RESUMO
A rapid method is presented for the gravimetric determination of molybdenum (as the oxinate) in ferromolybdenum and molybdenum additives. The sample is fused with a mixed flux of sodium peroxide and sodium carbonate in a zirconium crucible for complete decomposition. Leaching the cooled fusion cake with water provides instantaneous separation of molybdenum as sodium molybdate from iron(III) and other hydrous oxides. After filtration, the molybdenum is precipitated with oxine after addition of EDTA and oxalate to obviate interference from other metal oxinates, and determined gravimetrically. The precision and accuracy are comparable to those of referee methods.
RESUMO
A rapid, simple and accurate method for determining phosphorus photometrically in iron ores and related materials, obviating the use of perchloric acid, is described. The sample is fused with sodium peroxide in a zirconium crucible and the melt dissolved in hydrochloric acid. The molybdenum-blue complex is developed by the addition of ammonium molybdate and hydrazine sulphate and the absorbance is measured at 725 nm. The range of the method is from 0.005 to 1.0% P. A batch of 6 samples can be analysed in about 2 hr.
RESUMO
The diphenylcarbazide colorimetric method was evaluated by analyzing spiked PVC filters prepared by an AIHA-accredited consultant laboratory for chromium (VI). All seven participating laboratories received the samples and performed the analyses at the same time. Three laboratories simultaneously tested three alternative analytical procedures. Reduced amounts of chromium (VI) were found by both the consultant and participating laboratories when using the test procedure and one of the alternative methods. Two of the alternative analytical methods, both of which involve an alkaline extraction procedure, provided higher recoveries and more precise values for the test filters. It appears that the alkaline extraction procedure may be more appropriate for occupational health samples taken in steel industry environments which may include several interferents. Suggestions are made for further studies to determine the most appropriate analytical method.
Assuntos
Cromo/análise , Poluentes Ambientais/análise , Filtração , MétodosRESUMO
A rapid, simple and virtually universal technique is described for decomposing a wide range of materials such as ores, sinters, slags, ferro-alloys and other reagents and additives used in the steel industry, as well as environmental dusts and particulate matter. The procedure involves fusion with sodium peroxide, alone or with sodium carbonate (mixed flux) in a zirconium or vitreous carbon crucible. Treatment of the fused melt with water and acid results in complete dissolution. It avoids the tedious operations involved in dissolving residues left by other dissolution techniques. Losses of normally volatile elements such as arsenic, phosphorus, lead and zinc do not occur. Application of this technique is described, particularly for the photometric methods developed for determining arsenic, phosphorus, titanium and vanadium in iron ores in the ranges 0.0002-0.1% As, 0.002-0.6% P, 0.01-0.6% Ti, and 0.001-0.5% V. Both the precision and accuracy are excellent.
RESUMO
A method for the complexometric determination of aluminium in iron ore, sinter, concentrates and agglomerates encountered in international trade is described. The sample is fused in a zirconium crucible with a mixed flux of sodium carbonate and sodium peroxide. The fused mass is completely soluble in hydrochloric acid. The R(2)O(3) oxides are then precipitated with ammonia and redissolved in hydrochloric acid. Elements such as iron, titanium and zirconium are separated from aluminium by solvent extraction with cupferron and chloroform. After removal of traces of organic matter from the aqueous phase, the solution is treated with an excess of EDTA, which is then back-titrated with zinc solution (Xylenol Orange as indicator). Addition of ammonium fluoride then releases EDTA equivalent to the aluminium and this is titrated with zinc solution. The method is rapid. The precision and accuracy are excellent, and the results comparable with those obtained by the referee method.
RESUMO
A rapid method for determining total iron in iron ores, sinter and related materials without use of mercury compounds is described. Fusion of the sample with sodium peroxide in a zirconium crucible and subsequent treatment with acid yields total decomposition and a solution amenable to direct reduction to ferrous iron with a silver reductor and subsequent titration with dichromate. Results for NBS, BCS and ISO reference standard ores demonstrate the universal applicability of the method both for routine and referee analysis. There is no interference from vanadium and two samples can be analysed in 30 min.
RESUMO
A simple and precise method for the complexometric determination of aluminium in "Alzinoy" (a binary alloy of aluminium and zinc) is described. After dissolution of the sample in hydrochloric acid, aluminium, zinc and any lead and iron are complexed with excess of EDTA. The excess of EDTA is titrated with lead solution, with Xylenol Orange as indicator. Ammonium fluoride is then added to decompose the Al-EDTA complex, and the EDTA liberated is titrated with lead solution. Four samples can be analysed in about 45 min.
RESUMO
An automatic absorptiometric method is presented for the determination of silicon in iron ores, sinters, slags, iron and steel. The last two are dissolved in dilute sulphuric acid; the others are fused with sodium peroxide, then dissolved in hydrochloric acid. After suitable additions and dilution, the resulting solutions are treated identically in a Technicon AutoAnalyzer. The silicomolybdate formed is reduced to molybdenum blue with iron(II). Fluoride is added to provide a redox buffering system. The novelty of the method lies in selecting the sample sizes, conditions of fusion and/or dissolution and dilutions so that this universality is attained. Thus a single programme for the analyzer serves to determine, in any sequence, silicon in iron ores or sinters (1-6%), slags (3-10%), iron (0.4-2.5%) or steel (0.005-2%), the only change being in the tables used to translate transmittanee into per cent silicon. Both the precision and accuracy are satisfactory.
RESUMO
A rapid spectrophotometric method is presented for the determination of boron in steel by use of the fluoborate-Methylene Blue complex. The method is in principle similar to that of Rosotte, but modifications simplify the operation, obviate contamination and avoid problems with emulsion formation. Up to 20% Cr, 10% Ni, and 1% each of V, Mo and W present either individually or collectively do not interfere in the determination, making it applicable to alloy steels. The determination limit of the method has been lowered from 5 to 0.2 ppm boron. Samples are dissolved at room temperature in polythene bottles, solubilizing all forms of boron including boron nitride, and avoiding loss of relatively volatile boron compounds. The precision of the method is good. Six samples can be analysed in less than 2 hr.
RESUMO
A rapid spectrophotometric method employing zinc dibenzyldithiocarbamate is described for determining copper in a wide variety of steels. The acidity is not critical (0.5-2N) and the colour of the complex is stable for > 1 hr. The range of the method is 0.005-5% copper and 6 samples can be analysed in about an hour.
