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Method for determining content of calcium in nickel-calcium alloy by adopting fluorescence titrimetric method

A titration method, a technology of calcium content, applied in the field of chemical analysis, can solve problems such as difficulty in observing the change of green fluorescence in the upper part of the solution, inability to accurately determine the titration end point, blurred green fluorescence in the upper part, etc., achieving clear green fluorescence color and shortening the analysis period. , the effect of easy observation

Active Publication Date: 2017-06-13
JIANGSU LONGDA SUPERALLOY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the detection method of "GB / T5195.1-2006 Determination of Fluorite Calcium Fluoride", a black paper pad is used to make a black background under the beaker, and the black paper is only pasted on the bottom of the beaker, so the test solution is only on the bottom of the beaker. Obvious light difference is produced, that is, obvious green fluorescence is produced, and the green fluorescence in the upper part of the test solution is blurred; during the titration process, with the decrease of the ions to be measured, the green fluorescence gradually disappears from the bottom of the test solution; When the fluorescence in the upper part of the solution is blurred, it is difficult to observe the change of the green fluorescence in the upper part of the solution when the titration is near the end point, which makes it impossible to accurately judge the titration end point and cause certain errors in the titration results.

Method used

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  • Method for determining content of calcium in nickel-calcium alloy by adopting fluorescence titrimetric method
  • Method for determining content of calcium in nickel-calcium alloy by adopting fluorescence titrimetric method

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0020] Experimental equipment such as figure 1 As shown, the experimental apparatus comprises a beaker 3, an electric heating magnetic stirrer 4, a polytetrafluoroethylene magnet 5, a liquid to be tested 6, a titration solution 7, a burette 8 and an iron frame platform 11; the burette 8 is fixed on the iron frame platform 12, Iron stand platform 12 sides are provided with electrothermal magnetic force stirrer 4, place beaker 3 on the electric heat magnetic force stirrer 4, be provided with polytetrafluoroethylene magnet 5 in beaker 3; There is a liquid to be tested 6; it also includes a black lid bucket 1 and a lower black bucket 2; the top of the black lid bucket 1 has a round hole 9, and the black lid bucket 1 has a first observation window 10 from bottom to top; Lower black bucket 2 has the second observation window 11 equally from top to bottom.

Embodiment 2

[0022] The equipment described in Example 1 was used to determine the mass fraction of calcium in the nickel-calcium alloy.

[0023] (1) Weighing and dissolving of raw materials: Accurately weigh 0.2500g nickel-calcium alloy sample in a beaker, add 20mL volume concentration of 10% hydrochloric acid, drop 2mL volume concentration of 47% hydrofluoric acid, 3mL 98% sulfuric acid, 1g boric acid, heated to dissolve;

[0024] (2) Filtration: adjust the pH to 7-8 with 10g / L sodium hydroxide, add 20mL 50g / L copper-iron reagent while stirring, shake well, let stand for 30min, filter in a beaker with medium-speed filter paper, and add 0.5% copper Wash the beaker and precipitate with the reagent lotion for 3 to 5 times, and keep the filtrate.

[0025] (3) Reagent adjustment: drop a small piece of Congo red test paper into the filtrate, adjust to Congo red test paper with volume concentration of 10% ammonium hydroxide, add 0.2g ammonium tartrate, 10mL volume concentration is 49% triethan...

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Abstract

The invention relates to a method for determining the content of calcium in a nickel-calcium alloy by adopting a fluorescence titrimetric method and belongs to the technical field of chemical analysis. The method comprises the following steps: weighing raw material, dissolving, filtering, adjusting by a reagent and titrating to determine the content of the calcium in the nickel-calcium alloy. According to the method for determining the content of the calcium in the nickel-calcium alloy by adopting the fluorescence titrimetric method, a range of quantitatively detecting the content of the metal calcium in a nickel-calcium alloy test sample is 4 percent to 15 percent. A beaker containing a test solution is filled into a black barrel and a complete black packaging background is provided for the whole test solution, so that a green fluorescence color of the whole test solution is clear and consistent; the two black barrels can move up and down, so that testers can conveniently put in or take out beakers with different volumes; observation windows, which have the same size and are overlapped, are formed in side faces of the used black barrels so that the testers can conveniently observe. In a fluorescence titration process, a small quantity of iron ions in the solution can be separated in a manner of forming sediment or adding a screening agent for screening. By adopting the fluorescence titrimetric method, an analysis period is greatly shortened and analysis steps are simplified; meanwhile, the precision and accuracy of the detection method are improved.

Description

technical field [0001] The invention relates to a method for measuring calcium content in nickel-calcium alloy by fluorescence titration, which belongs to the technical field of chemical analysis. Background technique [0002] Nickel-calcium alloy has important applications in the smelting of nickel-based superalloys and the preparation of silicon electrode composite materials. The main components are 4%-15% of Ca, C<0.3%, Fe<0.5%, Cu<0.25, Si<1, and the rest For you. Ca in high-temperature alloys and a proper amount of calcium in nickel alloys mainly play the role of deoxidation, desulfurization and dephosphorization, as well as spheroidizing and dispersing primary carbides; it can also refine grains, prevent grain growth, and significantly improve casting performance , mechanical properties and thermoplasticity. For the determination of calcium content in nickel-calcium alloys, there is currently no relevant national or industry standard analysis method. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64G01N31/16
CPCG01N21/643G01N31/16G01N2021/6443
Inventor 年季强华剑刘青青吕水永
Owner JIANGSU LONGDA SUPERALLOY MATERIAL CO LTD
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