CN103528913A - Method for measuring rhodium content in rhodium-containing compound - Google Patents
Method for measuring rhodium content in rhodium-containing compound Download PDFInfo
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Abstract
The invention relates to a method for measuring the rhodium content in rhodium-containing compound. The method comprises the steps of: 1) roasting by using high-temperature air to decompose rhodium-containing compound to be rough rhodium oxide; 2) grinding the rough rhodium oxide, immersing with 1-6mol/L hydrochloric acid for 1-5h at 50-70 DEG C and filtering to obtain filter residue; 3) reducing the filter residue with high-temperature nitrogen to change the rhodium oxide into rhodium powder; 4) weighing the rhodium powder and calculating rhodium content in the rhodium-containing compound. By adopting the method, rhodium content in the rhodium-containing compound with regular rhodium content which can be decomposed to be oxide by heating can be accurately measured, addition of other reagents for separation of rhodium is not needed, measuring error caused by repeated dilution with a power-spectral method is avoided, and rigorous requirements of high-temperature and strong-oxidizing-property wet digestion on the equipment are avoided. The method is convenient to operate without introducing solid impurities and has the advantages of high accuracy and recovery rate.
Description
Invention field
The present invention relates to compound elemental rhodium assay, particularly relate to rhodium content assay method in a kind of rhodium-containing compound of conventional rhodium content.
Background technology
Platinum group metal, because all have the electronics that can lose gradually under certain condition on outer and time out orbit, forms multiple low price oxidation state, and while there is some part in solution, they can form stable complex.This distinct electrical minor structure of platinum group metal, makes it have good catalytic performance, is widely used in the fields such as environment-friendly materials, petrochemical complex, fine chemistry industry, bio-pharmaceuticals.Rhodium compound and complex thereof, have activity for reactions such as the hydrogenation of organic synthesis process, carbonyl addition, acyl hydrogenations, and it is widely used.Rhodium catalysis has become one of field the most active in organic and catalytic science.
Because the content of rhodium directly affects the catalytic efficiency of catalyzer, be an important indicator of evaluate catalysts catalytic performance, so particularly important to the Accurate Determining of rhodium content in rhodium-containing compound.
Jap.P. JP629262 has proposed, according to the principle of the pH value flex point of neutralization reaction formation, to utilize alkaline aqueous solution to carry out the method for the rhodium content in titration sulfuric acid system.Its principle is that the sulfuric acid neutralization reaction in OH-and rhodium plating solution forms first pH value flex point (a), and after the sulfuric acid in plating solution neutralizes completely, OH can form rhodium hydroxide (b) with rhodium sulfate reaction, generates precipitation, forms another pH value flex point.But because the old rhodium of hydroxide is amphiprotic substance, this kind of more difficult judgement of method terminal, error is larger.
GB/T1485-1979, platinum-rhodium alloy chemical analysis method adopts nitric acid six amminos to close trivalent cobalt salt and rhodium generates double salt precipitation to measure the method for rhodium (III), because thick rhodium (III) solution often contains a large amount of interference elements, causes analytical error.After have document to adopt precipitation, extraction separation method and complexing masking method to eliminate Au, Fe, the impact of Ir element on nitric acid six cobaltammine gravimetric determination rhodiums by improvement, and separated and masking condition has been carried out systematic research to it.Under selected condition, relative error≤± 5 ‰.The method is complicated, complex steps.
At present conventional instrumental analysis is as atomic absorption method (FAAS) and inductively coupled plasma mass spectrometry (ICP-MS)] need to rhodium-containing test solution repeatedly dilute hundreds of～several ten thousand times just can make rhodium concentration within 100PPM to be suitable for measurement, cause measurement result error larger.X ray fluorescence spectrometry, due to the interference of other element, affects the accuracy of result.
Summary of the invention
The present invention relates to rhodium content assay method in a kind of conventional rhodium content rhodium-containing compound.The rhodium compound that can be decomposed into oxide for Accurate Measurement heating, comprises rhodium in the rhodium compounds such as rhodium nitrate, halogenide, rhodium organic complex.The method is passed through pyrolytic, acidleach, and hydrogen reducing, weighs, and measures rhodium content in rhodium-containing compound.This method has been eliminated for rhodium separation being added to the needs of other reagent, and avoids spectrographic determination repeatedly to dilute and cause measuring error, has avoided high temperature, the harsh requirement of strong oxidizing property Wet to equipment.
The present invention is rhodium content assay method in a kind of rhodium-containing compound, it is characterized in that, comprises the steps:
1) adopt high temperature blowing air roasting rhodium-containing compound, make rhodium-containing compound resolve into thick rhodium oxide;
2) thick rhodium oxide is ground, with 1～6mol/L salt acid soak, 1～5h, temperature is 50～70 ℃, filters and obtains filter residue;
3) filter residue adopts the logical hydrogen reducing of high temperature, makes rhodium oxide become rhodium powder;
4) rhodium powder is weighed, calculate rhodium content in rhodium-containing compound;
Wherein, described rhodium-containing compound is for heating the rhodium compound that can be decomposed into oxide;
In step 1), sintering temperature is 650～1000 ℃, and roasting time is 0.5～5h;
Step 3) in, logical hydrogen reducing temperature is 600～800 ℃, and the recovery time is 0.5～3h.
According to rhodium content assay method in rhodium-containing compound of the present invention, in described rhodium-containing compound, preferred rhodium content is for being greater than 10%.
According to rhodium content assay method in rhodium-containing compound of the present invention, the test sampling amount of described rhodium-containing compound is preferably 1～10g.
A kind of or potpourri in described rhodium-containing compound selected from rhodium nitrate, halogenation rhodium and rhodium organic complex, preferably rhodium-containing compound is rhodium chloride.
In rhodium-containing compound of the present invention, rhodium content assay method compared with prior art, the inventive method adopts high-temperature roasting, Ore Leaching and hydrogen reduction method to measure rhodium content in high-load rhodium compound, easy to operate and do not introduce solid impurity, there is degree of accuracy high, the advantage that the recovery is good.
Embodiment
Embodiment 1
Take rhodium chloride 1g, at 700 ℃, roasting is 1 hour, cooling, obtains thick rhodium oxide; Thick rhodium oxide is ground, use 2mol/L salt acid soak 3 hours, temperature is 60 ℃, filters and obtains filter residue; Filter residue is placed in quartz boat and puts into tubular furnace, first in tubular furnace, leads to after nitrogen 10min, and logical hydrogen reducing, temperature is 700 degree, reduction 1h, makes rhodium oxide become rhodium powder; Rhodium powder is weighed, and weight is 0.3884g, calculates rhodium content in rhodium compound.
The computing formula of rhodium content is: Rh%=rhodium grain weight amount/rhodium chloride weight * 100%
Embodiment 2
Take rhodium chloride 5g, at 1000 ℃, roasting is 1 hour, cooling, obtains thick rhodium oxide; Thick rhodium oxide is ground, use 1mol/L salt acid soak 5 hours, temperature is 70 ℃, filters and obtains filter residue; Filter residue is placed in quartz boat and puts into tubular furnace, first in tubular furnace, leads to after nitrogen 10min, and logical hydrogen reducing, temperature is 800 degree, reduction 1h, makes rhodium oxide become rhodium powder; Rhodium powder is weighed, and weight is 1.9510g, calculates rhodium content in rhodium compound.
Embodiment 3
Take rhodium chloride 10g, at 650 ℃, roasting is 3 hours, cooling, obtains thick rhodium oxide; Thick rhodium oxide is ground, use 6mol/L salt acid soak 1 hour, temperature is 50 ℃, filters and obtains filter residue, washes with water; Filter residue is placed in quartz boat and puts into tubular furnace, first in tubular furnace, leads to after nitrogen 10min, and logical hydrogen reducing, temperature is 600 degree, reduction 3h, makes rhodium oxide become rhodium powder; Rhodium powder is weighed, and weight is 3.9122g, calculates rhodium content in rhodium compound.
Embodiment 4
Take rhodium nitrate 6g, at 800 ℃, roasting is 4 hours, cooling, obtains thick rhodium oxide; Thick rhodium oxide is ground, use 3mol/L salt acid soak 4 hours, temperature is 60 ℃, filters and obtains filter residue, washes with water; Filter residue is placed in quartz boat and puts into tubular furnace, first in tubular furnace, leads to after nitrogen 10min, and logical hydrogen reducing, temperature is 600 degree, reduction 3h, makes rhodium oxide become rhodium powder; Rhodium powder is weighed, and weight is 2.3862g, calculates rhodium content in rhodium compound.
Embodiment 5
Take rhodium dicarbonyl acetylacetonate 8g, at 1000 ℃, roasting is 2 hours, cooling, obtains thick rhodium oxide; Thick rhodium oxide is ground, use 2mol/L salt acid soak 4 hours, temperature is 70 ℃, filters and obtains filter residue, washes with water; Filter residue is placed in quartz boat and puts into tubular furnace, first in tubular furnace, leads to after nitrogen 10min, and logical hydrogen reducing, temperature is 700 degree, reductase 12 h makes rhodium oxide become rhodium powder; Rhodium powder is weighed, and weight is 3.1621g, calculates rhodium content in rhodium compound.
Claims (5)
1. a rhodium content assay method in rhodium-containing compound, is characterized in that, comprises the steps:
1) adopt roasting rhodium-containing compound under blowing air condition, make rhodium-containing compound resolve into thick rhodium oxide;
2) thick rhodium oxide is ground, with 1～6mol/L salt acid soak, 1～5h, temperature is 50～70 ℃, filters and obtains filter residue;
3) filter residue adopts the logical hydrogen reducing of high temperature, makes rhodium oxide become rhodium powder;
4) rhodium powder is weighed, calculate rhodium content in rhodium-containing compound;
Wherein, described rhodium-containing compound is for heating the rhodium compound that can be decomposed into oxide;
Step 1) in, sintering temperature is 650～1000 ℃, and roasting time is 0.5～5h;
Step 3) in, logical hydrogen reducing temperature is 600～800 ℃, and the recovery time is 0.5～3h.
2. rhodium content assay method in rhodium-containing compound according to claim 1, is characterized in that, in rhodium-containing compound, rhodium content is for being greater than 10%.
3. rhodium content assay method in rhodium-containing compound according to claim 1, is characterized in that, the test sampling amount of described rhodium-containing compound is 1～10g.
4. rhodium content assay method in rhodium-containing compound according to claim 1, is characterized in that, wherein one or more potpourris in described rhodium-containing compound selected from rhodium nitrate, halogenation rhodium and rhodium organic complex.
5. rhodium content assay method in rhodium-containing compound according to claim 5, is characterized in that, wherein rhodium-containing compound is rhodium chloride.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067475A (en) * | 2015-07-30 | 2015-11-18 | 成都欣华源科技有限责任公司 | Method for determining content of rhodium in water-soluble rhodium-phosphine complex |
| CN113008723A (en) * | 2021-02-03 | 2021-06-22 | 广东金正龙科技有限公司 | Method for detecting content of high-purity rhodium compound solution |
| CN113237789A (en) * | 2021-05-12 | 2021-08-10 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
| CN113267421A (en) * | 2021-06-29 | 2021-08-17 | 巴斯夫公司 | Method for determining noble metal content |
| CN114427998A (en) * | 2020-09-27 | 2022-05-03 | 中国石油化工股份有限公司 | Method for determining rhodium content in rhodium-containing waste residue |
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2013
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067475A (en) * | 2015-07-30 | 2015-11-18 | 成都欣华源科技有限责任公司 | Method for determining content of rhodium in water-soluble rhodium-phosphine complex |
| CN114427998A (en) * | 2020-09-27 | 2022-05-03 | 中国石油化工股份有限公司 | Method for determining rhodium content in rhodium-containing waste residue |
| CN113008723A (en) * | 2021-02-03 | 2021-06-22 | 广东金正龙科技有限公司 | Method for detecting content of high-purity rhodium compound solution |
| CN113237789A (en) * | 2021-05-12 | 2021-08-10 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
| CN113237789B (en) * | 2021-05-12 | 2023-07-28 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
| CN113267421A (en) * | 2021-06-29 | 2021-08-17 | 巴斯夫公司 | Method for determining noble metal content |
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Application publication date: 20140122 |