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Analysis method for determining high-content molybdenum element in metal material by potentiometric titration

A metal material, potentiometric titration technology, applied in chemical analysis by titration, electrochemical variables of materials, measuring devices, etc., can solve the problems of lack of rapid and accurate determination of high-content molybdenum in metal materials, etc.

Active Publication Date: 2020-07-07
SHANGHAI ELECTRIC POWER GENERATION EQUIPMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the above-mentioned shortcoming of the prior art, the object of the present invention is to provide a kind of analysis method that adopts potentiometric titration to measure the high-content molybdenum element in the metal material, for solving the lack of rapid and accurate determination of the high-content molybdenum element in the metal material in the prior art The problem with the method of analysis

Method used

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  • Analysis method for determining high-content molybdenum element in metal material by potentiometric titration
  • Analysis method for determining high-content molybdenum element in metal material by potentiometric titration
  • Analysis method for determining high-content molybdenum element in metal material by potentiometric titration

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Weigh 0.2g of metal material and place it in a 200mL beaker, add an appropriate amount of hydrochloric acid and nitric acid with a volume ratio of 6:1 to dissolve the mixed solution of hydrochloric acid and nitric acid to form the first solution.

[0100] Add 15mL of the mixed acid aqueous solution of sulfuric acid and phosphoric acid to the first solution, heat to 550°C to emit phosphoric acid fumes for 60 seconds, then remove it quickly, stop heating, and let the phosphoric acid fumes evaporate completely to form the second solution. Wherein, in the mixed acid aqueous solution of sulfuric acid and phosphoric acid, the volume ratio of sulfuric acid, phosphoric acid and water is 1:2:3. When the metal material is selected from one of nickel-based alloys, cobalt-based alloys, or metal materials containing tungsten and vanadium, 10 mL of phosphoric acid is additionally added to the first solution.

[0101] In the second solution, add 80mL phosphoric acid (if Fe in the seco...

Embodiment 2

[0105] This example is to compare the effect of phosphoric acid concentration.

[0106] Accurately pipette 25 mL of 1000 mg / mL molybdenum standard solution and place it in a 200 mL beaker, and follow the preparation process in Example 1 above to obtain the second solution sample to be tested. According to Table 2, different volumes of phosphoric acid were added to the 7 parts of the above-mentioned solution to be tested, and the subsequent measurement conditions were the same as in the above-mentioned Example 1. The specific test results are shown in Table 2.

[0107] The influence of table 2 phosphoric acid concentration on titration result

[0108]

[0109] It can be seen from Table 2 that when the concentration of phosphoric acid in the solution is less than 11.5mol / L, the first equivalence point disappears, and the measured result is low due to incomplete reduction of molybdenum. However, if the concentration of phosphoric acid is too high, the viscosity of the soluti...

Embodiment 3

[0111] This embodiment is to compare the influence of sulfuric acid concentration.

[0112] According to the preparation process in the above-mentioned Example 1, the second solution sample to be tested was obtained. According to Table 3, 0, 1, 2, 2.5, and 3 mL of sulfuric acid were added to 7 parts of the above-mentioned second solution samples, and the subsequent measurement conditions were the same as in the above-mentioned Example 1. The specific test results are shown in Table 3.

[0113] The influence of table 3 sulfuric acid concentration on titration result

[0114]

[0115] It can be seen from Table 3 that with the increase of sulfuric acid addition, the first equivalent point jump potential dropped from 325mV to 281mV. Adding more than 1mL of sulfuric acid can increase the potential jump, and adding 2mL of sulfuric acid can be used.

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Abstract

The invention provides an analysis method for determining a high-content molybdenum element in a metal material by potentiometric titration, which comprises the following steps: (1) dissolving the metal material in a mixed solution of hydrochloric acid and nitric acid to form a first dissolved solution; (2) adding a mixed acid aqueous solution of sulfuric acid and phosphoric acid into the first dissolved solution, heating until phosphoric acid smoke is emitted, and stopping heating to form a second dissolved solution; (3) adding phosphoric acid, sulfuric acid and a manganese sulfate aqueous solution into the second dissolved solution to form a third dissolved solution; and (4) adding an ammonium ferrous sulfate aqueous solution into the third dissolved solution to adjust the initial pointposition, putting an electrode, dropwise adding a potassium dichromate standard solution, and determining the content of the molybdenum element in the metal material according to the volume differenceof the two potential leaps by adopting an isovolumetric potentiometric titration mode. According to the technical scheme provided by the invention, the high-content molybdenum element in metal materials such as nickel-based alloy, cobalt-based alloy, medium-low alloy steel and ferromolybdenum can be accurately determined, and the accuracy of a determination result is improved.

Description

technical field [0001] The invention relates to an analysis and test method, in particular to an analysis method for measuring high-content molybdenum in metal materials by potentiometric titration. Background technique [0002] Whether the alloy composition in the metal meets the requirements will directly affect the performance of the material. As far as superalloys are concerned, due to the harsh and dangerous application environment, there are strict requirements on the performance of superalloys. If the performance does not meet the requirements, not only will it Cause immeasurable losses, and unpredictable accidents may occur. [0003] Molybdenum is an important alloying element. Molybdenum has the effect of solid solution strengthening and forming carbides and intermetallic compounds. If it is excessive, it will form a topological close-packed phase and affect the properties of the alloy. Adding molybdenum to the steel can make the steel have a uniform crystal struct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N27/44
CPCG01N31/164G01N27/44Y02E30/30
Inventor 刘思思丁丽锋李虹史文斌邓敏
Owner SHANGHAI ELECTRIC POWER GENERATION EQUIPMENT CO LTD
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