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Vanadium-nitrogen alloy resolution method

A vanadium-nitrogen alloy and a technology for extracting vanadium-nitrogen alloy, which is applied in the field of vanadium-nitrogen alloy detection, can solve the problems of detection failure, matrix effect and blank effect, and insufficient consideration of excessive solvent, etc., and achieve the goal of improving accuracy and broad industrial application prospects Effect

Inactive Publication Date: 2013-02-27
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The digestion of vanadium-nitrogen alloy samples has the following difficulties: most of Si and Al exist in the form of oxides, and any single or mixed acid cannot be completely digested under normal conditions; arsenic and lead are easy to volatilize and be contaminated; a large amount of gas is added to vanadium-nitrogen alloy Elements N and C are easily splashed and lost when melted at high temperature; if the method of melting and digesting in a muffle furnace below 950°C with an alkaline flux is used, and because the vanadium-nitrogen alloy contains a large amount of gas elements N and C, it will be lost at high temperature for a long time Melting reaction, easy to splash loss, low results, and large amount of alkaline flux (10-15 times the sample volume), high reagent blank, high salt concentration, unable to use modern methods such as ICP-AES, ICP-MS, AAS, etc. Analytical means of precision instruments; the matrix effect and blank of conventional digestion methods are seriously affected, which can easily lead to detection failure, etc.
The article "Determination of Silicon, Manganese, Phosphorus, Aluminum in Vanadium-Nitrogen Alloy by Microwave Digestion-Plasma Spectrometry" in "Fujian Analysis and Test" 2006, 15(2) discloses an analytical method for detecting some impurity elements in vanadium-nitrogen alloy , but there are still many defects in this method when digesting alloys, such as: incomplete digestion of some impurity elements due to improper concentration ratio, insufficient consideration of the influence of excess solvent, and the need for special anti-corrosion parts for testing instruments, etc.
[0003] So far, there is no relevant report on a digestion method that can efficiently, safely, quickly and completely digest vanadium-nitrogen alloys

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] The digestion of embodiment 1 No. 1-7 samples (No. 1-7 samples are the vanadium-nitrogen alloys of different batch numbers produced by Panzhihua Iron and Steel Co., Ltd.)

[0018] Weigh 0.5000g of No. 1, 2, 3, 4, 5, 6, and 7 vanadium-nitrogen alloy samples for the following digestion:

[0019] The sample is placed in the inner tank of microwave digestion, and 3.0mL HNO is added dropwise along the tank wall 3 , and gently shake the digestion tank to fully contact the acid with the sample and pre-react until there are no bubbles and NO 2 Brown smoke is produced, then add 9.0mL HCl and 1.5mL HF, 1.5mL H 3 PO 4 Then put the outer tank on, cover the lid and tighten it with a torque wrench, put it into the microwave digestion furnace according to the operation steps of the instrument, and connect the temperature and pressure sensors.

[0020] Set the microwave program to ramp up the temperature, and the pressure is controlled below 800psi. The whole process is divided into...

Embodiment 2

[0022] Example 2 Determination of sample impurity content after digestion

[0023] No. 1, 2, and 3 samples after the digestion of embodiment 1, carried out 8 times of independent ICP-AES analysis and determination respectively, carried out statistical processing to 8 times of measurement results, evaluated the digestion method of the present invention according to relative standard deviation to actual vanadium nitrogen Digestion treatment of alloy samples and the precision of ICP-AES method determination. The measurement results are shown in Table 1.

[0024] Table 1 Analysis results and precision of vanadium nitrogen alloy samples (n=8)

[0025]

[0026] It can be seen from Table 1 that the RSD% of each element is less than 3%, which shows that the method of the present invention has good digestion effect of vanadium nitrogen alloy, good reproducibility and high precision.

Embodiment 3

[0028] The vanadium-nitrogen alloy samples 4, 5, 6, and 7 after digestion in Example 1 were analyzed and measured by the ICP-AES method respectively. In addition, referring to the national standard analysis method of vanadium pentoxide, samples No. 4, 5, 6, and 7 were first digested with aqua regia to digest the vanadium-nitrogen alloy samples, and the residue was filtered with an alkaline mixed flux (Na 2 CO 3 +H 3 BO 3 =1+1) In the muffle furnace for 30 minutes of high-temperature melting reaction at 950°C, the residue melt was leached and dissolved with hydrochloric acid, and then combined with the original filtrate to make up volume, and finally an appropriate amount of test solution was taken and the acidity was adjusted. determined by chemical analysis methods. The comparison results of the analysis and detection of the two technical means are shown in Table 2.

[0029] Table 2 Analysis and detection results comparison

[0030]

[0031] As can be seen from Table ...

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Abstract

The method comprises: a) taking out the Vanadium-Nitrogen alloy to be tested from a sealed container; adding nitric acid to react until bubbles is free and the NO2 smoke is generated; b) adding hydrofluoric acid and phosphoric acid; then sealing them and using micro wave to clear up; c) adding hydrofluoric acid.

Description

technical field [0001] The invention relates to a vanadium-nitrogen alloy digestion method, which belongs to the field of vanadium-nitrogen alloy detection. Background technique [0002] As a new type of iron and steel metallurgical additive, vanadium-nitrogen alloy can greatly improve the strength of steel and save 20% of vanadium resources, so it has been widely valued at home and abroad. In order to control and improve the quality of vanadium-nitrogen alloy products, it is necessary to establish an analysis and inspection method for determining trace impurity elements such as silicon, aluminum, calcium, magnesium, iron, chromium, titanium, arsenic, and lead in vanadium-nitrogen alloys. To establish an analysis method, first What needs to be solved is the problem of digestion of the sample into a solution. The digestion of vanadium-nitrogen alloy samples has the following difficulties: most of Si and Al exist in the form of oxides, and any single or mixed acid cannot be c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/44
Inventor 成勇
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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