CN112730289A - Analysis method for determining palladium content in waste residues - Google Patents
Analysis method for determining palladium content in waste residues Download PDFInfo
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- CN112730289A CN112730289A CN202110061457.3A CN202110061457A CN112730289A CN 112730289 A CN112730289 A CN 112730289A CN 202110061457 A CN202110061457 A CN 202110061457A CN 112730289 A CN112730289 A CN 112730289A
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 41
- 239000002699 waste material Substances 0.000 title claims abstract description 22
- 238000004458 analytical method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 56
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000012488 sample solution Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000523 sample Substances 0.000 claims abstract description 15
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002835 absorbance Methods 0.000 claims abstract description 14
- 229960001701 chloroform Drugs 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- AKUVRZKNLXYTJX-UHFFFAOYSA-N 3-benzylazetidine Chemical compound C=1C=CC=CC=1CC1CNC1 AKUVRZKNLXYTJX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229960001657 chlorpromazine hydrochloride Drugs 0.000 claims abstract description 8
- 238000007865 diluting Methods 0.000 claims abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 239000011780 sodium chloride Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000000605 extraction Methods 0.000 claims abstract description 4
- 230000010355 oscillation Effects 0.000 claims abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims abstract 3
- 239000000919 ceramic Substances 0.000 claims description 6
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000012086 standard solution Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 17
- 238000011084 recovery Methods 0.000 description 5
- 238000009835 boiling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000003928 amperometric titration Methods 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 description 1
- 238000000835 electrochemical detection Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses an analysis method for determining palladium content in waste residue, which comprises the steps of calcining a waste residue sample at a high temperature, cooling to room temperature, adding a mixed solution of hydrochloric acid and nitric acid, heating to slightly boil at a low temperature, sequentially adding sodium chloride and 10% hydrochloric acid, completely dissolving, transferring to a 100ml volumetric flask, and diluting with distilled water to a scale to obtain a pretreated sample solution; taking 1ml of the pretreated sample solution, putting the pretreated sample solution into a 60ml separating funnel, adding 20ml of water, adjusting the pH value to 2 by using a 5% hydrochloric acid solution and a 5% sodium hydroxide solution, adding 2ml of a 1% chlorpromazine hydrochloride solution, shaking uniformly, standing for 10min to generate a red complex, adding 10ml of trichloromethane, carrying out oscillation extraction for 1min, taking a lower layer of trichloromethane solution after layering, taking a reagent blank as a reference, measuring the absorbance of the solution at 488nm by using a 1cm cuvette, and calculating the palladium content according to the absorbance and a standard regression curve. The method has low detection cost and can be suitable for detecting the content of 0.1-5 percent palladium.
Description
Technical Field
The invention relates to an analysis method for determining palladium content in waste residue.
Background
Palladium is used as a precious metal, is widely used in the fields related to chemistry, chemical industry and food, and has good recovery value, but the existing detection method has poor adaptability to the recovery of low-content palladium with the recovery rate of less than 3 percent or has high detection cost.
The common palladium content detection mainly adopts electrochemical detection methods such as a ferrous sulfate potentiometric titration method, a potassium permanganate amperometric titration method, a dimethylglyoxime gravimetric method and the like, is mainly applied to the detection of the palladium content within the range of 3-99 percent, and cannot meet the detection requirements of waste residues or certain low-content palladium content. Other methods such as graphite furnace atomic absorption spectrophotometry and inductively coupled plasma emission spectrometry are suitable for detecting the content of trace palladium, but the detection equipment cost is high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an analysis method for determining the palladium content in waste residues, which has low detection cost, is suitable for detecting 0.1-5% of palladium content and has high accuracy.
In order to achieve the purpose, the technical scheme of the invention is as follows: an analysis method for determining palladium content in waste residue is characterized in that a waste residue sample is calcined at high temperature, cooled to room temperature, added with mixed solution of hydrochloric acid and nitric acid, heated to slight boiling at low temperature, sequentially added with sodium chloride and 10% hydrochloric acid, completely dissolved, transferred to a 100ml volumetric flask, and diluted to scale by distilled water to obtain a pretreated sample solution;
taking 1ml of the pretreated sample solution, putting the pretreated sample solution into a 60ml separating funnel, adding 20ml of water, adjusting the pH value to 2 by using a 5% hydrochloric acid solution and a 5% sodium hydroxide solution, adding 2ml of a 1% chlorpromazine hydrochloride solution, shaking uniformly, standing for 10min to generate a red complex, adding 10ml of trichloromethane, carrying out oscillation extraction for 1min, taking a lower layer of trichloromethane solution after layering, taking a reagent blank as a reference, measuring the absorbance of the solution at 488nm by using a 1cm cuvette, and calculating the palladium content according to the absorbance and a standard regression curve.
Further, the standard regression curve is drawn by weighing 0.1666g of palladium chloride, adding 20ml of 10% hydrochloric acid solution, transferring the solution to a 100ml volumetric flask after the solution is completely dissolved, and diluting the solution to a scale with distilled water; taking 1ml of the solution in a 250ml volumetric flask, adding 10% hydrochloric acid solution to dilute the solution to a scale, transferring 0, 1, 2, 3, 4 and 5ml of palladium standard solution into a 60ml separating funnel by a pipette, adding 20ml of water, adjusting the pH to 2 by using 5% hydrochloric acid solution and 5% sodium hydroxide solution respectively, adding 2ml of 1% chlorpromazine hydrochloride solution, shaking uniformly and standing for 10min to generate red complexes, adding 10ml of trichloromethane respectively, shaking and extracting for 1min, taking a lower layer of trichloromethane solution after layering, taking a reagent blank as a reference, measuring the absorbance of the solution at 488nm by using a 1cm cuvette, and drawing a standard regression curve according to the absorbance and the standard concentration of palladium.
Further, the specific operation method of the pretreatment sample solution is that 20g of the waste residue sample is weighed and placed in a ceramic crucible, the whole is placed in a muffle furnace at 850 ℃ to be calcined for 5 hours, then the ceramic crucible is taken out to be cooled to room temperature, and the volume ratio of the materials is 3: 1, heating the mixed solution to slightly boil at low temperature, sequentially adding 0.1g of sodium chloride and 20ml of 10% hydrochloric acid, transferring the mixed solution to a 100ml volumetric flask after the mixed solution is completely dissolved, and diluting the mixed solution to a scale with distilled water to obtain a pretreated sample solution.
Furthermore, the weighing accuracy of the waste residue sample and the palladium chloride sample is 0.0001 g.
The invention has the beneficial effects that: a stable colored complex is formed by palladium with chlorpromazine hydrochloride at a lower acidity. According to the principle of spectrophotometry detection, the method can accurately measure the palladium content in the pretreated sample solution. In the detection process, the removal amount after pretreatment can be adjusted according to the concentration of the palladium content in the sample solution, so that the sample solution is more fit with the range of a standard regression curve, the detection precision is further improved, the detection cost is low, and the method is suitable for detection of 0.1-5% of palladium content.
Detailed Description
The present invention will be described in further detail with reference to the following examples.
An analysis method for determining the content of palladium in waste residue comprises the following specific steps:
first, sample pretreatment
1. 20g of a waste residue sample with an accuracy of 0.0001g is weighed and placed in a ceramic crucible and calcined in a muffle furnace at 850 ℃ for 5 h.
2. Taking out the ceramic crucible, cooling to room temperature, adding a mixture of 3: 1, heating to slight boiling at low temperature, adding 0.1g of sodium chloride and 20ml of 10% hydrochloric acid, fully dissolving, transferring to a 100ml volumetric flask, and diluting to the scale with distilled water.
Second, making a standard regression curve
3. 0.1666g of palladium chloride is accurately weighed, and after 20ml of 10% hydrochloric acid solution is added and fully dissolved, the solution is transferred to a 100ml volumetric flask and diluted to the mark with distilled water.
4. Taking 1ml of the solution obtained in the step 3, putting the solution into a 250ml volumetric flask, diluting the solution to a scale with a 10% hydrochloric acid solution, transferring 0, 1, 2, 3, 4 and 5ml of a palladium standard solution into a 60ml separating funnel by using a pipette, adding 20ml of water, adjusting the pH to be 2 by using a 5% hydrochloric acid solution and a 5% sodium hydroxide solution respectively, adding 2ml of a 1% chlorpromazine hydrochloride solution, shaking uniformly, standing for 10min to generate a red complex, adding 10ml of trichloromethane respectively, shaking, extracting for 1min, layering, taking a lower layer of trichloromethane solution, measuring the absorbance of the solution at 488nm by using a 1cm cuvette by using a reagent blank as a reference, and drawing a standard regression curve according to the absorbance and the palladium standard concentration.
Third, sample detection
5. And (3) putting 1ml of the pretreated waste residue sample obtained in the step (2) into a 60ml separating funnel, adding 20ml of water, adjusting the pH to 2 by using a 5% hydrochloric acid solution and a 5% sodium hydroxide solution, adding 2ml of a 1% chlorpromazine hydrochloride solution, shaking uniformly, standing for 10min to generate a complex, adding 10ml of trichloromethane, carrying out oscillation extraction for 1min, taking a lower layer of trichloromethane solution after layering, taking a reagent blank as a reference, measuring the absorbance of the solution at 488nm by using a 1cm cuvette, and calculating the palladium content according to the absorbance and a standard regression curve.
The recovery rate of palladium content was determined by plotting a standard regression curve with different palladium standards on samples of known palladium content, and the results are shown in the following table
| Palladium content of sample | Palladium standard | Test value | Recovery rate |
| 2.31％ | 0.2％ | 2.49％ | 90.0％ |
| 2.31％ | 0.4％ | 2.72％ | 102.5％ |
| 2.31％ | 0.6％ | 2.92％ | 101.7％ |
Compared with GB/T15072.4-2008 weight method for determining the amount of palladium in the noble metal alloy by chemical analysis method, the method of the invention is used for carrying out three comparison tests on standard samples with 0.92% and 2.80% palladium content respectively, and recording related palladium content detection analysis, wherein the related detection results are as follows:
from the table, the technical scheme of the invention has more advantages and higher accuracy in the aspect of low content detection.
The technical solutions provided by the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained herein by using specific examples, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, for a person skilled in the art, according to the embodiments of the present invention, there may be variations in the specific implementation manners and application ranges, and in summary, the content of the present description should not be construed as a limitation to the present invention.
Claims (4)
1. An analysis method for determining the content of palladium in waste residue is characterized in that: calcining a waste residue sample at a high temperature, cooling to room temperature, adding a mixed solution of hydrochloric acid and nitric acid, heating at a low temperature to slightly boil, sequentially adding sodium chloride and 10% hydrochloric acid, completely dissolving, transferring to a 100ml volumetric flask, and diluting with distilled water to a scale to obtain a pretreated sample solution;
taking 1ml of the pretreated sample solution, putting the pretreated sample solution into a 60ml separating funnel, adding 20ml of water, adjusting the pH value to 2 by using a 5% hydrochloric acid solution and a 5% sodium hydroxide solution, adding 2ml of a 1% chlorpromazine hydrochloride solution, shaking uniformly, standing for 10min to generate a red complex, adding 10ml of trichloromethane, carrying out oscillation extraction for 1min, taking a lower layer of trichloromethane solution after layering, taking a reagent blank as a reference, measuring the absorbance of the solution at 488nm by using a 1cm cuvette, and calculating the palladium content according to the absorbance and a standard regression curve.
2. The analytical method for determining the palladium content in waste residues according to claim 1, characterized in that: the standard regression curve is drawn by weighing 0.1666g of palladium chloride, adding 20ml of 10% hydrochloric acid solution, transferring the solution to a 100ml volumetric flask after the solution is completely dissolved, and diluting the solution to a scale with distilled water; taking 1ml of the solution in a 250ml volumetric flask, adding 10% hydrochloric acid solution to dilute the solution to a scale, transferring 0, 1, 2, 3, 4 and 5ml of palladium standard solution into a 60ml separating funnel by a pipette, adding 20ml of water, adjusting the pH to 2 by using 5% hydrochloric acid solution and 5% sodium hydroxide solution respectively, adding 2ml of 1% chlorpromazine hydrochloride solution, shaking uniformly and standing for 10min to generate red complexes, adding 10ml of trichloromethane respectively, shaking and extracting for 1min, taking a lower layer of trichloromethane solution after layering, taking a reagent blank as a reference, measuring the absorbance of the solution at 488nm by using a 1cm cuvette, and drawing a standard regression curve according to the absorbance and the standard concentration of palladium.
3. The analytical method for determining the palladium content in the waste residue according to claim 2, wherein: the specific operation method of the pretreatment sample solution comprises the steps of weighing 20g of waste residue sample, placing the waste residue sample in a ceramic crucible, placing the whole in a muffle furnace at 850 ℃ for calcining for 5 hours, taking out the ceramic crucible, cooling to room temperature, and adding the mixture in a volume ratio of 3: 1, heating the mixed solution to slightly boil at low temperature, sequentially adding 0.1g of sodium chloride and 20ml of 10% hydrochloric acid, transferring the mixed solution to a 100ml volumetric flask after the mixed solution is completely dissolved, and diluting the mixed solution to a scale with distilled water to obtain a pretreated sample solution.
4. The analytical method for determining the palladium content in waste residues according to claim 3, characterized in that: the weighing accuracy of the waste residue sample and the palladium chloride sample is 0.0001 g.
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| CN202110061457.3A CN112730289A (en) | 2021-01-18 | 2021-01-18 | Analysis method for determining palladium content in waste residues |
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| CN202110061457.3A CN112730289A (en) | 2021-01-18 | 2021-01-18 | Analysis method for determining palladium content in waste residues |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1720343A (en) * | 2002-12-02 | 2006-01-11 | 科学与工业研究会 | Method for recovering and adsorbing palladium from waste silicon oxide |
| CN102954942A (en) * | 2012-11-23 | 2013-03-06 | 四川中自尾气净化有限公司 | Palladium content testing method |
| CN106092934A (en) * | 2016-07-13 | 2016-11-09 | 东江环保股份有限公司 | The assay method of the bullion content in solid waste |
| CN113337723A (en) * | 2021-06-10 | 2021-09-03 | 广东先导稀材股份有限公司 | Method for separating and extracting silver, palladium, copper and germanium from silver separating slag |
-
2021
- 2021-01-18 CN CN202110061457.3A patent/CN112730289A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1720343A (en) * | 2002-12-02 | 2006-01-11 | 科学与工业研究会 | Method for recovering and adsorbing palladium from waste silicon oxide |
| CN102954942A (en) * | 2012-11-23 | 2013-03-06 | 四川中自尾气净化有限公司 | Palladium content testing method |
| CN106092934A (en) * | 2016-07-13 | 2016-11-09 | 东江环保股份有限公司 | The assay method of the bullion content in solid waste |
| CN113337723A (en) * | 2021-06-10 | 2021-09-03 | 广东先导稀材股份有限公司 | Method for separating and extracting silver, palladium, copper and germanium from silver separating slag |
Non-Patent Citations (1)
| Title |
|---|
| 安登魁 主编, 人民卫生出版社 * |
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