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Method for determining content of boron in boronation ash-free sample

An element content and boronization technology, applied in material excitation analysis, thermal excitation analysis, etc., can solve the problems of complex steps, interference in measurement, inappropriate operation, etc., to avoid pollution, avoid boron loss, and accurately determine the content.

Inactive Publication Date: 2015-03-25
重庆市盛馨种业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Previously, the SH / T0227-92 method was used to determine boron, the steps were complicated and unsuitable for operation, and the presence of zinc, phosphorus, aluminum and other elements interfered with the determination of boron

Method used

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  • Method for determining content of boron in boronation ash-free sample

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Experimental program
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Effect test

Embodiment 1

[0027] The conditions of the plasma atomic emission spectrometer, pressure melting bomb, and electric heating constant temperature drying oven are set, and the parameters of the RF generator of the plasma atomic emission spectrometer are: incident power 1000Kw; carrier gas flow rate: 0.651 / min; sampling rate: 1ml / min; Observation height: 15mm at the induction coil; Spectral bandwidth 0.044nm; Dilute 100ug / g boron standard solution step by step to 10.0, 0.20, 0.50, ug / gB; gB standard dilution solution, measured on the machine with the reagent blank as a reference, and draw the standard curve; accurately weigh the ash-free boronized sample in the cup of the pressure melting bomb; drip water into the cup of the pressure melting bomb to wet the sample and add Concentrated nitric acid 1ml, 30% hydrogen peroxide 1ml, then put the melting cup into the pressure melting bomb liner and tighten the cover; put it in an oven and keep the temperature at 100°C for 4 hours, take it out after t...

Embodiment 2

[0029] The conditions of the plasma atomic emission spectrometer, pressure melting bomb, and electric heating constant temperature drying oven are set, and the parameters of the RF generator of the plasma atomic emission spectrometer are: incident power 1000Kw; carrier gas flow rate: 0.651 / min; sampling rate: 1ml / min; Observation height: 15mm at the induction coil; Spectral bandwidth 0.044nm; Dilute 100ug / g boron standard solution step by step to 10.0, 0.20, 0.50, ug / gB; gB standard dilution solution, measured on the machine with the reagent blank as a reference, and draw the standard curve; accurately weigh the ash-free boronized sample in the cup of the pressure melting bomb; drip water into the cup of the pressure melting bomb to wet the sample and add Concentrated nitric acid 2ml, 30% hydrogen peroxide 1.5ml, then put the melting cup into the pressure melting bomb liner and tighten the cover; put it in an oven and keep the temperature at 120°C for 4 hours, take it out after...

Embodiment 3

[0031] The conditions of the plasma atomic emission spectrometer, pressure melting bomb, and electric heating constant temperature drying oven are set, and the parameters of the RF generator of the plasma atomic emission spectrometer are: incident power 1000Kw; carrier gas flow rate: 0.651 / min; sampling rate: 1ml / min; Observation height: 15mm at the induction coil; Spectral bandwidth 0.044nm; Dilute 100ug / g boron standard solution step by step to 10.0, 0.20, 0.50, ug / gB; gB standard dilution solution, measured on the machine with the reagent blank as a reference, and draw the standard curve; accurately weigh the ash-free boronized sample in the cup of the pressure melting bomb; drip water into the cup of the pressure melting bomb to wet the sample and add Concentrated nitric acid 3ml, 30% hydrogen peroxide 2ml, then put the melting cup into the pressure melting bomb liner and tighten the cover; put it in an oven and keep the temperature at 150°C for 4 hours, take it out after t...

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Abstract

The invention relates to a method for determining the content of boron in a boronation ash-free sample. The method comprises the following steps: setting and preparing a working condition of instruments; gradually diluting boron standard solution of a given volume into a plurality of parts; respectively and precisely absorbing a plurality of standard diluted solutions, carrying out the computer determination by adopting reagent blank as reference, and drawing a standard curve; accurately measuring the boronation ash-free sample, and adding the boronation ash-free sample into a pressure melting shell cup; dropwise adding a water moisturizing sample into the pressure melting shell cup, adding concentrated nitric acid and hydrogen perioxide, and then placing the melting shell cup into a pressure melting shell liner, and tightening a cover; placing the pressure melting shell liner with the melting cup in a drying oven, carrying out the heat treatment on the sample, taking out the pressure melting shell after the pressure melting shell is cooled, adding the sample solution in a volume bottle of an appropriate volume by making volume constant, and carrying out the computer determination. According to the method, the sample is processed by adopting the pressure melting shell, and the sample is dissolved in a closed manner, so that not only can the environmental pollution be avoided, but also the loss of the volatile boron can be avoided, and accuracy in content determination can be realized.

Description

technical field [0001] The invention relates to a method for determining the content of elements, in particular to a method for determining the content of boron in boronized ashless. Background technique [0002] In recent years, boron-containing lubricating oils and additives have been applied to various fields. The addition of boron to the additive not only plays an anti-wear role, but also improves the sealing properties of rubber products; adding boron to the fluorine-containing lubricating oil can prevent the expansion of the fluorine oil. Previously, the SH / T0227-92 method was used for the determination of boron. The steps were complicated and unsuitable for operation, and the presence of zinc, phosphorus, aluminum and other elements interfered with the determination of boron. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a method for determining the content of the sample by pressure bomb solution, which...

Claims

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Application Information

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IPC IPC(8): G01N21/71
Inventor 张洪卫
Owner 重庆市盛馨种业有限公司