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Digestion method and detection method of vanadium-nitrogen-titanium-iron mixed alloy cored wire

A technology of vanadium-nitrogen-titanium-iron and detection method, which is applied in the preparation of test samples, measurement of color/spectral characteristics, thermal excitation analysis, etc.

Active Publication Date: 2016-03-30
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

[0004] For vanadium-nitrogen-titanium-iron mixed alloy cored wire, if traditional chemical analysis methods such as titration are used to manually measure the content of a few major elements such as vanadium, titanium, nitrogen, aluminum, etc., not only the human resources are consumed, but also the operation steps are many. The process is long, the inspection cycle is long, there are many human factors, the analysis cost is high, and other trace alloys or impurity elements lack corresponding detection and analysis methods, which to a certain extent affect and restrict the quality control and improvement of VT cored wire products

Method used

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  • Digestion method and detection method of vanadium-nitrogen-titanium-iron mixed alloy cored wire
  • Digestion method and detection method of vanadium-nitrogen-titanium-iron mixed alloy cored wire
  • Digestion method and detection method of vanadium-nitrogen-titanium-iron mixed alloy cored wire

Examples

Experimental program
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Effect test

example 1

[0025] Digestion of VT cored wire samples

[0026] Weigh 0.1000g of the VT cored wire sample (hereinafter referred to as sample No. 1) into the microwave digestion inner tank, add 1.0mL concentrated nitric acid and 3.0mL concentrated hydrochloric acid, shake the container to disperse the sample evenly, and let it stand for 3 minutes in the open state Time pre-reaction; then wash the container wall with 5mL water in sequence, then add 1.0mL concentrated sulfuric acid drop by drop along the container wall, and continue to pre-react for 1 minute in the open state; finally put the outer tank and cover it And tighten it with a torque wrench to ensure a good seal. Put the sealed digestion container into the microwave digestion furnace according to the instrument operation steps, connect the temperature and pressure sensors, and perform microwave digestion and complexation reaction. This example adopts the microwave reaction method of ramping up the temperature, and the pressure is ...

example 2

[0033] The sample to be digested is 0.1500g VT cored wire sample (hereinafter referred to as sample No. 2), add 2.0mL concentrated nitric acid and 6.0mL concentrated hydrochloric acid, pre-react for 5 minutes; wash the container wall with 8mL water in sequence, and then Add 2.0mL concentrated sulfuric acid drop by drop to the wall of the vessel, and continue the pre-reaction for 2 minutes; finally, close the container for microwave digestion; set the microwave heating condition as ramp temperature rise, and the pressure is less than 800psi; Raise the temperature to 220°C for 3 minutes and keep it warm for 3 minutes to carry out enhanced digestion. After cooling to room temperature, dilute with water and set the volume to 250mL.

[0034] Other than that, the VT cored wire sample was digested in the same manner as in Example 1 and the solution was detected by ICP-OES.

example 3

[0036] The digestion sample is 0.1200g VT cored wire sample (hereinafter referred to as sample No. 3), add 1.5mL concentrated nitric acid and 4.5mL concentrated hydrochloric acid, and pre-react for 4 minutes; wash the container wall with 6mL water sequentially, and then Add 1.5mL concentrated sulfuric acid drop by drop, and continue the pre-reaction for 1 minute; finally, close the container for microwave digestion; set the microwave heating condition as ramp temperature rise, and the pressure is less than 800psi; first, heat up to 185°C for 13 minutes and keep it warm for 9 minutes for high-temperature digestion, and finally heat up for 2 minutes Heat at 215°C and keep it warm for 2 minutes for enhanced digestion. After cooling to room temperature, dilute with water to 200mL.

[0037] In addition, the VT cored wire sample was digested in the same manner as in Example 1 and subjected to ICP-OES detection.

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Abstract

The invention provides a digestion method and a detection method for a vanadium-nitrogen-titanium-iron mixed alloy cored wire. The digestion method comprises the following steps: putting a cored wire into a container, adding a concentrated nitric acid and a concentrated hydrochloric acid to the container; carrying out first time of pre-reaction under an open state; adding a concentrated sulfuric acid and carrying out second time of pre-treatment under the open state; carrying out digestion and complexation reaction by microwave in a closed state, so as to obtain a solution. The detection method comprises the following steps: cooling the solution, diluting and fixing volume to obtain a sample solution; determining the content of elementary compositions in one or more sample solutions by using inductively coupled plasma atomic emission spectrometry, flame atomic absorption spectrometry, titration, spectrophotometry and an electrochemical process. The digestion method and the detection method have the advantages of being safe to operate, simple and rapid, efficient and complete, fewer in man-made factors, and easy to accurately control and repeatedly reappear, and technical indexes such as the accuracy, the precision and the like of an analysis result are improved.

Description

technical field [0001] The invention relates to the technical field of alloy element detection, in particular to a digestion method and a detection method for a vanadium nitrogen titanium iron mixed alloy cored wire. Background technique [0002] At present, wire feeding treatment has become an effective method to improve the intrinsic quality of cast steel. The wire feeding technology has been able to feed more than ten kinds of metal wires and alloy core wires, and is widely used in steelmaking processes to effectively reduce the content of oxygen, sulfur and other elements in steel and the total amount of non-metallic inclusions, and has the functions of carburization, micro Alloying, changing the shape of inclusions, etc., can also be used for desulfurization, spheroidization, inoculation, and modification and degassing of aluminum alloys in the casting production process. The application of wire feeding technology has been widely popularized in various enterprises in t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/44G01N21/71G01N21/31
Inventor 成勇彭慧仙袁金红
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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