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Method for quickly determining rhenium in chemical sediment

A rapid determination and chemical technology, applied in the field of chemical analysis and detection, can solve the problems such as the failure to realize the rapid detection and analysis of rhenium in the precipitated rhenium slag, the inability to meet high-load production and production control, and the unstable rhenium content and grade. Control, analysis speed is fast, and the effect of ensuring analysis accuracy

Inactive Publication Date: 2020-01-10
广西金川有色金属有限公司 +1
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  • Claims
  • Application Information

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Problems solved by technology

However, due to the extremely unstable rhenium content and grade in the dirty acid stock solution produced by smelting flue gas acid production, the rhenium content in the precipitated rhenium slag also fluctuates greatly, and the subsequent production of ammonium rhenate is easily affected by the grade of rhenium in the precipitated rhenium slag. Therefore, in the production process, it is necessary to accurately and quickly determine the rhenium in the sinking rhenium slag, so as to provide data support for the production of ammonium rhenate
[0003] At present, there are existing detection methods for rhenium in sinking rhenium slag, such as hydrochloric acid-nitric acid airtight digestion method adopted by Yunnan Copper Industry, after digesting samples for 8 hours, and then using spectrophotometric colorimetry; in addition, there is also the use of sodium peroxide alkali fusion decomposition The method of spectrophotometric determination of the sample, although the detection time is shortened compared with the hydrochloric acid-nitric acid airtight digestion method, the process is more complicated and inconvenient to operate; at the same time, the existing detection standards for rhenium include GB / T15079.11-94 molybdenum The determination of the amount of rhenium by the chemical analysis method of concentrates, and the determination of the amount of rhenium by the analysis method of ammonium perrhenate in YS / T836-2012, but the above methods have not realized the rapid detection and analysis of rhenium in the sinking rhenium slag, and the detection efficiency is obviously insufficient. Meet the needs of high-load production and production control

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  • Method for quickly determining rhenium in chemical sediment
  • Method for quickly determining rhenium in chemical sediment

Examples

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Embodiment 1

[0025] A method for rapid determination of rhenium in chemical industry precipitation rhenium slag, it comprises the steps:

[0026] (1) Preparation of rhenium standard solution: Weigh 1.5537g of potassium perrhenate in a beaker, dissolve it with 100mL of water, then add 50ml of nitric acid with a concentration of 1.42g / ml, then transfer it into a 1000mL volumetric flask, add water to dilute to the mark, Mix well to get rhenium standard solution Ⅰ with a concentration of 1mg / ml; take 10ml of rhenium standard solution Ⅰ in a 100mL volumetric flask, then add 10mL of nitric acid, then add water to dilute to the mark, and mix well to get 100μg / ml rhenium standard Solution II;

[0027] (2) Sample treatment: Weigh 0.2000g of the sample to be tested, put it in a 500ml beaker, then add 5ml of nitric acid with a concentration of 1.42g / ml, 1ml of bromine with a concentration of 1.18g / ml, and cover with a watch glass , and then heated in a water bath at a temperature of 45°C until the s...

Embodiment 2

[0034] A method for rapid determination of rhenium in chemical industry precipitation rhenium slag, it comprises the steps:

[0035] (1) Preparation of rhenium standard solution: Weigh 1.5537g of potassium perrhenate in a beaker, dissolve it with 100mL of water, then add 50ml of nitric acid with a concentration of 1.42g / ml, then transfer it into a 1000mL volumetric flask, add water to dilute to the mark, Mix well to get rhenium standard solution Ⅰ with a concentration of 1mg / ml; take 10ml of rhenium standard solution Ⅰ in a 100mL volumetric flask, then add 10mL of nitric acid, then add water to dilute to the mark, and mix well to get 100μg / ml rhenium standard Solution II;

[0036] (2) Sample treatment: Weigh 0.2000g of the sample to be tested, put it in a 500ml beaker, then add 5ml of nitric acid with a concentration of 1.42g / ml, 1ml of bromine with a concentration of 1.18g / ml, and cover with a watch glass , and then heated in a water bath at a temperature of 40°C until the s...

Embodiment 3

[0043] A method for rapid determination of rhenium in chemical industry precipitation rhenium slag, it comprises the steps:

[0044] (1) Preparation of rhenium standard solution: Weigh 1.5537g of potassium perrhenate in a beaker, dissolve it with 100mL of water, then add 50ml of nitric acid with a concentration of 1.42g / ml, then transfer it into a 1000mL volumetric flask, add water to dilute to the mark, Mix well to get rhenium standard solution Ⅰ with a concentration of 1mg / ml; take 10ml of rhenium standard solution Ⅰ in a 100mL volumetric flask, then add 10mL of nitric acid, then add water to dilute to the mark, and mix well to get 100μg / ml rhenium standard Solution II;

[0045] (2) Sample treatment: Weigh 0.2000g of the sample to be tested, put it in a 500ml beaker, then add 5ml of nitric acid with a concentration of 1.42g / ml, 1ml of bromine with a concentration of 1.18g / ml, and cover with a watch glass , and then heated in a water bath at a temperature of 50°C until the s...

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Abstract

The invention discloses a method for quickly determining rhenium in chemical sediment, and the method comprises four steps such as preparation of a rhenium standard solution, sample processing, debugging of a measuring instrument, drawing of a rhenium standard curve, and determination of a sample, and especially comprises the following steps of preparing the rhenium standard solution by using potassium perrhenate, dissolving the sample under test of rhenium by using nitric acid and bromine to obtain the solution under test, determining the rhenium content in the standard series solution and the solution under test by using an inductively coupled plasma emission spectrometer, and determining the rhenium content in the sample under test by drawing the rhenium standard curve and calculation analysis. The method provided by the invention can quickly and accurately determine the content of rhenium in the sediment.

Description

technical field [0001] The invention belongs to the field of chemical analysis and detection, and in particular relates to an analysis method for rapidly determining rhenium in chemical industry sinking rhenium slag. Background technique [0002] The dirty acid stock solution produced by the existing copper smelting flue gas acid production still contains rare and valuable resources. In order to realize the full recovery and utilization of resources, the stock solution containing solid suspended matter and high metal impurities is usually treated, and then treated with The rhenium element in the sewage acid is recovered by chemical method, the enrichment of rhenium is realized, and the precipitated rhenium slag is formed, and then the crude ammonium rhenate is produced by wet leaching-extraction comprehensive process, and then 99% ammonium rhenate product is obtained through further refining and purification . However, due to the extremely unstable rhenium content and grade...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/28
CPCG01N21/73G01N1/28
Inventor 杨晶丽尹文梅陈淑霞朱海燕史光源
Owner 广西金川有色金属有限公司
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