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Catalytic digestion, enrichment and separation column and catalytic digestion, enrichment and separation cup and preparation method thereof

A separation column and separation cup technology, applied in the field of analytical chemistry, can solve the problems of environmental pollution, high cost of solid phase extraction agents, and easy loss

Active Publication Date: 2019-09-27
SHENYANG LIGONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among these separation and enrichment methods, the co-precipitation method is easy to cause losses and the recovery rate is low; liquid-liquid extraction generally uses a large amount of organic solvents, which endangers the health of the operator and pollutes the environment; the cost of solid-phase extraction agents is high; First digestion and then separation and enrichment, step by step, the sample solution needs to be transferred multiple times, the operation is cumbersome, and it is easy to cause losses

Method used

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  • Catalytic digestion, enrichment and separation column and catalytic digestion, enrichment and separation cup and preparation method thereof
  • Catalytic digestion, enrichment and separation column and catalytic digestion, enrichment and separation cup and preparation method thereof
  • Catalytic digestion, enrichment and separation column and catalytic digestion, enrichment and separation cup and preparation method thereof

Examples

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Embodiment 1

[0067] A method for preparing a catalytic digestion enrichment separation column, the process flow chart is shown in figure 1 , including the following steps:

[0068] 1. Take 1000g of 325 mesh diatomite, immerse it in 0.5mol / L nitric acid solution containing 10% hydrogen peroxide, heat and boil for 20min, separate solid and liquid, wash diatomite to near neutrality, and obtain impurity-removing and pore-expanding diatomaceous earth;

[0069] Soak the diatomite after impurity removal and pore expansion in the aqueous solution of chelating dispersant containing 80g / L urea, 15g / L acetic acid and 40g / L citric acid, ultrasonically vibrate for 25min, and place in a In a closed container, vacuumize the container to a vacuum degree of -0.09MPa, keep it for 120min, open the vent valve to restore the pressure in the container to normal pressure, let it stand for 24h, filter, and dry the filtered solid matter at 60°C. Obtain the modified diatomite for subsequent use;

[0070] 2. Take...

Embodiment 2

[0085] A method for preparing a catalytic digestion enrichment separation column, comprising the following steps:

[0086] 1. Take 1000g of 325 mesh diatomite, immerse it in 0.5mol / L nitric acid solution containing 10% hydrogen peroxide, heat and keep boiling slightly for 20min, separate the solid and liquid, wash the diatomite with water until it is nearly neutral, and get the impurity removal Diatomaceous earth behind the hole;

[0087] Soak the diatomite after impurity removal and pore expansion in the aqueous solution of chelating dispersant containing 80g / L urea, 15g / L acetic acid and 40g / L citric acid, ultrasonically vibrate for 25min, and place in a In a closed container, vacuumize the container to a vacuum degree of -0.1MPa, keep it for 120min, open the vent valve to restore the pressure in the container to normal pressure, let it stand for 24h, filter, and dry the filtered solid matter at 80°C. Obtain the modified diatomite for subsequent use;

[0088] 2. Take 250g ...

Embodiment 3

[0103] A method for preparing a catalytic digestion enrichment separation column, comprising the following steps:

[0104] 1. Take 1000g of 325 mesh diatomite, immerse it in 0.5mol / L nitric acid solution containing 10% hydrogen peroxide, heat and boil for 20min, separate solid and liquid, wash diatomite to near neutrality, and obtain impurity-removing and pore-expanding diatomaceous earth;

[0105] Soak the diatomite after impurity removal and pore expansion in the aqueous solution of chelating dispersant containing 80g / L urea, 15g / L acetic acid and 40g / L citric acid, ultrasonically vibrate for 25min, and place in a In a closed container, vacuumize the container, the vacuum degree is -0.09MPa, keep it for 120min, open the vent valve, let the pressure in the container return to normal pressure, let it stand for 24h, filter, and dry the filtered solid matter at 70°C, Obtain the modified diatomite for subsequent use;

[0106] 2. Take 250g of 325 mesh alumina, soak and activate ...

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Abstract

The invention provides a catalytic digestion, enrichment and separation column and a catalytic digestion, enrichment and separation cup and a preparation method thereof, and belongs to the field of analytical chemistry. The catalytic digestion, enrichment and separation cup is an integrated device for sample pretreatment and separation and enrichment of trace components through conventional wet digestion. The preparation method of the catalytic digestion, enrichment and separation cup comprises the steps that calcium nitrate and tetrabutyl titanate are directly impregnated on diatomite separately by adopting a pre-impregnation method, then an iron-chromium-aluminum alloy wire is used as a support and an internal hot wire, a silk is taken as a temperate and a doping source, the catalytic digestion, enrichment and separation column, loaded with nano calcium titanate and nano strontium titanate, with a special hole structure is prepared and placed in a special high beaker, and the catalytic digestion, enrichment and separation cup is prepared. The catalytic digestion, enrichment and separation cup has the advantages that the cost is low, the catalytic digestion efficiency is high, the digestion, enrichment and separation are carried out synchronously, explosive boiling prevention and splashing loss prevention are achieved, the recovery rate is high, the operation is simple, the acid dosage is less, the performance is stable, and economic, environmental and social benefits are very high.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and specifically relates to a catalytic digestion and enrichment separation column, a catalytic digestion and enrichment separation cup and a preparation method thereof. Background technique [0002] In the field of analytical chemistry and environmental monitoring, when performing the determination of trace metal elements in samples (water samples, soil samples, solid waste, food and biology, etc.), pretreatment steps such as digestion, separation and enrichment are essential It is also the key to determine the speed and accuracy of sample analysis. [0003] The role of digestion treatment is to destroy organic matter and transform the analyte elements in various valence states into forms that are convenient for determination. Digestion methods include dry ashing and wet digestion, and wet digestion is currently the most commonly used sample pretreatment method in routine analysis. The so-c...

Claims

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Application Information

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IPC IPC(8): B01D15/20C02F1/28G01N1/40G01N1/44
CPCB01D15/20C02F1/281G01N1/4022G01N1/44
Inventor 张东张艳丽林远芳刘胜博王赫轮刘念
Owner SHENYANG LIGONG UNIV