Determination of ascorbic acid by potassium iodate

Summary Results are given for a two stage oxidation in the ascorbic acid-KIO₃ reaction under controlled conditions of acidity. The first step corresponds to the Landolt reaction and the second end point is obtained by the classical Andrews method. The reproducibility and accuracy of the results calculated on the basis of the two successive end points constitute an interesting new feature of this redox reaction involving the use of KIO₃ as a primary standard for the determination of ascorbic acid.Our sincere thanks are due to Professor S. S. Joshi for kind interest in the work and to the National Institute of Sciences of India for award of a Research Fellowship to one of us (G. S. D.).     

Determination of sulphide by anion-exchange with lead iodate

A quick anion-exchange reaction, suitable for the determination of sulphide, has been found to occur on stirring a suspension of lead iodate (solubility product, K(s0) = 1.2 x 10(-13)) with sulphide solution at pH 5-8. After removal of the precipitates of lead iodate and lead sulphide (K(s0) = 3.4 x 10(-28)), the iodate released can be determined by its reaction with acidified iodide to give tri-iodide which is either titrated with thiosulphate or measured spectrophotometrically as its blue complex with starch. Chloride, bromide, iodide, fluoride, oxalate, sulphate, thiocyanate and phosphate do not interfere. Thiosulphate, sulphite, nitrite and thiols do not give an anion-exchange reaction but do interfere in the redox reaction of iodate with acidified iodide. However, this is avoided if they are first oxidized with bromine (the liberated iodate remains unaffected before iodometry.     

碘酸钾滴定法测定ITO粉末材料中的锡

建立了以锌粉-氢氧化钠熔融样品,盐酸浸取,用盖氏漏斗作为还原装置,铁粉和铝粒将锡还原,碘酸钾滴定法测定ITO粉末材料中锡的分析方法。方法测定结果稳定,精密度好,相对标准偏差为0.42%~0.67%,加标回收率在99.8%~101%,能够满足ITO粉末中锡的测定要求。     

碘酸钾滴定法测定铜阳极泥分银渣中的锡

建立了碘酸钾滴定法测定铜阳极泥分银渣中锡的含量。通过硝酸溶解,过滤除铜,还原铁粉置换分离锑、铋、砷等元素,消除了铜阳极泥分银渣中的铜、锑、砷等杂质元素对锡测定的干扰。方法加标回收率在99.7%~100%。精密度实验结果表明,相对标准偏差(RSD,n=11)小于1.1%。操作过程简单,能满足生产的需要。     

Determination of the purity of potassium iodate by constant-current coulometry

This paper describes a method of determining the purity of potassium iodate by constant-current coulometry. The determination can be divided into two steps. First, a Na₂S₂O₃ solution is prepared and its reductive value is determined. Second, the purity value of an oxidimetric quantity of potassium iodate is determined. This paper discusses the conditions of the reaction process and evaluates type A and B standard uncertainty of this method. The expanded relative uncertainty of this method is 0.02% (k=2). Received: 15 June 2000 Accepted: 27 December 2001     

Determination of iodate and periodate at the microgram level by a kinetic method

A procedure is reported for the kinetic determination of iodate/periodate mixtures based on the reduction of these anions by the iron(II)/dipyridylglyoxal dithiosemicarbazone complex in an acidic medium. The reaction is monitored spectrophotometrically at 410 nm (absorption maximum of the iron(III) complex formed). Mixtures of these anions at μg ml^?1 levels for iodate/periodate ratios from 5:1 to 1:4 can be determined with a r.s.d, of ca. 3%. Molybdate is used to mask periodate to allow iodate to be determined alone. The sum of both anions is obtained in the absence of molybdate. Chromate, hypochlorite and hexacyanoferrate(III) interfere seriously.     

Determination of iodate and sulphate in iodized common salt by ion chromatography with conductivity detection

A simple, rapid and accurate method for the determination of iodate in iodized common salts has been developed. The quantitative determination of iodate was accomplished by anion exchange chromatography with conductimetric detection. The method requires a sample pretreatment for the removal of large excess of chloride from the sample matrix. Onguard silver cartridges were found most suitable for this purpose. The sulphate content in the salt was simultaneously determined. The lower limits for the determination of iodate and sulphate in solution are 0.5 and 0.05 mug ml(-1), respectively. Quantitative recovery of the anions in synthetic samples has been obtained and the interferences from different cations and anions have been studied. The method has been successfully applied to the determination of iodate and sulphate in the commercially available salts. The concentrations of iodate measured by this method are in good agreement with those claimed by the manufacturer.     

Instrumental neutron activation analysis of dry atmospheric fall-out and rain-water

An automated precipitation sampler and an instrumental neutron activation analysis (i.n.a.a.) method for the determination of some major and trace elements in dry atmospheric fall-out and rain-water are presented. The sampler features a rain detector which makes separate collection of dry atmospheric fall-out and rain-water possible. The sampler is equipped with u.v. lamps in order to avoid algal growth during extended collection periods. After collection, the samples are separated into water-soluble and insoluble fractions. The soluble fraction is preconcentrated before analysis by freeze-drying. The i.n.a.a. method involves the measurement of both short- and long-lived radioactivities so that a total of 35 elements can be determined. The possibility of losses during freezedrying and the accuracy of the i.n.a.a. method were investigated for 7 elements by analysis of a soluble fraction with an independent method, viz. inductively coupled plasma atomic emission spectrometry.     

Determination of optical properties of hexagonal lithium iodate crystal by use of NQR and IR spectroscopy

The NQR Zeeman effect of ¹²⁷I (± $\text{1}\text{2}$ ←→ ± $\text{3}\text{2}$ transition) for the LiIO₃ crystal of hexagonal modification has been investigated, and the EFTG asymmetry parameter for nuclei of ¹²⁷I determined. Measurements of optical properties of the z-cut crystal in polarized light within the region of stretching vibrations and their overtones for IO^?₃ revealed that transmission (reflection) depends on the direction of the incident light wave electric vector. The results obtained indicate that crystals of LiIO₃ grown from aqueous solutions show anomalous biaxiality.     

碘酸铯的晶体结构

大多数碘酸盐具有良好的电光、非线性光学和压电性能,因此,人们对碘酸盐的结构和性能进行了广泛的研究,已测定了锂、钠、钾、铷等碱金属碘酸盐的晶体结构,并观察到CsIO_3粉末也具有较强的倍频效应.由于难以生长单晶和结构上呈现赝立方对称性,至今人们还未确定出其晶体结构.因此,碱金属碘酸盐随碱金属原子半径的增大,其晶体结构类型发生变化的规律并没有完全阐明,解决 CsIO_3的晶体结构,对了解碱金属碘酸盐结构类型的变化具有一定的意义.     

Recoil iodine-128 in anhydrous copper iodate

The thermal annealing of the damage caused by /n,/ reaction has been investigated for anhydrous copper iodate in crystalline phase. Solvent extraction and fractional precipitation methods were employed to distinguish the recoil species containing recoil iodine-128 atoms. The role of reaction intermediates have been discussed.     

Utilization of flow injection with hydrazine reduction and photometric detection for the determination of nitrate in rain-water

The hydrazine reduction method for determination of nitrate at the parts per million level is adapted to flow injection sample processing of rain-water. Reagent composition and physical variables were evaluated and optimized. Forty samples per hour can be processed. A precision of better than 3% is possible in the range of 1.0–10.0 ppm nitrate. Results for nitrate obtained from 9 rain-water samples agreed favorably with those determined by ion chromatography.     

Thermal decomposition kinetics of potassium iodate

The effect of gamma ray irradiation on the rate and kinetics of thermal decomposition of potassium iodate (KIO₃) has been studied by thermogravimetry (TG) under non-isothermal conditions at different heating rates (3, 5, 7, and 10 K min^?1). The thermal decomposition data were analyzed using isoconversional methods of Flynn–Wall–Ozawa, Kissinger–Akahira–Sunose, and Friedman. Irradiation with gamma rays increases the rate of the decomposition and is dependent on the irradiation dose. The activation energy decreases on irradiation. The enhancement of the rate of the thermal decomposition of KIO₃ upon irradiation is due to the combined effect of the production of displacements and extended lattice defects and chemical damage in KIO₃. Non-isothermal model fitting method of analysis showed that the thermal decomposition of irradiated KIO₃ is best described by the contracting sphere model equation, with an activation energy value of ~340 kJ mol^?1.     

Thermal decomposition kinetics of potassium iodate

The thermal decomposition of potassium iodate (KIO₃) has been studied by both non-isothermal and isothermal thermogravimetry (TG). The non-isothermal simultaneous TG–differential thermal analysis (DTA) of the thermal decomposition of KIO₃ was carried out in nitrogen atmosphere at different heating rates. The isothermal decomposition of KIO₃ was studied using TG at different temperatures in the range 790–805 K in nitrogen atmosphere. The theoretical and experimental mass loss data are in good agreement for the thermal decomposition of KIO₃. The non-isothermal decomposition of KIO₃ was subjected to kinetic analyses by model-free approach, which is based on the isoconversional principle. The isothermal decomposition of KIO₃ was subjected to both conventional (model fitting) and model-free (isoconversional) methods. It has been observed that the activation energy values obtained from all these methods agree well. Isothermal model fitting analysis shows that the thermal decomposition kinetics of KIO₃ can be best described by the contracting cube equation.     

Thermal decomposition kinetics of potassium iodate

The rate and kinetics of the thermal decomposition of potassium iodate (KIO₃) has been studied as a function of particle size, in the range 63?C150???m, by isothermal thermogravimetry at different temperatures, 790, 795, 800 and 805?K in nitrogen atmosphere. The theoretical and experimental mass loss data are in good agreement for the thermal decomposition of all samples of KIO₃ at all temperatures studied. The isothermal decomposition of all samples of KIO₃ was subjected to both model-fitting and model-free (isoconversional) kinetic methods of analysis. It has been observed that the activation energy values are independent of the particle size. Isothermal model-fitting analysis shows that the thermal decomposition kinetics of all the samples of KIO₃ studied can be best described by the contracting cube equation.     

Indirect determination of iodate by atomic-absorption spectrophotometry

An indirect method for determination of trace iodate in certain high-purity chemicals by atomic-absorption spectrophotometry (AAS) is described. Iodate forms a stable ion-association complex [Hg(dipy)(2)](IO(3))(2) in neutral medium, which can be extracted into methyl isobutyl ketone with 99% efficiency. The extract can be analysed for mercury (and hence indirectly for iodate) by flameless AAS. The limit of detection for iodate by this method is 7.5 ng. Apparent recoveries of 92-112% have been obtained for spikes of 0.25-0.70 mug of iodate.