次亚磷酸钠分离-重铬酸钾容量法测定钨尾矿中砷含量

选矿中产生的钨尾矿长期堆放,经过雨水冲刷,钨尾矿中的砷会进入到水土中,造成环境污染,准确测定钨尾矿中砷含量,利于监测钨尾矿中砷对环境的污染程度。采用硝酸-氯酸钾饱和溶液和氟化铵溶液分解样品,再用硫酸溶液冒烟赶尽硝酸,在盐酸介质中,以硫酸铜为催化剂,用次亚磷酸钠将砷离子还原成元素态,析出的砷过滤分离,除去其他杂质。在硫酸溶液中,用过量的重铬酸钾标准溶液滴定溶解单质砷,过量的重铬酸钾以二苯胺磺酸钠为指示剂,用硫酸亚铁标准溶液反滴定。通过优化样品溶解条件和砷沉淀还原条件,建立了次亚磷酸钠分离-重铬酸钾容量法测定钨尾矿中砷含量的分析方法。通过测定滤液中的砷含量,考察了滤液中砷含量对砷测定结果的影响,可忽略不计,表明实验中砷沉淀完全。通过沉淀单质砷,过滤使砷与杂质元素分离,消除了杂质元素对砷测定的影响。运用重铬酸钾容量法测定3个钨尾矿样品中的砷,并进行加标回收实验,测定结果的相对标准偏差（RSD,n=11）在0.14%～2.1%,加标回收率在97%～101%。方法操作简单、精密度高,适合钨尾矿中高含量砷的测定,测定结果与碱融分离-碘量法结果基本一致。     

Regioselective iodination of aromatic compounds with potassium iodide in the presence of benzyltriphenylphosphonium perchlorate

A simple and efficient method for the selective iodination of various aromatic compounds by using potassium iodide in the presence of benzyltnphenylphosphonium perchlorate,is reported.This method provides several advantages such as good selectivity between ortho and para positions of aromatic compounds and high yields of the products.     

Volumetric estimation of potassium permanganate and potassium dichromate in mixtures with oxalic acid

1. A simple method has now been developed for the volumetric estimation of potassium permanganate and potassium dichromate in mixtures The method consists in taking an aliquot volume of the mixture in an Erlenmeyer flask, adding sufficient quantities of sulphuric acid and manganous sulphate (catalyst) and titrating with a standard solution of sodium oxalate or oxalic acid run in from the burette, until the colour changes from orange-red to yellow. The oxalic acid run ingives a measure of the permanganate present in the mixture Then the mixture in the flask is titrated with a standard solution of Mohr's salt using diphenylbenzidine as indicator. The volume of Fe⁺² solution run in the second stage gives a measure of the dichromate present in the original mixture. 2. The reverse titration does not give accurate results, because it is affected by the induced reaction between oxalic acid and dichromate which is induced by the reaction between oxalic acid and permanganate during the first stage of the reaction. This induced reaction has been studied in some detail.     

重铬酸钾容量法测定地质样品中的有机碳

目前,地质样品中有机碳的测定方法有干烧法（高温电炉灼烧）和湿烧法（重铬酸钾氧化）两大类。另外还有ICP-AES法、微波消解法、过硫酸钾法、电导法、石墨电热消解法、比色法等,然而这些有机碳测定方法仍然存在许多不尽如人意的地方。干烧法要求实验条件苛刻,操作繁琐,不易掌握,受碳酸盐的干扰。湿烧法虽然操作比较简单,但方法受样品中还原性物质的干扰,如氯根、亚铁等,上述方法都有待完善和优化改进。如：探索因不同样品基体差异而产生的干扰元素消除方法;寻找更合适的指示剂;本文采 用重铬酸钾-容量法测定地质样品中的有机碳,在220±10℃恒温电热板上,用0.4 mol/mL重铬酸钾溶解样品。通过优化熔矿温度、熔矿时间、熔剂浓度的优化选择,进行了氯离子的干扰试验。样品中含氯化物低的样品通过加入0.1 g硫酸银消除,样品中含氯化物高的样品通过高温灼烧减量消除。氧化指示剂选用邻菲啰啉或苯二氨基苯甲酸。本方法适用于土壤、水系沉积物、岩石等地质调查样品中有机碳的测定,方法相对标准偏差（RSD）在0.80%～4.41%之间,准确度（RE）在-3.15%～+1.15%之间。通过标准物质验证,方法技术指标满足地质行业规范DZ/T0130.4-2006中有机碳的分析要求,建立了一种简单、快捷、经济、准确的测定地质样品中有机碳的测定方法,满足地球化学调查批量样品生产的需要。     

Coulometric investigation of the drying methods for the standard reference materials potassium dichromate and sodium carbonate

The water content of dried potassium dichromate and sodium carbonate, which had been heated at various temperatures and then cooled in a "desiccated" atmosphere of argon, was measured by a coulometric microdetermination method. The amounts of water in the dried standard reference materials depended mainly on the heating temperature and only a little on the desiccant used. The dichromate and carbonate contained less than 50 ppm of water when they were heated at temperatures higher than 200 degrees and 250 degrees respectively and then cooled in an atmosphere of argon desiccated with magnesium perchlorate. Sulphuric acid was not advisable as the desiccant for sodium carbonate.     

Thermal properties of potassium dichromate

Thermosonimetry, DTA, high temperature XRD and hot stage microscopy have been used to study the thermal behaviour of K₂Cr₂O₇. A rapid triclinic to monoclinic phase transformation occurs at 543 K slowly reversible at 508 K. Severe crystallite fracturing is associated with the reverse transition and manifests anomalous X-ray intensities which have been previously interpreted as metastable phase formation. On reheating, the transformation occurs at 528 K. Possible interpretations of the temperature hystereses are given.

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Zusammenfassung Thermosonimetrie, DTA, Hochtemperatur-XRD und Mikroskopie in heißem Zustand wurden zur Untersuchung des thermischen Verhaltens von K₂Cr₂O₇ eingesetzt. Eine schnelle Phasenänderung von der triklinen zur monoklinen Form findet bei 543 K statt, welche bei 508 K langsam reversibel ist. Der schwere Kristallbruch ist mit dem umgekehrten Übergang verbunden und weist anomale Röntgenstrahlen-Intensitäten auf, welche früher als Bildung einer metastabilen Phase gedeutet wurden. Bei wiederholtem Aufheizen geht die Änderung bei 528 K vor sich. Mögliche Deutungen der Temperaturhysterese werden gegeben.

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Résumé On a étudié le comportement thermique de K₂Cr₂O₇ par thermosonimétrie, ATD, diffraction des rayons X à haute température et microscopie avec platina chauffante. Une transformation rapide de la phase triclinique à la phase monoclinique a lieu à 543 K et est lentement réversible à 508 K. Un fractionnement important des cristallites est associé à la transition inverse et se manifeste par des intensités anormales des raies de diffraction X, ce qui a été préalablement interprété comme la formation d'une phase métastable. Lors d'un nouvel échauffement, la transformation a lieu à 528 K. Diverses interprétations possibles de l'hystérèse de température sont proposées.

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₂₂₇ - , , - . 543 - , 508 . - , . 528 . .

     

A comparative study on chemical treatment of jute fiber: potassium dichromate, potassium permanganate and sodium perborate trihydrate

Studies have been carried out on chemical treatments of jute fibers in order to hinder moisture absorption, which causes incompatibility with a non-polar polymer, and to increase the surface roughness for mechanical interlocking. The objective of this research is to improve the interfacial adhesion between jute fibers and polypropylene by oxidative treatments. On this basis, jute fibers were treated with potassium dichromate (PD), potassium permanganate (PM) and sodium perborate trihydrate (SP). Fourier transform infrared spectrometry (FTIR), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy were used to characterize jute fibers. The effects of chemical treatments were also revealed by assessment of moisture absorbability, yarn tensile properties and interfacial shear strength with polypropylene. FTIR and XPS analyses confirmed oxidative modification of jute fibers using any of the surface treatments. It was observed that the proportion of O=C groups increased, whereas that of O–H groups decreased after oxidative modifications. Tensile strength and elasticity modulus results decreased after oxidative treatments, whereas PD, PM and SP enhanced the interfacial shear strength values by 25, 61 and 71 %, respectively. Only SP treatment influenced moisture absorbability results significantly. The surface roughness of untreated jute fibers shows increments after chemical treatments due to partial removal of surface cementings. According to the findings obtained from surface characterization methods and physical tests, the highest interfacial adhesion with better compatibility with polypropylene was achieved after SP treatment by providing the highest surface roughness values and hydrophobic character of jute fiber.     

Dissolving metal reductions with sodium potassium alloy in the presence of 18-crown-6

The dissolving metal reduction of organic compounds can be performed in THF utilizing sodium potassium alloy in the presence of a catalytic amount of 18-crown-6.     

Determination of the rate of reaction between potassium iodide and potassium peroxodisulphate with the econoburette: a green chemistry and microscale titrations

Measurement for a rate of reaction for about 30?min at a 5?min interval between KI and K₂S₂O₈ aqueous solutions with conventional burette in industries and academics consumes about 3.375?g K₂S₂O₈/250?mL?:?4.15?g KI/250?mL?:?11.6?mL (CH₃COOH, glacial)/100?mL?:?1?g starch/10?mL?:?0.62?g Na₂S₂O₃ (sodium thiosulphate)/250?mL?:?50?mL ice cold water. The number after the oblique in mL depicts an amount of aqueous solution where the amounts of chemicals in grams are dissolved. Similar determinations with econoburette reduced their amounts in 0.0675?g K₂S₂O₈/5?mL?:?0.083?g KI/5?mL:?0.5?mL (CH₃COOH, glacial)/5?mL?:?0.05?g starch/0.5?mL?:?0.025?g Na₂S₂O₃/2?mL?:?2.5?mL ice cold water. The reduction in amounts is about 50 times, and similarly the time and operational efforts are reduced in the same proportion. The econoburette is a ‘green chemistry’ instrument which performs valuable titration with microlitre of substances. The micro level amount of titer and titrant consumed less time in performing a volumetric tititration and also prevented much use of materials. In general, after titration a significant quantity of indicators, additives, titer and titrant are consumed and drained out in a sink with the possibility of causing pollution. The econoburette reduces such wastage of materials by up to 90%, with high accuracy in results. The rate constant k?=?0.0431?sec^?1?L^–1?mol^?1 remained fairly constant for successive measurements with time but with the conventional burette larger deviations were noted at 298.15 Kelvin temperature.     

The preparation of sodium and potassium borohydrides by the reduction of boron halides by sodium and potassium hydrides in the presence of aluminum triethyl

Summary It was found that sodium and potassium hydrides readily react with boron halides in hydrocarbon solvents in the presence of aluminum triethyl to form the borohydrides of sodium and potassium, respectively.     

Volumetric estimation of indigo and indigo sulphonic acid with potassium dichromate

Summary The reaction between indigo sulphonate and chromic acid has been studied under various conditions, with a view to its analytical application. When indigo sulphonate is treated with an excess of chromic acid in 0.7 N sulphuric acid, indigo is quantitatively oxidised to isatin. The excess of unreacted chromic acid can be determined iodimetrically or by titration with standard ferrous ammonium sulphate solution. At higher acid concentration, the reaction is not quantitative, the chromic acid consumed being somewhat less than the theoretical.     

Thermometric titration of uranium(iv)with potassium dichromate

A thermometric method is presented for the redox titration of uranium(IV) with dichromate. The investigation was made primarily to determine the applicability of the thermometric method to redox titrations in solutions that contain ions deleterious to electrodes used in electrometric methods. A relative standard error of ±1% attainable in the titration of quantities of uranium(lV) of the order of 5 mg. Less than l 5 min is required to complete a titration. Fluoride ion can be tolerated in the solution provided that sufficient aluminium(111) is added to complex all the fluoride.     

Potentiometric titration of gold in ores with potassium iodide

Summary A direct potentiometric titration method for the determination of gold in ores and alloys is described. It is based on the reduction of Au(III) with iodide ions yielding accurate and reproducible results. Detection limit and sensitivity were 0.06 and 0.032 mg/l Au, respectively. The linear response range was between 0.1 and 120 mg/l Au. The method can be used for the routine assay of gold in different kind of samples.