CN102023154A - Method for detecting the content of palladium in carbon catalyst - Google Patents
Method for detecting the content of palladium in carbon catalyst Download PDFInfo
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- CN102023154A CN102023154A CN2009100349670A CN200910034967A CN102023154A CN 102023154 A CN102023154 A CN 102023154A CN 2009100349670 A CN2009100349670 A CN 2009100349670A CN 200910034967 A CN200910034967 A CN 200910034967A CN 102023154 A CN102023154 A CN 102023154A
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Abstract
The invention belongs to the technical field of analytical chemistry, and provides a method for detecting the content of palladium in carbon catalyst. The method comprises the following steps: weighing 0.15 gram of sample, putting the sample into a beaker, adding perchloric acid, hydrochloric acid and hydrogen nitrate in a proper proportion, covering the beaker with a watch glass, heating the beaker on an electric hot plate until white smoke disappears and the solution is clear, meanwhile adding about 0.15 gram of activated carbon powder, adding perchloric acid, hydrochloric acid and hydrogen nitrate in a proper proportion, preparing blank liquid and standard liquid, dispelling the interference of reagent and matrix, and analyzing samples by plasma emission spectrometer. The method is advantageous in that: the method shortens the sample processing time to an hour or less from traditional a few days, thus the sample processing time is shortened remarkably; by preparing blank liquid and standard liquid, the influence of the reagent and matrix on analysis is dispelled; and the method of the invention is capable of providing timely and accurate data for scientific research and production.
Description
Technical field: the invention belongs to the chemical analysis technology field, relate to palladium-carbon catalyst perchloric acid oxidation treatment technology, and eliminate matrix and disturb, thereby reach the method for analyzing palladium content fast and accurately by blank, standard laboratory preparation.
Technical background: the palladium-carbon catalyst preprocess method has Microwave Digestion, the muffle furnace method of making charcoal usually.These methods have all that time-consuming length, palladium easily lose, power consumption is big, and during instrument detecting because the influence of reagent and charcoal base can bring matrix to disturb, accuracy is measured in influence.
Palladium content analysis report seldom in the palladium-carbon catalyst.Sinopec Yangzi Petrochemical Co's patent, the number of applying for a patent CN200710022937.9 introduces: a kind of microwave clearing ICP method is measured the method for palladium content in the palladium-carbon catalyst, it is to take by weighing sample 0.1-0.2 to restrain in the micro-wave digestion jar, add the wetting sample of secondary deionized water, add 5mlHCl and 3mlHNO again
3, build lid, insert in the protective sleeve and put the safety spring sheet; compress whole counteracting tank, prepare blank sample simultaneously, put into microwave dissolver then; start microwave dissolver, open program control system, with program setting be: pressure 35bar, power 500W, heating schedule are to be warming up to 200 ℃, 30 minutes constant temperature in 5 minutes; cooling; after clearing up EOP (end of program), temperature reaches room temperature, takes out counteracting tank and acid solution is rushed to 2ml; constant volume records palladium content at last on ICP then.
Urumqi Petro-Chemical Branch, Chinese Petroleum-Natural Gas Co Ltd's patent, the number of applying for a patent CN02157951.2 introduces: palladium content method in a kind of fast measuring palladium-carbon catalyst, carry out: the first step, the palladium-carbon catalyst sample of required mensuration is carried out pre-service according to the following steps; Second goes on foot, above-mentioned pretreatment sample formulations prepared from solutions is become with the required working sample solution of spectrophotometric determination: above-mentioned pretreatment sample solution is put to room temperature carried out obtaining working sample solution behind molten surely dilution and the adding chromogenic reagent; The 3rd step, with the said determination sample solution with spectrophotometer in its absorbance A of 406nm place mensuration; The 4th step, be content: C=K with palladium concentration C in following worker's formula calculating palladium-carbon catalyst
1* A+K
0
Summary of the invention: the present invention is directed to these drawbacks palladium content analysis method in a kind of quick, accurate, economic mensuration palladium-carbon catalyst is provided.
Technical solution of the present invention is as follows: the method for palladium content in the rapid and accurate determination palladium-carbon catalyst is characterized in that comprising following consecutive steps:
A, the preparation of palladium standard stock solution: take by weighing the 0.1g Metal Palladium, with the molten sample of chloroazotic acid, constant volume makes 100mg/l in the 1L volumetric flask
The standard stock solution.
B, bioassay standard preparation: take by weighing 0.15g (being accurate to 0.1mg) dry activated carbon powder in the 250mL beaker, add the palladium standard stock solution that 10mL has prepared, again 5-8mL perchloric acid, 5-8mL hydrochloric acid and 3-6mL nitric acid are poured in the clean beaker of a processing and mixed, again mixed solution is slowly added and be equipped with in the beaker of active carbon powder, heating is smoldered to the powdered carbon disappearance, and the solution clarification.Thin up boils and handles 3min to 50mL, and constant volume makes the palladium standard model in the 100mL volumetric flask.
C, blank preparation: take by weighing 0.15g (being accurate to 0.1mg) dry activated carbon powder in the 250mL beaker, again 5-8mL perchloric acid, 5-8mL hydrochloric acid and 3-6mL nitric acid are poured in the clean beaker of a processing and mixed, again mixed solution is slowly added and be equipped with in the beaker of active carbon powder, heating is smoldered to the powdered carbon disappearance, and the solution clarification.Thin up boils and handles 3min to 50mL, and constant volume makes blank sample in the 100mL volumetric flask.
D, specimen preparation: get the 10g sample with inquartation, be ground to below the 75 μ m, sieve, dry to constant mass at 130 ℃, take by weighing the dry sample of 0.15g (being accurate to 0.1mg) in the 250mL beaker, 5-8mL perchloric acid, 5-8mL hydrochloric acid and 3-6mL nitric acid are added in the beaker, heating is smoldered to the powdered carbon disappearance again, and the solution clarification.Thin up boils and handles 3min to 50mL, and constant volume makes testing sample in the 100mL volumetric flask.
E, plasma emission spectrometer is started shooting behind the preheating 0.5h, the massfraction that 340.458nm place palladium characteristic spectral line is measured palladium is chosen in igniting.
F, analysis result are calculated as follows:
The massfraction of palladium is in w, and numerical value calculates by formula with percentage (%) expression:
w＝C×10
-6×100/(m×1/V)
In the formula: C---testing sample solution palladium concentration, mg/l;
V---volumetric flask volume, ml;
M---sample weighting amount, g;
W---the massfraction of palladium element in the sample, %.
The inventive method is handled the charcoal base by the perchloric acid oxidation, certain proportion hydrochloric acid, nitric acid stripping palladium, the sample preparation time was shortened in 1 hour from traditional several days, shortened the processing time of sample greatly, and, eliminated the influence of reagent and matrix to analyzing by preparation blank solution and titer.For research and production provide quick, accurate, economic analytical approach.
Utilize the present invention can realize accurately, measure quickly and accurately palladium content in the palladium-carbon catalyst, and spectrophotometer thereby cost are lower owing to having adopted, can estimate palladium-carbon catalyst situation in process engineering so on the one hand, guarantee the quality of production, on the other hand can quantitative assessment to the palladium content of the palladium-carbon catalyst that lost efficacy, the recovery of palladium is played directive function.The analysis means aspect adopts the inductively coupled plasma emission spectrometer to analyze, and it is low that it has a detection limit of analysis, and the range of linearity is wide, characteristics such as precision height.
Embodiment: following by specific embodiment explanation the present invention.
Embodiment one:
Research institute's palladium-carbon catalyst palladium Determination on content.
1, experiment device therefor
The model iCAP6300Radial of inductively coupled plasma emission spectrometer U.S. Thermo company
Electric hot plate
Electronic balance
The quartzy pure water distiller of secondary
Baking oven
The standard sub-sieve
2, experiment reagent
Perchloric acid is analyzed pure
The salt acid analysis is pure
Nitric acid is analyzed pure
Secondary distillation water (self-control)
Metal Palladium silk (99.99%)
3, sample preparation step
Get 0.1489g through grinding, sieve, this catalyst sample of 130 ℃ of constant weights adds perchloric acid, hydrochloric acid, nitric acid successively in the 250ml beaker, and heating is smoldered to the powdered carbon disappearance, and the solution clarification.Add secondary distillation water 50ml, heated and boiled 3min, constant volume is in the 100ml volumetric flask.Claim the 0.15g active carbon powder simultaneously, prepare blank solution and titer (10mg/l) by above-mentioned steps.
4, sample determination
Plasma emission spectrometer is started shooting behind the preheating 0.5h, and igniting is chosen 340.458nm place palladium characteristic spectral line and is measured, and is blank with the blank solution for preparing.Sequentially determining blank solution, titer, liquid to be measured.Have bales catch except that blank and computing function because instrument carries software, can directly obtain liquor concentration to be measured.Its result is: 7.30mg/l
5, the result calculates
Utilize formula: w=C * 10
-6* 100/ (m * 1/V)
In the formula:
C---testing sample solution palladium concentration, mg/l;
V---volumetric flask volume, ml;
M---sample weighting amount, g;
W---the massfraction of palladium element in the sample, %.
The palladium constituent content is in the sample by calculating: 0.49%
Embodiment two:
Use factory's one industry to use the front and back catalyzer
2# industry used back upper strata 3# industry to use back middle level 4# industry to use back lower floor before sample situation: 1# industry was used
The sample preparation step; Take by weighing 1#, 2#, 3#, 4# respectively through grinding, sieve.The catalyst sample of 130130 ℃ of constant weights, its sample weighting amount is respectively 0.1541g, 0.1573g, 0.1504g, 0.1520g adds in four 250ml beakers, adds perchloric acid, hydrochloric acid, nitric acid successively, and heating is smoldered to the powdered carbon disappearance, and the solution clarification.Add secondary distillation water 50ml, heated and boiled 3min, constant volume is in the 100ml volumetric flask.Take by weighing the 0.15g active carbon powder simultaneously, prepare blank solution and titer (10mg/l) by above-mentioned steps.Plasma emission spectrometer is started shooting behind the preheating 0.5h, and igniting is chosen 340.458nm place palladium characteristic spectral line and is measured, and is blank with the blank solution for preparing.Sequentially determining blank solution, titer, liquid to be measured.Have bales catch except that blank and computing function because instrument carries software, can directly obtain liquor concentration to be measured.Its result is respectively: 6.32mg/l, 6.45mg/l, 6.31mg/l, 7.35mg/l.Utilize formula: w=C * 10
-6* 100/ (m * 1/V)
In the formula:
C---testing sample solution palladium concentration, mg/l;
V---volumetric flask volume, ml;
M---sample weighting amount, g;
W---the massfraction of palladium element in the sample, %.
The palladium constituent content is respectively in the sample by calculating: 0.41%, 0.41%, 0.42%, 0.48%.
Embodiment three:
Fresh catalyst before using factory's two industry to use
Get 0.1607g through grinding, sieve, this catalyst sample of 130 ℃ of constant weights adds perchloric acid, hydrochloric acid, nitric acid successively in the 250ml beaker, and heating is smoldered to the powdered carbon disappearance, and the solution clarification.Add secondary distillation water 50ml, heated and boiled 3min, constant volume is in the 100ml volumetric flask.Claim the 0.15g active carbon powder simultaneously, prepare blank solution and titer (10mg/l) by above-mentioned steps.Take by weighing the 0.15g active carbon powder simultaneously, prepare blank solution and titer (10mg/l) by above-mentioned steps.Plasma emission spectrometer is started shooting behind the preheating 0.5h, and igniting is chosen 340.458nm place palladium characteristic spectral line and is measured, and is blank with the blank solution for preparing.Sequentially determining blank solution, titer, liquid to be measured.Have bales catch except that blank and computing function because instrument carries software, can directly obtain liquor concentration to be measured.Its result is 7.71mg/l.
Utilize formula: w=C * 10
-6* 100/ (m * 1/V)
In the formula:
C---testing sample solution palladium concentration, mg/l;
V---volumetric flask volume, ml;
M---sample weighting amount, g;
W---the massfraction of palladium element in the sample, %.
The palladium constituent content is respectively in the sample by calculating: 0.48%.
Claims (1)
1. method of measuring palladium content in the palladium-carbon catalyst is characterized in that comprising following consecutive steps:
A) palladium standard stock solution preparation: take by weighing the 0.1g Metal Palladium, with the molten sample of chloroazotic acid, constant volume makes 100mg/l standard stock solution in the 1L volumetric flask.
B) bioassay standard preparation: take by weighing 0.15g dry activated carbon powder in the 250mL beaker, add the palladium standard stock solution that 10mL has prepared, again 5-8mL perchloric acid, 5-8mL hydrochloric acid and 3-6mL nitric acid are poured in the clean beaker of a processing and mixed, mixed solution is slowly added again and be equipped with in the beaker of active carbon powder, heating is smoldered to the powdered carbon disappearance, and the solution clarification, thin up is to 50mL, boil and handle 3min, constant volume makes the palladium standard model in the 100mL volumetric flask;
C) blank preparation: take by weighing 0.15g dry activated carbon powder in the 250mL beaker, again 5-8mL perchloric acid, 5-8mL hydrochloric acid and 3-6mL nitric acid are poured in the clean beaker of a processing and mixed, again mixed solution is slowly added and be equipped with in the beaker of active carbon powder, heating is smoldered to powdered carbon and is disappeared, and solution clarification, thin up are boiled and are handled 3min to 50mL, constant volume makes blank sample in the 100mL volumetric flask;
D) specimen preparation: get the 10g sample with inquartation, be ground to below the 75 μ m, sieve, dry to constant mass at 130 ℃, the sample that takes by weighing the 0.15g drying is in the 250mL beaker, again 5-8mL perchloric acid, 5-8mL hydrochloric acid and 3-6mL nitric acid are poured in the clean beaker of a processing and mixed, again mixed solution is slowly added and be equipped with in the beaker of active carbon powder, heating is smoldered to powdered carbon and is disappeared, and solution clarification, thin up are boiled and are handled 3min to 50mL, constant volume makes testing sample in the 100mL volumetric flask;
E) plasma emission spectrometer is started shooting behind the preheating 0.5h, the massfraction that 340.458nm place palladium characteristic spectral line is measured palladium is chosen in igniting;
F) analysis result is calculated as follows:
The massfraction of palladium is in w, and numerical value is calculated as follows with percentage (%) expression:
w＝C×10
-6×100/(m×1/V)
In the formula: C---testing sample solution palladium concentration, mg/l;
V---volumetric flask volume, ml;
M---sample weighting amount, g;
W---the massfraction of palladium element in the sample, %.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104697986A (en) * | 2015-03-30 | 2015-06-10 | 西部新锆核材料科技有限公司 | Method for measuring lithium content in zirconium and zirconium alloy |
| CN110296948A (en) * | 2019-08-09 | 2019-10-01 | 新乡双鹭药业有限公司 | The remaining measuring method of palladium metal in a kind of drug |
| CN112014380A (en) * | 2020-09-03 | 2020-12-01 | 中国科学院长春应用化学研究所 | Pretreatment and quantitative analysis method for quickly, efficiently and accurately measuring palladium content in palladium-carbon catalyst |
| CN113267485A (en) * | 2020-10-27 | 2021-08-17 | 水口山有色金属有限责任公司 | Method for measuring platinum and palladium in noble metal solution sample suitable for gold and silver production |
| CN114280034A (en) * | 2021-12-24 | 2022-04-05 | 浙江微通催化新材料有限公司 | Application of oxygen bomb combustion method in determination of waste palladium-carbon-palladium content and determination method |
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2009
- 2009-09-16 CN CN2009100349670A patent/CN102023154A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104697986A (en) * | 2015-03-30 | 2015-06-10 | 西部新锆核材料科技有限公司 | Method for measuring lithium content in zirconium and zirconium alloy |
| CN107462567A (en) * | 2015-03-30 | 2017-12-12 | 国核宝钛锆业股份公司 | A kind of method for determining lithium content in zirconium and zircaloy |
| CN107462567B (en) * | 2015-03-30 | 2019-04-09 | 国核宝钛锆业股份公司 | A method of lithium content in measurement zirconium and zircaloy |
| CN110296948A (en) * | 2019-08-09 | 2019-10-01 | 新乡双鹭药业有限公司 | The remaining measuring method of palladium metal in a kind of drug |
| CN112014380A (en) * | 2020-09-03 | 2020-12-01 | 中国科学院长春应用化学研究所 | Pretreatment and quantitative analysis method for quickly, efficiently and accurately measuring palladium content in palladium-carbon catalyst |
| CN113267485A (en) * | 2020-10-27 | 2021-08-17 | 水口山有色金属有限责任公司 | Method for measuring platinum and palladium in noble metal solution sample suitable for gold and silver production |
| CN114280034A (en) * | 2021-12-24 | 2022-04-05 | 浙江微通催化新材料有限公司 | Application of oxygen bomb combustion method in determination of waste palladium-carbon-palladium content and determination method |
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Application publication date: 20110420 |