium chloride. Using this methodology, the optimal values for concentration of sucrose, ammonium sulphate, yeast extract, dipotassium hydrogen phosphate, and sodium chloride were 5.31%, 0.11%, 0.07%, 0.05%, and 0.15% (w/v), respectively. This optimized medium has projected a theoretically production of pullulan of 4.44%, biomass yield of 1.03%, and sugar utilization of 97.12%. The multiple correlation coefficient ‘R’ was 0.9976, 0.9761 and 0.9919 for pullulan production, biomass production, and sugar utilization, respectively. The value of R being very close to one justifies an excellent correlation between the predicted and the experimental data.     

Polarographic determination of impurities in high-purity phosphorus

Square-wave and radio-frequency polarographic techniques in phosphoric acid-potassium chloride media are applied to the simultaneous determination of copper, lead and cadmium in highpurity red phosphorus down to a level of 0.1 ppm. In addition ca. 0.01 ppm of cadmium is determined by R.F. polarography in potassium sulphate base electrolyte after cation-exchange separation.     

Uranium in phosphate rock and derivates

It is well known that phosphate rock contains a small amount of uranium. During the production of phosphate fertilizers, most uranium present is found in the phosphate fraction. Uranium was determined in the 70–200 ppm range in the phosphate rock and the final products by nuclear and classical methods.     

Sur la thermogravimétrie des précipités analytiques : Dosage du Glucinium (Béryllium)

The authors have studied, by means of the chevenard thermobalance, the pyrolysis of the hydroxide, crystalline sulphate, amorphous sulphate and ammoniacal phosphate of beryllium. They recommend the apparatus for carrying out the automatic determination of beryllia after heating to 951° only, instead of 1200° C. They give reasons why weighing as anhydrous sulphate is far from being satisfactory and indicate their preference for the pyrophosphate.     

Bestimmung von geringen Mengen Arsen in Kupfer und Kupfersalzen

Zusammenfassung Es wird ein für routinemäßige Analysen geeignetes Verfahren zur Bestimmung kleiner Arsenmengen in Kupfer, Kupfer(I)- und Kupfer(II)-verbindungen beschrieben, mit dessen Hilfe Arsengehalte bis hinab zu 0,4 ppm, unter geeigneten Bedingungen bis zu 0,1 ppm bestimmt werden können. Die Methode beruht auf der Anreicherung des Arsens durch Mitfällung als Arsenat mit Magnesiumammoniumphosphat und anschließender Destillation als Arsenwasserstoff. Die Bestimmung erfolgt spektralphotometrisch mit Silberdiäthyldithiocarbamidat.

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Summary A method for the determination of small amounts of arsenic in copper, cupric and cuprous salts is described. Normaly values down to 0.4 ppm arsenic are detectable by this procedure, or even 0.1 ppm under special conditions. The method is especially well suitable for routine tests. The procedure is based on concentrating the arsenic by co-precipitation as arsenate with magnesium ammonium phosphate followed by a distillation of the arsenic via hydrogen arsenide and on the photometrical determination with silver diethyldithiocarbamate.