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Analysis method for determining content of palladium in waste residues

An analysis method and waste residue technology, which is applied in the analysis field of determining palladium content in waste residue, can solve the problems of high cost of detection equipment, poor adaptability of palladium, failure to meet the detection requirements of palladium content, etc.

Pending Publication Date: 2021-04-30
CHONGQING THRIVE CHEM
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Problems solved by technology

[0002] As a precious metal, palladium is widely used in chemistry, chemical industry, and food related fields, and has good recovery value, but the existing detection methods are not suitable for recovering low-content palladium below 3% or the detection cost is high
[0003] Commonly used palladium content detection mainly uses ferrous sulfate potentiometric titration method, potassium permanganate amperometric titration method, dimethylglyoxalxime gravimetric method and other electrochemical detection methods, and its main application range is 3%-99% palladium content detection , unable to meet the detection requirements of waste slag or some low-level palladium content
Others such as graphite furnace atomic absorption spectrophotometry, inductively coupled plasma emission spectrometry, etc. are suitable for the detection of trace palladium content, but the cost of detection equipment is relatively high

Method used

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  • Analysis method for determining content of palladium in waste residues

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Embodiment Construction

[0011] The present invention will be further described in detail below in conjunction with specific embodiments.

[0012] An analytical method for measuring palladium content in waste residue, the specific steps include:

[0013] 1. Sample pretreatment

[0014] 1. Weigh 20g of the waste residue sample with an accuracy of 0.0001g, place it in a ceramic crucible, and calcinate it in a muffle furnace at 850°C for 5h.

[0015] 2. Take out the ceramic crucible and cool it down to room temperature, add 5ml of a mixed solution of hydrochloric acid and nitric acid with a volume ratio of 3:1, heat at low temperature to slightly boil, add 0.1g of sodium chloride, 20ml of 10% hydrochloric acid, fully dissolve and transfer to a 100ml volumetric flask , diluted to the mark with distilled water.

[0016] 2. Make a standard regression curve

[0017] 3. Accurately weigh 0.1666g of palladium chloride, add 20ml of 10% hydrochloric acid solution to fully dissolve, transfer to a 100ml volumetr...

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Abstract

The present invention discloses an analysis method for determining content of palladium in waste residues. The analysis method comprises the following steps: calcining a waste residue sample at high temperature, cooling to room temperature, adding a mixed solution of hydrochloric acid and nitric acid, heating at low temperature until the mixed solution is slightly boiled, sequentially adding sodium chloride and 10% hydrochloric acid, completely dissolving, transferring into a 100ml volumetric flask, and diluting with distilled water to a scale to obtain a pretreated sample solution; adding 1ml of the pretreated sample solution into a 60ml separating funnel, adding 20ml of water, adjusting the pH value to be 2 by using a 5% hydrochloric acid solution and a 5% sodium hydroxide solution, adding 2ml of a 1% chlorpromazine hydrochloride solution, uniformly shaking and standing for 10min to generate a red complex, adding 10ml of trichloromethane, carrying out oscillation extraction for 1min, taking a lower trichloromethane solution after layering, and taking reagent blank as a reference; and measuring the absorbance of the solution at 488 nm by using a 1 cm cuvette, and calculating the palladium content according to the absorbance and the standard regression curve. The method is low in detection cost and can be suitable for detecting the content of 0.1%-5% palladium.

Description

technical field [0001] The invention relates to an analysis method for measuring palladium content in waste residue. Background technique [0002] As a precious metal, palladium is widely used in chemistry, chemical industry, and food-related fields, and has good recovery value. However, the existing detection methods are not suitable for recovering low-content palladium below 3% or the detection cost is high. [0003] Commonly used palladium content detection methods are mainly electrochemical detection methods such as ferrous sulfate potentiometric titration method, potassium permanganate amperometric titration method, dimethylglyoxaloxime gravimetric method, etc., and its main application range is 3%-99% palladium content detection , unable to meet the detection requirements of waste slag or some low-level palladium content. Others, such as graphite furnace atomic absorption spectrophotometry and inductively coupled plasma emission spectrometry, are suitable for the dete...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N1/38
CPCG01N21/3103G01N1/38
Inventor 张伟张玉梅汪洋罗洋甘建强朱治瑾唐凌
Owner CHONGQING THRIVE CHEM
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