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Method for determining nitrate ions in high-iron and copper matrix samples

A technology of nitrate ion and determination method, which is applied in the direction of color/spectral characteristic measurement, etc., can solve the problems of measurement interference, no national standard, and few documents, and achieve the effect of easy operation, good stability and high accuracy

Pending Publication Date: 2022-02-08
金川镍钴研究设计院有限责任公司 +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] During the process of nitric acid treatment of low-nickel matte, an intermediate material will be produced. This material is a high-iron and copper matrix sample. When the nitrate ion is determined by UV-visible spectrophotometry, iron and copper will significantly interfere with the determination, while for There is currently no national standard for the analysis and determination of nitrate ions in this sample, and there are few related literatures. Therefore, a method for the determination of nitrate ions in high iron and copper matrix samples is now proposed to solve this technical problem.

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  • Method for determining nitrate ions in high-iron and copper matrix samples
  • Method for determining nitrate ions in high-iron and copper matrix samples
  • Method for determining nitrate ions in high-iron and copper matrix samples

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Embodiment 1

[0078] The present embodiment provides a kind of assay method of nitrate ion in high iron, copper substrate sample, comprises the following steps:

[0079] (1) The contents of iron and copper matrix in the test sample are 50.93g / L and 41.81g / L respectively.

[0080] (2) Sample dilution treatment: Take 10 mL of the sample with a pipette, put it in a 100 mL volumetric flask, add 0.1 mL of sulfuric acid (1+1) dropwise, use pure water without nitrate ions to make up the volume, shake well, and then After diluting to 10000 times, let stand for 5min.

[0081] (3) Sample colorimetry: then move the solution into a 1cm quartz cuvette, and perform colorimetry at a wavelength of 210nm and 275nm, respectively, at absorbance A 总 and A Fe275 They were 1.196 and 0.147 respectively, and the reagent blank was tested together with the absorbance A 0 is 0.002.

[0082] (4) Result calculation:

[0083] a. Deduct the iron matrix interference according to the dual wavelength method, that is, a...

Embodiment 2

[0087] The present embodiment provides a kind of assay method of nitrate ion in high iron, copper substrate sample, comprises the following steps:

[0088] (1) The contents of iron and copper matrix in the test sample are 5.16g / L and 23.06g / L respectively.

[0089] (2) Sample dilution treatment: Take 10 mL of the sample with a pipette, put it in a 100 mL volumetric flask, add 0.1 mL of sulfuric acid (1+1) dropwise, use pure water without nitrate ions to make up the volume, shake well, and then After diluting to 1000 times, let stand for 5min.

[0090] (3) Sample colorimetry: then move the solution into a 1cm quartz cuvette, and perform colorimetry at a wavelength of 210nm and 275nm respectively, and the absorbance A 总 and A Fe275 They were 1.028 and 0.143 respectively, and the reagent blank was tested together with the absorbance A 0 is 0.002.

[0091] (4) Result calculation:

[0092] a. Deduct the iron matrix interference according to the dual wavelength method, that is,...

Embodiment 3

[0096] The present embodiment provides a kind of assay method of nitrate ion in high iron, copper substrate sample, comprises the following steps:

[0097] (1) The contents of iron and copper matrix in the test sample are 75.38g / L and 14.82g / L respectively.

[0098] (2) Sample dilution treatment: Take 10 mL of the sample with a pipette, put it in a 100 mL volumetric flask, add 0.1 mL of sulfuric acid (1+1) dropwise, use pure water without nitrate ions to make up the volume, shake well, and then After diluting to 10000 times, let stand for 5min.

[0099] (3) Sample colorimetry: then move the solution into a 1cm quartz cuvette, and perform colorimetry at a wavelength of 210nm and 275nm, respectively, at absorbance A 总 and A Fe275 Respectively 0.927, 0.211, the reagent blank was tested together, the absorbance A 0 is 0.002.

[0100] (4) Result calculation:

[0101] a. Deduct the iron matrix interference according to the dual wavelength method, that is, according to the formu...

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Abstract

The invention discloses a method for determining nitrate ions in high-iron and copper matrix samples, relates to the technical field of metallurgical analysis, and solves the problem of inaccurate nitrate ion determination caused by iron and copper interference in the analysis and determination process of the nitrate ions in the high-iron and copper matrix samples. The determination method comprises the following steps: selecting a sample determination system as a sulfuric acid system, selecting a dual-wavelength method with wavelengths of 210 nm and 275 nm, successfully deducting the interference of the iron matrix, deducting the interference of the copper matrix at the nitrate determination wavelength of 210 nm and within a certain concentration range and the absorbance of the copper ions conform to the Lambert-Beer law, and finally calculating the concentration of the nitrate ions through a formula. According to the determination method provided by the invention, the determination interference of copper and iron matrixes on the nitrate ions is successfully deducted, an analysis method which meets the process requirements and can realize rapid determination of the nitrate ions is developed, and the determination method has the characteristics of high analysis and test speed, low cost, good stability, high accuracy and convenience in operation.

Description

technical field [0001] The invention relates to the technical field of metallurgical analysis, more specifically to the technical field of nitrate ion determination. Background technique [0002] At present, there are many methods for the determination of nitrate maturity, mainly including ion chromatography, electrochemical method, photometric method, reduction method, catalytic kinetic method, spectroscopic method, flow injection analysis method and other analytical methods. Among them, the photometric method can be widely used due to the advantages of simple instruments, high sensitivity and low cost, and does not need to add color reagents and auxiliary reagents. [0003] The principle of using UV-Vis spectrophotometry to measure nitrate is that nitrate contains -N=O group, which has strong absorption in the ultraviolet region, and the relationship between the absorbance and its content follows the Lambert-Beer law. [0004] During the process of nitric acid treatment o...

Claims

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Application Information

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IPC IPC(8): G01N21/33
CPCG01N21/33
Inventor 马天飞孔令军宗红星张鹏席海龙陈彩霞张建玲郭京权
Owner 金川镍钴研究设计院有限责任公司
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