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

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  • Solid oxidant and preparation method and application thereof
  • Solid oxidant and preparation method and application thereof
  • Solid oxidant and preparation method and application thereof

Examples

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Example Embodiment

[0035] The second aspect of the present invention provides a preparation method of the above solid oxidant, the preparation method comprising:

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

[0037] (2) Mix the adsorbent dispersion with the solution of the soluble salt of the subgroup elements of the fourth period, and disperse uniformly 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) Evaporate the mixed suspension system to dryness, collect the remaining solid, and calcinate the solid to obtain a treated solid;

[0040] (5) Co-grind the treated solid, the positive tetravalent oxide of Group IV metal and the carbon-free grinding aid to obtain the solid oxidant.

[0041] In the process of converting the soluble salt of the subgroup element in the fourth period into the hydroxide of the subgroup element in the fourth period, the presence of the adsorbent can i...

Example Embodiment

[0056] Example 1

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

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

[0059] 3) Under vigorous stirring, add dropwise the 0.05M NaOH solution prepared in advance with analytical pure NaOH and deionized water to the mixed system obtained in step 2), while monitoring the pH of the system until the pH of the system is adjusted to 9-10, get 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 4h; after cooling, use it The solid product was washed with ionized water and dried at 80°C fo...

Example Embodiment

[0062] Example 2

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

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

[0065] 3) Under vigorous stirring, add dropwise the 0.05M NaOH solution prepared in advance with analytical pure NaOH and deionized water to the mixed system obtained in step 2), while monitoring the pH of the system until the pH 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 4h; after cooling, use it The solid product was washed with...

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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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