Thermogravimetric investigation of manganese(ii), silver and thorium diliturates

Thermolysis curves for manganese(II), silver and thorium diliturates were obtained. Manganese diliturate precipitated as the octahydrate and dehydrated in two steps. Silver diliturate formed as a monohydrate from aqueous solutions. Thorium diliturate formed as a hydrate containing 20 moles of water and dehydrated in two steps.Methods for the thermogravimetric determination of manganese(II) and thorium by precipitation as the diliturates are suggested.     

Thermogravimetric investigation of scandium,yttrium and the rare earth metal diliturates

Thermolysis curves for scandium, yttrium, lanthanum, cerium(III), neodymium, samarium, gadolinium, dysprosium and erbium diliturates are described, Scandium diliturate forms a 15-hydrate which dehydrates in 3 steps. The other diliturates all form 12-hydrates which dehydrate smoothly. All of the anhydrous diliturates are thermally stable to about 240°.Solubilities in water for scandium, yttrium, lanthanum, cerium(lll), neodymium, samarium. gadolinium, dysprosium and erbium diliturates are given. Scandium diliturate is the most soluble and neodymium diliturate the least soluble. Solubilities of rare earth diliturates not investigated can be predicted approximately.Methods for thermogravimetric determination of yttrium, lanthanum, neodymium, samarium, gadolinium, dyprosium, and erbium as the diliturates have been developed. The precipitates are quite dense, easily handled and filterable. Weighing as the diliturate salts gives these determinations a very favorable gravimetric factor.     

Thermogravimetric investigation of the alkaline earth diliturates

Thermolysis curves for calcium, strontium and barium diliturates were obtained. Calcium dilituratc forms an octahydrate from aqueous solution while strontium, dilituratc forms a. heptahydrate and barium diliturate forms a tetrahydrate.Methods for the thermogravimetrie determination of strontium and barium were developed and found to be quite accurate; calcium can only be determined semi-qnartitatively by precipitation as the diliturate salt.     

Thermogravimetric determination of ethylenediamine and quinine with dilituric acid: Solubilities of some polymethylenediamine diliturates

The thermolysis curve's of ethylenediamine, trimethylenediamine, tetramethylenediamine pentamethylenediamine, trimethylamine and quinine diliturates were determined. These curves established that (either the hydrated or the anhydrous form of ethylenediamine and quinine diliturate is stable enough for their gravimetric use to be possible. Both ethylenediamine and quinine were determined by precipitation with alcoholic dilituric acid .solution. In addition the solubilities of some polymethylenediamine diliturates were determined.     

Optical crystallographic properties of some chemotherapeutic compounds used in tuberculosis

Summary The optical properties of isonicotinic acid hydrazide, isonicotinic acid hydrazide diliturate, 1-isonicotinyl-2-benzylidene hydrazide, 1 -isonicotinyl-2-isopropyl hydrazide, Tibione, and Tibione-p-nitrophenyl hydrazone have been determined. The melting points, densities, and molar refractions of these compounds have been determined. The optical properties are valuable for identification purposes.

---

Zusammenfassung Die optischen Eigenschaften der Kristalle von Isonikotinsäurehydrazid, Isonikotinsäurehydraziddiliturat, 1-Isonikotinyl-2-benzylidenhydrazid (Isoteben), 1-Isonikotinyl-2-isopropylhydrazid, 4-Acetylaminobenzaldehydthio-semicarbazon (Tibion, Conteben) und Tibion-p-nitrophenylhydrazpn wurden bestimmt. Außerdem wurden für diese Verbindungen Bestimmungen von Schmelzpunkt, Dichte und Molekularrefraktion ausgeführt. Die optischen Eigenschaften der Kristalle eignen sich für die Feststellung der Identität,

---

Résumé Détermination des propriétés optiques des points de fusion, des densités et des réfractions moléculaires de l'hydrazide isonicotinique, du diliturate de l'hydrazide isonicotinique, de Pisonicotinyl-1, benzylidene-2 hydrazide, de l'isonicotinyl-1, isopropyl-2 hydrazide, de la tibione et de la p-nitrophénylhydrazone de la tibione. Les propriétés optiques sont utilisables pour l'identification de ces composés.

---

---

Dedicated to Prof.Hans Lieb on occasion of his 70th birthday.     

复杂高铋物料中铅的Na2EDTA滴定法测定

复杂高铋物料中,铋、砷、锑、锡四元素含量高且共存时会影响铅的测定。特别是铋含量高时对铅的测定影响大。实验用EDTA—酒石酸联合掩蔽铋、砷、锑、锡,在稀硫酸介质中以硫酸钾为沉淀剂,使铅生成硫酸铅钾复盐沉淀而与铋、砷、锑、锡、铁、铜、锌、铝、钴、镍等干扰离子分离,沉淀以乙酸-乙酸钠浸取,二甲酚橙为指示剂,Na2EDTA滴定法测定铅。试验进一步优化了测定条件,确定最佳条件：硫酸（1 1）加入量为7mL、硫酸钾用量为5g、煮沸时为5min、沉淀陈化时间为2h、EDTA 50g/L 加入量为10mL、酒石酸用量为0.5g,铅的回收率99.70% ～100.65%。将实验方法应用于测定复杂高铋物料中铅,标样BY0111-1与给定值一致,相对标准偏差（n=11）RSD 0.20%～0.23%,满足生产测试要求。     

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。     

Diethylenetetra-ammonium sulphatocerate as volumetric reagent: Iodine monochloride method. Indirect determinations

In presence of 4N to N hydrochloric acid, diethylenetetra-ammnonium sulphatocerate was used as a volumetric reagent to determine indirectly potassium iodate, potassium metaperiodate, potassium dichromate, potassium bromate, ceric sulphate, hydrogen peroxide, lead dioxide and chloramine-B by the iodine monochloride method. An excess of potassium iodide added to each of the substances in the acid medium was, titrated back with a standard solution of diethylene-tetra-ammonium suphatocerate. Chloroform was used as an indicator. It was coloured violet owing to the liberation of iodine during the titralion and became very pale yellow at the end-point because of the formation of iodine monochloride.     

Determination of Lead(II) by a Nitrocellulose Membrane Fluorescent Biosensor Based on G-Quadruplex Conformational Changes

A simple, label-free fluorescence method was developed for the sensitive determination of lead(II) using a nitrocellulose membrane biosensor. The surface of the nitrocellulose membrane was modified by glutaraldehyde to conjugate streptavidin, followed by the immobilization of a DNA probe via a biotin modifier. The biotinylated DNA probe can fold into a G-quadruplex structure in the presence of potassium ion that selectively binds to N-methyl mesoporphyrin IX and yields a strong fluorescence signal. The presence of lead(II) can induce a conformational change of the G-quadruplex to a more compact structure, which results in the release of potassium ion and N-methyl mesoporphyrin IX with a concomitant reduction of the fluorescence signal. The biosensor displayed a detection limit as low as 10 nM with excellent selectivity for lead(II) over other metal ions. The developed biosensor was employed for the determination of lead(II) in spiked river water.     

Liesegang rings of lead chromate Part II

Faint rings of lead chromate are formed in gelatin gel when a solution of lead nitrate diffuses in gelatin gel containing potassium chromate. These rings become well defined in the presence of a coagulant like potassium nitrate. Well definedLiesegang rings of insoluble substances in gel media can be obtained if the substance can exist in the colloidal state in the media and is coagulable by the diffusing ion.     

氢化物发生—原子荧光法测定地球化学样品中痕量铅

研究了铁氰化碱性体系下痕量氢的化物发生－原子荧光测定的方法。本方法克服了在酸性样品溶液中加入铁氰化钾后对样品分析产生的问题，具有操作简便。分析结果重现性好等特点。对二十六个国家一级地球化学标准物质进行了分析，获得满意结果。     

Evaluation of oxidant media for the determination of lead in food slurries by hydride generation atomic absorption spectrometry

Several oxidant media were evaluated for the generation of lead hydride from slurry samples and their application to the determination of lead in vegetables and fish by hydride generation atomic absorption spectrometry. Three oxidant - acid media were compared: hydrogen peroxide - nitric acid, ammonium persulphate - nitric acid and potassium dichromate - lactic acid. The powdered samples were suspended in Triton X-100 and shaken with 10.0 g of blown zirconia spheres until a slurry was formed. The potassium dichromate - lactic acid medium was the most satisfactory for the determination of lead in fish and vegetables, providing the lowest detection limits as a result of its high sensitivity and low blank values. The ammonium persulphate - nitric acid medium gave good accuracy, precision and selectivity for vegetables (1-2 p.p.m. of lead); however, with fish (0.1-1 p.p.m. of lead) it was only a semi-quantitative medium for the determination of lead owing to its lack of sensitivity and selectivity. The hydrogen peroxide - nitric acid medium was unsatisfactory for the generation of lead hydride from slurry samples because of decomposition of hydrogen peroxide by the organic matter in the sample.     

Eine bifunktionelle Bleititration mit Kaliumchromatl?sung

Ohne Zusammenfassung

---

Bifunctional titration of lead with potassium chromate solution

     

碱金属钾对Ni基催化剂纤维素水蒸气气化活性的影响

采用两段式催化气化方式研究了生物质热解气化过程中碱金属的挥发对Ni基催化剂活性的影响。实验结果表明,负载K盐的纤维素水蒸气催化气化过程中,K挥发后会在催化剂表面沉积,而少量K的存在和表面沉积不但能够提高镍基催化剂的抗积炭能力,而且有助于提高其催化活性,产生更多的氢气。然而纤维素中K的浓度过大,将会抑制Ni基催化剂的效果;K在催化剂上的沉积随催化剂循环次数的增加而增加,K的含量愈高,对催化剂的抑制效果愈明显,从而缩短了催化剂的使用寿命。     

Volumetric studies in oxidation-reduction reactions: Oxidation with chloramine-t. indirect determinations

Chloramine-T has been used as an oxidizing agent in hydrochloric acid medium for the indirect volumetric determination of hydrogen peroxide, lead dioxide, selenium dioxide, sodium formate, potassium meta-periodate, potassium permanganate and potassium dichromate using iodine monochloride as a catalyst, prcoxidizer and an indicator. Chloroform is coloured pink owing to the liberation of iodine during the titration and becomes very pale yellow at the end-point because of the formation of iodine monochloride.     

Effects of potassium distributions in carbonizations of bituminous coal

The carbonization of coal/KOH mixtures were investigated to identify the influence of potassium distributions on characteristics of the final products. The products were characterized using TGA, BET, TEM and adsorption of lead from its aqueous solutions with initial concentrations of 10–100 ppm. For the activated carbon obtained at 600 °C, the potassium distribution affected both the BET surface areas (661–1994 m²/g) and the meso- and micro-pore volumes ratios (0.48–0.91). There were also evolutions of nanostructures of both straight and curved tubular morphologies as evidenced by TEM micrograph. The samples exhibited different adsorptive capacities when tested in adsorption of lead from aqueous solutions. The adsorption followed second order kinetics and the equilibrium data were better described by empirical Freudlich isotherm model. The amount of lead adsorbed ranges from 4.3 to 47.3 mg/g. Thus, different degrees of potassium effects led to activated carbons with different surface and adsorptive properties.     

The polarographic determination of indium in zinc-base alloys : The determination of indium in zinc and in “lead-free” zinc alloys

The use of a potassium iodide base electrolyte for the separation of the polarographic steps due to indium and cadmium is discussed and theoretical data relating to the interference of the step due to lead with that due to indium are presented. An experimental study is given together with details of the attempted removal of lead interference. A method is presented for the polarographic determination of indium in zinc alloys, applicable when the lead concentration is small compared with that of indium.     

Determination of penicillins by desulphurization with lead and edta titration

A new, simple, accurate and rapid method is described for the determination of total penicillins in pharmaceutical preparations. The method is based on desulphurization with potassium plumbite whereby one mole of lead sulphide is formed per mole of penicillin. The excess of lead ions is titrated with EDTA at pH 4.5, with use of the lead ion-selective electrode. Results are reproducible within +/- 0.5% and compare favourably with those obtained by the procedures of the United States and British Pharmacopoeias.     

Flow-injection chemiluminescence determinations for human blood lead using controlled reagent release technology

A flow-through CL method for the determination of lead combined with controlled-reagent-release technology has been developed. Chemiluminescence (CL) reagents luminol and potassium permanganate were immobilized on anion exchange resin by electrostatic interaction. Lead ion was determined by its enhancing effect on the CL reaction between luminol and potassium permanganate. Both luminol and potassium permanganate were eluted from the anion exchange resin column by sodium phosphate solution. The linear range of the system was 10 μg mL^?1, and the detection limit was 5?×?10^–9 g mL^?1 lead (3σ). A complete analysis could be performed in 1 min with a relative SD 3.2% (1.0?×?10^–7 g mL^?1, n?=?9). The column shows remarkable stability and can be reused over 350 times and 21 days. The method has been applied to determine lead in human blood samples.     

Size fractionation of metals in wine using ultrafiltration

Ultrafiltration has been used to examine the size fractionation of lead, copper, iron, aluminium, calcium, potassium and sodium in white and red wines. Fractionation patterns demonstrated that the behaviour of lead is significantly diferent to the other metals considered. In red wine, there was a sudden decrease for lead between 100 000 and 30 000 nominal molecular weight cut off (NMWCO) and in white wine, a gradual decrease in the lead concentration was observed from 100 000 NMWCO. Iron was the only other metal which showed, for red wine, a size distribution pattern with a reduction in the iron concentration between 30 and 50% from 100 000 to 1000 NMWCO. Potential binding agents for lead and iron are discussed. The absence of any fractionation pattern for the other metals examined has been interpreted in terms of the metals existing as aquated cations (potassium and sodium), metal tartrate complexes (aluminium, copper and calcium) and either tartrate or phosphate for iron in white wine. The possibility of ultrafiltration disturbing kinetically facile processes, particularly for copper and calcium, is identified.