Method for measuring nickel content in low alloy steel by spectrophotometry

A spectrophotometric method, low-alloy steel technology, applied in color/spectral characteristic measurement, analysis through chemical reaction of materials, material analysis through observation of the influence of chemical indicators, etc., can solve the difficulty of ensuring accurate measurement results Accuracy and precision, interference and other issues

Active Publication Date: 2013-07-10
北京北机机电工业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the actual operation process, it is difficult to ensure the accuracy and precision of the measurement results due to the serious interference of elements such as iron and copper in the matrix to the determination of nickel.

Method used

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  • Method for measuring nickel content in low alloy steel by spectrophotometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1 Weigh 0.5000 g of the sample (standard sample 1#), accurate to 0.0001 g.

[0054] Put the sample to be weighed in a 100mL steel measuring bottle, add 5mL of a mixture of concentrated hydrochloric acid and concentrated nitric acid, heat, and when the sample is nearly dissolved, add distilled water in portions, 1mL each time, until small bubbles in the solution can be observed Stop adding distilled water until the bubbles disappear and start to appear. At this time, add a total of 5 mL of distilled water, and continue heating until the sample is completely dissolved.

[0055] Add 5mL of perchloric acid to the dissolved sample, evaporate until fumes of perchloric acid are emitted, and cool slightly. Add 20mL of distilled water to dissolve the salt, dilute to the mark with water, and shake well to obtain solution a.

[0056] Accurately pipette 10.00mL test solution from solution a into a 100mL volumetric flask, add 7mL potassium sodium tartrate, 7mL ammonium citr...

Embodiment 2

[0063] Example 2 Weigh 0.5000 g of the sample (standard sample 1#), accurate to 0.0001 g.

[0064] The process of dissolving the sample is the same as in Example 1.

[0065] Add 5mL of perchloric acid to the dissolved sample, evaporate until fumes of perchloric acid are emitted, and cool slightly. Add 20mL of distilled water to dissolve the salt, dilute to the mark with water, and shake well to obtain solution a.

[0066] Accurately pipette 10.00mL test solution from solution a into a 100mL volumetric flask, add 10mL potassium sodium tartrate, 10mL ammonium citrate, 10mL sodium hydroxide, 2mL ammonium persulfate, 10mL dimethylglyoxime, dilute to the mark with water, mix uniform; wherein, the order of adding the masking agent is: first add sodium potassium tartrate, then ammonium citrate.

[0067] Place it for 10-20min, that is, after the chelation reaction is sufficient, use the reference solution as a reference, measure the color at 530nm on a spectrophotometer, and measure...

Embodiment 3

[0072] Example 3 Weigh 0.5000 g of the sample (standard sample 1#), accurate to 0.0001 g.

[0073] The process of dissolving the sample is the same as in Example 1.

[0074] Add 5mL of perchloric acid to the dissolved sample, evaporate until fumes of perchloric acid are emitted, and cool slightly. Add 20mL of distilled water to dissolve the salt, dilute to the mark with water, and shake well to obtain solution a.

[0075] Accurately pipette 10.00mL test solution from solution a into a 100mL volumetric flask, add 12mL sodium potassium tartrate, 12mL ammonium citrate, 10mL sodium hydroxide, 2mL ammonium persulfate, 10mL dimethylglyoxime, dilute to the mark with water, mix uniform; wherein, the order of adding the masking agent is: first add sodium potassium tartrate, then ammonium citrate.

[0076] Place it for 10-20min, that is, after the chelation reaction is sufficient, use the reference solution as a reference, measure the color at 530nm on a spectrophotometer, and measure...

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Abstract

The invention provides a method for measuring nickel content in low alloy steel by spectrophotometry. The method comprises the steps of: (1) dissolving a sample; (2) adding a proper amount of perchloric acid till smoking, and adding distilled water so as to obtain a solution a: (3) adding potassium sodium tartrate and ammonium citrate into the solution to serve as dual masking agents; (4) adding a strong base, then adding ammonium persulfate as an oxidizing agent, and then adding a dimethylglyoxime developer so as to react with nickel to generate a red chelate; (5) conducting measuring: zeroing the solution obtained in step (4) with a reference solution, carrying out color comparison at a position of 530nm on a spectrophotometer, thus measuring absorbance A1; (6) calculating the nickel content according to the absorbance A1. By applying dual masking agents, the method of the invention substantially improves the accuracy and precision of a measured result on the basis of guaranteeing rapid measuring.

Description

technical field [0001] The invention relates to a method for measuring nickel content in low-alloy steel, in particular to a method for measuring nickel content in low-alloy steel by using a spectrophotometric method. Background technique [0002] Nickel is one of the important elements in alloy steel, which can increase the elasticity, ductility and corrosion resistance of steel, so that alloy steel has high mechanical properties. At present, the determination of nickel content in alloy steel mainly includes gravimetric method, spectrophotometric method, combined titration method and spectroscopic method. Among them, spectrophotometric method is currently the most widely used method due to its fast analysis speed, low-cost instrument, and simple operation. method. However, in the actual operation process, it is difficult to ensure the accuracy and precision of the measurement results because the elements such as iron and copper contained in the matrix have seriously interf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/78G01N21/31
Inventor 贾海平王春玲李木其
Owner 北京北机机电工业有限责任公司
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