CN107099676A - A kind of method of platinum, palladium, rhodium iridium in small sulfonium ensaying separation and concentration Platinum in Ore race element - Google Patents
A kind of method of platinum, palladium, rhodium iridium in small sulfonium ensaying separation and concentration Platinum in Ore race element Download PDFInfo
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- CN107099676A CN107099676A CN201710337416.6A CN201710337416A CN107099676A CN 107099676 A CN107099676 A CN 107099676A CN 201710337416 A CN201710337416 A CN 201710337416A CN 107099676 A CN107099676 A CN 107099676A
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- sulfonium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
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- 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
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to element sepatation beneficiation technologies field in the test of noble metal pyrogenic process, ore, the method for disclosing platinum, palladium, rhodium iridium in a kind of small sulfonium ensaying separation and concentration Platinum in Ore race element, including：For non-sulfide ore, testing sample is weighed, nickel oxide, sodium carbonate, borax, glass dust, A, B, C is added, mixed；After high-temperature fusion, sulfonium button can be obtained；Sulfonium is buckled in hot water and soaks loose, hydrochloric acid is added and decomposes sulfonium button powder to solution clarification, carry out subsequent analysis；For sulphide ore, weigh testing sample, it is fired after, carry out dispensing enrichment by step one.The present invention by adjusting sulfonium preparative materials scheme, make the sulfonium button of acquisition through hot-water soak can weathering it is loose, without Mechanical Crushing, it is to avoid sample loss and sample pollute mutually so that measurement result more accurately and reliably, improves testing efficiency.
Description
Technical field
The invention belongs to element sepatation beneficiation technologies field in the test of noble metal pyrogenic process, ore, more particularly to a kind of small sulfonium
The method of platinum, palladium, rhodium iridium in ensaying separation and concentration Platinum in Ore race element.
Background technology
For the measure of platinum family element, separation and enrichment are extremely important.It is platinum family element Accurate Determining
Premise, it can not only make substantial amounts of matrix element and interference element and element sepatation, and be enriched with the platinum family element of trace,
So as to be conducive to determining.Assaying of firing method is the most effectual way of platinum family element separation and concentration, is also internationally recognized method.
Existing enrichment method (being typically according to GB/T17418.7-2010) can enter to the platinum, palladium, rhodium iridium in rock forming mineral
Row enrichment, but Mechanical Crushing need to be carried out mostly by the sulfonium button obtained after the enrichment of its proportion scheme, then carry out subsequent analysis survey
Trial work is made, and process is cumbersome, easily cause sulfonium button loss and sulfonium button between cross pollution.
The content of the invention
The problem of existing for prior art, the invention provides a kind of small sulfonium ensaying separation and concentration Platinum in Ore race element
The method of middle platinum, palladium, rhodium iridium.
The present invention is achieved in that a kind of side of platinum, palladium, rhodium iridium in small sulfonium ensaying separation and concentration Platinum in Ore race element
Method, it is characterised in that the method for platinum, palladium, rhodium iridium in the small sulfonium ensaying separation and concentration Platinum in Ore race element, including following step
Suddenly：
Step one, for non-sulfide ore, the testing sample that 5g~10.0g has been broken to 200 mesh is weighed, wide-mouth bottle is filled in tool
In, add 2.0g nickel oxide, 15g sodium carbonate, 15g boraxs, 10g glass dust, 4.5gA, 0.1g B, 1.5g C；Shake up, pour into resistance to
In fiery crucible, it is put into Muffle furnace and is incubated, then heating and heat preservation, crucible is taken out, melt is poured into swage, sulfonium is taken out after cooling
Button；It is put into beaker and adds hot water, as being boiled on electric hot plate, adds hydrochloric acid and decompose sulfonium button powder to solution clarification, after progress
Continuous analysis；
For sulphide ore, weigh and treat 5g~10.0g test sample product, pour into square porcelain boat, be placed in Muffle furnace, roasted by low temperature
Burn, take out after cooling by step one progress dispensing enrichment.
Further, for non-sulfide ore, the testing sample that 5g~10.0g has been broken to 200 mesh is weighed, it is wide in 200ml tool plugs
In mouth bottle, 2.0g nickel oxide, 15g sodium carbonate, 15g boraxs, 10g glass dust, 4.5gA, 0.1g B, 1.5g C are added.
Further, pour into fire-clay crucible, be put into have warmed up and be incubated half an hour into 850 DEG C of Muffle furnace, then be warming up to
1000 DEG C of insulation half an hour, take out crucible.
Further, melt is poured into swage, sulfonium button is taken out after cooling, be put into addition 100ml hot water in 400ml beakers,
It is completely loose as half an hour is boiled on electric hot plate, add 100ml hydrochloric acid and decompose sulfonium button powder to solution clarification, carry out follow-up
Analysis.
Further, the step 2, is specifically included：
For sulphide ore, the testing sample that 10.0g has been broken to 200 mesh is weighed, pours into square porcelain boat, is placed in Muffle furnace
In, rise to 680 DEG C by low temperature and be calcined 2 hours, take out after cooling by step one progress dispensing enrichment.
Advantages of the present invention and good effect are：
The present invention by adjusting sulfonium preparative materials scheme, make the sulfonium button of acquisition through hot-water soak can weathering it is loose, without
Mechanical Crushing, it is to avoid polluted mutually between the loss of sulfonium button and sulfonium button so that measurement result is more accurately and reliably, it is adaptable to batch sample
Product are tested, and testing efficiency can be made to improve 50%.
Brief description of the drawings
Fig. 1 is the method for platinum, palladium, rhodium iridium in small sulfonium ensaying separation and concentration Platinum in Ore race element provided in an embodiment of the present invention
Flow chart.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is described in detail below in conjunction with the accompanying drawings.
As shown in figure 1, platinum, palladium, rhodium iridium in small sulfonium ensaying separation and concentration Platinum in Ore race element provided in an embodiment of the present invention
Method, including：
S101:For non-sulfide ore, the testing sample that 5g~10.0g has been broken to 200 mesh is weighed, in 200lm tool plug wide-mouths
In bottles, 2.0g nickel oxide, 15g sodium carbonate, 15g boraxs, 10g glass dust, 4.5g " A ", 0.1g " B ", 1.5g " C " are added, is shaken up,
Pour into fire-clay crucible, be put into have warmed up and be incubated half an hour into 850 DEG C of Muffle furnace, then to be warming up to 1000 DEG C of insulations half small
When, crucible is taken out, melt is poured into swage, sulfonium button is taken out after cooling, is put into 400ml beakers and adds about 100ml hot water, extremely
Can be completely loose in boiling half an hour on electric hot plate, add 100ml hydrochloric acid and decompose sulfonium button powder to solution clarification, carry out follow-up
Analysis.
S102:For sulphide ore, the testing sample that 5g~10.0g has been broken to 200 mesh is weighed, pours into square porcelain boat, puts
In Muffle furnace, rise to 680 DEG C by low temperature and be calcined 2 hours, take out after cooling by S101 progress dispensing enrichments.
Wherein, A is that ferrous sulfide, B are that sulphur, C are wheat flour.
The application principle of the present invention is further described with reference to specific embodiment.
Embodiment 1：The separation and concentration of platinum, palladium, rhodium iridium is carried out to national standard material GBW07101 using the present invention program, will
Sample mixes with dispensing and shape such as button can must be obtained after high melt buckled in the sulfonium of steel grey；Sulfonium button is put into beaker, adds hot water
Slowly weathering is loose into powder afterwards；Heating boil after half an hour can weathering it is complete.
Experiment shows：Proportion scheme as given by the present invention carries out ensaying, and gained sulfonium button can use the direct weathering of hot water, no
Operating process must be reduced through crusher in crushing, improve production efficiency, it is to avoid loss and dirt during sample broke
Dye.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (5)
1. a kind of method of platinum, palladium, rhodium iridium in small sulfonium ensaying separation and concentration Platinum in Ore race element, it is characterised in that the small sulfonium
The method of platinum, palladium, rhodium iridium, comprises the following steps in ensaying separation and concentration Platinum in Ore race element：
Step one, for non-sulfide ore, 5g~10.0g testing samples are weighed, in tool plug wide-mouth bottle, addition 2.0g nickel oxide,
15g sodium carbonate, 15g boraxs, 10g glass dust, 4.5gA, 0.1g B, 1.5g C；Shake up, pour into fire-clay crucible, be put into Muffle
It is incubated in stove, then heating and heat preservation, crucible is taken out, melt is poured into swage, sulfonium button is taken out after cooling；It is put into beaker and adds heat
Water, as being boiled on electric hot plate, adds hydrochloric acid and decomposes sulfonium button powder to solution clarification, carry out subsequent analysis；
Step 2, for sulphide ore, weighs and treats 5g~10.0g test sample product, pour into square porcelain boat, be placed in Muffle furnace, by low
Temperature roasting, dispensing enrichment is carried out after taking-up cooling by step one.
2. the method for platinum, palladium, rhodium iridium, its feature in small sulfonium ensaying separation and concentration Platinum in Ore race element as claimed in claim 1
It is, for non-sulfide ore, weighs the testing sample that 5g~10.0g has been broken to 200 mesh, in 200ml tool plug wide-mouth bottles, adds
2.0g nickel oxide, 15g sodium carbonate, 15g boraxs, 10g glass dust, 4.5gA, 0.1g B, 1.5g C.
3. the method for platinum, palladium, rhodium iridium, its feature in small sulfonium ensaying separation and concentration Platinum in Ore race element as claimed in claim 1
It is, pours into fire-clay crucible, be put into have warmed up and be incubated half an hour into 850 DEG C of Muffle furnace, then is warming up to 1000 DEG C of insulations
Half an hour, take out crucible.
4. the method for platinum, palladium, rhodium iridium, its feature in small sulfonium ensaying separation and concentration Platinum in Ore race element as claimed in claim 1
It is, melt is poured into swage, sulfonium button is taken out after cooling, addition 100ml hot water in 400ml beakers is put into, as electric hot plate
On boil half an hour, it is completely loose, add 100ml hydrochloric acid and decompose sulfonium button powder to solution and clarify, carry out subsequent analysis.
5. the method for platinum, palladium, rhodium iridium, its feature in small sulfonium ensaying separation and concentration Platinum in Ore race element as claimed in claim 1
It is that the step 2 is specifically included：
For sulphide ore, the testing sample that 10.0g has been broken to 200 mesh is weighed, pours into square porcelain boat, is placed in Muffle furnace, by
Low temperature rises to 680 DEG C and is calcined 2 hours, takes out after cooling by step one progress dispensing enrichment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710337416.6A CN107099676A (en) | 2017-05-15 | 2017-05-15 | A kind of method of platinum, palladium, rhodium iridium in small sulfonium ensaying separation and concentration Platinum in Ore race element |
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| CN201710337416.6A CN107099676A (en) | 2017-05-15 | 2017-05-15 | A kind of method of platinum, palladium, rhodium iridium in small sulfonium ensaying separation and concentration Platinum in Ore race element |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110983028A (en) * | 2019-11-21 | 2020-04-10 | 云龙县铂翠贵金属科技有限公司 | Method for recovering platinum group metal from automobile exhaust purification waste catalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102706860A (en) * | 2012-06-29 | 2012-10-03 | 广州有色金属研究院 | Chemical analysis method of rhodium content |
| CN103940805A (en) * | 2014-04-16 | 2014-07-23 | 万宝矿产有限公司 | Method for determining precious metal in platinum-palladium ores |
| CN105954264A (en) * | 2016-07-07 | 2016-09-21 | 长春黄金研究院 | Method for determining contents of platinum and palladium in gold ore |
-
2017
- 2017-05-15 CN CN201710337416.6A patent/CN107099676A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102706860A (en) * | 2012-06-29 | 2012-10-03 | 广州有色金属研究院 | Chemical analysis method of rhodium content |
| CN103940805A (en) * | 2014-04-16 | 2014-07-23 | 万宝矿产有限公司 | Method for determining precious metal in platinum-palladium ores |
| CN105954264A (en) * | 2016-07-07 | 2016-09-21 | 长春黄金研究院 | Method for determining contents of platinum and palladium in gold ore |
Non-Patent Citations (2)
| Title |
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| 李刚等: ""镍锍试金富集-中子活化分析测定地质样品中的铂族元素"", 《河南化工》 * |
| 武汉地质学院等编著: "《岩石矿物分析教程》", 30 July 1980, 地质出版社出版 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110983028A (en) * | 2019-11-21 | 2020-04-10 | 云龙县铂翠贵金属科技有限公司 | Method for recovering platinum group metal from automobile exhaust purification waste catalyst |
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Application publication date: 20170829 |