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Platinum characteristic complexing agent, preparation method and application for extracting, and enriching and testing platinum

An extraction, enrichment and complexing agent technology, applied in the field of analytical chemistry, can solve the problems of insufficient sensitivity to meet the requirements of platinum determination, poor platinum selectivity, etc., and achieve the effect of safe separation of metal ions, low detection limit and low pollution

Inactive Publication Date: 2014-02-26
YUNNAN MINZU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many reports on the photometric determination of platinum with heterocyclic azo reagents, but the selectivity of heterocyclic azo reagents to platinum is poor, and for some samples with low platinum content, the sensitivity of ordinary photometric methods cannot meet the requirements of platinum determination.

Method used

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  • Platinum characteristic complexing agent, preparation method and application for extracting, and enriching and testing platinum
  • Platinum characteristic complexing agent, preparation method and application for extracting, and enriching and testing platinum

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preparation example Construction

[0024] The preparation method of the platinum characteristic complexing agent of the present invention comprises the operations such as diazonium salt synthesis, diazonium salt coupling, product purification, specifically has the following steps:

[0025] For the synthesis of the diazonium salt, mix and stir 0.01 mol of 4-amino-4′hydroxyazobenzene and 4~6 mL of concentrated hydrochloric acid, cool to 0~10°C, add dropwise 0.01 mol of NaNO 2 Aqueous solution, keep the temperature constant and stir well until the diazotization reaction is complete;

[0026] For the coupling of the diazonium salt, add 0.01 mole of 8-aminoquinaldine to the diazonium salt synthesized in step A, keep the temperature constant, adjust the pH value of the reaction system to 4~5, react for 1.5 h, and then adjust The pH value of the reaction system is 7 ~ 8, until the coupling reaction is complete;

[0027] For the purification of the product, the product in step B is suction filtered, washed with water ...

Embodiment 1

[0041] 8-quinaldine azo-p-hydroxy-diazoaminoazobenzene complexing agent Synthesis and identification of

[0042] Diazotization: Add 6.0 mL of concentrated hydrochloric acid to 0.01 mL of 4-amino-4′hydroxyazobenzene, stir to form a paste, cool to 0 ~ 5°C; dropwise add 0.01 mol of NaNO 2 Aqueous solution, stirred for 1 h, and the diazotization was completely checked with starch-potassium iodide test paper.

[0043] Coupling: Weigh 0.01 mol of 8-aminoquinaldine, slowly add it to the above diazonium salt, adjust the pH to 4 ~ 5 with saturated sodium acetate, stir for 1.5 h, then adjust the pH to 7 ~ 8, let stand overnight, Suction filtration, wash twice with water and 50% ethanol respectively, and dry at low temperature to obtain the crude product, which can be recrystallized 2 to 3 times with ethanol to obtain the pure product with a yield of 36%.

[0044] Compound melting point: 232-235 °C. Infrared spectrum (KBr pellet): at 3560 cm -1 There is an -OH absorption peak at ; 3...

Embodiment 2

[0046] - Determination of platinum in environmental water samples

[0047] Weigh 0.1-0.2 g of cyanide slag sample into a polytetrafluoroethylene microwave digestion bottle, add 1 mL of concentrated nitric acid and 3 mL of concentrated hydrochloric acid, and digest in a microwave digestion furnace with a power of 800 W for 10 min; The plate was heated and evaporated to nearly dryness, dissolved the residue with 10 mL of 1% hydrochloric acid, transferred to a 50 mL colorimetric tube, and transferred to a 100 mL colorimetric tube; then added 0.1% 8-quinaldine azo-p Hydroxyl-diazoaminoazophenylethanol solution 4 mL, adjust the pH value to neutral with 10% sodium hydroxide, then add 5 ml acetic acid-sodium acetate buffer solution with pH=4.0, shake well, let stand for 10 min, The chromogenic solution passed through the pre-activated MCI-GEL CHP20 solid-phase extraction column at a flow rate of 10 mL / min. After enrichment, the column was centrifuged and dehydrated, and eluted with 1...

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Abstract

The invention discloses a platinum characteristic complexing agent, a preparation method and the application for extracting, and enriching and testing platinum. The platinum characteristic complexing agent is 8-quinaldine azo-hydroxy-diazo aminoazobenze. The preparation method comprises the following steps of: synthesizing diazonium salt, coupling the diazonium salt, and purifying a product. The platinum characteristic complexing agent and trace platinum in a sample have a high-selectivity coloring and complexing reaction, so that a stable red complex can be generated; and the interfering ion can be separated after the extraction and enrichment of solid phase, so that the platinum content can be accurately and quantitatively tested. The platinum characteristic complexing agent can be used for enriching, separating and testing of trace platinum in the environment water sample, the cyaniding tailings and the ore sample, the absorption contrast ratio is high (system delta lambda=140nm), the quick coloring can be realized within 5min under room temperature, and the coloring complexing product is high in stability, and can be stabilized for 8-10h; the enriching sensitivity is high; and the analysis interference resistance is high. The defect that the separation method such as the liquid-liquid extraction, the ion exchange and the like in the prior art needs a mass of high-purity organic solvent can be overcome, and the platinum characteristic complexing agent has the advantages of being high in enrichment multiple, free from emulsification, safe to separate, and small in pollution.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and more specifically, the invention relates to a platinum characteristic complexing agent and a preparation method thereof, as well as an application in solid-phase extraction enrichment and determination of platinum. Background technique [0002] Due to its excellent performance, platinum has become an indispensable and precious raw material in high-tech fields such as going to the sky, going to the ground, and going to the sea. Because of its high price, it is generally only used to manufacture the most critical and core components, so it has the reputation of "industrial vitamin". At the same time, platinum is an environmentally harmful element. Excessive intake of platinum by the human body will affect the effectiveness of other beneficial elements in the body, such as liver and kidney damage, emphysema, bronchitis, endocrine disorders, loss of appetite, insomnia and other problems. There...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D215/40G01N21/31G01N1/40
Inventor 叶艳青胡秋芬张英杰郭俊明杨海英
Owner YUNNAN MINZU UNIV
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