Complexometric reagent as well as preparation method and application thereof

A reagent and complexation technology, applied in the field of analytical chemistry, can solve problems such as difficult emulsification and lack of complexation reagents, and achieve high recovery and good selectivity

Inactive Publication Date: 2011-09-21
YUXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, solid phase extraction has the advantages of high enrichment multiple, less environmental pollution, not easy to emulsify, and saves time. However, there is still a lack of stable and easy-to-operate complexing reagents.

Method used

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  • Complexometric reagent as well as preparation method and application thereof
  • Complexometric reagent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] - Determination of palladium in environmental water samples

[0032] Take an appropriate amount of clean water sample (less than 230 mL) in a 250 mL volumetric flask, add 4 mL of cetyltrimethylammonium bromide solution, 10 mL of hydrochloric acid, 5 mL of 2-(2-quinoline azo )-4,5-dimethylaniline ethanol solution, diluted with water to the mark, shaken well, and left for 10 min, the solution passed through the activated solid phase extraction cartridge at a flow rate of 20 mL / min, and after passing Use 1.0 mL ethanol (containing 1% acetic acid) at a flow rate of 5 mL / min to elute the complexes enriched on the small column, and the palladium in the eluent is determined according to the selected atomic absorption conditions. The measurement results were compared with inductively coupled plasma mass spectrometry (ICP-MS).

[0033] Samples with high organic content are digested and then measured; take an appropriate amount of palladium-containing waste liquid in a 100 mL ca...

Embodiment 2

[0035] - Determination of palladium in slag

[0036]Weigh 0.2 g of cyanide slag sample into a polytetrafluoroethylene microwave digestion bottle, add 1.0 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; Heat and evaporate to near dryness, dissolve the residue with 20 mL of 5% hydrochloric acid, add 4 mL of cetyltrimethylammonium bromide solution, 5 mL of 2-(2-quinolineazo)-4 , 5-Dimethylaniline ethanol solution, shake well, let it stand for 10 min; the solution passes through the activated solid phase extraction column at a flow rate of 20 mL / min, and after passing through the column, use 1.0 at a flow rate of 5 mL / min mL of ethanol (containing 1% acetic acid) was used to elute the enriched complex on the small column, and the palladium in the eluate was determined according to the selected atomic absorption conditions. The measurement results were compared with inductively...

Embodiment 3

[0038] - Determination of Palladium in Carbon Palladium Catalyst

[0039] Weigh 0.200 g of carbon-palladium catalyst into a porcelain crucible, place it in a muffle furnace at 750°C and burn for 25 min, transfer it to a small beaker after cooling, add 3 ml of concentrated sulfuric acid and 3 ml of perchloric acid, heat until smoking, Then add 5 ml of aqua regia to dissolve the residue and evaporate to near dryness, add 4 ml of concentrated hydrochloric acid and evaporate to near dryness, repeat three times, dissolve the residue with 20 mL of 5% HCl, add 4 mL of cetyltrimethyl bromide to the solution Ammonium ammonium solution, 5 mL of 2-(2-quinolineazo)-4,5-dimethylaniline ethanol solution, shake well, let stand for 10 min, and pass the solution through the activated After passing through the solid phase extraction column, use 1.0 mL ethanol (containing 1% acetic acid) to elute the enriched complex on the column at a flow rate of 5 mL / min. The palladium in the eluent is select...

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Abstract

The invention discloses a complexometric reagent as well as a preparation method and application thereof. The reagent has a chemical structure shown as in a novel general formula (I). The method comprises the following steps of: dissolving 2-aminoquinoline into absolute ethyl alcohol; adding sodium amide, heating in a water bath and reflowing; adding isoamyl nitrite, then reflowing and cooling to obtain diazo salt; adding 3,4-dimethylaniline in a diazo salt solution, stirring under the condition of introducing carbon diode, standing overnight, decompressing to evaporate most of ethanol and filtering precipitate to obtain a crude product; and recrystallizing with ethanol for 2-3 times to obtain the required complexometric reagent. The complexometric reagent can generate a stable complex compound with palladium. Therefore, the invention provides a novel method for detecting the palladium, wherein the detection limit can reach ng/L level. The detection result is contrasted by adopting an inductance coupling plasma mass spectroscopy (ICP-MS) method and is proved to be consistent.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, more specifically, the invention relates to a complexing reagent for palladium separation and enrichment. At the same time, the present invention also relates to the preparation method and application of the complexing reagent. technical background [0002] Palladium reserves are small and scattered in nature, and generally must be enriched in advance, and then determined by various analytical methods. In the prior art, enrichment methods include fire assay gold method, co-precipitation method, electrodeposition method, ion exchange method, solvent extraction method, solid phase extraction method and the like. Among them, solid-phase extraction has the advantages of high enrichment multiple, less environmental pollution, less emulsification, and time saving, but there is still a lack of complexation reagents that are stable and easy to operate. Contents of the invention [0003] The purpos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/38G01N30/08
Inventor 羊波李银科胡秋芬杨光宇
Owner YUXI NORMAL UNIV
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