Method for measuring molybdenum content in molybdenum waste residues

A determination method and waste residue technology, applied in the field of analytical chemistry, can solve the problems of not meeting the needs of rapid determination of molybdenum waste residues, the detection range cannot cover molybdenum waste residues, and the experience requirements of inspectors are high, so as to meet product quality supervision and inspection, promotion and application value. Great, reduce the effect of environmental pollution

Pending Publication Date: 2020-06-19
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The lead molybdate gravimetric method uses various reagents such as ammonia water, nitric acid, and lead acetate to digest samples, and at the same time requires operations such as precipitation, filtration, drying, and ashing.
[0005] To sum up, none of the existing detection technologies are applicable to molybdenum waste residues, and the detection range cannot cover the molybdenum content (5%-20%) in molybdenum waste residues, and the detection technologies are all traditional manual analysis methods, which require various Digestion samples with chemical reagents consume many types and large amounts of reagents, many operation steps, cumbersome process, high labor intensity, long time-consuming, high experience requirements for inspectors, and do not meet the rapid determination needs of molybdenum waste slag resource recovery and trade process

Method used

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  • Method for measuring molybdenum content in molybdenum waste residues
  • Method for measuring molybdenum content in molybdenum waste residues

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Experimental program
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Effect test

Embodiment 1

[0041] In the embodiment of the present invention, the inductively coupled plasma optical emission spectrometer is an Agilent 5110.

[0042] 1. Digestion and preparation of molybdenum waste residue samples

[0043] 1. Put the sample in an agate mortar and grind it by hand, pass through an 80-mesh sieve, take 10g-20g of the sieved sample according to the quartering method, put it in a 500ml glass beaker, and keep it in a drying oven at 110°C for 2 hours. Drying, place the dried sample in a desiccator to cool to room temperature;

[0044] 2. Configure anhydrous sodium carbonate and borax mixed solvent (according to the mass ratio of 2.5:1);

[0045] 3. Weigh 0.10 g of molybdenum waste slag cooled to room temperature in step 1, place it in a platinum crucible filled with 2.0 g of mixed flux in advance, and then cover with 1.5 g of mixed flux. Place the platinum crucible in a high-temperature furnace and heat it up to 920°C for 20 minutes. Take out and cool to room temperature....

Embodiment 2

[0055] Embodiment 2 precision test

[0056] Two molybdenum waste slag samples were respectively prepared and analyzed for 6 independent detection sample solutions, and the results of the 6 measurements were statistically processed, and the precision of the present invention was evaluated according to the relative standard deviation (RSD%). The measurement results are shown in Table 2.

[0057] Table 2: Analytical method precision (n=6)

[0058]

[0059] It can be seen from Table 2 that the RSD (relative standard deviation) is not more than 2.0%, indicating that the present invention has good precision. It can be seen in Table 2 that the determination results of the two analytical lines of molybdenum element for the same sample are basically the same.

Embodiment 3

[0060] The recovery rate of standard addition of embodiment 3 method The recovery rate is the important index of characterizing the accuracy of the method, in two molybdenum content known molybdenum waste residue samples (content is respectively 6.57% and 12.45%), add the molybdenum standard solution of different content to carry out Spike recovery test. According to the experimental method, three parts of 0.10 g of a molybdenum waste slag sample were weighed for high-temperature melting, and three kinds of molybdenum standard solutions (1 mg / mL) with different content gradients were added before constant volume. During instrumental analysis, input the sample mass on the software, measure the molybdenum content of the spiked mixture, and calculate the spiked recovery rate. The test results are listed in Table 3.

[0061] Table 3: Spike recoveries for methods

[0062]

[0063] As can be seen from Table 3, the recovery rate of the method established by the present invention ...

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Abstract

The invention relates to a method for measuring the content of molybdenum in molybdenum waste residues, belonging to the technical field of analytical chemistry. Firstly, molybdenum waste residues tobe detected are digested to obtain a molybdenum waste residue sample, then the molybdenum waste residue sample is combined with an inductively coupled plasma-emission spectrometer, instrument workingparameters such as atomizer pressure, plasma emission power and observation height are optimized through tests, and an element analysis spectral line to be detected is optimized, so that the detectionperformance of a matrix element molybdenum is improved. The method is wide in application, wide in detection concentration, high in anti-interference capability, simple to operate, easy to master andexcellent in technical indexes such as accuracy, precision and recovery rate. Rapid and accurate analysis of the molybdenum content in the molybdenum waste residue is realized, and the sample can bedetected within 6 hours.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for determining molybdenum content in molybdenum waste slag. Background technique [0002] Molybdenum is a very important refractory rare metal element. It is an important element that constitutes alloy additives and inorganic functional materials (such as catalysts). It is widely used in iron and steel, nonferrous metals, petrochemicals and other fields. [0003] A large amount of molybdenum waste slag will be produced during the beneficiation, smelting and processing of molybdenum metal and related molybdenum products. As a recyclable resource, molybdenum waste slag can be re-refined metal molybdenum and related products. Among them, the molybdenum content in molybdenum waste residue is about 5% to 20%, which has good resource recovery value. The content of molybdenum element is the main basis for determining the resource recovery process and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/44
CPCG01N21/73G01N1/44
Inventor 何鹏飞李景滨唐伟
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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