The oxidation of thallium(I) by selenious acid

A new and simple method for the quantitative determination of thallium based on the oxidation of TI(I) to TI(III) by selenious acid has been described. The precipitated selenium is weighed directly. Furthermore, the thallic hydroxide obtained by the addition of excess alkali to the filtrate is dissolved in HCl and determined iodometrically. The excess selenious acid in the filtrate is also estimated iodometrically or by gravimetric method after reduction to metallic selenium. Under the specified operative conditions the results are reproducible and accurate within the limits of experimental error.     

Reduction of selenious acid by hydrazine sulphate. Volumetric determination of selenium

Summary A volumetric method of estimating selenium, depending upon the reduction of selenious acid by excess hydrazine sulphate solution and titration of the excess against KIO₃ to the iodine monochloride end point, has been described. Determination of tellurium on these lines is suggested.The author is indebted to Professor S. S.Joshi for facilities and kind interest in the work. The award of a Scientific Man Power Committee Research Fellowship is also gratefully acknowledged.     

Determination of bismuth by forced-flow liquid chromatography

Bismuth(III) is retained on a cation-exchange column from dilute acid and is then separated from most other metal ions by elution with 0.5M hydrobromic acid. The elution curve can be measured spectrophotometrically and automatically recorded. This separation method is rapid and is selective for bismuth.     

Oxidation of 6-methyl-2,4-dioxypyrimidine with selenious acid

The yield orotic aldehyde at the oxidation of 6-methyl-2,4-dihydroxypyrimidine was found to increase when selenious acid is used as an oxidizer. A comparative analysis of 6-methyl-2,4-dioxypyrimidine oxidation with selenium dioxide and selenious acid was performed using the ab initio quantum chemical method in the 6-31G** basis.     

Determination of bismuth oxide in and on high-purity bismuth

Bismuth is dissolved in mercury on shaking with ammonium nitrate solution in a nitrogen atmosphere; bismuth oxide is insoluble and so can be separated by flotation and dissolved in nitric acid for spectrophotometric determination as tetraiodobismuthate(III). The method is applied to various bismuth samples containing about 0.01% Bi₂O₃, the relative standard deviation being 7–11%.     

Chemical amplification method for the determination of selenious acid with bismuthiol II

Summary An amplification method is described for the determination of selenious acid with bismuthiol II. A 9.4 fold amplification is achieved.     

Determination of mercury in bismuth by neutron activation analysis

A method has been developed for the determination of traces of mercury in bismuth by neutron activation analysis. After sample irradiation at a flux of 7 · 10¹³ n cm^-2 s^-1 for 20 min, mercury was separated from bismuth by addition of ammonium sulfide and re-dissolution of bismuth (matrix) sulfide with nitric acid, and filtration of sulfur containing mercury on a membrane filter. The activity of the 68- or 68–77-keV region, counted with a Ge(Li) or NaI(Tl) detector, was used for quantitative measurements. The method was applied to bismuth samples containing 0.1–100 p.p.m. of mercury.     

Determination of bismuth in lead by neutron activation analysis

Neutron activation analysis for bismuth in lead was performed through the separation and measurement of²¹⁰Po, using two different extraction procedures. The reproducibility of the results was good for lead containing bismuth in higher concentrations. For high purity lead, variations in the bismuth content have been found by different analyses of the same sample, owing to inhomogeneity in the distribution of the Bi metal traces. An independent analysis of the same lead samples gave comparable Bi concentrations.     

Determination of chloride ion in bismuth oxide by capillary electrophoresis

A procedure is developed for determining chloride ion in bismuth(III) oxide by capillary electrophoresis with indirect photometric detection after precipitating the major component of the sample as bismuthyl acetate. The mixture containing chromate ion and diethanolamine is used as a separating electrolyte. The detection limit for chloride ions in the developed procedure is 5 × 10^?4%, the relative standard deviation is 15%. The absence of a systematic error is confirmed by atomic absorption and laser mass spectrometry.     

Polarographic and voltammetric behavior of selenious acid and its use in analysis

Solution chemistry of Se(IV), in particular the acid-base properties, salt and complex formation, chemical reduction and reaction of Se(IV) with organic and inorganic sulfur compounds are briefly summarized. The electrochemical reduction of Se(IV) on dropping and stationary mercury electrodes is dealt with in some detail. The effects of antecedent acid-base equilibria and of consecutive reactions of the reduction product, Se(2-), adsorption of their products, and effects of added metal ions are discussed. The principles and applications of stripping analyses for determination of ultratraces of Se(IV) are summarized. The behavior on unreactive (Au, Pt, carbon) and reactive (Hg, Ag, Cu) electrodes are compared.     

Determination of traces of bismuth in copper by anodic stripping voltammetry

Summary Procedures are described for the determination of bismuth impurities in. copper using anodic stripping voltammetry on a hanging mercury drop electrode. Bismuth was previously separated from copper by cation or anion exchange in hydrochloric acid. The method was applied to the analysis of commercially available high purity copper, showing satisfactory sensitivity and accuracy. The detection limit was about 2×10^–9 M bismuth in solution for a pre-electrolysis time of 15 min (–0.5 V vs. Ag/AgCl); this corresponds to 0.004 ppm of bismuth for a 1 g sample and a final volume of 10 ml after separation.

---

Bestimmung von Wismutspuren in Kupfer durch anodische Amalgamvoltammetrie

Zusammenfassung Mit hängendem Quecksilbertropfen. Wismut wird vor der Bestimmung durch Kationen oder Anionenaustausch aus salzsaurer Lösung vom Kupfer abgetrennt. Das Verfahren wurde zur Analyse von handelsüblichem hochreinem Kupfer angewendet. Mit einer Vorelektrolysedauer von 15 min (–0,5 V gegen Ag/AgCl) konnten noch 2×10^–9 M Bi bestimmt werden; das entspricht 0,004 ppm Bi für eine 1 g-Probe bei einem Endvolumen von 10 ml nach der Trennung.

     

分光光度法测定铝合金中的微量铋

研究了在75℃条件下偶氮氯膦(Ⅲ)在HClO4介质中与Bi(Ⅲ)显色生成稳定红色络合物测定微量铋的高灵敏方法。该络合物的最大吸收波长为510nm,摩尔吸光系数ε510=1.567×105L.mol-1.cm-1,Bi(Ⅲ)在0~0.60μg/mL范围内符合比耳定律。已用于铝合金样品中微量铋的测定。     

Spectrophotometric study of bismuth with N-(2-acetamido)iminodiacetic acid (ADA): Determination of bismuth in pharmaceutical formulations

A new method for the Spectrophotometric determination of bismuth using N-(2-acetamido)iminodiacetic acid as complexometric agent is proposed. The complex is formed in a wide pH range, 5.5–7.5, and has a maximum absorption at 265 nm. Beer's law is obeyed in the interval 3.8–17.9 μg of bismuth(III)/ml, with a minimum photometric error of 2.3. The molar absorptivity is 9.1 × 10³ liters/cm mol. The stoichiometry of the reaction takes place in the metal-to-ligand ratio 1:2. The interferences produced by the more common ions are studied. The method has been successfully applied to the determination of bismuth in pharmaceutical formulations.     

Determination of impurities in bismuth by solid-liquid extraction and emission spectrography

Summary A high-purity bismuth metal or bismuth nitrate sample is dissolved in nitric acid and converted to solid basic bismuth nitrate by heating. Impurities such as iron, cobalt, copper, and zinc at the low ppm or ppb level are extracted from the solid with water and determined by DC arc emission spectrography.

---

Zusammenfassung Hochgereinigtes Wismutmetall oder Wismutnitrat werden in Salpetersäure gelöst und durch Erhitzen in festes basisches Wismutnitrat übergeführt. Verunreinigungen wie Eisen, Kobalt, Kupfer und Zink in ppm- oder ppb-Mengen werden aus der festen Probe mit Wasser extrahiert und emissionsspektrographisch bestimmt.

     

枸橼酸铋雷尼替丁胶囊有效成份的紫外分光光度法的测定

提出了对枸橼酸铋雷尼替丁胶囊有效成份进行紫外分光光度测定的新方法，该方法简便、快速、准确度高，能用于纯度较高的样品分析，可作为枸橼酸铋雷尼替丁胶囊药品质量标准控制方法。     

Determination of zinc in high purity bismuth by thermal neutron activation

A neutron activation analysis for the determination of zinc in bismuth was developed. After irradiating the samples for 44 days at 4·10¹¹n/cm²/sec, zinc was separated quantitatively by hexone extraction and precipitation as quinaldate. The sensitivity of the method was estimated as 0.05 p.p.m. No zinc could be detected in the high purity bismuth samples. An addition method of analysis showed that the precision was 1.2%.     

Amperometry with two polarisable electrodes-XI Determination of bismuth by EDTA titration

Optimum conditions have been found for a highly selective determination of bismuth via EDTA titration with biamperometric indication of the end-point. The influence of the applied potential, pH and stirring on the accuracy and selectivity of the determination has been studied. In a medium of 0.4M nitric acid only high concentrations of iron(III) and copper(II) interfere with the determination of bismuth. Zirconium, thallium(III) and indium interfere even in small concentrations. The average error of the determination of 5-100 mg of bismuth (when titrated with 0.05M EDTA solution) is +/-0-1 % rel. and for the determination of 0.5-10 mg it is +/-0.3% rel. (0.005M EDTA). The method has been verified by the analysis of a Wood's metal of known composition.     

Determination of trace bismuth by flow injection-hydride generation collection-atomic absorption spectrometry

Bismuth hydride gas was collected on-line and determined via a new flow injection-hydride generation collection-flame atomic absorption spectrometry system. The performance of the gas-liquid separator, hydride gas collection time, acidity of the sample solution, NaBH(4) concentration, and the effects of concomitant interferents were investigated to optimize the conditions of this new method. Interferences from concomitant elements were investigated, and recoveries of 94.7-105.3% for 10 ng mL(-1) Bi were obtained after the addition of 0.2% ascorbic acid-thiourea masking reagents. The sensitivity of this new method was one order of magnitude higher than the continuous flow-hydride generation-flame atomic absorption method with a detection limit of 0.25 ng mL(-1) and a precision of 2.3%. The method was evaluated by determining trace bismuth in standard biological reference material human hair GBW07601, and the results were consistent with the certified value. The proposed method was then employed to determine trace bismuth in ten colored gelatin samples; recoveries of 94.2-105.8% were obtained.