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Preparation of modified active carbon

A technology of activated carbon and modification, applied in the field of preparation of modified activated carbon, can solve the problems of large operator injury, low recovery rate, performance difference, etc., and achieve the effects of low cost, easy operation and strong pertinence

Inactive Publication Date: 2009-06-24
NATIONAL MARINE ENVIRONMENTAL MONITORING CENTRE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of activated carbon to separate organochlorine pesticides and polychlorinated biphenyls has achieved certain results. However, due to the different production processes of activated carbon, its performance is significantly different, the repeatability of the separation results is poor, and the eluent after separation also has certain effects. question
For example, a micro-activated carbon column chromatography separation method uses an acetone-ether mixture with a volume ratio of 70:30 as the eluent to elute organochlorine pesticides, and benzene as the eluent to elute polychlorinated biphenyls, wherein Ether as the eluent is harmful to the operator, and the eluent benzene has a high boiling point, and the loss of PCBs is relatively large during the heating and rotary evaporation concentration, and the recovery rate of the determination is on the low side

Method used

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  • Preparation of modified active carbon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1. Preparation of activated carbon glass chromatography column

[0036] Wood carbonization: Put the wood block in the muffle furnace and keep it at 150℃ for 12h; then heat it to 275℃ and keep it for 12h; then continue to raise the temperature to 400℃ and keep it for 24h; finally, heat it up to 500℃ and keep it 8h. Turn off the muffle furnace, and when the temperature drops to the greenhouse, take out the charcoal block.

[0037] Grinding and sieving: the carbonized charcoal block is crushed into pieces, crushed by a pulverizer, ground in a mortar, and passed through a sieve of 40 mesh to 100 mesh to obtain charcoal powder.

[0038] Acid-base soaking: Take 10g of the above wood charcoal powder and place it in a beaker. After soaking and stirring with 100mL of 2mol / L hydrochloric acid solution, ultrasonically shake for 30min, let it stand for 30min to make it penetrate completely, and then rinse with tap water and distilled water to Neutral; After pouring out the wate...

Embodiment 2

[0041] Example 2: Using activated carbon glass chromatography column to separate organochlorine pesticides and PCBs in marine biological samples

[0042] Weigh 20.0g of marine biological sample (wet sample) and 20g of anhydrous sodium sulfate (mixed), place them in a 100mL glass conical flask with stopper, and add 30mL of a 1:1 mixture of n-hexane and acetone. Place the extraction in an ultrasonic extraction instrument for 20 minutes, then transfer the entire amount of the extract to a rotary evaporator; then add 20 mL of a 1:1 hexane-acetone mixture into a stoppered glass conical flask, and ultrasonically extract for 10 minutes ; Combine the above two extracts in the same rotary evaporator, evaporate in a 45 ℃ water bath, concentrate until nearly dry, add 1 mL of n-hexane and mix well to obtain a marine biological sample containing PCBs and organochlorine pesticides. N-hexane extraction liquid.

[0043] Transfer the entire amount of the above-mentioned marine biological sample n-...

Embodiment 3

[0044] Example 3. Separation of organochlorine pesticides and PCBs in marine sediment samples using activated carbon glass chromatography columns

[0045] Weigh 10.0g of marine sediment sample (dry sample) and 10g of anhydrous sodium sulfate, mix them, place them in a 100mL glass conical flask with stopper, and add 30mL of a 1:1 mixture of n-hexane and acetone. Carry out ultrasonic extraction, and use activated carbon glass chromatography column to separate organochlorine pesticides and PCBs in the sample. The operation steps are the same as those in Example 2 (but in a constant volume of 2mL n-hexane solution, 1g of high-purity copper powder should be added , Ultrasonic oscillation for 5min, standing for 12h, after desulfurization, can be measured by capillary GC-ECD).

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Abstract

The invention discloses a method for preparing modified activated charcoal. The method comprises the following process steps that: a woody material is dried, thermally decomposed and carbonized at a high temperature; charcoal blocks after carbonization are crushed, ground and sieved so as to obtain charcoal powder; the charcoal powder which is ground and sieved is adequately soaked in a hydrochloric acid solution and a sodium hydroxide solution in turn; the charcoal powder which is soaked in the hydrochloric acid solution and the sodium hydroxide solution and dried is activated in a high-temperature furnace; and the activated charcoal powder after high-temperature activation and anhydrous sodium sulfate are put into a glass chromatography column containing acetone in turn so as to prepare an activated charcoal glass chromatography column. The method for preparing the modified activated charcoal has the advantages of low cost, easy operation and applicability to the separation of sixteen types of organic chloride pesticides and ten types of polychlorinated biphenyls in marine environmental samples (marine organisms, marine sediments and seawater).

Description

Technical field [0001] The invention relates to a preparation method of activated carbon, in particular to a preparation method of modified activated carbon used to separate organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in marine environmental samples. Background technique [0002] The organic pollutants in the ocean have a great impact on the ecological environment and human health. In particular, organochlorine pesticides and polychlorinated biphenyls, which are highly toxic and long-lasting, can cause serious harm to marine biological resources and may cause cancer when entering the human body. And life-threatening diseases such as blood counts. The monitoring of organochlorine pesticides and PCBs in the ocean has become an important aspect of marine environmental monitoring. [0003] The detection of the types and content of organochlorine pesticides and PCBs in marine environmental samples can provide important scientific data for the formulation of p...

Claims

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Application Information

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IPC IPC(8): C01B31/08
Inventor 徐恒振姚子伟翟立斐周传光
Owner NATIONAL MARINE ENVIRONMENTAL MONITORING CENTRE
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