Digestion method and detection method for iron ore

A detection method, iron ore technology, applied in the direction of measuring device, test sample preparation, color/spectral characteristic measurement, etc., can solve the problems of complex matrix, interference accuracy, explosion hazard, etc., and achieve high detection accuracy and low System error, the effect of less reagent consumption

Inactive Publication Date: 2010-09-22
PANGANG GROUP VANADIUM TITANIUM & RESOURCES +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] ① After microwave digestion, a suspension will be formed, and there are many residues in the suspension, which makes the digestion not thorough enough
Mainly reflected in two points: First, microwave digestion usually requires the use of hydrofluoric acid, however, the hydrofluoric acid remaining in the digestion solution will seriously corrode the detection instruments used in subsequent detection steps
If the detection instrument is replaced with special parts with anti-corrosion ability, it will usually reduce the important technical performance such as transmission atomization efficiency, and the method of reducing the corrosion of hydrofluoric acid by boric acid complexation will increase the types of salt in the solution to be tested , which makes the matrix of the solution to be tested more complex, which leads to more factors that interfere with the detection and affects the accuracy of the detection results; the second is that after microwave digestion, the high content of silicon in the vanadium ilmenite is not removed

Method used

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  • Digestion method and detection method for iron ore
  • Digestion method and detection method for iron ore
  • Digestion method and detection method for iron ore

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The iron ore digestion method according to one aspect of the present invention comprises the steps: (1) placing the iron ore to be tested in a container, adding hydrofluoric acid and nitric acid into the container, sealing the container, and then using microwaves for the first Once digested, a suspension is formed; (2) the suspension is transferred to another container, and perchloric acid is added to the other container, and then the other container is heated in an open system, and then added to the other container Add hydrogen peroxide into the other container to use the nitric acid remaining in the suspension and the added perchloric acid and hydrogen peroxide to digest the residue in the suspension for the second time, so as to obtain a completely digested solution .

[0034] According to the digestion method of iron ore on the one hand of the present invention, hydrofluoric acid and nitric acid consumption can be according to the quality of iron ore to be measured ...

example 1

[0045] The hydrofluoric acid, nitric acid, perchloric acid, hydrogen peroxide and water used in this example are all of superior grade. The microwave digestion system used is Mars5 produced by CEM Company of the United States, and the ICP-AES is iCAP6300 of Thermo Fisher Corporation of the United States. Inductively coupled plasma atomic emission spectrometer.

[0046] Digestion of vanadium ilmenite

[0047] In this example, the sample to be tested is the ore sample of vanadium-titanium iron ore (produced by Panzhihua Iron and Steel Group) (hereinafter referred to as No. 1 sample), and its main components include: TiO 2 =9.0%, V 2 o 5 =0.3%, Al 2 o 3 =10%, Fe=26%.

[0048] Weigh 0.2500g vanadium-titanite raw ore sample in the microwave digestion inner tank, first add 1.0 mL of concentrated hydrofluoric acid (HF) with a mass percentage concentration of 40% and a mass percentage concentration of 65% along the inner tank wall concentrated nitric acid (HNO 3 ) 3.5mL. The...

example 2

[0053] In this example, the sample to be tested is the ore sample of vanadium-titanium iron ore (produced by Panzhihua Iron and Steel Group) (hereinafter referred to as No. 2 sample), and its main components include: TiO 2 =11%, V 2 o 5 =0.5%, Al 2 o 3 =10%, Fe=33%. In addition, in this example, except that the mass of the sample is 0.1000 g, the reagent dosages are: 1.0 mL of concentrated HF with a concentration of 47% by mass, concentrated HNO with a concentration of 68% by mass 3 3.0mL, concentrated perchloric acid 1.0mL, H 2 o 2 0.6mL and (1+2) dilute hydrochloric acid 15.0mL. The microwave heating program is set to raise the temperature of the material in the container to 190°C in 5 minutes, and then keep it warm for 8 minutes. The rest of the steps and parameters are the same as those in Example 1. Through the observation of the sample digestion results, it was found that the obtained digestion solution was clear and free of residues.

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Abstract

The invention provides a digestion method and a detection method for iron ore. The digestion method comprises the following steps: adding an iron ore sample in which hydrofluoric acid and nitric acid (or sulfuric acid) are mixed, then carrying out high-pressure closed microwave digestion to obtain a suspension; and heating the suspension in an unclosed system to secure the second digestion with residual nitric acid (or residual sulfuric acid) and added perchloric acid and hydrogen peroxide, thereby obtaining a solution which is digested fully. The detection method comprises the following steps: preparing a solution with the digested solution, and detecting the prepared solution by inductive coupling plasma atomic emission spectrometry, thereby obtaining content of each element of the iron ore sample. The invention has the advantages of high efficiency, high accuracy, and simple and fast process. Especially, the invention realizes accurate detection of key element content in iron ore, such as As, Pb, Zn, W, Sn, Ca, Mg, Cu, Co, Ni, Cr and Mo which affect product quality of iron and steel smelting and vanadium/titanium extraction.

Description

technical field [0001] The invention relates to the technical field of analysis and detection of compounds, more specifically, to iron ore categories, especially to digestion methods and detection methods of various types of vanadium-ilmenite. Background technique [0002] Vanadium ilmenite (including raw ore, concentrate, tailings, sinter, pellet ore and oxidized ilmenite, etc. containing vanadium, titanium, and iron, hereinafter also referred to as vanadium ilmenite samples) is different from ordinary Iron ore, its composition and phase structure are very complex, and usually contains about 10% TiO 2 and a few percent of V 2 o 5 . For example, there are very rich vanadium-titanium magnetites in the Panxi region of my country. These vanadium-titanium magnetites are multi-element paragenetic ores with complex compositions and phase structures, and the composition of different ore sites is also quite different. In addition to containing major elements such as Fe, V, Ti, Si...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N21/17G01N21/31
Inventor 成勇
Owner PANGANG GROUP VANADIUM TITANIUM & RESOURCES
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