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 . .

     

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.     

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.     

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.     

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.     

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.     

Determination of iodide with chloramine-T

A method is described for the estimation of iodide, based on its oxidation to iodate by the addition of excess of chloramine-T, destruction of the excess of chloraniine-T with dimethyl sulphoxide and determination of the iodate iodometrically. In addition, the dimethyl sulphoxide eliminates any interference from bromide or bromate.     

Spectrophotometric determination of paracetamol in drug formulations by oxidation with potassium dichromate

A rapid spectrophotometric method for determination of paracetamol is described, based on oxidation with dichromate for 15 min in 6M sulphuric acid at 80 degrees , and measurement (at 580 nm) of the chromium(III) formed. The method is applied to the determination of paracetamol in drugs prescribed for colds, coughs and flu. Of the common pharmaceuticals associated with paracetamol, only ascorbic acid and acetylsalicylic acid interfere. The results have been statistically compared with those obtained by the official (BP) and cerium(IV) methods.     

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.     

Shaken not stirred; oxidation of alcohols with sodium dichromate

Efficient and selective oxidation of primary alcohols to the corresponding aldehydes with sodium dichromate at room temperature under solvent-free conditions by shaking is described. This new procedure can also successfully oxidise secondary alcohols.     

消解氨溶-火焰原子发射光谱法测定丁苯橡胶中的钾、钠

和浓硝酸消解了丁苯橡胶样品,再用氨水溶解消解产物。取适量消解产物的氨溶液,加入消电离剂Li^ 配制成试液,以工作曲线法测定。对样品处理方法、消解产物的溶解性质、线性范围、干扰及检出限进行了考察。测定结果的相对标准偏差小于3．9％,加标回收率为97．3％－103．7％。建立了快速同时测定丁苯橡胶中钾、钠的火焰原子发射光谱法。     

Coulometric assay of the primary standards potassium dichromate and ammonium hexanitratocerate

The high-precision coulometric titration apparatus of Eckfeldt and Shaffer (Leeds & Northrup Company) has been used for the precision assay of two primary standard materials for oxidation-reduction work. The purity found for NBS 136b Potassium Dichromate. 99.975 %, standard deviation 0.002 %, checks the earlier value of Marinenko and Taylor. Ammonium hexanitratocerate, if low in thorium, is also an excellent primary standard, two recent commercial preparations having purities of 99.972 and 99.984%, a higher standard deviation, 0.005 %, reflecting a minor difficulty in end-point detection caused by platinum oxide formation on the indicating electrodes.