Method for quickly measuring content of phosphorus, lead and zinc in industrial ferrous dust
A rapid determination of zinc content technology, applied in the field of chemical analysis, can solve the problems of unfavorable environmental protection and occupational health, matrix interference, cumbersome sample decomposition operation, etc.
Active Publication Date: 2013-12-11
ANGANG STEEL CO LTD
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[0003] At present, the determination of lead and zinc in slag and ore generally adopts flame atomic absorption spectrometry, and the determination of phosphorus adopts extraction and separation spectrophotometry, phosphorus molybdenum heteropoly acid photometry, etc. These methods can only measure one element method sample at a time The decomposition operation is cumbersome and the inspection cycle is long. It takes at least three days for analysts to complete the analysis of P, Pb, and Zn in a sample of iron-containing dust and mud. The linear range of the test is narrow, and the above wet chemical analysis process uses a large amount of organic reagents and other chemical reagents, which are not conducive to environmental protection and occupational health; X-ray fluorescence spectrometry analysis of elements such as lead, zinc and phosphorus containing iron impurities, because the detection limit of P, Pb, Zn and other elements by X-ray fluorescence spectroscopy is 0.1%, cannot It meets the precision requirements of smelting analysis. At the same time, because there is no standard sample of the same matrix to make a working curve, the matrix interference is serious and accurate quantitative analysis cannot be performed. The method is only suitable for on-line production stability monitoring, but cannot provide accurate quantitative analysis for process adjustment and quality analysis. method
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[0027] The present invention further illustrates the content of the invention through the examples, but is not limited by the examples.
[0028] Equipment used: IRIS Advantage ER / S full-spectrum direct-reading plasma emission spectrometer (TJA, USA); AURULAR-600 pressure self-controlled closed microwave sample dissolution system, power 1200W;
[0029] Reagents used: high-purity water; chemical reagents are of superior grade. Hydrochloric acid, nitric acid (ρ1.42g / mL), perchloric acid (ρ1.67g / mL), hydrofluoric acid.
[0030] Phosphorus, lead, zinc standard stock solution: use the National Standard Center to develop national standard reagents, 1mg / mL.
[0031] Determination of phosphorus, lead and zinc content in gas ash, blast furnace ash, dedusting ash and converter mud:
[0032]Each sample sample is dried at 105°C, cooled, weighed 0.1O00g (accurate to 0.1mg) in a magnetic dish covered with a layer of quantitative filter paper, and in a high-temperature furnace, gradually in...
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The invention discloses a method for quickly measuring the content of phosphorus, lead and zinc in industrial ferrous dust. The method comprises the steps of sample decomposition, setting the instrument analysis parameters of an ICP (Inductively Coupled Plasma) spectrometer, interference correction, making a working curve, and analyzing the content of to-be-measured elements in a measured sample by using an ICP spectral method, wherein the sample decomposition comprises sample pre-decarburizing treatment and sample pressure-microwave digestion. The invention provides a new method for improving the speed and the accuracy in a chemical test of hazardous elements in metallurgical dust.
Description
technical field [0001] The invention belongs to the field of chemical analysis, in particular to a method for quickly measuring the content of harmful elements phosphorus, lead and zinc in iron-containing dust and sludge in the iron and steel industry by using an ICP-AES method. Background technique [0002] Iron and steel enterprises will inevitably produce some iron-containing waste in the production process, such as blast furnace dust, converter dust, sintering dust, blast furnace gas ash, etc., and efficiently recycle the effective elements in iron and steel metallurgical dust to realize all The recycling of iron-containing dust and mud resources is undoubtedly an important part of the development of circular economy in the iron and steel industry. In recycling, metallurgical waste such as iron-containing dust and sludge can be made into iron-containing sludge pellets to replace part of the sintering and pelletizing raw materials for ironmaking, but the phosphorus and le...
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IPC IPC(8): G01N21/31G01N1/44G01N1/34
Inventor 于媛君杨丽荣王铁顾继红亢德华邓军华
Owner ANGANG STEEL CO LTD