钢渣中游离氧化镁含量的测定

研究和提出了以硝酸铵-乙醇作为提取剂提取活性氧化镁（即游离氧化镁）的分析方法。通过正交实验,选取了最佳的提取条件。样品平行测定的相对标准偏差在0.51%～2.13%之间,回收率实验结果为98.2%～99.0%,表明该实验的精密度和准确度均较好。采用硝酸铵-乙醇作为提取剂提取游离氧化镁的分析方法,实现了钢渣中游离氧化镁的快速、准确测定,为钢渣的回收再利用提供了依据。     

碳酸盐法测定钢渣中活性氧化镁含量

采用碳酸盐法测定钢渣中活性氧化镁含量。研究了碳酸盐法测定钢渣中活性氧化镁反应的可行性和测定的准确性。结果表明:二氧化碳在水中可以将氧化镁和氢氧化镁转化成可溶性镁离子,然后用EDTA标准溶液滴定其含量,氧化镁、氢氧化镁与二氧化碳的反应率均达到97%以上;二氧化碳与钢渣反应时间应大于105min,新余热焖钢渣中活性氧化镁质量分数为1.44%;压蒸后钢渣中氢氧化镁质量分数为1.86%,与原钢渣中活性氧化镁测定结果保持一致,相对误差小于1%。     

读者园地

问 :1 .燃烧 -碘量法测定钢铁中硫 ,可用碘标准溶液或用碘酸钾标准溶液滴定 ,两者有何不同 ?2 .燃烧 -碘量法测定钢铁中硫时 ,对淀粉吸收液有何要求 ?——读者　　李纬　　　　答 1 :用燃烧 -碘量法测定硫 ,将试样在氧气中燃烧生成的 SO2 导入吸收液中生成 H2 SO3 ,以淀粉为指示剂 ,用碘或碘酸钾标准溶液进行滴定 ,根据所消耗的标准溶液量计算出试样中硫含量 ,两者原理是相同的。用碘标准溶液滴定 ,试剂配制方便 ,适用于测定含硫量 w( S)≥ 0 .0 1 %的试样。对含硫量 w( S)≤ 0 .0 1 %的试样最好用碘酸钾 -碘化钾标准溶液滴定 ,因为它比…     

EDTA滴定法测定稀土镁硅铁中氧化镁

本文用EDTA络合滴定法测定稀土镁硅铁中氧化镁含量。试样经重铬酸钾溶解、浸取、分离，在pH10时，以铬黑T为指示剂，EDTA标准溶液定量对钙、镁合量铬合滴定。在pH≥12时，以钙试剂为指示剂，EDTA标液定量滴定钙量，同时做空白试剂试验，用差减法计算氧化镁量。方法特点，不必挥铬，EDTA滴定，终点明确，结果的精密度好，相对标准偏差在1．52％以内，     

碱分离-EDTA络合滴定法测定铝及铝合金中的镉

建立碱分离–EDTA络合滴定法测定铝及铝合金中镉含量的方法。样品用盐酸溶液(1+1)和30%过氧化氢溶解,经氢氧化钠、氨水两次沉淀分离铝、钛、铁、铬、铜、镍、锰等元素,在pH 5.5的弱酸性介质中,以1-(2-吡啶偶氮)-2-萘酚乙醇溶液作指示剂,用乙二胺四乙酸二钠标准滴定溶液滴定镉,计算得镉含量。干扰试验表明,经过两次分离后铝基体和其它杂质元素均不干扰镉的测定。将该方法用于铝及铝合金中质量分数在3.00%～12.00%之间镉的测定,测定结果的相对标准偏差为0.16%～0.68%(n=9),加标回收率为99.2%～100.3%。该方法精密度、准确度良好,简便快速,适用于铝及铝合金中镉含量为3.00%～12.00%样品的测定。     

碘化法提金工艺中碘及碘离子连续测定研究

建立了一种碘化法提金液中碘及碘离子的连续测定方法,调节溶液酸度,用硫代硫酸钠滴定溶液中碘,在滴定完碘的溶液中,以曙红为指示剂,以硝酸银定量滴定溶液中的碘离子,扣除碘生成的碘离子即可得到溶液中的碘离子。采用定量模拟碘化法提金液验证方法的有效性,同时进行加标回收及精密度实验,加标回收率为98.1%~103%,相对标准偏差(RSD,n=10)在0.19%~0.67%,方法精密度好,可满足碘化提金液中碘及碘离子的分析测定。     

氢氧化钠-碘化钾振荡吸收快速测定氯化炉气中氯气和二氧化碳

本文采用注射器取样,氢氧化钠-碘化钾振荡吸收Cl、HCl、CO_2以百里酚酞作指示剂,盐酸滴定过量氢氧化钠后,再用甲基橙作指示剂,盐酸滴定以测定二氧化碳;最后用硫代硫酸钠滴定析出的碘而测定Cl_2。方法简便、快速,重现性及准确性较好。共存氯化氢及三氧化硫气体不影响测定。     

工业锡酸钠中游离碱的测定

工业锡酸钠中的游离碱(氢氧化铵),一般含量在2±1%,多采用酚酞作指示剂,用硝酸标准溶液作滴定剂酸碱滴定法测定。然而,由于Na_2SnO_3及空气中二氧化碳的影响,致使结果误差较大。为此,本文拟定了用氯化钡沉淀锡酸根,以百里酚酞作指示剂用盐酸标准溶液作滴定剂,酸碱滴定游离碱的方法。方法也适用于含锡电镀液中游离碱的测定。     

银量法测定混合卤化物中的碘离子

碘和淀粉在有碘离子存在时显蓝色。在滴定分析中,这一显色机理已被应用于无汞定铁法的预还原过程和指示碘化钾溶液滴定银离子的终点。本文利用上述显色原理指示硝酸银溶液滴定碘离子的终点,在滴定前加入指示剂碘-淀粉,溶液呈蓝色:     

萘醌分析方法的探讨

萘醌是萘氧化制苯酐过程中的重要副产物,其含量是苯酐生产工艺控制的指标之一。它的分析在国外一般采用色谱法使其与其它组份同时测定,操作简便,准确度高;在国内大都仍采用碘量法或光电比色法测定。不同分析方法的比较:1.碘量法:其原理是萘醌在溶液中与过量盐酸作用产生游离氯,氯与碘化钾作用析出的碘用硫代硫酸钠滴定,以淀粉为指示剂。     

Investigation of iodine liberation process in redox titration of potassium iodate with sodium thiosulfate

Potassium iodate is often used as a reference material to standardize a sodium thiosulfate solution which is a familiar titrant for redox titrations. In the standardization, iodine (triiodide) liberated by potassium iodate in an acidic potassium iodide solution is titrated with a sodium thiosulfate solution. The iodine liberation process is significantly affected by the amount of acid, that of potassium iodide added, the waiting time for the liberation, and light; therefore, the process plays a key role for the accuracy of the titration results. Constant-voltage biamperometry with a modified dual platinum-chip electrode was utilized to monitor the amount of liberated iodine under several liberation conditions. Coulometric titration was utilized to determine the concentration of a sodium thiosulfate solution on an absolute basis. Potassium iodate was assayed by gravimetric titration with the sodium thiosulfate solution under several iodine liberation conditions. The liberation process was discussed from the changes in the apparent assay of potassium iodate. The information of the appropriate titration procedure obtained in the present study is useful for any analysts utilizing potassium iodate to standardize a thiosulfate solution.     

The formulation of the electron and proton balance equations for solving complicated equilibrium problems in redox titrations

 A plain, didactically convenient formulation of the electron balance and of the proton balance equations, suitable for complicated redox titration systems with redox, acid-base, precipitation and complexation side-reactions is discussed. Two typical examples, the standardisation of a permanganate solution by titration of iron(II), and the standardisation of a iodine solution by titration of sodium arsenite, are presented. Received: 30 January 1996/Accepted: 9 February 1996     

The formulation of the electron and proton balance equations for solving complicated equilibrium problems in redox titrations

 A plain, didactically convenient formulation of the electron balance and of the proton balance equations, suitable for complicated redox titration systems with redox, acid-base, precipitation and complexation side-reactions is discussed. Two typical examples, the standardisation of a permanganate solution by titration of iron(II), and the standardisation of a iodine solution by titration of sodium arsenite, are presented. Received: 30 January 1996/Accepted: 9 February 1996     

Sodium meta-vanadate as volumetric reagent: Iodine monochloride method

In hydrochloric acid medium sodium meta-vanadate was used as a volumetric reagent for the determination of copper, zinc, cobalt, mercury, and lead. Cu⁺², Zn⁺² and Co⁺²were precipitated as complex mercurythiocyanates, Hg⁺² as mercuric zinc thiocyanate and Pb⁺² as Iodide. The thiocyanates were dissolved in concentrated hydrochloric acid and titrated against standard sodium meta-vanadate solution in the presence of iodine monochloride as a pie.oxidizer and catalyst. In titration of the iodide against the meta-vanadate. it was not necessary to add iodine monochloride to the titrant because it is formed during the titration. Chloroform was used as an indicator. It was pink owing to the liberation of iodine during the titration and became pale yellow at the end-point because of the formation of iodine monochlonde.     

Prerequisites for attaining 1:1 stoichiometry between water and iodine using dimethylformamide as solvent in coulometric Karl Fischer titrations

Summary Conditions for attaining 1:1 stoichiometry between water and iodine in a non-alcoholic, dimethylformamide-based Karl Fischer reagent have been investigated. It has been made clear that the stoichiometric ratio is determined by the rate of the main KF-reaction consuming iodine, in relation to the rate of the side reaction between water and sulphur trioxide, which is a reaction product of the KF-reaction. The rate constants for these reactions were determined to be 9.8±0.6 M^–2s^–1 and 0.072±0.007 M^–1s^–1, respectively. It is shown theoretically as well as experimentally by means of coulometric titrations that the attainment of a 1:1 stoichiometric ratio requires that the titration is carried out at very high iodine concentrations.Dedicated to Professor Dr. Wilhelm Fresenius on the occasion of his 80th birthday     

Precise coulometric titration of sodium thiosulfate and development of potassium iodate as a redox standard

In this paper, we determine the effective purity of potassium iodate as a redox standard with a certified value linked to the international system of units (SI units). Concentration measurement of sodium thiosulfate solution was performed by precise coulometric titration with electrogenerated iodine, and an assay of potassium iodate was carried out by gravimetric titration based on the reductometric factor of sodium thiosulfate assigned by coulometry. The accuracy of the coulometric titration method was evaluated by examining the current efficiency of iodine electrogeneration, stability of sodium thiosulfate solutions and dependence on the amount of sodium thiosulfate solution used. The measurement procedure for gravimetric titration of potassium iodate with sodium thiosulfate was validated based on determination of a reference material of known purity (potassium dichromate determined by coulometry with electrogenerated ferrous ions) using the same gravimetric method. Solutions of 0.2 and 0.5 mol/L sodium thiosulfate were stable over 17 days without stabilizer. Investigation of the dependency of titration results on the amount of sodium thiosulfate solution used showed no significant effects, no evidence of diffusion of the sample, and no effect of contamination appearing during the experiment. Precise coulometric titration of sodium thiosulfate achieved a relative standard deviation of less than 0.005% under repeating conditions (six measurements). For gravimetric titration, the results obtained for the effective purity of potassium dichromate were sufficiently close to its certified value to allow confirmation of the validity of the gravimetric titration was confirmed. The relative standard deviation of gravimetric titration for potassium iodate was less than 0.011% (nine measurements), and a redox standard with a certified value linked to SI units was developed.     

Mechanism and reaction rate of the karl fischer titration reaction: Part V. Analytical Implications

The Karl Fischer titration procedure for the determination of water has been studied. In view of the results of previous investigations, a methanolic sodium acetate—sulfur dioxide solution is recommended as solvent and an iodine solution in methanol as titrant. The advantages of this procedure over a conventional Karl Fischer titration are: a much more rapidly reacting reagent, the possibility of a visual end-point detection, a titrant of constant titre over a long period of time, and the absence of the disagreeable odour of pyridine.     

Semiconducting organic polymer from polyacrylamide–Cu++ chelate and iodine

Semiconducting organic polymer was obtained by the modification of polyacrylamide (PAAm)–Cu⁺⁺ chelate with iodine in acetone. Favorable conditions for preparing the chelate effective for the conduction were investigated. Surface resistivities were affected by the amounts of cupric salts and iodine, satisfactory results being given by about 25 wt % of the salts based on PAAm and more than 1 wt % of iodine on the chelate. The conductivity was also varied with the degree of neutralization of the chelate in solution, and optimal values were obtained by addition of about an equimolar amount of potassium hydroxide to cupric salts. Effective structures of the polymer chelate in solution were assumed on the basis of the visible and the NMR spectra and potentiometric titration.     

Study of acid and reductant functions of hydrazine sulphate by iodate-iodide mixture

Summary Hydrazine sulphate was found to liberate two atoms of iodine per molecule, when treated with an excess of iodate and iodide, and this was determined by thiosulphate or arsenious oxide in borax-boric acid buffer. The study of the action of iodate-iodide mixture on hydrazine sulphate at different stages of neutralisation and decomposition was carried out and iodometric relationships were verified. An interesting titration involving hydrazine sulphate both as a titrant and the titrating solution following its different reactions towards iodate-iodide mixture and iodine, is described. Hydrazine sulphate is found to be a satisfactory standard for the titration of iodine in presence of an alkaline buffer.Sincere thanks of the authors are due to Dr. S. S. Joshi, D. Sc. (London), for kind interest in the work.