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.     

EDTA滴定法连续测定铅精矿中铅和锌

建立了EDTA滴定法连续测定铅精矿中铅和锌的方法。试样用盐酸、硝酸、硫酸和氯酸钾分解。铅通过硫酸铅沉淀与其他干扰元素分离,沉淀溶解于乙酸-乙酸钠溶液中。在滤液中加入氨水、氟化钾使铁等干扰元素沉淀并与锌溶液分离。用二甲酚橙作指示剂,EDTA分别滴定溶液中的铅和锌。研究中测定了能力验证NILPT(2010)-0211铅精矿样品10-1和10-2中铅和锌,结果满意。     

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.     

Determination of Sulphate by Titrimetric and Colorimetric Measurement of Equivalent Displaced Zinc Ion

Abstract

Two methods are described for the determination of sulphate in the range of 200 μg to 100 mg by dissolving precipitated barium sulphate in excess of EDTA at pH 12.5. A titrimetric procedure involves back titration of excess EDTA with a standard zinc solution, while a complementary spectrophotometric method makes use of the stability of the barium EDTA complex in the presence of an excess of zinc ions; the latter are reacted with zincon and are equivalent to the amount of sulphate present.     

Complexometric determination of aluminium in iron ore,sinter, concentrates and agglomerates

A method for the complexometric determination of aluminium in iron ore, sinter, concentrates and agglomerates encountered in international trade is described. The sample is fused in a zirconium crucible with a mixed flux of sodium carbonate and sodium peroxide. The fused mass is completely soluble in hydrochloric acid. The R₂O₃ oxides are then precipitated with ammonia and redissolved in hydrochloric acid. Elements such as iron, titanium and zirconium are separated from aluminium by solvent extraction with cupferron and chloroform. After removal of traces of organic matter from the aqueous phase, the solution is treated with an excess of EDTA, which is then back-titrated with zinc solution (Xylenol Orange as indicator). Addition of ammonium fluoride then releases EDTA equivalent to the aluminium and this is titrated with zinc solution. The method is rapid. The precision and accuracy are excellent, and the results comparable with those obtained by the referee method.     

A new approach for obtaining total tryptophan recovery in plasma samples deproteinized with sulphosalicylic acid.

The treatment of plasma with a sodium dodecy sulphate solution before deproteinization with sulphosalicylic acid is described. With this treatment, the liberation of tryptophan from plasma albumin is complete and its determination can be made directly, together with that of other amino acids and related compounds, by automatic ion-exchange chromatography, eliminating the need for an extra analysis for the accurate determination of this amino acid. Results of tryptophan recovery tests, carried out both on plasma samples simply deproteinized with sulphosalicylic acid and on other samples pre-treated with sodium dodecylsulphate solution are reported. These results are also compared with those obtained when trichloroacetic acid was used as deproteinizing agent. A recovery study on a human albumin (fraction V) solution containing a known amount of tryptophan is also described.     

Determination of fluoride in zinc concentrates, processing products and solutions with an ion-specific electrode

Determination of fluoride in hydrometallurgical zinc-plant processing products and solutions with a fluoride-ion electrode is described. Various types of buffers were tested, to find a suitable common buffer for use in analysis of all types of substances generated at the zinc plant. The method involves decomposition of samples either by fusion with sodium hydroxide or by leaching with perchloric acid to bring fluoride into solution. The fluoride concentration is measured directly with a fluoride-specific electrode. In standard addition tests 100% recovery was obtained when a citric acid/sodium nitrate buffer was used. Validation tests gave satisfactory results.     

Bestimmung von Sulfat mit Hilfe einer modifizierten FIA-Methode und Vergleich mit der Methode DIN 38405 Teil 5

Summary In general the DIN-method 38405, Part 5 is stipulated and used to determine sulphate in drinking and waste water. Since the processes of complexometric titration after ion exchange and precipitation described in those methods are rather time consuming and the number of samples to take is constantly increasing, it is opportune to adopt more rapid methods. For this purpose, flow injection analysis (FIA) is also suitable in addition to ion-chromotography.We have therefore revised and modified the analysis method ASTN 15/84, published by Tecator. This is based on the following principle:Methylthymolblue added to barium ions in an alkaline and alcoholic solution results in a blue complex with a peak at about 620 nm.Sulphate contained in the sample will precipitate out of the complex barium sulphate and the loss of coloration can be measured photometrically. In the revised version the method is especially suitable for routine tests. In order to prove that the results obtained are equivalent to those of the DIN-method, the equivalence of both methods has been examined according to DIN 38402, Part 71.The test has shown that the same results are obtained with both methods. Significant differences are not ascertainable.     

Selective complexometric determination of mercury with sulphite as indirect masking reagent

A complexo-titrimetric method for the determination of mercury(II) in the presence of other metal ions is described, based on the selective masking ability of sulphite ion towards Hg(II). Mercury in a given sample solution is initially complexed with a known excess of EDTA and the surplus EDTA titrated with zinc sulphate solution at pH 5.0–6.0 (hexamine), using xylenol orange (or methylthymol blue) as indicator. An excess of solid sodium sulphite is then added to decompose the Hg(II)-EDTA complex and the released EDTA is titrated with standard zinc sulphate solution. Reproducible and accurate results are obtained for 9.9–99 mg Hg with relative errors < 0.35% and standard deviations < 0.05 mg. The effects of various cations and anions are studied.     

Quantitative precipitation of large amounts of sodium as sodium zinc uranyl acetate and its determination by an indirect complexometric method

Up to 40 mg of sodium can be quantitatively precipitated as sodium zinc uranyl acetate if enough reagent of appropriate composition is added to make the concentrations of zinc and uranium in the mother liquor at least 1.25 and 0.14M respectively. In practice, the reagent solution contains 100 g of uranyl acetate and 300 g of zinc acetate per litre and the volume added (ml) must be at least 15 times that of the solution to which it is added or 1.5 times the number of mg of sodium present, whichever is the greater. The triple salt can then be dissolved in water and the zinc selectively titrated with EDTA at pH 5.3, with Xylenol Orange as indicator. The uranium is masked with ammonium fluoride. Most constituents of ceramics and other silicates, including barium, strontium, magnesium, potassium, sulphate, phosphate and arsenate, do not interfere.     

Non-aqueous titration of quinine and quinidine sulphates by use of barium perchlorate

A simple non-aqueous titration method has been devised for determining the sulphates of quinine and quinidine. The sulphate is precipitated by addition of excess of barium perchlorate solution in acetic and the liberated alkaloid is then titrated in 1:2 anhydrous acetic-dioxan mixture, with an acetic acid solution of perchloric acid. The end-point is determined either visually with Crystal Violet as indicator or potentiometrically with a glass-Ag/AgCl combination electrode. The method is accurate, precise and suitable for routine analysis of pure materials and tablets.     

The titrimetric determination of sulphate,thiosulphate and polythionates in mining effluents

A titrimetric procedure is described for the determination of various forms of sulphur (sulphate, sulphite, thiosulphate, dithionate, tri- and tetrathionates after conversion to sulphate) in mining effluents. Metal ions are removed, after an oxidizing step, by a cationexchange resin, and the sulphate is precipitated with a known excess of 0.01 M barium chloride at pH 3.5. The excess of barium is back-titrated with standard 0.01 M ethylenediaminetetraacetic acid (EDTA) solution to a o-cresolphthalein complexone end-point at pH 11.0. The results obtained are in good agreement with those obtained by lengthy gravimetric procedures. Indirectly, dithionate can be determined, and sulphate and oxidizable thio salts such as thiosulphate and di-, tri-, and tetrathionates can be distinguished.     

Complexometric estimation of ferric iron

Summary Ferric iron has been determined alone or in presence of barium chloride, calcium chloride, magnesium sulphate, mercuric chloride, manganese sulphate, strontium nitrate, chromic sulphate or zinc sulphate by titrating it with EDTA, using potassium thiocyanate-p-anisidine indicator. In these complexometric titrations, the quantitative results obtained by using potassium thiocyanate-p-anisidinie indicator are comparable with those obtained with Bindschedler's green indicator; and the metallic salts mentioned above do not interfere in the estimation of ferric iron by this method.     

Direct titration of potassium ferricyanide with hydrazine sulphate in presence of zinc sulphate determination of hydrazine

Operative conditions for direct titration of potassium ferricyanide solution with a solution of hydrazine sulphate which contains zinc sulphate are described. The results are comparable with those obtained by the standard iodate procedure. The chief advantages of the present method of estimating hydrazine are (1) titration in slightly acidic medium and (2) no indicator is required. Determination of substituted hydrazines, hydroxylamine and other reducing substances on similar lines is suggested.     

Sulphate determination after its reduction to hydrogen sulphide and volatile separation by molecular absorption spectrometry

A rapid spectrophotometric method for sulphate determination in a discontinuous mode is described. The method is based on sulphate reduction to hydrogen sulphide followed by its volatilization and absorption in an alkaline solution. The reduction is obtained when a sulphate sample is heated to 287 degrees C for 15 min, with a mixture of Fe(o)/KI and phosphoric acid. The resulting gas is swept by nitrogen flow into a 0.1 M sodium hydroxide solution and the absorbance of the sulphide ions is measured directly at 230 nm. The proposed method enabled us to determine 50-700 mug of total sulphate with a relative standard deviation of the order of 5%. The method has been applied for the determination of sulphates in liquid (mineral waters) and solid (gypsiferous soils) samples.     

Errors in the determination of silica in lead-bearing samples caused by preliminary separation of lead sulphate

Some procedures for the gravimetric determination of silica in lead-bearing samples involve the extraction of lead sulphate with ammonium acetate. Results for silica are then low because some silica is dissolved in ammonium acetate solution. Correct results can be obtained only by avoiding fuming with sulphuric acid. If samples contain a large proportion of insoluble silica, preliminary fusion with sodium hydroxide is recommended.     

Spectrophotometric determination of chloride in barium sulphate precipitates following isolation of the analyte

A spectrophotometric method was developed for the determination of chloride concentrations between 0.2 and 5 mgL^?1 in barium sulphate precipitates, obtained by precipitation of sulphate in concentrations of 50 to 250 mgL^?1 or even lower. The proposed method involves prior dissolution of the barium sulphate precipitate in hot conc. sulphuric acid and collection of the released hydrogen chloride by means of gaseous nitrogen. The analytical calibration function was obtained by the least-squares procedure from 10 determinations at each of three concentration levels of a standard solution of chloride. The lack of fit of experimental points to the least-squares straight line was found to be negligible at a significance level of 5%. Blank measurements were required in all instances as the blank absorbance varied with time.     

EDTA滴定法测定含锌物料中氧化锌

采用氯化铵-氨水体系溶解试样,干过滤后,向移取的滤液中加入氯化钡和硫酸共沉淀铅离子,过滤分离硫酸铅沉淀,向滤液中加人抗坏血酸、氟化钾、硫代硫酸钠等掩蔽剂掩蔽少量干扰元素。在pH=5~6的乙酸-乙酸钠缓冲溶液中,以二甲酚橙为指示剂,用EDTA标准滴定溶液滴定测得结果为氧化锌、水溶性锌和镉合量,扣除由原子吸收光谱法测得的水溶性锌量和镉量,即为氧化锌量。对总氨浓度、氯化铵-氨水浓度比、溶液加入量、搅拌时间、共存离子干扰、精密度等进行了实验,建立了EDTA滴定法测定含锌物料中氧化锌物相的分析方法。实验证明,氧化锌含量在24%~83%时,方法精密度(RSD)为0.25%~0.54%,加标回收率在99%~104%,完全满足含锌物料中氧化锌的测定要求。     

Gravimetric determination of gold with sodium salt of n-(n-bromo-c-tetradecyl betainyl)-c-tetradecylbetaine

The sodium salt of N-(N-bromo-C-tetradecyl betainyl)-C-tetradecyl betaine is presented as a gravimetrie reagent for the determination of gold. Two complexes have been isolated; one, precipitated from hydrochloric acid solution, containing 22.14% gold; the other, from hydrobromic acid solution, containing 18.01% gold. Both complexes may be dried to constant weight at 85° C, thus giving the advantage of a favorable weight factor. Determinations from hydrobromic acid solutions are more rapid and offer several other advantages. Optimum conditions have been established. The number of interfering ions is small and a method for thie separation of gold from these ions was developed. A procedure for the determination of gold in ore concentrates was applied to several samples with satisfactory results.