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Mixed flux and method for measuring silicon content of silicon iron by perchloric acid dehydration gravimetric method

A technology of perchloric acid dehydration and gravimetric method, which is applied in the field of analytical chemistry, can solve problems such as the determination of silicon content without flux, and achieve the effects of simple operation, accurate measurement results and fewer components

Inactive Publication Date: 2013-11-13
PANZHIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Through literature search, in the field of analytical chemistry, there is no flux made by directly mixing anhydrous sodium carbonate and potassium nitrate at present, and there is no flux provided by the present invention for the determination of silicon content in ferrosilicon samples

Method used

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  • Mixed flux and method for measuring silicon content of silicon iron by perchloric acid dehydration gravimetric method
  • Mixed flux and method for measuring silicon content of silicon iron by perchloric acid dehydration gravimetric method

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preparation example Construction

[0025] The preparation method of the mixed flux of the present invention: first weigh analytical pure potassium nitrate and grind it into powder in a mortar, then weigh analytical pure anhydrous sodium carbonate and potassium nitrate in proportion, mix evenly, and bottle for later use.

[0026] Perchloric acid dehydration gravimetric method of the present invention measures the method for silicon content in ferrosilicon, comprises the steps:

[0027] a. Mix the ferrosilicon sample to be tested with the mixed flux described in any of the above, and then wrap it into a spherical ball sample with filter paper (those skilled in the art can understand that it should be wrapped as tightly as possible, and the tighter the better ), put into a porcelain crucible filled with graphite powder (those skilled in the art can understand that graphite powder should be burnt at 800-900°C);

[0028] b. Put the porcelain crucible containing the sample into the muffle furnace, slowly raise the te...

Embodiment 1

[0038] Take the same ferrosilicon standard sample YSB11601-99 (Si%=72.95) using anhydrous sodium carbonate: potassium nitrate (weight ratio) 5:1, 7:1, 8:1, 10:1, 15:1 mixture The solvent decomposition samples were measured in parallel three times to check the precision of the determination method. The method is as follows, and the results are shown in Table 1.

[0039] a. Divide the slow quantitative filter paper with a diameter of 12.5cm into two halves, take half and fold it into a funnel shape, and put it on a 30ml crucible. b. Add 5 grams of the mixed flux of the present invention to the folded filter paper in a. Sweep 0.2000g of the ferrosilicon sample into the mixed flux in b, so that the sample is fully mixed with the mixed flux, and d pack the filter paper described in a, b, and c into spherical balls. f Put the sample ball described in d in a 100ml porcelain crucible filled with graphite powder and ground smooth. g Put the porcelain crucible containing the sample des...

Embodiment 2

[0044] Get three ferrosilicon sample quality and be 0.2000 grams, according to the method process of embodiment one, get anhydrous sodium carbonate: potassium nitrate=10: 1 mixed flux decomposes sample, carry out three parallel measurements, check the precision of its assay method The results are shown in Table 2.

[0045] Table 2 Analysis results of different ferrosilicon samples with the same mixed flux

[0046]

[0047] As can be seen from the data in Table 1, the mixed flux of the present invention is used to measure the silicon content in ferrosilicon, and the measurement results have good reproducibility; the extreme difference is less than 0.3%. Blank values ​​are very low and negligible.

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Abstract

The invention discloses a mixed flux and a method for measuring the silicon content of silicon iron by a perchloric acid dehydration gravimetric method and applied to decomposition of an early-stage sample, and belongs to the field of chemistry. The mixed flux consists of anhydrous sodium carbonate and nitrate potash, wherein the weight ratio of the anhydrous sodium carbonate to the nitrate potash is (6-11):1. The method for measuring the silicon content of the silicon iron comprises the following steps: a, mixing a silicon iron sample to be measured and the mixed flux uniformly, wrapping the mixture by using filter paper into a spherical sample, and placing the sample into a porcelain crucible with graphite powder; b, placing the porcelain crucible with the sample into a muffle furnace, slowly heating to 900 DEG + / -10 DEG C and preserving heat for 15-20 minutes; c, taking out the porcelain crucible subjected to heat preservation in the step b and cooling to below 50 DEG C, wherein the sample is shaped like a button; and d, placing the button-shaped sample into hydrochloric acid and leaching, and in the subsequent steps, operating the leaching liquid according to an analysis method in national standard GB4333.1-84. According to the mixed flux and the method, the sample can be fused and decomposed effectively, so that the measuring result is more accurate.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a mixed flux and a method for decomposing a sample in the early stage of determining the silicon content in ferrosilicon by a perchloric acid dehydration gravimetric method. Background technique [0002] The current national standard GB4333.1-84 "Chemical Analysis of Ferrosilicon by Perchloric Acid Dehydration Gravimetric Method for Determination of Silicon Content", the mixed flux sodium carbonate used in the early sample processing operation: sodium peroxide = 1:2 (mass ratio) is not very good The sample is decomposed accurately, and it is easy to produce sample splashing, which makes the result low, and this method is difficult to operate. The application number is 200810149787.2 Chinese patent: a molten metallurgical sample analysis flux and the flux disclosed in its preparation and use method. In practice, boric acid: sodium carbonate = 1:2 (mass ratio) is use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N5/04
Inventor 冯向琴邹华超周兰花陈绿英孙艳
Owner PANZHIHUA UNIV
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