CN115420585A - Digestion method suitable for accurate analysis of trace elements in sulfide minerals - Google Patents
Digestion method suitable for accurate analysis of trace elements in sulfide minerals Download PDFInfo
- Publication number
- CN115420585A CN115420585A CN202211028427.3A CN202211028427A CN115420585A CN 115420585 A CN115420585 A CN 115420585A CN 202211028427 A CN202211028427 A CN 202211028427A CN 115420585 A CN115420585 A CN 115420585A
- Authority
- CN
- China
- Prior art keywords
- digestion tank
- sulfide minerals
- digestion
- hydrochloric acid
- sulfide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
Landscapes
- 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)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a digestion method suitable for accurately analyzing trace elements of sulfide minerals, and relates to the technical field of chemical industry. The digestion method suitable for accurately analyzing the trace elements of the sulfide minerals comprises the following steps of: crushing sulfide ores and then selecting materials according to the volume; step two, adding hydrochloric acid to carry out primary acid washing to dissolve most of soluble substances in the sulfide minerals; removing sulfur elementary substance generated in the reaction process of the hydrochloric acid and the sample and substances which cannot react with the hydrochloric acid; and step four, carrying out element analysis on the digested mineral solution. By adding hydrochloric acid and nitric acid, the phenomenon that a sulfur simple substance is separated out to wrap a mineral sample to influence subsequent reaction when the nitric acid reacts with the sulfurized mineral is avoided, so that the digestion rate of the sulfurized mineral is improved, meanwhile, concentrated nitric acid is added and heated to dissolve the sulfur simple substance originally existing in the sulfurized mineral, and residual chloride ions in the previous reaction can be removed to avoid influencing the analysis result of the subsequent sample.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a digestion method suitable for accurately analyzing trace elements of sulfide minerals.
Background
The abundance of mineral trace elements in the sulfide is an important characteristic for reflecting material evolution information at different diagenesis and mineralization stages, and is important support data for researching diagenesis conditions, diagenesis mechanisms and diagenesis models, and the trace elements of the sulfide imply geological, geochemistry, thermodynamics and other information in the formation process of submarine hydrothermal activity, so that the research on the trace element characteristics of sulfide minerals is also an important link in the exploration work of metal deposit resources.
At present, the sulfide minerals are generally required to be digested before the sulfide mineral element analysis is carried out, but the digestion of the sulfide minerals cannot guarantee the accurate analysis of trace elements at present, and further cannot meet the data support requirements of researches such as mining conditions and the like of sulfide mineral trace element characteristics and metal deposit resource exploration, so that a digestion method suitable for the sulfide minerals is urgently needed to ensure the reliability of trace element analysis results, and further the deep research and resource exploration work of metal resources is promoted.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a digestion method suitable for accurately analyzing trace elements of sulfide minerals, and solves the problem that solid impurities remain in a solution when the sulfide minerals are digested at present.
(II) technical scheme
In order to realize the purpose, the invention is realized by the following technical scheme: a digestion method suitable for accurately analyzing trace elements of sulfide minerals comprises the following steps:
crushing sulfide ores and then selecting materials according to the volume;
step two, adding hydrochloric acid to carry out primary acid washing to dissolve most of soluble substances in the sulfide minerals;
removing sulfur elementary substance generated in the reaction process of the hydrochloric acid and the sample and substances which cannot react with the hydrochloric acid;
and step four, performing element analysis on the digested mineral solution.
Preferably, the first step is specifically: selecting the sulfide minerals to be detected, putting the sulfide minerals into a vertical mill, crushing the sulfide minerals through the vertical mill, selecting 50-60mg of the sulfide minerals with the particle size of less than 70 mu m in the crushed minerals as raw materials by using a high-efficiency powder concentrator integrated with the vertical mill, and putting the raw materials into a digestion tank prepared in advance.
Preferably, the second step is specifically: after the digestion tank is moved to a ventilation position, 3ml of hydrochloric acid with the concentration of 10% is added into the digestion tank, and the interior of the digestion tank is stirred to enable the hydrochloric acid and the mineral sample to be fully mixed so as to enable the minerals in the digestion tank to be initially dissolved.
Preferably, the reaction process after the hydrochloric acid is added in the second step can generate toxic and malodorous gaseous hydrogen sulfide, and operators need to protect the mouth and eyes and be in a downwind position to avoid poisoning.
Preferably, the third step is specifically: adding 1ml of concentrated nitric acid with the concentration of 68% into the digestion tank, putting the digestion tank into an oven, heating to 150 ℃, keeping the temperature for 20min, adding 2mg of barium chloride into the digestion tank, stirring the digestion tank for 3-5min, standing for 5min, and taking out solid impurities in the digestion tank.
Preferably, the third step is followed by: and (3) observing whether solid impurities still exist in the digestion tank, if so, preparing aqua regia, adding 1ml of aqua regia into the digestion tank to dissolve gold existing in the solution, then adding 3ml of nitric acid with the concentration of 5% into the digestion tank, and standing the digestion tank for 1-2 hours.
Preferably, the step four specifically comprises: and (4) putting the digested mineral solution into a polytetrafluoroethylene plastic bottle, and analyzing the digested sample by using inductively coupled plasma mass spectrometry.
(III) advantageous effects
The invention provides a digestion method suitable for accurately analyzing trace elements of sulfide minerals. The method has the following beneficial effects:
according to the invention, hydrochloric acid is added firstly, and then nitric acid is added, so that the phenomenon that a large amount of sulfur elementary substance is separated out to wrap a mineral sample to influence the subsequent reaction when the nitric acid reacts with the sulfurized mineral is avoided, the digestion rate of the sulfurized mineral is improved, meanwhile, concentrated nitric acid is added and heated to dissolve the sulfur elementary substance originally existing in the sulfurized mineral, and chloride ions remained in the previous reaction can be removed to avoid influencing the analysis result of the subsequent sample.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides a digestion method suitable for accurately analyzing trace elements of sulfide minerals, which comprises the following steps:
firstly, selecting materials according to the volume after crushing sulfide ores;
secondly, adding hydrochloric acid to carry out primary acid washing to dissolve most of soluble substances in the sulfide minerals;
removing sulfur elementary substance generated in the reaction process of the hydrochloric acid and the sample and substances which cannot react with the hydrochloric acid;
and step four, carrying out element analysis on the digested mineral solution.
The first step is specifically as follows: selecting a sulfide mineral to be detected, putting the sulfide mineral into a vertical mill, crushing the sulfide mineral through the vertical mill, selecting 50-60mg of the sulfide mineral with the particle size of less than 70 mu m in the crushed mineral as a raw material by using an efficient powder concentrator integrated with the vertical mill, and putting the raw material into a digestion tank prepared in advance.
The particle size of the sulphide mineral is controlled to increase the contact area of the same mass of sulphide mineral and the digestion reagent as much as possible, thereby accelerating the digestion rate of the sulphide mineral.
The second step is specifically as follows: after the digestion tank is moved to a ventilation position, 3ml of hydrochloric acid with the concentration of 10% is added into the digestion tank, and the interior of the digestion tank is stirred to enable the hydrochloric acid and the mineral sample to be fully mixed so as to enable the minerals in the digestion tank to be initially dissolved.
Most of metal substances in the sulfide minerals are dissolved into solution with chloride ions as anions by adding hydrochloric acid, and substances which do not react with the hydrochloric acid are precipitated at the lower side in the solution.
In the second step, toxic and malodorous gaseous hydrogen sulfide is generated in the reaction process after the hydrochloric acid is added, and operators need to well protect the mouth and eyes and keep the mouth and eyes at a leeward position to avoid poisoning.
The hydrogen sulfide is a highly toxic gas, and high-concentration hydrogen sulfide can cause death when being inhaled by a human body seriously.
The third step is specifically as follows: adding 1ml of concentrated nitric acid with the concentration of 68% into the digestion tank, putting the digestion tank into an oven, heating to 150 ℃, keeping the temperature for 20min, adding 2mg of barium chloride into the digestion tank, stirring the digestion tank for 3-5min, standing for 5min, and taking out solid impurities in the digestion tank.
Concentrated nitric acid can react with sulfur simple substance under the condition of heating to generate nitrogen peroxide, sulfuric acid and water, and barium chloride is added to react with sulfuric acid to generate barium sulfate, so that sulfate ions in the solution are replaced.
The third step is as follows: and (3) observing whether solid impurities still exist in the digestion tank, if so, preparing aqua regia, adding 1ml of aqua regia into the digestion tank to dissolve gold existing in the solution, then adding 3ml of nitric acid with the concentration of 5% into the digestion tank, and standing the digestion tank for 1-2h.
The aqua regia is obtained by uniformly mixing concentrated hydrochloric acid and concentrated nitric acid 3
The fourth step is specifically as follows: and (4) putting the digested mineral solution into a polytetrafluoroethylene plastic bottle, and analyzing the digested sample by using inductively coupled plasma mass spectrometry.
The second embodiment:
the embodiment of the invention provides a digestion method suitable for accurately analyzing trace elements of sulfide minerals, which comprises the following steps:
crushing sulfide ores and then selecting materials according to the volume;
step two, adding hydrochloric acid to carry out primary acid washing to dissolve most of soluble substances in the sulfide minerals;
removing sulfur elementary substance generated in the reaction process of the hydrochloric acid and the sample and substances which cannot react with the hydrochloric acid;
and step four, performing element analysis on the digested mineral solution.
The first step is specifically as follows: selecting the sulfide minerals to be detected, putting the sulfide minerals into a vertical mill, crushing the sulfide minerals through the vertical mill, selecting 55mg of the sulfide minerals with the particle size of less than 70 mu m in the crushed minerals as raw materials by using a high-efficiency powder concentrator integrated with the vertical mill, and putting the raw materials into a digestion tank prepared in advance.
The particle size of the sulfide mineral is controlled to increase the contact area of the same mass of sulfide mineral and the digestion reagent as much as possible, so that the digestion rate is accelerated.
The second step is specifically as follows: after the digestion tank is moved to the ventilation position, 3ml of hydrochloric acid with the concentration of 8% is added into the digestion tank, and the digestion tank is stirred so that the hydrochloric acid and the mineral sample are fully mixed to enable the minerals in the digestion tank to be initially dissolved.
Most of metal substances in the sulfide minerals are dissolved into solution with chloride ions as anions by adding hydrochloric acid, and substances which do not react with the hydrochloric acid are precipitated at the lower side in the solution.
In the second step, toxic and malodorous gaseous hydrogen sulfide is generated in the reaction process after the hydrochloric acid is added, and operators need to well protect the mouth and eyes and keep the mouth and eyes at a leeward position to avoid poisoning.
The hydrogen sulfide is a highly toxic gas, and the high-concentration hydrogen sulfide can cause death when being inhaled by a human body seriously.
The third step is specifically as follows: adding concentrated nitric acid 1ml with concentration of 68% into the digestion tank, placing the digestion tank into an oven, heating to 150 deg.C, maintaining for 20min, adding barium chloride 2mg into the digestion tank, stirring for 4min, standing for 5min, and taking out solid impurities.
Concentrated nitric acid can react with sulfur simple substance under the condition of heating to generate nitrogen peroxide, sulfuric acid and water, and barium chloride is added to react with sulfuric acid to generate barium sulfate, so that sulfate ions in the solution are replaced.
The third step is followed by: and (3) observing whether solid impurities still exist in the digestion tank, if so, preparing aqua regia, adding 1ml of aqua regia into the digestion tank to dissolve gold existing in the solution, then adding 3ml of nitric acid with the concentration of 5% into the digestion tank, and standing the digestion tank for 1-2 hours.
The aqua regia is obtained by uniformly mixing concentrated hydrochloric acid and concentrated nitric acid 3.
The fourth step is specifically as follows: and (4) putting the digested mineral solution into a polytetrafluoroethylene plastic bottle, and analyzing the digested sample by using inductively coupled plasma mass spectrometry.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A digestion method suitable for accurately analyzing trace elements of sulfide minerals is characterized by comprising the following steps: the method comprises the following steps:
crushing sulfide ores and then selecting materials according to the volume;
step two, adding hydrochloric acid to carry out primary acid washing to dissolve most of soluble substances in the sulfide minerals;
removing sulfur elementary substance generated in the reaction process of the hydrochloric acid and the sample and substances which cannot react with the hydrochloric acid;
and step four, carrying out element analysis on the digested mineral solution.
2. The digestion method suitable for accurate analysis of trace elements in sulfide minerals according to claim 1, which is characterized by comprising the following steps: the first step is specifically as follows: selecting the sulfide minerals to be detected, putting the sulfide minerals into a vertical mill, crushing the sulfide minerals through the vertical mill, selecting 50-60mg of the sulfide minerals with the particle size of less than 70 mu m in the crushed minerals as raw materials by using a high-efficiency powder concentrator integrated with the vertical mill, and putting the raw materials into a digestion tank prepared in advance.
3. The digestion method suitable for accurate analysis of trace elements of sulfide minerals according to claim 1, characterized in that: the second step is specifically as follows: after the digestion tank is moved to a ventilation position, 3ml of hydrochloric acid with the concentration of 10% is added into the digestion tank, and the interior of the digestion tank is stirred to enable the hydrochloric acid and the mineral sample to be fully mixed so as to enable the minerals in the digestion tank to be initially dissolved.
4. The digestion method suitable for accurate analysis of trace elements of sulfide minerals according to claim 1, characterized in that: in the second step, toxic and malodorous gaseous hydrogen sulfide is generated in the reaction process after the hydrochloric acid is added, and operators need to well protect the mouth and eyes and keep the mouth and eyes at a leeward position to avoid poisoning.
5. The digestion method suitable for accurate analysis of trace elements of sulfide minerals according to claim 1, characterized in that: the third step is specifically as follows: adding 1ml of concentrated nitric acid with the concentration of 68% into the digestion tank, putting the digestion tank into an oven, heating to 150 ℃, keeping the temperature for 20min, adding 2mg of barium chloride into the digestion tank, stirring the digestion tank for 3-5min, standing for 5min, and taking out solid impurities in the digestion tank.
6. The digestion method suitable for accurate analysis of trace elements in sulfide minerals according to claim 1, which is characterized by comprising the following steps: the third step is followed by: and (3) observing whether solid impurities still exist in the digestion tank, if so, preparing aqua regia, adding 1ml of aqua regia into the digestion tank to dissolve gold existing in the solution, then adding 3ml of nitric acid with the concentration of 5% into the digestion tank, and standing the digestion tank for 1-2h.
7. The digestion method suitable for accurate analysis of trace elements of sulfide minerals according to claim 1, characterized in that: the fourth step is specifically as follows: and (4) putting the digested mineral solution into a polytetrafluoroethylene plastic bottle, and analyzing the digested sample by using inductively coupled plasma mass spectrometry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211028427.3A CN115420585A (en) | 2022-08-25 | 2022-08-25 | Digestion method suitable for accurate analysis of trace elements in sulfide minerals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211028427.3A CN115420585A (en) | 2022-08-25 | 2022-08-25 | Digestion method suitable for accurate analysis of trace elements in sulfide minerals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115420585A true CN115420585A (en) | 2022-12-02 |
Family
ID=84199851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211028427.3A Pending CN115420585A (en) | 2022-08-25 | 2022-08-25 | Digestion method suitable for accurate analysis of trace elements in sulfide minerals |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115420585A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116754349A (en) * | 2023-08-16 | 2023-09-15 | 四川赛科检测技术有限公司 | ICP-OES-based digestion method for lithium sulfide impurity elements and content determination method thereof |
-
2022
- 2022-08-25 CN CN202211028427.3A patent/CN115420585A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116754349A (en) * | 2023-08-16 | 2023-09-15 | 四川赛科检测技术有限公司 | ICP-OES-based digestion method for lithium sulfide impurity elements and content determination method thereof |
| CN116754349B (en) * | 2023-08-16 | 2023-11-21 | 四川赛科检测技术有限公司 | ICP-OES-based digestion method for lithium sulfide impurity elements and content determination method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| AU2012297534B2 (en) | Process of leaching precious metals | |
| Abbruzzese et al. | Thiosulphate leaching for gold hydrometallurgy | |
| Whitehead et al. | Application of 1-alkyl-3-methyl-imidazolium ionic liquids in the oxidative leaching of sulphidic copper, gold and silver ores | |
| Ubaldini et al. | Process flow-sheet for gold and antimony recovery from stibnite | |
| Crundwell et al. | A mathematical model of the leaching of gold in cyanide solutions | |
| Yang et al. | Study on oxygen pressure thiosulfate leaching of gold without the catalysis of copper and ammonia | |
| Nogueira et al. | Selective process of zinc extraction from spent Zn–MnO2 batteries by ammonium chloride leaching | |
| Melashvili et al. | Dissolution of gold during pyrite oxidation reaction | |
| CN115420585A (en) | Digestion method suitable for accurate analysis of trace elements in sulfide minerals | |
| Wang et al. | Leaching of gold from a free milling gold ore in copper-citrate-thiosulfate solutions at elevated temperatures | |
| Tuncuk | Lab scale optimization and two-step sequential bench scale reactor leaching tests for the chemical dissolution of Cu, Au & Ag from waste electrical and electronic equipment (WEEE) | |
| Heidel et al. | Galena oxidation investigations on oxygen and sulphur isotopes | |
| Zhang et al. | Effect of pH on desulphurization of spent lead paste via hydrometallurgical process | |
| Rao et al. | A new look at characterisation and oxidative ammonia leaching behaviour of multimetal sulphides | |
| CN109055760A (en) | A kind of method of the high arsenic germanium material Ti recovery of high zinc | |
| Teimouri et al. | Using experimental design and response surface methodology (RSM) to optimize gold extraction from refractory sulphidic gold tailings with ionic liquids | |
| Ni et al. | Simultaneous determination of ultra-trace Pt, Pd, Rh and Ir in geochemical samples by inductively coupled plasma mass spectrometry following tin fire assay preconcentration and microwave digestion | |
| CN110408786A (en) | A kind of method that the catalysis of electrolytic manganese anode slag prepares manganese sulfate solution and recycles lead | |
| AU2011360586A1 (en) | Energy efficient recovery of precious metals and base metals | |
| Gajam et al. | A kinetic study of enargite dissolution in ammoniacal solutions | |
| Kursunoglu et al. | Recovery of manganese from spent batteries using guar meal as a reducing agent in a sulfuric acid medium | |
| Fisher et al. | Comparison of chalcocite dissolution in the oxygenated, aqueous sulfate and chloride systems | |
| Lehmann et al. | A comparative study of the dissolution of hexagonal and monoclinic pyrrhotites in cyanide solution | |
| Porvali et al. | Thiosulfate-copper-ammonia leaching of pure gold and pressure oxidized concentrate | |
| Zandevakili et al. | Leaching optimization of Sarcheshmeh copper concentrate by application of Taguchi experimental design method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |