CN102954942A - Palladium content testing method - Google Patents
Palladium content testing method Download PDFInfo
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- CN102954942A CN102954942A CN2012104845188A CN201210484518A CN102954942A CN 102954942 A CN102954942 A CN 102954942A CN 2012104845188 A CN2012104845188 A CN 2012104845188A CN 201210484518 A CN201210484518 A CN 201210484518A CN 102954942 A CN102954942 A CN 102954942A
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Abstract
The invention discloses a method for determining palladium by spectrophotometry. The method comprises the following steps that liquid to be tested and standard solution are prepared; the liquid to be tested and the standard solution measure the absorbancy A of test solution at a wavelength of 635nm; a standard curve is established according to the standard palladium solution with different concentrations and the corresponding absorbancy, and the slope k and the intercept b of the regression equation of the standard curve are calculated; and the amount of palladium m is calculated to be equal to kA plus b according to the equation. According to the palladium content testing method, the palladium can be directly determined without separating platinum, rhodium and other substances when the platinum, rhodium and other substances which do not affect the absorbancy at the wavelength of 635nm exist in a tested substance, and a process is simple and quick; the resistance to the interference of platinum, rhodium and the like is strong, the impact of an appropriate amount of platinum, rhodium and the like on a determination result is small, and the method is particularly applicable to the determination in a production process of a catalytic converter; the content of palladium is determined to be high and can reach 500mu.g; and compared with existing stannous chloride-acetone-potassium iodide spectrophotometry, the used amount of stannous chloride is only one tenth, so that the pollution is reduced, and the inspection cost is saved.
Description
Technical field
The invention belongs to field of spectral analysis technology, particularly utilize the method for spectrophotometry palladium content.
Background technology
Present detection method to palladium content has multiple, inductively coupled plasma spectrometry analytic approach (ICP method), and atomic absorption spectrography (AAS) (AAS), dimethylglyoxime is separated out-the EDTA compleximetry, stannous chloride-acetone-potassium iodide list wavelength spectrophotometric method etc.
Inductively coupled plasma spectrometry analytic approach and atomic absorption spectrography (AAS): the instrument price of use is up to hundreds thousand of, disposable having high input, consume spare unit and gas, analysis cost is high, to separate first other interference element during mensuration, process is complicated, and other element interference measurement when not separating affects the accurate of result.
Dimethylglyoxime is separated out-the EDTA compleximetry: be only applicable to the higher solution of palladium concentration, and will use methenyl choloride in measuring, it has pollution, and is national management and control goods and materials.
Stannous chloride-acetone-potassium iodide: this is the method for a comparative maturity.But, separate first other interference element, such as platinum, rhodium, then could measure.This method, separating step is many, and process is complicated, and the error of generation is large, affects equally the accurate of measurement result.
Summary of the invention
The present invention discloses a kind of method of Spectrophotometric Determination of Palladium according to the deficiencies in the prior art.The problem to be solved in the present invention provides a kind of method quick, convenient, that accurately utilize spectrophotometric to detect to palladium content.
The present invention is achieved through the following technical solutions:
Spectrophotometric Determination of Palladium comprises:
Liquid preparation to be detected, accurately take by weighing the determinand dissolving, pipette respectively the blank contrasting fluid of above-mentioned lysate and equal volume in two 25ml volumetric flasks, and add simultaneously respectively 5ml concentration and be the hydrochloric acid of (1+6), after shaking up, slowly to add 1.0ml concentration be the 0.5mol/L stannous chloride solution and shake up gently simultaneously, is that the hydrochloric acid of (1+6) is diluted to scale with concentration, shakes up stand-by;
Absorbance measurement, above-mentioned liquid to be detected was placed 15 minutes, used the 1cm cuvette, measured the test solution absorbance A in wavelength 635nm place;
Standard formulation, same method prepares the palladium standard solution of variable concentrations with preparing liquid phase to be detected, and the production standard curve, calculates slope k and the intercept b of typical curve regression equation;
Calculate, according under establish an equation and calculate the palladium amount: m=kA+b, wherein m is the palladium amount.
Palladium optimum detection scope palladium amount m:0-500 μ g of the present invention.Namely when carrying out spectrophotometry, the optimal amts of palladium in detecting solution is 0-500 μ g/25ml, and be high such as content in the reality detection thing, can be by detection after the method dilution of in proportion dilution.
The present invention is to containing interference component platinum or rhodium or containing simultaneously platinum and rhodium has good Detection accuracy in the determinand.
The present invention utilizes in hydrochloric acid medium, and palladium (II) (divalence palladium ion) forms green complex compound with stannous chloride, and in wavelength 635nm place mensuration absorbance, through evidence: platinum and/or rhodium do not affect detection in wavelength 635nm place absorbance under the similarity condition.
The present invention utilizes similarity condition, uses palladium standard substance production standard curve, calculates slope and the intercept of typical curve regression equation; To measure the palladium amount.Can use above-mentioned detection method to other interfering materials that do not affect detection in wavelength 635nm place absorbance and detect the palladium amount.
Helpfulness of the present invention: when the present invention has realized having platinum, rhodium etc. not to affect the material of wavelength 635nm place absorbance in detecting thing, the material such as Separation of Platinum, rhodium and directly measuring not, process is simply, fast; The interference performances such as anti-platinum, rhodium are strong, and the existence of an amount of platinum, rhodium etc. is little on the measurement result impact, is specially adapted to measure in the catalytic converter production run; The content of measuring palladium is high, can reach 500 μ g; Stannous chloride-the acetone that has with oneself-potassium iodide spectrophotometric method relatively, the stannous chloride consumption also only has 1/10, need not use expensive potassium iodide, the acetone of national management and control, has reduced pollution, has saved inspection cost.
Description of drawings
Fig. 1 is the palladium typical curve that experiment obtains.
Embodiment
Below by embodiment the present invention is conducted further description; the present embodiment only is used for the present invention is further detailed; but can not be interpreted as limiting the scope of the invention, those skilled in the art can make some nonessential improvement and adjustment belongs to the scope of protection of the invention according to the content of the invention described above.
Spectrophotometric Determination of Palladium comprises:
Liquid preparation to be detected, accurately take by weighing the determinand dissolving, pipette respectively the blank contrasting fluid of above-mentioned lysate and equal volume in two 25ml volumetric flasks, and add simultaneously respectively 5ml concentration and be the hydrochloric acid of (1+6), after shaking up, slowly to add 1.0ml concentration be the 0.5mol/L stannous chloride solution and shake up gently simultaneously, is that the hydrochloric acid of (1+6) is diluted to scale with concentration, shakes up stand-by;
Absorbance measurement, above-mentioned liquid to be detected was placed 15 minutes, used the 1cm cuvette, measured the test solution absorbance A in wavelength 635nm place;
Standard formulation, same method prepares the palladium standard solution of variable concentrations with preparing liquid phase to be detected, and the production standard curve, calculates slope k and the intercept b of typical curve regression equation;
Calculate, according under establish an equation and calculate the palladium amount: m=kA+b, wherein m is the palladium amount.
Palladium optimum detection scope palladium amount m:0-500 μ g.Namely when carrying out spectrophotometry, the optimal amts of palladium in detecting solution is 0-500 μ g, and be high such as content in the reality detection thing, can be by detection after the method dilution of in proportion dilution.
Embodiment 1
The making of palladium typical curve:
Palladium standard solution (100mg/L)
Pipette respectively palladium standard solution 0,1.00 with graduated pipette, 2.00,3.00,4.00, in 5.00mL to the 6 25ml volumetric flask, slowly to add concentration be the 1.0ml stannous chloride solution of 0.5mol/L and shake up gently simultaneously, is diluted to scale with concentration for (1+6) hydrochloric acid, shake up, placed 15 minutes, and used the 1cm cuvette, measure the test solution absorbance A in wavelength 635nm place.
Use the 1cm cuvette, take reagent blank as reference solution, measure absorbance A in wavelength 635nm place.Take palladium amount (unit is as μ g) as ordinate, corresponding absorbance A(unit is %) for horizontal ordinate, at the drawing standard curve, calculate slope k and the intercept b of typical curve regression equation.
Embodiment 2
The palladium content detection
Measurement range: palladium amount 0-500 μ g; High such as content in the reality detection thing, can be by detection after the method dilution of in proportion dilution.
Stannous chloride solution configuration (0.5mol/L): take by weighing 11.3g stannous chloride (SnCl
22H
2O), add concentration and be (1+6) hydrochloric acid solution 100ml dissolving preparation.
Accurately take by weighing the determinand dissolving, pipette respectively equal volume test solution and blank solution in two 25ml volumetric flasks, and add simultaneously respectively 5ml concentration and be the hydrochloric acid of (1+6), after shaking up, slowly adding 1.0ml concentration is to shake up gently 0.5mol/L stannous chloride solution and while, be diluted to scale with concentration for the hydrochloric acid of (1+6), shake up stand-by; Above-mentioned liquid to be detected was placed 15 minutes, used the 1cm cuvette, measured the test solution absorbance A in wavelength 635nm place
According under establish an equation and calculate palladium amount: m=kA+b, wherein m is the palladium amount, k is the slope of typical curve regression equation, b is the intercept of typical curve regression equation.
Embodiment 3
Concrete test example
Test sample content: 430 μ g, contain platinum, rhodium chaff interference.
Two absorbance such as following tables that Duplicate Samples is measured: table 1
| Sample number | Sample 1 | Sample 2 |
| Absorbance A (%) | 36.92 | 36.55 |
| Sample determination content (μ g) | 422.9 | 418.7 |
| Relative error (%) | -1.65 | 2.63 |
Table 1 explanation error at measurment meets the requirements.
Standard curve determination data: table 2
| Palladium amount (ug) | Absorbance A (%) |
| 0 | 0 |
| 100 | 8.34 |
| 200 | 17.18 |
| 300 | 26.28 |
| 400 | 34.92 |
| 500 | 43.69 |
The production standard curve: such as Fig. 1, the slope k of typical curve regression equation=11.389: intercept; B=2.4679.
Typical curve: m=11.389A+2.4679
Linearly dependent coefficient R satisfies R
2=0.9999, the description standard curve linear is relevant fine.
Embodiment 4
Under condition determination, by adding the platinum standard solution as the method for chaff interference, add 250 μ g platinum, the absorbance of platinum only is 0.11%; Add 240 μ g platinum, the absorbance of platinum is 0.81% only, further specifies the inventive method disturbing factor little, and testing result is accurate.
Claims (3)
1. palladium detection method of content is characterized in that comprising:
Liquid preparation to be detected, accurately take by weighing the determinand dissolving, pipette respectively the blank contrasting fluid of above-mentioned lysate and equal volume in two 25ml volumetric flasks, and add simultaneously respectively 5ml concentration and be the hydrochloric acid of (1+6), after shaking up, slowly to add 1.0ml concentration be the 0.5mol/L stannous chloride solution and shake up gently simultaneously, is that the hydrochloric acid of (1+6) is diluted to scale with concentration, shakes up stand-by;
Absorbance measurement, above-mentioned liquid to be detected was placed 15 minutes, used the 1cm cuvette, measured the test solution absorbance A in wavelength 635nm place;
Standard formulation, same method prepares the palladium standard solution of variable concentrations with preparing liquid phase to be detected, and the production standard curve, calculates slope k and the intercept b of typical curve regression equation;
Calculate, according under establish an equation and calculate the palladium amount: m=kA+b, wherein m is the palladium amount.
2. palladium detection method of content according to claim 1 is characterized in that: described palladium measurement range palladium amount m:0-500 μ g/25ml.
3. palladium detection method of content according to claim 2 is characterized in that: contain interference component platinum and/or rhodium in the described determinand.
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| CN2012104845188A CN102954942A (en) | 2012-11-23 | 2012-11-23 | Palladium content testing method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103575676A (en) * | 2013-11-07 | 2014-02-12 | 广州有色金属研究院 | Method for analyzing palladium in palladium-carbon catalyst |
| CN106841180A (en) * | 2015-12-03 | 2017-06-13 | 北京有色金属研究总院 | A kind of method for continuously measuring of Platinum in Ore, palladium |
| CN112730289A (en) * | 2021-01-18 | 2021-04-30 | 重庆欣欣向荣精细化工有限公司 | Analysis method for determining palladium content in waste residues |
| JP7290783B1 (en) | 2022-11-14 | 2023-06-13 | 松田産業株式会社 | metal recovery system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1510412A (en) * | 2002-12-23 | 2004-07-07 | 中国石油天然气股份有限公司乌鲁木齐 | Method for rapidly determining palladium content in palladium-carbon catalyst |
| JP2010237051A (en) * | 2009-03-31 | 2010-10-21 | Sumitomo Metal Mining Co Ltd | Method for quantifying hydroxyl group on surface of metal powder |
-
2012
- 2012-11-23 CN CN2012104845188A patent/CN102954942A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1510412A (en) * | 2002-12-23 | 2004-07-07 | 中国石油天然气股份有限公司乌鲁木齐 | Method for rapidly determining palladium content in palladium-carbon catalyst |
| JP2010237051A (en) * | 2009-03-31 | 2010-10-21 | Sumitomo Metal Mining Co Ltd | Method for quantifying hydroxyl group on surface of metal powder |
Non-Patent Citations (1)
| Title |
|---|
| 丘星初等: ""钯-镍镀液中钯的光度测定"", 《电镀与精饰》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103575676A (en) * | 2013-11-07 | 2014-02-12 | 广州有色金属研究院 | Method for analyzing palladium in palladium-carbon catalyst |
| CN106841180A (en) * | 2015-12-03 | 2017-06-13 | 北京有色金属研究总院 | A kind of method for continuously measuring of Platinum in Ore, palladium |
| CN112730289A (en) * | 2021-01-18 | 2021-04-30 | 重庆欣欣向荣精细化工有限公司 | Analysis method for determining palladium content in waste residues |
| JP7290783B1 (en) | 2022-11-14 | 2023-06-13 | 松田産業株式会社 | metal recovery system |
| JP2024071280A (en) * | 2022-11-14 | 2024-05-24 | 松田産業株式会社 | Metal collection system |
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Application publication date: 20130306 |