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Solid oxidant and preparation method and application thereof

An oxidant and solid technology, applied in the field of solid oxidant and its preparation, achieves the effects of simple equipment, convenient use, and stable chemical properties

Active Publication Date: 2019-04-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the problems currently used in accelerator mass spectrometers 14 The defects of the oxidizing agent in the pre-treatment of sample graphitization in the C measurement provide a high conversion rate of carbon element into carbon dioxide, and will not produce steam that pollutes the sample, and it does not need to increase the gas path of the sample processing device, and the oxidizing agent is easy to operate and Its preparation method; it provides a more efficient and reliable option for the graphitization pretreatment of samples in AMS

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preparation example Construction

[0035] The second aspect of the present invention provides the preparation method of above-mentioned solid oxidizing agent, and this preparation method comprises:

[0036] (1) dispersing the adsorbent in water to obtain an adsorbent dispersion;

[0037] (2) Mix the adsorbent dispersion with the solution of the soluble salt of the fourth period subgroup element, and disperse evenly to obtain a mixed system;

[0038] (3) adjusting the pH value of the mixed system to be alkaline to obtain a mixed suspension system;

[0039] (4) Evaporating the mixed suspension system to dryness, collecting the remaining solid, and calcining the solid to obtain the treated solid;

[0040] (5) co-grinding the treated solid, the tetravalent oxide of the main group IV metal and a carbon-free grinding aid to obtain the solid oxidant.

[0041] In the process of transforming the soluble salts of the fourth-period subgroup elements into hydroxides of the fourth-period subgroup elements by the action of...

Embodiment 1

[0057] 1) Weigh 10 g of diatomaceous earth and add it into a sufficient amount of deionized water, and ultrasonically treat it to form a dispersion system;

[0058] 2) Weigh 15.7g CuSO 4 ·5H 2 O (analytically pure), add an appropriate amount of deionized water to dissolve, fully mix with the diatomite dispersion system obtained in step 1), keep stirring, and obtain a mixed system;

[0059] 3) Under vigorous stirring, add dropwise the 0.05M NaOH solution prepared in advance with analytically pure NaOH and deionized water to the mixed system obtained in step 2), and monitor the pH value of the system at the same time until the pH value of the system is adjusted to 9-10, to obtain a mixed suspension system;

[0060] 4) Slowly evaporate the mixed suspension system obtained in step 3), collect the remaining solid mixture after evaporation, transfer the solid to a porcelain crucible, and place it in an air atmosphere at 500°C for 4 hours; after cooling, use The solid product was ...

Embodiment 2

[0063] 1) Weigh 10g of active γ-alumina and add it into a sufficient amount of deionized water, and ultrasonically treat it to form a dispersion system;

[0064] 2) Weigh 26g Fe 2 (SO 4 ) 3 ·xH 2 O (analytically pure, Fe content is 21-23wt%), add an appropriate amount of deionized water to dissolve, fully mix with the active γ-alumina dispersion system obtained in step 1), and keep stirring to obtain a mixed system;

[0065] 3) Under vigorous stirring, add dropwise the 0.05M NaOH solution prepared in advance with analytically pure NaOH and deionized water to the mixed system obtained in step 2), and monitor the pH value of the system at the same time until the pH value of the system is adjusted to 8. Obtain a mixed suspension system;

[0066] 4) Slowly evaporate the mixed suspension system obtained in step 3), collect the remaining solid mixture after evaporation, transfer the solid to a porcelain crucible, and place it in an air atmosphere at 500°C for 4 hours; after cool...

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Abstract

The invention, which belongs to the field of <14>C detection, discloses a solid oxidant and a preparation method and application thereof. On the basis of the total weight of the solid oxidant, the solid oxidant comprises the following components: 20 to 40wt% of IV-main-group metal positive tetra-valent oxide, 20 to 60wt% of fourth-cycle sub-group element oxide, 20 to 40wt% of adsorbents, and 1 to10wt% of carbon-free grinding auxiliary agents, wherein the sum of weights of all components does not exceed 100wt%. The disclosed oxidant has advantages of improved oxidation effect, no pollution onthe follow-up prepared sample, and simple usage by being compared with the traditional oxidant and thus is worthy of promotion.

Description

technical field [0001] The present invention relates to 14 The field of C detection, more specifically, relates to a solid oxidant and a preparation method thereof, and the solid oxidant in an accelerator mass spectrometer 14 Application of sample graphitization pretreatment in C measurement. Background technique [0002] 14 C is an important radioactive isotope of carbon, which widely exists in various organisms, environmental samples, polymers and other organic products. right 14 The measurement of C is of great significance in archaeology, geology, meteorology, medicine, biology, materials, energy and other fields. Existing available for determination 14 The methods for C content include proportional scintillation method (PSM), beta ionization (BI) or accelerated mass spectrometry (AMS) method. Among them, the proportional scintillation method needs to convert the C in the sample into benzene series for detection, which requires a large amount of sample, and the con...

Claims

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Application Information

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IPC IPC(8): G01N1/28
CPCG01N1/28
Inventor 高昂范彦如高静
Owner CHINA PETROLEUM & CHEM CORP
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