Method for determining content of boron in boride

A kind of determination method, the technology of boron content

Inactive Publication Date: 2017-05-31
SHANDONG NON METALLIC MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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But this method is only for the determinati

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  • Method for determining content of boron in boride
  • Method for determining content of boron in boride

Examples

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Embodiment 1

[0025] Determination of Boron Oxide Content in Boron Nitride

[0026] Weigh 1g of ERM-ED103 sample (accurate to 0.1mg), dissolve it in hot water at 70°C for 40min, then suction filter while it is hot, collect the filtrate in a 500mL Erlenmeyer flask, transfer it to a three-necked flask after cooling under running water, add 5g of mannitol, and add Rotor, titrate the reaction liquid with 0.05mol / L NaOH standard solution, use the pH standard solution to calibrate the pH meter, measure the pH change of the solution with the pH meter, and collect data every 30s. The titration curve takes the titration volume as the abscissa, and the pH value and The derivative is the ordinate, and the titration curve is derived, and the maximum point of the derivative is selected as the titration end point, and the corresponding consumed NaOH solution volume is the reaction end volume. The boron oxide content is calculated by formula (1).

[0027] Titrate with 0.05mol / L NaOH standard solution, th...

Embodiment 2

[0031] Determination of total boron content in boron nitride

[0032] Weigh 0.1g (accurate to 0.1mg) of the ERM-ED103 sample into a nickel crucible, add 3g of NaOH solid, cover, slightly open the cover, put it into the muffle furnace, heat up to 700°C, melt for 10min, after cooling, use Lip the molten material in hot water into a 250mL beaker, add calcium carbonate in portions and keep stirring until no bubbles are generated, boil on an electric stove for 3 minutes, then filter with suction after cooling slightly, wash the flask with hot water 5 times, wash the precipitate 10 times, collect Add 1 drop of (1+1) hydrochloric acid and 1 drop of methyl red to the filtrate in a 500mL Erlenmeyer flask, boil for 5 minutes, transfer to a three-necked flask after cooling under running water, and titrate with 0.1mol / L NaOH solution until it turns from reddish to just Yellow (not counting the volume), add 5g mannitol, add the rotor, use pH standard solution to calibrate the acidity meter...

Embodiment 3

[0036] Determination of Boron Oxide in Boron Carbide

[0037] Weigh 0.5g (accurate to 0.1mg) of ERM-ED102 sample, dissolve it in hot water at 70°C for 40 minutes, then filter while hot, collect the filtrate in a 500mL Erlenmeyer flask, transfer it to a three-necked flask after cooling under running water, add 5g of mannitol, Add the rotor, use the pH standard solution to calibrate the acidity meter, use 0.02mol / L NaOH solution for titration, use the acidity meter to measure the pH change of the solution, and collect data every 30s. The titration curve takes the titration volume as the abscissa, and the pH value Its derivative is the ordinate, and the titration curve is derived, and the maximum point of the derivative is selected as the titration end point, and the corresponding consumed NaOH solution volume is the reaction end volume. The boron oxide content is calculated by formula (1).

[0038] Titrate with 0.02mol / L NaOH standard solution, the sampling pH time interval is ...

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Abstract

The invention belongs to the technical field of testing. A mathematic derivation method is adopted; a titration end point is accurately judged by utilizing pH (Potential of Hydrogen) value jump nearby the titration end point, probable errors are reduced and the testing accuracy is improved. A method for determining the content of boron in boride, provided by the invention, comprises the following steps of pre-treating a sample, titrating and processing data, wherein NaOH with the concentration of 0.01mol/L to 0.2mol/L as a titration solution; a pH value is collected by utilizing a pH meter and the collection interval is 10s to 50s; a titration curve takes a titration volume as a transverse coordinate and the pH value and a derivative thereof as a longitudinal coordinate; the maximum point of the derivative is used as the titration end point; the corresponding volume of the consumed NaOH solution is used as the volume of the titration end point; the contents of boron oxide, free boron and total boron are calculated respectively. The method provided by the invention can be used for eliminating judgment on the titration end point by artificial subjective factors and a testing result is accurate and reliable. The method is applicable to determination of the contents of the boron oxide, the free boron and the total boron in the boride.

Description

technical field [0001] The invention belongs to the technical field of testing, and relates to a substance content measurement technology, in particular to a boron content measurement technology in borides. Background technique [0002] The traditional method for the determination of boron content in borides is to use phenolphthalein as an indicator, use acid-base neutralization reaction, and confirm the reaction end point by observing the color change of the solution during titration. There are two problems in this method. Firstly, phenolphthalein is used as the indicator of this reaction, and its color change range is between 8.2 and 10.0. The color will not change until the pH reaches 8. At this time, the volume of NaOH consumed will be obviously higher than that of boric acid. The volume when the reaction is complete; secondly, when the boron content is large, the color change of the solution is more obvious and the accuracy is higher, but when the boron content is low, ...

Claims

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Application Information

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IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 冀克俭李颖巩琛李本涛黄辉邓卫华李艳玲赵晓刚高岩立邵鸿飞
Owner SHANDONG NON METALLIC MATERIAL RES INST
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