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Method for measuring trace amount of inorganic impurities in boric acid

A determination method and boric acid technology, applied in the field of analytical chemistry, can solve the problems of easy introduction of other impurities, cumbersome processing, and unfavorable boric acid sample analysis, and achieve the effect of improving pretreatment speed, simple operation steps, and fast and efficient determination.

Active Publication Date: 2016-02-10
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These techniques are either limited to specific ions, or use corrosive reagents, which are easy to introduce other impurities, and the subsequent treatment is cumbersome
K.Dash et al. published in 2003 on the 1002 volume of "JournalofChromatographyA" reported the use of methanol vapor and boric acid matrix to react to generate volatile trimethyl borate, then absorb the trimethyl borate obtained with glycerol to To achieve the purpose of eliminating the boric acid matrix, but this method requires the use of special equipment, and the pretreatment time can be as long as 7 hours, which is not conducive to the analysis of large quantities of boric acid samples

Method used

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  • Method for measuring trace amount of inorganic impurities in boric acid
  • Method for measuring trace amount of inorganic impurities in boric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Accurately weigh 1g (accurate to 0.0001g) of boric acid sample and place it in a PFA jar;

[0023] (2) The mass ratio of the boric acid sample and the spectrally pure methanol reagent is 1:8, directly adding the spectrally pure methanol reagent into the open PFA jar, and stirring evenly;

[0024] (3) Place the PFA jar in a boiling water bath at 78°C and heat it for 80 minutes, then stop heating to obtain a boric acid sample solution;

[0025] (4) After the boric acid sample solution is cooled, use secondary deionized water to make up the volume in a 5mL volumetric flask;

[0026] (5) ICP-OES was used to analyze the content of lithium, sodium, potassium, magnesium and calcium in the boric acid sample solution after constant volume.

[0027] Among them, the test conditions of ICP-OES are as follows:

[0028] Power 1100W; Plasma gas 13L / min; Auxiliary gas 0L / min; Sheath gas 0.3L / min; Atomizing gas 0.8L / min; The most sensitive line was used; the light chamber was pur...

Embodiment 2

[0031] (1) Accurately weigh 1g (accurate to 0.0001g) of boric acid sample and place it in a PFA jar;

[0032] (2) The mass ratio of the boric acid sample and the spectrally pure methanol reagent is 1:18, and the spectrally pure methanol reagent is directly added to the open PFA jar, and stirred evenly;

[0033] (3) Place the PFA jar in a boiling water bath at 120°C and heat it for 45 minutes, then stop heating to obtain a boric acid sample solution;

[0034] (4) After the boric acid sample solution is cooled, use secondary deionized water to make up the volume in a 5mL volumetric flask;

[0035] (5) ICP-OES was used to analyze the content of lithium, sodium, potassium, magnesium and calcium in the boric acid sample solution after constant volume.

[0036] Among them, the test conditions of ICP-OES are as follows:

[0037] Power 1100W; Plasma gas 13L / min; Auxiliary gas 0L / min; Sheath gas 0.3L / min; Atomizing gas 0.8L / min; The most sensitive line was used; the light chamber wa...

Embodiment 3

[0040] (1) Accurately weigh 1g (accurate to 0.0001g) of boric acid sample and place it in a PFA jar;

[0041] (2) The mass ratio of the boric acid sample and the spectrally pure methanol reagent is 1:12, and the spectrally pure methanol reagent is directly added to the open PFA jar, and stirred evenly;

[0042] (3) Place the PFA jar in a boiling water bath at 100°C and heat it for 60 minutes, then stop heating to obtain a boric acid sample solution;

[0043] (4) After the boric acid sample solution is cooled, use secondary deionized water to make up the volume in a 5mL volumetric flask;

[0044] (5) ICP-OES was used to analyze the content of lithium, sodium, potassium, magnesium and calcium in the boric acid sample solution after constant volume.

[0045] Among them, the test conditions of ICP-OES are as follows:

[0046] Power 1100W; Plasma gas 13L / min; Auxiliary gas 0L / min; Sheath gas 0.3L / min; Atomizing gas 0.8L / min; The most sensitive line was used; the light chamber was ...

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Abstract

The invention provides a method for measuring the trace amount of inorganic impurities in boric acid. The method comprises the following steps: (1) weighing a certain amount of a boric acid sample, and placing the weighed sample on a PFA wide-mouth bottle; (2) directly adding an optically-pure methanol reagent into the PFA wide-mouth bottle, and evenly stirring; (3) placing the PFA wide-mouth bottle in a water bath with a constant temperature of 78 to 120 DEG C, and heating the PFA wide-mouth bottle for 45 to 80 minutes until the boric acid sample is completely dissolved to obtain a boric acid sample solution, wherein during the heating process, the opening of the wide-mouth bottle is opened; (4) cooling the boric acid sample solution, transferring the boric acid sample solution to a volumetric flask, and filling water to a meter volume; (5) using inductively coupled plasma-optical emission spectrometer (ICP-OES) to analyze the content of inorganic impurity elements in the boric acid sample solution after the step (4). The provided method can rapidly and efficiently detect the trace amount of inorganic impurities in boric acid and is especially suitable for analyzing a large amount of boric acid samples.

Description

technical field [0001] The invention relates to the field of analytical chemistry methods, in particular to a method for determining trace inorganic impurities in boric acid. Background technique [0002] High-purity boric acid is often used as a high-purity reagent and a raw material for producing various high-purity borate crystals. However, the production process of high-purity boric acid determines that boric acid products may contain some inorganic impurity elements, such as lithium, sodium, magnesium, calcium, sulfur, phosphorus, silicon, iron, etc. In the nuclear industry, high-purity boric acid can be used as neutron moderator, collector and coolant, so there are strict requirements on its purity. However, boric acid has a high matrix concentration, and its solubility at room temperature is only 5.74g / 100mL. , because the boric acid matrix is ​​easy to crystallize and precipitate, it is easy to block the nebulizer, and the excessively diluted boric acid solution wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/28
Inventor 谢增春万小红朱刘
Owner 昆明先导新材料科技有限责任公司
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