Method for determining content of iron in nickel-based high temperature alloy

A technology for nickel-based superalloy and iron content, which is applied in the direction of chemical analysis by titration, which can solve the problems of time-consuming and labor-intensive, environmental pollution of waste liquid production, and complicated steps.

Inactive Publication Date: 2015-11-18
SHANGHAI ELECTRIC POWER GENERATION EQUIPMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method for determining the iron content in alloys is mainly based on the national standard "GB / T223.73-2008 Determination of Iron and Steel and Alloy Iron Content Titanium Trichloride-Potassium Dichromate Titration Method", but the method used in this standard is The manual volumetric titration method is only suitable for the determination of iron content with a mass fraction of 0.50% to 8.00% in superalloys and precision alloys
The method steps are cumbersome, time-consuming and labor-intensive
Moreover, this method needs to add a variety of indicators, and its waste liquid will pollute the production environment
At the same time, this method needs to judge the end point according to the color mutation of the indicator, and record the end point reading, which often causes systematic errors due to the judgment of the color mutation of the indicator and the inaccurate reading of the end point of the titration volume, reducing the precision and accuracy of the measurement results. Spend
In addition, there is no report on the method of determining iron content in nickel-based superalloys by double-jump potentiometric titration

Method used

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  • Method for determining content of iron in nickel-based high temperature alloy
  • Method for determining content of iron in nickel-based high temperature alloy
  • Method for determining content of iron in nickel-based high temperature alloy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] Take by weighing 0.5000g of nickel base superalloy sample 1# (IARM53D, standard fixed value: 6.86%), add the mixed acid solution (wherein, hydrochloric acid solution, nitric acid solution The volume ratio of the added amount is = 6-8:1, and the volume ratio of the added amount of hydrochloric acid solution, nitric acid solution, and hydrofluoric acid solution is 150-400:25-50:3, so that the added amount of hydrochloric acid solution is about 35.5ml, The amount of nitric acid solution added is about 4.5ml, and the amount of hydrofluoric acid solution added is about 0.25ml), and heated and dissolved at 120°C for 5 hours to completely dissolve the sample. Then add 20ml of 70-72% perchloric acid solution to heat and reflux for 4 minutes to oxidize the chromium and iron elements in the nickel-based superalloy and dehydrate the niobic acid. After heating to reflux, evaporate to nearly dryness, and after cooling slightly, dissolve the soluble salts in the sample with 200ml of ...

Embodiment 2

[0093] Take by weighing 0.5000g of nickel base superalloy sample 2# (IARM53D, standard fixed value: 6.86%), add the mixed acid solution (wherein, hydrochloric acid solution, nitric acid solution The volume ratio of the amount added is = 7:1, and the volume ratio of the amount of hydrochloric acid solution, nitric acid solution, and hydrofluoric acid solution is 175-350:25-50:3, so that the amount of hydrochloric acid solution added is about 35ml, and the amount of nitric acid solution added The amount is about 5ml, and the amount of hydrofluoric acid solution is about 0.3ml), and heated and dissolved at 150°C for 4 hours to completely dissolve the sample. Then add 10ml of 70-72% perchloric acid solution to heat and reflux for 5 minutes to oxidize the chromium and iron elements in the nickel-based superalloy and dehydrate the niobic acid. After heating to reflux, evaporate to nearly dryness, and after cooling slightly, dissolve the soluble salts in the sample with 200ml of hot ...

Embodiment 3

[0097] Dilute the obtained sample digestion solution 2* to 130ml. Follow the same procedure as above for sample processing to prepare sample blank test solution.

[0098] Add 1.5ml of 25% sodium tungstate solution dropwise to the sample digestion solution 2* and the sample blank solution respectively, and then add dropwise a 1% titanium trichloride solution to make the sample digestion solution 2* After the solid blue color and the sample blank solution respectively appear, stop the dropwise addition. The sodium tungstate solution is added dropwise in order to ensure that the titanium trichloride completely reduces the ferric iron to ferrous iron for subsequent reactions. Adding the titanium trichloride solution dropwise is to completely reduce the ferric iron in the sample digestion solution 2* to ferrous iron.

[0099] Then use an automatic potentiometric titrator to titrate the sample digestion solution 2* and the sample blank solution respectively with a potassium dichro...

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Abstract

The invention provides a method for determining the content of iron in nickel-based high temperature alloy. The method comprises the following steps: 1, processing a nickel-based high temperature alloy sample with a hydrochloric acid-nitric acid-hydrofluoric acid mixed acid as a digestion agent, perchloric acid as an oxidant and ammonium hydroxide as a precipitating agent to obtain a sample digestion solution; and 2, determining the content of iron in the digestion solution through adopting a two jump potentiometric titration technology. The method for determining the content of iron in nickel-based high temperature alloy takes shorter time and less force than manual direct titration, is simple and feasible, uses two potential jumps to determine the end point without using the color abrupt change of an indicator, omits the reading of the titration result, eliminates system errors brought by the indicator and the end point reading, and improves the accuracy and precision of the determination result.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis of metal materials, and relates to a method for measuring the iron content in nickel-based superalloys, in particular to a method for measuring the iron content in nickel-based superalloys by using a double-jump potentiometric titration method. Background technique [0002] Nickel-based superalloys are the most widely used and highest high-temperature strength alloys among superalloys. They are based on nickel (the content is generally greater than 50%), and have high strength and good resistance in the range of 650-1000 °C. Oxidation, gas corrosion resistance superalloy. Compared with iron-based superalloys, it has better oxidation resistance and gas corrosion resistance. However, nickel-based superalloys contain many other elements besides nickel, and these elements have a significant impact on the properties of nickel-based superalloys. Therefore, it is extremely important to accura...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
Inventor 张颖李虹史文斌
Owner SHANGHAI ELECTRIC POWER GENERATION EQUIPMENT CO LTD
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