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Method for measuring impurity elements arsenic, tin antimony in ferromolybdenum

A technology of ferromolybdenum and elements, applied in the direction of material excitation analysis, thermal excitation analysis, etc., can solve the problems of result influence, long cycle, product scrapping, etc., and achieve the effect of simple pretreatment process

Active Publication Date: 2009-05-20
CHINA ERZHONG GRP DEYANG HEAVY IND
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Problems solved by technology

[0003] In the past, due to the inability to detect arsenic in ferromolybdenum, the acceptance index for the range of arsenic content could not be specified in the procurement contract
Because the existing methods for detecting tin and antimony do not specify the sum of iron and molybdenum in the standard solution, changes in the content of molybdenum often have a significant impact on the results of antimony in production, and it is necessary to re-prepare the standard solution to calibrate the instrument
In order to accurately detect arsenic, tin, and antimony, some people try to separate and enrich arsenic, tin, and antimony from the solution with an extractant, but only for research, because the operation is cumbersome and the cycle is long, and it cannot meet the inspection requirements of mass production
[0004] So far, because there is no suitable method for the simultaneous determination of the harmful impurity elements arsenic, tin, and antimony in ferromolybdenum, the supplier cannot completely provide the detection report of the harmful impurity elements arsenic, tin, and antimony in ferromolybdenum, purchase and use At the same time, it is also impossible to specify a complete acceptance index for the harmful impurity elements arsenic, tin, and antimony, which leads to product scrapping and re-feeding due to excessive harmful impurity elements in ferromolybdenum.

Method used

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  • Method for measuring impurity elements arsenic, tin antimony in ferromolybdenum

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preparation example Construction

[0024] Preparation of standard series solutions: Accurately weigh 5 parts of pure iron 30.0mg~50.0mg and pure molybdenum 50.0mg~70.0mg, so that the sum of the two is close to 100mg, and iron and molybdenum have appropriate content gradients. Add 0.0500ml-1.600ml of arsenic diluted standard solution, 0.010ml-1.000ml of tin diluted standard solution, and 0.010ml-1.000ml of antimony diluted standard solution to make arsenic, tin, and antimony have appropriate content gradients. Add 20ml of hydrochloric acid-nitric acid mixed acid, heat at a temperature not higher than 120°C, and blow water at the right time to replenish the lost water. After the sample is completely dissolved, cool down, dilute with water to 100ml, and shake well.

[0025] Preparation of ferromolybdenum control sample solution: When the content of one or more elements in the sample obviously exceeds the content of the standard series solution, prepare a control sample solution with an appropriate composition acco...

Embodiment 1

[0028] Embodiment 1: the situation that individual sample detection finds inferior molybdenum iron:

[0029] The upper limit of the calibration curve for arsenic is 0.16% and detections in production clearly outside that range: shows about 1% arsenic, is the direct read reliable? For this extreme situation, according to the sample display results, a control sample solution of 40% iron, 58% molybdenum, and 1.00% arsenic can be prepared for quality control. , the monitoring solution for measuring arsenic 1.00% shows a value of 0.95%, which is already low, so the sample showing 1.02% arsenic in the sample should actually be reported as the calibration result of 1.07%:

[0030] 1.00%÷0.95%×1.02%=1.07%

[0031] Table 1 Reproducibility and accuracy of analysis of low-quality ferromolybdenum samples (w%, n=10)

[0032]

Embodiment 2

[0033] Embodiment 2: The situation that batches of samples detect and find inferior molybdenum ferromolybdenum:

[0034] The upper limit of the calibration curve for arsenic is 0.16%, but the batch test results in production obviously exceed this range: inferior ferromolybdenum shows arsenic 1.02%, 0.28%, etc., is the result of direct reading reliable? When this extreme situation occurs, according to the sample display results such as iron 41.30%, molybdenum 56.70%, arsenic 1.02%, tin 0.005%, antimony 0.008%, and iron 34.38%, molybdenum 62.97%, arsenic 0.28%, tin 0.003% , antimony 0.030%, etc., add a standard solution of 40% iron, 58% molybdenum, and 1.00% arsenic, and calibrate the instrument together with the original standard solution. For samples with data such as 0.27%, the arsenic display value after adding a standard solution to recalibrate is 1.07%, 0.28%, etc., and the analysis results can be read directly.

[0035] Table 2 The reproducibility and accuracy of random ...

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Abstract

The invention provides a method for determining arsenic, tin and antimony in ferromolybdenum, which belongs to the field of quantitative analysis in analytical chemistry. The method for determining arsenic, tin and antimony in ferromolybdenum comprises the steps of dissolving a ferromolybdenum specimen in mixed acid of hydrochloric acid and nitric acid, using standard serial solutions to draw a working curve on an inductively-coupled plasma atomic emission spectrometer, deducting interference among elements and background interference through a computer program correction mode and determining arsenic, tin and antimony which are trace detrimental impurity element in a specimen solution. The method does not need to perform separation, enrichment and other fussy operation during specimen pretreatment and only needs to suck the ferromolybdenum specimen solution into an instrument for determination, and the percentage content of trace arsenic, tin and antimony in the specimen can be simultaneously displayed after tens of seconds. The content range that can be directly determined by the method is as follows: 0.005 to 1.00 percent of arsenic, 0.001 to 0.20 percent of tin and 0.001 to 0.10 percent of antimony.

Description

technical field [0001] The invention relates to a method for determining harmful impurity elements arsenic, tin and antimony in ferromolybdenum, belonging to the field of quantitative analysis in analytical chemistry. Background technique [0002] Ferromolybdenum is an important raw material for manufacturing heavy pressure vessels, nuclear power equipment and other products. Before feeding, it is necessary to detect the content of harmful impurity elements such as arsenic, tin, antimony, and select high-quality raw materials for feeding to ensure product quality. Otherwise, it may threaten the safe use of pressure vessels, nuclear power equipment and other products. [0003] In the past, due to the inability to detect arsenic in ferromolybdenum, the acceptance index for the range of arsenic content could not be stipulated in the procurement contract. Because the existing methods for detecting tin and antimony do not specify the sum of iron and molybdenum in the standard s...

Claims

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Application Information

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IPC IPC(8): G01N21/73
Inventor 刘金祥
Owner CHINA ERZHONG GRP DEYANG HEAVY IND
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