CN109142018A - A kind of method of the quick measurement containing rhodium content in rhodium material - Google Patents

A kind of method of the quick measurement containing rhodium content in rhodium material Download PDF

Info

Publication number
CN109142018A
CN109142018A CN201810765344.XA CN201810765344A CN109142018A CN 109142018 A CN109142018 A CN 109142018A CN 201810765344 A CN201810765344 A CN 201810765344A CN 109142018 A CN109142018 A CN 109142018A
Authority
CN
China
Prior art keywords
rhodium
content
rhodium material
cooled
measurement
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
Application number
CN201810765344.XA
Other languages
Chinese (zh)
Inventor
郭振中
徐涛
李小婷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KUNSHAN HONGFUTAI ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
Original Assignee
KUNSHAN HONGFUTAI ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by KUNSHAN HONGFUTAI ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd filed Critical KUNSHAN HONGFUTAI ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
Priority to CN201810765344.XA priority Critical patent/CN109142018A/en
Publication of CN109142018A publication Critical patent/CN109142018A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/42Low-temperature sample treatment, e.g. cryofixation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/73Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches

Landscapes

  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Immunology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The present invention provides a kind of quickly method of the measurement containing rhodium content in rhodium material, the following steps are included: by after tentatively the crushing and grind containing rhodium material of embrittlement processing, activated metal is added, is put into porcelain crucible after mixing evenly, then covers sodium chloride on surface, it is cooled to room temperature after roasting, it is transferred in beaker, chloroazotic acid is slowly added in beaker, after heating for dissolving, it is cooled to room temperature, obtains rhodium-containing liquid;By rhodium-containing liquid after being filtered, washed, filtrate constant volume obtains the content containing rhodium in rhodium material according to formula rhodium-containing liquid volume V × rhodium concentration C/M*1000 containing rhodium material with the concentration of rhodium in ICP inductive coupling plasma emission spectrograph analysis rhodium-containing liquid.The present invention forms alloy by that will contain rhodium material and zinc activated metal powder, after directly being dissolved with chloroazotic acid, it is obtained using ICP inductive coupling plasma emission spectrograph measure and calculation containing rhodium content in rhodium material, preparation method is simple, controllability is strong, interference is few, measures precise and high efficiency, sensitivity and favorable reproducibility.

Description

A kind of method of the quick measurement containing rhodium content in rhodium material
Technical field
The invention belongs to rhodium determination techniques fields, and in particular to a method of quickly measurement is containing rhodium content in rhodium material.
Background technique
Rhodium element belongs to platinum group, and yield is very rare, only takes up an area mass fraction in shell 0.0000000001%, rhodium material is from a wealth of sources, and broad categories mostly exist with alloy form, and the performance of rhodium is very excellent, has Stable resistance and good conductive, thermally conductive, acid-alkali-corrosive-resisting, high-temperature oxidation resistance and high catalytic activity, automotive electronics, The fields such as aerospace, medical and health are all widely used.
Rhodium has chemical inertness, and the solubility in chloroazotic acid is extremely low, is that measurement, recycling, separation and the purifying technique of rhodium increase Difficulty is added.The dissolving method of rhodium mainly has medium temperature chlorinating dissolution method, hot pressing dissolution method, electrochemical solution, microwave to disappear at present Solution, alloy activation dissolution method and sodium bisulfate/potassium-diluted acid dissolution method etc., wherein the application of alloy activation dissolution method is more wide It is general.Alloy activation dissolution is to melt the metals such as aluminium, iron, zinc, tin and noble metal at high temperature to form alloy or intermetallic Object removes base metal with diluted acid, then obtains precious metal solution with strong oxidizing property acid dissolution, then by analysis method or extract work Skill is measured precious metal solution or purifies.
The disclosed method that Purification of Platinum rhodium is recycled from the waste material of platiniferous rhodium of Chinese patent CN 101260469A, by platinum rhodium After waste material carries out pulverization process, with zinc powder Hybrid Heating, chloroazotic acid is added in the congruent melting at 800 DEG C after cooling, heating is boiled to complete It melts, after small fire is evaporated solution, concentrated hydrochloric acid dissolution is added, is evaporated again, continuous 3 times, until catching up with nitre complete, after obtaining pre-treatment Solution, then will in the solution after pre-treatment be added sodium hydroxide solution adjust pH value to 1.5-3.5, be handed over through strong acidic ion Resin column is changed, the base metal in solution is removed, the solution for removing base metal is subjected to three-level extraction with tributyl phosphate, is contained There is the pure extraction raffinate of rhodium, sodium hypochlorite/hydrogen peroxide oxidant will finally be added in the pure extraction raffinate containing rhodium, heated oxide removes iridium, Processing is further purified through extration resin again, obtains pure rhodium liquid, formic acid/hydrazine hydrate finally is added also into pure rhodium liquid Former agent, heating reduction, forms rhodium black, adds hydrogen heating reduction, obtains pure rhodium powder.One disclosed in Chinese patent 106011495A The melting method of kind rhodium powder, after rhodium powder is mixed with metal powder, ball-milling treatment carries out mechanical activation, is then dissolved out using hydrochloric acid Base metal obtains rhodium material after separation of solid and liquid, then rhodium material is placed in ultrasonic wave, melts, obtains through chloroazotic acid at 80-90 DEG C To rhodium liquid.By above-mentioned in the prior art it is found that the crystallization of rhodium can be reduced by handling rhodium powder and activated metal powder metallurgyization Degree and intermolecular combination energy, enhance the reactivity of rhodium, improve by the rate of acid leach solution, but will close at present Golden activation method is for inductive coupling plasma emission spectrograph measurement rhodium content using actually rare.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of quickly method of the measurement containing rhodium content in rhodium material, pass through by Alloy is formed containing rhodium material and zinc activated metal powder, after directly being dissolved with chloroazotic acid, is emitted using ICP inductively coupled plasma body Spectrometer measure and calculation is obtained containing rhodium content in rhodium material, and preparation method is simple, and controllability is strong, and interference is few, is measured accurate high Effect, sensitivity and favorable reproducibility.
In order to solve the above technical problems, the technical scheme is that
A kind of method of the quick measurement containing rhodium content in rhodium material, it is characterised in that: the following steps are included:
(1) rhodium material will be contained and carry out brittle processing, obtain embrittlement processing contains rhodium material;
(2) tentatively crushing containing rhodium material by the embrittlement processing of step (1) preparation, after the grinding of the grinder of 200 mesh, according to work Property metal powder and the weight ratio containing rhodium material be 2-4:1, be added 150 mesh active metal powder, stirred evenly with glass bar After be put into porcelain crucible, then surface cover one layer of sodium chloride, at 600-700 DEG C roast 2-3h after be cooled to room temperature, obtain Contain rhodium material after roasting;
(3) by being added in beaker containing rhodium material after the roasting of step (2) preparation, chloroazotic acid is slowly added in beaker, is heated molten Xie Hou is cooled to room temperature, and obtains rhodium-containing liquid;
(4) by the rhodium-containing liquid of step (3) preparation after being filtered, washed, filtrate constant volume is sent out with ICP inductively coupled plasma body The concentration for penetrating rhodium in spectrometer analysis rhodium-containing liquid, according to formula rhodium-containing liquid volume V × rhodium concentration C/M* containing rhodium material 1000 obtain the content containing rhodium in rhodium material.
As a preferred embodiment of the above technical solution, in the step (1), the technique of embrittlement processing are as follows: will contain rhodium material 0 ~- 120 DEG C are low-temperature grinding 5-15min under 0.02-0.1MPa with pressure.
As a preferred embodiment of the above technical solution, in the step (1), the technique of embrittlement processing are as follows: rhodium material will be contained from room Temperature drop pre-processes 2-10min to 0 ~ -5 DEG C at pressure 0.02-0.04MPa, be then cooled to the rate of 5-10 DEG C/min - 40 ~ -80 DEG C, 2-4min is pre-processed at pressure 0.03-0.05MPa, finally -60 are cooled to the rate of 10-13 DEG C/min ~ - 120 DEG C, 1-11min is pre-processed at pressure 0.08-0.1MPa.
As a preferred embodiment of the above technical solution, in the step (2), active metal powder is zinc powder, aluminium powder or glass putty One of or it is several, active metal powder and embrittlement processing the weight ratio containing rhodium material be 3:1.
As a preferred embodiment of the above technical solution, in the step (2), cover one layer of sodium chloride with a thickness of 1-2mm, chlorination Sodium is the sodium chloride powder that purity is 99.5%.
As a preferred embodiment of the above technical solution, in the step (2), the temperature of roasting is 650 DEG C, time 2h.
As a preferred embodiment of the above technical solution, in the step (3), chloroazotic acid include volume ratio be 1:3 31% hydrochloric acid and 65% nitric acid, chloroazotic acid and material ratio containing rhodium material are 8-10L:1kg.
As a preferred embodiment of the above technical solution, in the step (3), the rate being slowly added to is 5-20mL/min, heating Temperature be 60 DEG C, time 15min.
As a preferred embodiment of the above technical solution, in the step (3), the technique of washing are as follows: solvent is pure water, pH value 6- 7, it washs 2-3 times.
As a preferred embodiment of the above technical solution, in the step (3), in ICP inductive coupling plasma emission spectrograph The concentration of rhodium standard reserving solution is 1mg/mL, location parameter are as follows: wavelength 343.489nm.
Compared with prior art, the invention has the following advantages:
(1) quick method of the measurement containing rhodium content in rhodium material of the invention is that brittle pretreatment is carried out by the material to rhodium-containing Being handled respectively by low temperature declines the binding force between the component in the material of rhodium-containing, crystallinity decline, reduces preliminary crisp The difficulty for changing processing and grinding, the powder after making grinding is finer and smoother, the abundant alloy of activated metal after being more advantageous to, to mention The rate of dissolution and dissolution rate of high chloroazotic acid then ensure that the stability and repeatability of measuring method.
(2) quick method of the measurement containing rhodium content in rhodium material of the invention is by the way that activated metal is added, and sodium chloride is close Envelope, prevents during heating, and activated metal and rhodium absorb the dioxygen oxidation in air, influences the content of rhodium measurement, then Through high-temperature fusion, so that activated metal and rhodium is formed alloy, improve solubility of the rhodium in chloroazotic acid, avoid and use other solvents Or technique, process flow is simplified, and after directly dissolving alloy with chloroazotic acid, is directly sent out using ICP inductively coupled plasma body The concentration of rhodium in spectrometer analysis rhodium-containing liquid is penetrated, so that the content containing rhodium in rhodium material be calculated.
(3) preparation method of the invention is compared with rhodium solution prepared by traditional hydrochloric acid/sulfuric acid and peroxide, in solution Rhodium content stablize, rhodium-containing liquid washs through pure water, distilled water and sterile water in batches respectively, and content is pure, hardly by artificial The influence of factor is not also influenced by the noble metals such as other palladiums in material, ensure that the accurate fixed of measurement, and by metal activation with ICP inductive coupling plasma emission spectrograph combines, and preparation method is simple and efficient, and ICP inductively coupled plasma body is sent out It penetrates before spectrometer measurement, with pure water, the rhodium-containing liquid in impurity is sufficiently filtered into liquid, reduce mistake, Cause content relatively low, therefore good via the stability of the rhodium content of ICP inductive coupling plasma emission spectrograph measurement, speed Fastly, controllability is strong, and the interference by human factor and external environment is few, and measurement is sensitive containing rhodium content precise and high efficiency in rhodium material Property and favorable reproducibility.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1:
(1) rhodium material will be contained and is down to 0 DEG C from room temperature, 2min is pre-processed at pressure 0.02MPa, then with the rate of 5 DEG C/min - 40 DEG C are cooled to, 2min is pre-processed at pressure 0.03MPa, finally -60 DEG C are cooled to the rate of 10 DEG C/min, in pressure 1min is pre-processed under 0.08MPa.
By tentatively crushing containing rhodium material for embrittlement processing, after the grinding of the grinder of 200 mesh, according to zinc powder and contain rhodium material Weight ratio be 2:1, be added 150 mesh zinc powder, be put into porcelain crucible after mixing evenly with glass bar, then surface cover one layer With a thickness of 99.5% sodium chloride powder of 1mm, it is cooled to room temperature after roasting 2h at 600 DEG C, the rhodium-containing object after being roasted Material.
It (2) is 8L:1kg according to chloroazotic acid and material ratio containing rhodium material, by body by being added in beaker containing rhodium material after roasting The chloroazotic acid that 31% hydrochloric acid and 65% nitric acid that product ratio is 1:3 are constituted under 5mL/min rate to be slowly added in beaker, at 60 DEG C After dissolving by heating 15min, it is cooled to room temperature, obtains rhodium-containing liquid.
(3) by rhodium-containing liquid through filtering, with pure water 2 times that pH value is 6.4, filtrate constant volume, with ICP inductive coupling etc. Ionomer emission spectrum instrument analyzes the concentration of rhodium in rhodium-containing liquid, test parameter are as follows: wavelength 343.489nm, finally according to public affairs Formula rhodium-containing liquid volume V × rhodium concentration C/M*1000 containing rhodium material obtains the content containing rhodium in rhodium material.
Embodiment 2:
(1) rhodium material will be contained and is down to -5 DEG C from room temperature, 10min is pre-processed at pressure -0.04MPa, then with 10 DEG C/min's Rate is cooled to -80 DEG C, and 4min is pre-processed at pressure 0.05MPa, is finally cooled to -120 DEG C with the rate of 13 DEG C/min, 1min is pre-processed under pressure 0.1MPa.
By tentatively crushing containing rhodium material for embrittlement processing, after the grinding of the grinder of 200 mesh, according to zinc powder and contain rhodium material Weight ratio be 4:1, be added 150 mesh zinc powder, be put into porcelain crucible after mixing evenly with glass bar, then surface cover one layer With a thickness of 99.5% sodium chloride powder of 2mm, it is cooled to room temperature after roasting 3h at 700 DEG C, the rhodium-containing object after being roasted Material.
It (2) is 10L:1kg according to chloroazotic acid and material ratio containing rhodium material by being added in beaker containing rhodium material after roasting, it will The chloroazotic acid that 31% hydrochloric acid and 65% nitric acid that volume ratio is 1:3 are constituted under 20mL/min rate to be slowly added in beaker, 60 After dissolving by heating 15min at DEG C, it is cooled to room temperature, obtains rhodium-containing liquid.
(3) by rhodium-containing liquid through filtering, with pure water 3 times that pH value is 6.9, filtrate constant volume, with ICP inductive coupling etc. Ionomer emission spectrum instrument analyzes the concentration of rhodium in rhodium-containing liquid, test parameter are as follows: wavelength 343.489nm, finally according to public affairs Formula rhodium-containing liquid volume V × rhodium concentration C/M*1000 containing rhodium material obtains the content containing rhodium in rhodium material.
Embodiment 3:
(1) rhodium material will be contained and is down to -2 DEG C from room temperature, 8min is pre-processed at pressure 0.03MPa, then with the rate of 7 DEG C/min - 60 DEG C are cooled to, 4min is pre-processed at pressure 0.04MPa, finally -100 DEG C are cooled to the rate of 12 DEG C/min, in pressure 2min is pre-processed under 0.09MPa.
By tentatively crushing containing rhodium material for embrittlement processing, after the grinding of the grinder of 200 mesh, according to zinc powder and contain rhodium material Weight ratio be 3:1, be added 150 mesh zinc powder, be put into porcelain crucible after mixing evenly with glass bar, then surface cover one layer With a thickness of 99.5% sodium chloride powder of 1.5mm, it is cooled to room temperature after roasting 2.5h at 650 DEG C, the rhodium-containing after being roasted Material.
It (2) is 9L:1kg according to chloroazotic acid and material ratio containing rhodium material, by body by being added in beaker containing rhodium material after roasting The chloroazotic acid that 31% hydrochloric acid and 65% nitric acid that product ratio is 1:3 are constituted under 10mL/min rate to be slowly added in beaker, at 60 DEG C After lower heating for dissolving 15min, it is cooled to room temperature, obtains rhodium-containing liquid.
(3) by rhodium-containing liquid through filtering, with pure water 3 times that pH value is 6.5, filtrate constant volume, with ICP inductive coupling etc. Ionomer emission spectrum instrument analyzes the concentration of rhodium in rhodium-containing liquid, test parameter are as follows: wavelength 343.489nm, finally according to public affairs Formula rhodium-containing liquid volume V × rhodium concentration C/M*1000 containing rhodium material obtains the content containing rhodium in rhodium material.
Embodiment 4:
(1) rhodium material will be contained and is down to 0 DEG C from room temperature, 2min is pre-processed at pressure 0.04MPa, then with the rate of 10 DEG C/min - 40 DEG C are cooled to, 2min is pre-processed at pressure 0.05MPa, finally -60 DEG C are cooled to the rate of 13 DEG C/min, in pressure 1min is pre-processed under 0.1MPa.
By tentatively crushing containing rhodium material for embrittlement processing, after the grinding of the grinder of 200 mesh, according to zinc powder and contain rhodium material Weight ratio be 2.5:1, be added 150 mesh zinc powder and glass putty, be put into porcelain crucible after mixing evenly with glass bar, then on surface 99.5% sodium chloride powder that a layer thickness is 1.6mm is covered, is cooled to room temperature after roasting 2h at 630 DEG C, after obtaining roasting Contain rhodium material.
It (2) is 8.5L:1kg according to chloroazotic acid and material ratio containing rhodium material by being added in beaker containing rhodium material after roasting, it will The chloroazotic acid that 31% hydrochloric acid and 65% nitric acid that volume ratio is 1:3 are constituted under 15mL/min rate to be slowly added in beaker, 60 After dissolving by heating 15min at DEG C, it is cooled to room temperature, obtains rhodium-containing liquid.
(3) by rhodium-containing liquid through filtering, with pure water 2 times that pH value is 6.3, filtrate constant volume, with ICP inductive coupling etc. Ionomer emission spectrum instrument analyzes the concentration of rhodium in rhodium-containing liquid, test parameter are as follows: wavelength 343.489nm, finally according to public affairs Formula rhodium-containing liquid volume V × rhodium concentration C/M*1000 containing rhodium material obtains the content containing rhodium in rhodium material.
Embodiment 5:
(1) rhodium material will be contained and is down to -5 DEG C from room temperature, 10min is pre-processed at pressure 0.02MPa, then with the speed of 5 DEG C/min Rate is cooled to -80 DEG C, and 4min is pre-processed at pressure 0.03MPa, is finally cooled to -120 DEG C with the rate of 10 DEG C/min, is pressing 1min is pre-processed under power 0.08MPa.
By tentatively crushing containing rhodium material for embrittlement processing, after the grinding of the grinder of 200 mesh, according to zinc powder and contain rhodium material Weight ratio be 3.5:1, be added 150 mesh zinc powder, be put into porcelain crucible after mixing evenly with glass bar, then surface cover one Layer is cooled to room temperature, the rhodium-containing after being roasted with a thickness of 99.5% sodium chloride powder of 1.8mm after roasting 3h at 690 DEG C Material.
It (2) is 9.5L:1kg according to chloroazotic acid and material ratio containing rhodium material by being added in beaker containing rhodium material after roasting, it will The chloroazotic acid that 31% hydrochloric acid and 65% nitric acid that volume ratio is 1:3 are constituted under 12mL/min rate to be slowly added in beaker, 60 After dissolving by heating 15min at DEG C, it is cooled to room temperature, obtains rhodium-containing liquid.
(3) be with pH value by rhodium-containing liquid through filtering 7 pure water for 3 times, filtrate constant volume, with ICP inductive coupling etc. from Daughter emission spectrometer analyzes the concentration of rhodium in rhodium-containing liquid, test parameter are as follows: wavelength 343.489nm, finally according to formula Rhodium-containing liquid volume V × rhodium concentration C/M*1000 containing rhodium material obtains the content containing rhodium in rhodium material.
Embodiment 6:
(1) rhodium material will be contained and is down to -1 DEG C from room temperature, 7min is pre-processed at pressure 0.02MPa, then with the speed of 10 DEG C/min Rate is cooled to -40 DEG C, and 2min is pre-processed at pressure 0.05MPa, is finally cooled to -80 DEG C with the rate of 13 DEG C/min, is pressing 3min is pre-processed under power 0.09MPa.
By tentatively crushing containing rhodium material for embrittlement processing, after the grinding of the grinder of 200 mesh, according to zinc powder and contain rhodium material Weight ratio be 3.6:1, be added 150 mesh zinc powder and aluminium powder, be put into porcelain crucible after mixing evenly with glass bar, then on surface 99.5% sodium chloride powder that a layer thickness is 1.7mm is covered, is cooled to room temperature, is roasted after roasting 2.5h at 630 DEG C Afterwards contain rhodium material.
It (2) is 9L:1kg according to chloroazotic acid and material ratio containing rhodium material, by body by being added in beaker containing rhodium material after roasting The chloroazotic acid that 31% hydrochloric acid and 65% nitric acid that product ratio is 1:3 are constituted under 12mL/min rate to be slowly added in beaker, at 60 DEG C After lower heating for dissolving 15min, it is cooled to room temperature, obtains rhodium-containing liquid.
(3) be with pH value by rhodium-containing liquid through filtering 6 pure water for 2 times, filtrate constant volume, with ICP inductive coupling etc. from Daughter emission spectrometer analyzes the concentration of rhodium in rhodium-containing liquid, test parameter are as follows: wavelength 343.489nm, finally according to formula Rhodium-containing liquid volume V × rhodium concentration C/M*1000 containing rhodium material obtains the content containing rhodium in rhodium material.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as At all equivalent modifications or change, should be covered by the claims of the present invention.

Claims (10)

1. a kind of quickly method of the measurement containing rhodium content in rhodium material, it is characterised in that: the following steps are included:
(1) rhodium material will be contained and carry out brittle processing, obtain embrittlement processing contains rhodium material;
(2) tentatively crushing containing rhodium material by the embrittlement processing of step (1) preparation, after the grinding of the grinder of 200 mesh, according to work Property metal powder and the weight ratio containing rhodium material be 2-4:1, be added 150 mesh active metal powder, stirred evenly with glass bar After be put into porcelain crucible, then surface cover one layer of sodium chloride, at 600-700 DEG C roast 2-3h after be cooled to room temperature, obtain Contain rhodium material after roasting;
(3) by being added in beaker containing rhodium material after the roasting of step (2) preparation, chloroazotic acid is slowly added in beaker, is heated molten Xie Hou is cooled to room temperature, and obtains rhodium-containing liquid;
(4) by the rhodium-containing liquid of step (3) preparation after being filtered, washed, filtrate constant volume is sent out with ICP inductively coupled plasma body The concentration for penetrating rhodium in spectrometer analysis rhodium-containing liquid, according to formula rhodium-containing liquid volume V × rhodium concentration C/M* containing rhodium material 1000 obtain the content containing rhodium in rhodium material.
2. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 1, it is characterised in that: the step Suddenly in (1), the technique of embrittlement processing are as follows: low-temperature grinding 5- under rhodium material is 0.02-0.1MPa in 0 ~ -120 DEG C and pressure will be contained 15min。
3. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 2, it is characterised in that: the step Suddenly in (1), the technique of embrittlement processing are as follows: rhodium material will be contained from room temperature and be down to 0 ~ -5 DEG C, located in advance at pressure 0.02-0.04MPa 2-10min is managed, then -40 ~ -80 DEG C is cooled to the rate of 5-10 DEG C/min, pre-processes 2- at pressure 0.03-0.05MPa 4min is finally cooled to -60 ~ -120 DEG C with the rate of 10-13 DEG C/min, pre-processes 1- at pressure 0.08-0.1MPa 11min。
4. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 1, it is characterised in that: the step Suddenly in (2), active metal powder is one of zinc powder, aluminium powder or glass putty or several, at active metal powder and embrittlement The weight ratio containing rhodium material of reason is 3:1.
5. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 1, it is characterised in that: the step Suddenly in (2), cover one layer of sodium chloride with a thickness of 1-2mm, sodium chloride is the sodium chloride powder that purity is 99.5%.
6. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 1, it is characterised in that: the step Suddenly in (2), the temperature of roasting is 650 DEG C, time 2h.
7. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 1, it is characterised in that: the step Suddenly in (3), chloroazotic acid includes 31% hydrochloric acid and 65% nitric acid that volume ratio is 1:3, and chloroazotic acid and material ratio containing rhodium material are 8-10L: 1kg。
8. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 1, it is characterised in that: the step Suddenly in (3), the rate being slowly added to is 5-20mL/min, and the temperature of heating is 60 DEG C, time 15min.
9. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 1, it is characterised in that: the step Suddenly in (4), the technique of washing are as follows: solvent is pure water, and pH value 6-7 is washed 2-3 times.
10. a kind of quickly method of the measurement containing rhodium content in rhodium material according to claim 1, it is characterised in that: described In step (4), the concentration of rhodium standard reserving solution is 1mg/mL, location parameter in ICP inductive coupling plasma emission spectrograph Are as follows: wavelength 343.489nm.
CN201810765344.XA 2018-07-12 2018-07-12 A kind of method of the quick measurement containing rhodium content in rhodium material Pending CN109142018A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810765344.XA CN109142018A (en) 2018-07-12 2018-07-12 A kind of method of the quick measurement containing rhodium content in rhodium material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810765344.XA CN109142018A (en) 2018-07-12 2018-07-12 A kind of method of the quick measurement containing rhodium content in rhodium material

Publications (1)

Publication Number Publication Date
CN109142018A true CN109142018A (en) 2019-01-04

Family

ID=64800353

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810765344.XA Pending CN109142018A (en) 2018-07-12 2018-07-12 A kind of method of the quick measurement containing rhodium content in rhodium material

Country Status (1)

Country Link
CN (1) CN109142018A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109884036A (en) * 2019-03-08 2019-06-14 国家硅材料深加工产品质量监督检验中心东海研究院 A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz
CN111999150A (en) * 2020-09-16 2020-11-27 励福(江门)环保科技股份有限公司 Method for measuring rhodium content in rhodium-ruthenium alloy
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

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102912128A (en) * 2012-11-05 2013-02-06 中国海洋石油总公司 Method for separating and purifying rhodium through anion exchange resin

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102912128A (en) * 2012-11-05 2013-02-06 中国海洋石油总公司 Method for separating and purifying rhodium through anion exchange resin

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
周翠红: "低温破碎技术及其在资源回收中的应用", 《北京石油化工学院学报》 *
宫嘉辰等: "电感耦合等离子体发射光谱法测定铂钯合金中的铑和铱", 《有色矿冶》 *
陈海焱等: "低温粉碎系统的研究", 《西南工学院学报》 *
陈达平: "《贵金属回收工艺学》", 30 September 1991 *
黄礼煌: "《贵金属提取新技术》", 30 November 2016, 冶金工业出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109884036A (en) * 2019-03-08 2019-06-14 国家硅材料深加工产品质量监督检验中心东海研究院 A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz
CN111999150A (en) * 2020-09-16 2020-11-27 励福(江门)环保科技股份有限公司 Method for measuring rhodium content in rhodium-ruthenium alloy
CN111999150B (en) * 2020-09-16 2023-10-03 励福(江门)环保科技股份有限公司 Method for measuring rhodium content in rhodium-ruthenium alloy
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

Similar Documents

Publication Publication Date Title
CN109142018A (en) A kind of method of the quick measurement containing rhodium content in rhodium material
CN107758752B (en) A method of preparing chloro-iridic acid
CN111926195B (en) Method for preparing high-purity platinum powder from platinum alloy waste
CN111054933A (en) Method for preparing high-purity rhodium powder from platinum-rhodium waste
JP5132226B2 (en) Ruthenium recovery method
CN103626240B (en) Lower concentration complexity prepares the method for ruthenium trichloride containing ruthenium waste liquid
CN109115567A (en) A kind of method of iridium content in quick measurement material containing iridium
CN107226488A (en) A kind of preparation method of high-purity iridium dioxide
CN108655415A (en) A kind of new process preparing high-purity platinum
CN111304457A (en) Efficient activation dissolving method for rhodium powder
CN104259483A (en) Method for recycling iridum-rhodium alloy waste material
CN107868964A (en) The preparation method of alloy powder
CN105965030A (en) Technique for recovering gold from gold iodide liquid waste
CN105127414B (en) A kind of preparation method of core shell structure silver nickel coat nano-powder material
CN107586966B (en) Method for quickly activating and dissolving insoluble noble metal
Theron et al. Dissolution and quantification of tantalum-containing compounds: comparison with niobium
CN105648232A (en) Method for refining gold by using I2 and KI
CN106834691A (en) A kind of copper anode mud wet-treating comprehensive recycling process
CN104561559A (en) Method for separating and purifying ruthenium from ruthenium-containing wastes
CN108950211B (en) A method of recycling silver and copper from waste and old chip
JPH01136910A (en) Manufacture of granular fine metal powder
CN110387476B (en) Method for leaching and recovering high-purity potassium from electromagnetic enhanced yellow phosphorus electro-precipitator dust
CN109110828A (en) A method of efficiently preparing solid nitrosyl nitric acid ruthenium
CN108330291A (en) A kind of process for separating and purifying of platinum
CN112974834B (en) Plasma torch cathode material precursor powder, preparation method thereof and plasma torch cathode

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190104