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A method for analyzing free carbon

An analytical method and technology for free carbon, applied in the field of analytical chemistry, can solve the problem that free carbon cannot be directly measured, and achieve the effects of being easy to master, expanding the scope of application, and easy to operate.

Inactive Publication Date: 2011-12-21
PANZHIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the reports in the existing literature, free C basically needs to be analyzed by instruments, and when there are many kinds of carbon in the sample, the instrument cannot directly measure the content of free carbon. The simple laboratory, the sample contains a variety of carbons, and the instrumental analysis method has certain limitations

Method used

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  • A method for analyzing free carbon
  • A method for analyzing free carbon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Get three vanadium carbide sample quality and be m=0.2000 gram, carry out three parallel tests according to the method of the present invention: first add the water wetting of about 10mL, add the sulfuric acid solution of 10mL (the volume ratio of sulfuric acid and water is about 1: 1 ), and then add 50g / L potassium permanganate solution, resulting in 2 drops of excess red in the solution, which does not fade after standing for 3 minutes, and oxidizes low-valent oxygen-containing vanadium to vanadium pentoxide.

[0056] Add about 0.5g of urea, adjust sodium nitrite with 1% solution until the solution is red, remove 2 drops of excess, and reduce the manganese dioxide and excess potassium permanganate produced by the reaction to Mn 2+ , the excess sodium nitrite is removed with urea, and the vanadium carbide and vanadium pentoxide are not reduced; filter, transfer the filter paper and the residue into a porcelain crucible, put it in a muffle furnace, and burn it to constan...

Embodiment 2

[0062] Since there is no vanadium carbide standard sample and high-purity vanadium carbide substance, the free carbon in the simulated vanadium carbon standard sample is measured to verify the accuracy of the determination of the present invention.

[0063] Simulated vanadium-carbon standard sample method: use vanadium-iron standard sample (V%=54.20%), and high-purity carbon powder (C%=99.85%) to synthesize vanadium-carbon in vanadium carbide, according to the composition of vanadium carbide: carbon: vanadium The mass ratio is about 4: 1 simulation, accurately weigh 175.00g ferrovanadium standard sample and 25.00g high-purity carbon powder, fully mix, the prepared standard sample, in this standard sample: V%=47.42%, C%= 12.48%.

[0064] Weigh three copies of the above-mentioned vanadium-carbon standard samples with masses of 0.1000g, 0.1500g, and 0.2000g respectively, and carry out parallel determination of free carbon content according to the method of Example 1 of the presen...

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Abstract

The invention relates to a method for analyzing free carbon and belongs to the field of analytical chemistry. A pure chemical analysis method is established; by the method, a carbon sulfur determination instrument is not required; and the method is simple and convenient to operate, and easy to master. The invention adopts the technical scheme that: the method comprises the following steps of: weighting a sample of which mass is m for pre-processing; wetting the sample by using water, adding an acidic solution, and then adding a potassium permanganate solution and adding two drops more when the red color of the solution appears till the red color does not disappear in 3 minutes; adding a sodium nitrite solution, adding two drops more when the red color of the solution disappears, and removing the excess sodium nitrite by using urea; filtering, moving filter paper and residues into a porcelain crucible together, putting into a muffle furnace, firing at the temperature of 550 to 610 DEG C till constant weight, cooling to room temperature, and weighting mass m1; putting into the muffle furnace again, firing at the temperature of 850 to 950 DEG C till the constant weight, cooling to the room temperature, and weighting mass m2; and calculating the percentage content of the free carbon, namely C%=(m1-m2) / m*100%.

Description

technical field [0001] The invention relates to a method for analyzing free carbon, belonging to the field of analytical chemistry. Background technique [0002] The process of high-purity vanadium carbide new products is mainly obtained by using ammonium polyvanadate or ammonium vanadate under the reduction of carbon, and vacuum roasting at a high temperature above 1000°C. The main components of the product are vanadium carbide, vanadium suboxide and free carbon. However, due to the different process conditions, the conversion rate of vanadium is different, and the quality of the products is also very different. The different degrees of vanadium conversion lead to various forms of vanadium in the product, and it is difficult to accurately analyze the content of vanadium carbide. Because, if the conversion rate of vanadium into vanadium carbide is analyzed from the phase analysis of vanadium, and thus the content of vanadium carbide is deduced, the analysis steps will be v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04G01N1/28
Inventor 冯向琴方民宪刘秀刘松利邹建新陶洪早
Owner PANZHIHUA UNIV
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