Methods for digesting and detecting titanium concentrate, titanium slag or titanium carbide slag

A detection method, titanium carbide technology, applied in the direction of measuring device, test sample preparation, color/spectral characteristic measurement, etc., can solve problems such as inapplicability, and achieve the effect of improving product quality

Inactive Publication Date: 2013-11-27
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the problem that the above existing technology and the digestion and testing of titanium-rich materials cannot be applied to sample digestion and element detection of ilmenite, titanium slag, and titanium carbide slag, the present invention realizes the Complete digestion of titanium concentrate, titanium slag, titanium carbide slag, and accurate determination of trace and trace impurity elements Nb, Zr, V, Cu, Co, Ni, Cr, Pb, As, Cd

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  • Methods for digesting and detecting titanium concentrate, titanium slag or titanium carbide slag
  • Methods for digesting and detecting titanium concentrate, titanium slag or titanium carbide slag

Examples

Experimental program
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Embodiment 1

[0038] The hydrofluoric acid, hydrochloric acid, hydrogen peroxide and water used in this example are all of superior grade, the microwave digestion system used is Mars5 manufactured by CEM Company of the United States, and the ICP-AES instrument is the iCAP6300 inductor of Thermo Fisher Corporation of the United States Coupled plasma atomic emission spectrometer.

[0039] Digestion of titanium concentrate

[0040] In this embodiment, the sample to be tested is titanium concentrate (hereinafter referred to as sample No. 1).

[0041] Weigh 0.1000g of the titanium concentrate sample to be tested, first rinse the wall of the container with 3.0mL of water and shake the container to promote the suspension and dispersion of the sample; then, add 2.0mL of hydrofluoric acid with a mass percentage concentration of 40% to 47% The percentage concentration is 36%-38% hydrochloric acid, and the container is sealed. Use microwave heating method and set the conditions to raise the tempera...

Embodiment 2

[0046] In this embodiment, the sample to be tested is a titanium slag sample (produced by Panzhihua Iron and Steel Group) (hereinafter referred to as sample No. 2).

[0047]Weigh 0.5000g of the sample to be tested, rinse the wall of the vessel with 5.0mL of water and suspend and disperse the sample; add 5.0mL of hydrofluoric acid and 10.0mL, then set the microwave condition to 10min and raise the temperature to 150°C, and keep it warm for 8min for the first digestion reaction; After the reaction is over, cool the container at 95°C and slowly empty the gas in the closed container while it is hot. After opening the container, add 4.0mL hydrogen peroxide while it is hot. The microwave condition is set to 8min and the temperature is raised to 210°C, and the temperature is kept for 10min for the second digestion. reaction. In addition, the titanium slag sample was digested in the same manner as in Example 1 and detected with an ICP-AES instrument.

Embodiment 3

[0049] In this embodiment, the sample to be tested is a titanium carbide slag sample (produced by Panzhihua Iron and Steel Group) (hereinafter referred to as sample No. 3). In this example, the sample mass is 0.2500g, and the reagent dosages are: 3.5mL water, 3.5mL hydrofluoric acid, 6.0mL hydrochloric acid, 3.0mL hydrogen peroxide; the first microwave program is set to take 9min to raise the temperature to 130°C , keep warm for 6 minutes; the second microwave program is set to take 6 minutes to raise the temperature to 190°C, and keep warm for 8 minutes. In addition, the titanium carbide slag sample was digested in the same manner as in Example 1 and detected with an ICP-AES instrument.

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Abstract

The invention discloses methods for digesting and detecting titanium concentrate, titanium slag or titanium carbide slag. The method for digesting the titanium concentrate, the titanium slag or the titanium carbide slag comprises the following steps of: weighing a sample to be detected, placing the sample to be detected in a container, washing a container wall of the container by using an appropriate amount of deionized water, and shaking the container to make the sample be suspended and dispersed; adding hydrofluoric acid and hydrochloric acid into the container, closing the container, and performing first-time digestion reaction by using microwave; after the first-time digestion reaction is finished, cooling the container, and when the temperature of the container is reduced to 90 to 95 DEG C, emptying acid gas and a volatile reaction product in the closed container; opening the container, adding hydrogen peroxide while the container is hot, and then immediately closing the container; performing second-time digestion reaction by using the microwave; and after the second-time digestion reaction is finished, cooling the container to room temperature, directly diluting by using water and fixing the volume, and thus obtaining a solution of the sample to be detected. According to the methods, the sample is completely digested, and the accuracy, precision, working efficiency and analysis speed of detection data can be improved.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection of compounds, more specifically, the invention relates to a digestion method and a detection method of various types of titanium concentrates, titanium slags and titanium carbide slags as basic raw materials of the titanium industry. Background technique [0002] Although ilmenite, titanium slag, and titanium carbide slag are the same as other titanium-containing products such as rutile and titanium-rich materials, they belong to the high-titanium matrix samples and are used as the basic raw materials for the production of titanium dioxide, titanium sponge, and other titanium industrial products. However, their titanium dioxide matrix content and the types and contents of coexisting impurity elements are quite different, so the objects, requirements and goals of corresponding detection and analysis are not the same. [0003] At present, the titanium dioxide matrix and constant impur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/44G01N21/73G01N27/62G01N21/31G01N27/626
Inventor 成勇袁金红胡金荣
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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