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Method for testing content of boron trioxide in glass containing zinc and lead

A technology of diboron trioxide and testing methods, which is applied in the direction of analyzing materials through chemical reactions and material analysis through observing the impact on chemical indicators, and can solve problems affecting the accuracy of test results and interfering with measurement. Achieve the effect of clear discoloration point, easy to control, and eliminate the interference of gender elements

Inactive Publication Date: 2011-05-04
NO 53 RES INST OF CHINA NORTH IND GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is used when amphoteric elements such as zinc and lead are contained. The amphoteric elements interfere with the determination and affect the accuracy of the test results.
[0005] "Determination of B in glass by acid-base neutralization titration 2 o 3 Improvement of "("Glass", Volume 27, Issue 3, 2000) uses EDTA to complex the interfering amphoteric elements to reduce the influence of interfering elements and increase measurement accuracy, but EDTA itself is a weak acid, and excess EDTA will also participate Acid-base neutralization reaction affects the accuracy of test results

Method used

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  • Method for testing content of boron trioxide in glass containing zinc and lead
  • Method for testing content of boron trioxide in glass containing zinc and lead
  • Method for testing content of boron trioxide in glass containing zinc and lead

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Accurately weigh 0.5g of glass (containing lead and zinc) sample, add 4g of sodium hydroxide to melt in a nickel crucible, soak the melt with hot water, add 2 drops of methyl red indicator, and neutralize with 1mol / L hydrochloric acid Until the system turns reddish, calcium carbonate is added until the system turns yellow, and the precipitate is filtered to obtain solution A.

[0031] Add 10 mL of 0.1 mol / L Ca-EDTA solution to solution A, adjust the solution to reddish with 0.1 mol / L hydrochloric acid, and obtain solution B.

[0032] Titrate solution B with 0.1mol / L sodium hydroxide standard solution to turn yellow (do not record the reading), add 2g mannitol, 10 drops of 1:1 bromothymol blue and phenol red mixed indicator, and oxidize with 0.1mol / L hydroxide Titrate the sodium standard solution to purple; then add 2g mannitol, the purple color disappears, continue to titrate with 0.1mol / L sodium hydroxide standard solution, and repeat this, until the purple color of th...

Embodiment 2

[0040] Accurately weigh 0.5g glass sample (containing lead and zinc), add about 5g potassium hydroxide and melt it in a nickel crucible. Extract the molten material with hot water, add 2 drops of methyl red indicator dropwise, neutralize with 2mol / L nitric acid until the system turns reddish, add sodium carbonate until the system turns yellow, filter the precipitate to obtain solution A.

[0041] Add 15 mL of 0.1 mol / L Ca-EDTA solution to solution A, adjust the solution to reddish with 0.2 mol / L hydrochloric acid, and obtain solution B.

[0042] Neutralize solution B with 0.05mol / L sodium hydroxide until the solution turns yellow, add 2g of mannitol, 10 drops of 1:0.5 bromothymol blue and phenol red mixed indicator, and titrate with 0.1mol / L sodium hydroxide standard solution to purple; then add 2g of mannitol, purple disappears, continue to titrate with 0.1mol / L sodium hydroxide standard solution, and so on, until the purple color of the test solution does not disappear after...

Embodiment 3

[0047] Accurately weigh 0.5g glass sample (containing lead and zinc), add about 5g potassium hydroxide and melt it in a nickel crucible. Extract the molten material with hot water, add 2 drops of methyl red indicator dropwise, neutralize with 5mol / L hydrochloric acid until the system turns reddish, add potassium carbonate until the system turns yellow, filter the precipitate, and obtain solution A.

[0048] Add 25 mL of 0.1 mol / LCa-EDTA solution to solution A, adjust the solution to reddish with 0.5 mol / L hydrochloric acid, and obtain solution B.

[0049] Neutralize solution B with 0.11mol / L sodium hydroxide solution until the system turns yellow, add 2g mannitol, 10 drops of 1:1.5 bromothymol blue and phenol red mixed indicator, use 0.2mol / L sodium hydroxide standard The solution is titrated to purple; add 2g of mannitol again, the purple color disappears, continue to titrate with 0.2mol / L sodium hydroxide standard solution, and so on, until the purple color of the test solut...

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Abstract

The invention relates to a method for testing the content of boron trioxide in glass containing zinc and lead, belonging to the technical field of chemical analysis testing. The method comprises the following steps: dissolving a sample by using a conventional glass treatment method (alkali fusion method) to convert boron into borates, dissolving the fused mass in dilute acid, adding carbonates, and separating the borates from other impurity elements; and complexing the amphoteric elements (zinc and lead) by using Ca-EDTA (Ethylene Diamine Tetraacetic Acid); and adding mannitol to quantitively convert boric acid into alcohol boric acid with strong degree of dissociation, and accurately controlling the titration end-point by using a mixed indicator of bromothymol blue and phenol red. The testing method has the advantage of clear discolored points, is easy to control, and can effectively eliminate the interference of amphoteric elements (zinc, lead and the like) in the glass, thereby obviously enhancing the measurement accuracy and repetitiveness. The relative standard deviation of the test is reduced to below 0.5%, and the standard recovery rate is higher than 98%.

Description

1. Technical field [0001] The invention belongs to the technical field of chemical analysis and testing, and relates to the determination of the content of diboron trioxide in powder samples, in particular to the determination of the content of diboron trioxide in zinc-lead-containing glass powder. 2. Background technology [0002] Diboron trioxide is a commonly used raw material for low-temperature sealing glass, which can reduce the expansion coefficient of glass, improve the thermal and chemical stability of glass, increase the refractive index of glass, improve the mechanical properties of glass, accelerate the clarification of glass, reduce the crystallization ability. However, boron trioxide is highly volatile, and when the content is too high, it will produce SiO-rich 2 The devitrified material skin will reduce the performance of the material. Therefore, accurate determination of boron trioxide content is of great significance to the quality control of glass materia...

Claims

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Application Information

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IPC IPC(8): G01N21/79
Inventor 冀克俭邓卫华周彤华兰刘元俊李艳玲邵鸿飞张蕾
Owner NO 53 RES INST OF CHINA NORTH IND GRP
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