Analytical reagent for measuring heavy metal and method for preparing same

A technology for analyzing reagents and diazonium salts, which is applied in the field of environmental analytical chemistry, can solve the problems that the sensitivity of ordinary liquid chromatography cannot meet the requirements of determination, the complexes formed are not stable enough, and the practical application is not widely used, and the determination results are reliable. , the effect of improving the sensitivity and improving the detection sensitivity

Inactive Publication Date: 2013-01-09
汉龙莱科环境工程有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some of these reagents form complexes that are not stable enough, some have low sensitivity, and are not widely used in practice; and for some environmental samples with low content of heavy metal elements, the sensitivity of ordinary liquid chromatography cannot meet the requirements of determination.

Method used

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  • Analytical reagent for measuring heavy metal and method for preparing same
  • Analytical reagent for measuring heavy metal and method for preparing same
  • Analytical reagent for measuring heavy metal and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] ——Synthesis and identification of analytical reagents

[0034] Mix and stir 0.01mol of 4-acetylaniline and 5mL of concentrated hydrochloric acid (it can be scaled up or down in proportion, and the addition of reagents should also scale up or down accordingly), cool to 0-10°C, and add 0.02mol of NaNO dropwise 2 Aqueous solution, keep the temperature constant and stir well until the diazotization reaction is complete. Add 0.01 moL of 8-aminoquinaldine to the synthesized diazonium salt, keep the temperature constant, adjust the pH value of the reaction system to 4-5, react for 1.5 hours, then adjust the pH value of the reaction system to 7-8, until The coupling reaction is complete; the reaction product is suction filtered and dried at low temperature to obtain the crude product, which can be recrystallized 2 to 3 times with ethanol to obtain the pure product.

[0035] The melting point of the compound is 186-189°C. Infrared spectrum (KBr pellet): 3385 and 3354cm -1 wit...

Embodiment 2

[0037] ——Determination of lead, cadmium and mercury in environmental water samples

[0038] For clean water samples, according to the actual content of several heavy metal elements, take an appropriate amount of water samples, acidify them with nitric acid and use them directly for determination; for waste water with high organic content, take an appropriate volume of water samples to concentrate to 10mL, and add 1mL of concentrated nitric acid and 3mL of hydrogen peroxide were digested in a microwave digestion furnace with a power of 800W for 10min; after digestion, heated and evaporated on a hot plate to nearly dryness, dissolved the residue with 10mL of 1% hydrochloric acid, and transferred it to a 50mL volumetric flask for For measurement.

[0039] Add 5mL of the ethanol solution of the reagent of the present invention with a concentration of 0.1% in the sample solution to be tested, adjust the pH value to near neutrality, then add 10mL of acetic acid-sodium acetate buffer...

Embodiment 3

[0041] - Determination of lead, cadmium and mercury in soil

[0042] Weigh 0.5-1.0g of soil sample into a polytetrafluoroethylene microwave digestion bottle, add 2mL perchloric acid and 5mL hydrofluoric acid, and digest in a microwave digestion furnace with a power of 800W for 15min; after digestion, heat and evaporate on an electric heating plate When it is nearly dry, dissolve the residue with 10mL of 1% hydrochloric acid and transfer it to a 50mL volumetric flask; it is used for determination.

[0043] Add 5mL of the ethanol solution of the reagent of the present invention with a concentration of 0.1% to the sample solution to be tested, adjust the pH value to near neutrality, then add 10mL of acetic acid-sodium acetate buffer solution with pH=4., dilute with water to near scale, and constant volume to 50mL. The solution passes through the activated reversed-phase solid-phase extraction column (the material is reversed-phase microporous resin) at a flow rate of 10ml / min. A...

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Abstract

The invention discloses an analytical reagent for measuring heavy metal. The analytical reagent has a chemical structure with a general formula (I) and can react with lead, cadmium and mercury to generate stable complexes, the complexes can be separated on a reversed phase liquid chromatographic column, the trace amount of lead, cadmium and mercury in an environmental sample can be accurately measured by a visible photometric detector, and the limit of detection of the method reaches ng/L level. The measuring results obtained by using the analytical reagent coincide with those obtained by adopting the inductively coupled plasma mass spectrum (ICP-MS), which shows that the measuring results are reliable.

Description

technical field [0001] The invention belongs to the field of environmental analysis chemistry, more specifically, the invention relates to a new analysis reagent. At the same time, the invention also relates to the preparation method of the reagent and its application in the determination of lead, cadmium and mercury in environmental water samples, soil and plant samples. Background technique [0002] Lead, cadmium, and mercury are heavy metal elements that are relatively harmful in the environment. Lead can damage the blood and decompose red blood cells. At the same time, it spreads to the organs and tissues of the whole body through the blood and enters the bones, causing radial nerve paralysis and finger tremors. Cadmium poisoning can cause muscle atrophy, joint deformation, unbearable bone pain, inability to sleep, and pathological fractures. Mercury can damage the nerve center and lead to nervous disorders, restlessness, and extreme pain. Therefore, the accurate deter...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/40G01N30/02
Inventor 彭廷纯吴献花白勇徐娟刘小宇
Owner 汉龙莱科环境工程有限公司
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