CN108982562A - The preparation method of cobalt internal standard XRF analysis sheet glass based on assisted ejection agent - Google Patents
The preparation method of cobalt internal standard XRF analysis sheet glass based on assisted ejection agent Download PDFInfo
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- CN108982562A CN108982562A CN201810876639.4A CN201810876639A CN108982562A CN 108982562 A CN108982562 A CN 108982562A CN 201810876639 A CN201810876639 A CN 201810876639A CN 108982562 A CN108982562 A CN 108982562A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
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Abstract
The preparation method of the present invention relates to a kind of cobalt internal standard XRF analysis sheet glass based on assisted ejection agent.Its scheme is: 0.1g cobalt sesquioxide, 6~7g lithium tetraborate and 0.1g assisted ejection agent being mixed, the lithium tetraborate containing cobalt and assisted ejection agent, abbreviation mixture I are obtained.1g lithium carbonate, the agent of 0.15~0.2g assisted ejection, 0.05~0.08g iodide and 0.5g sample are mixed, the lithium carbonate containing iodine and assisted ejection agent, abbreviation mixture II are obtained.5~6g mixture I is placed in platinum crucible, mixture II is placed into, is covered with remaining mixture I.Platinum crucible equipped with mixture I and mixture II is placed in high temperature furnace, is pre-oxidized at 680~720 DEG C, takes out, moves in another high temperature furnace, is melted at 980~1050 DEG C；It takes out, natural cooling, removes, demoulding obtains the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent.Environmental-friendly, the at low cost and period of the invention is short, and the accuracy analyzed with made product is high.
Description
Technical field
The invention belongs to cobalt internal standard XRF analysis sheet glass preparation technical fields.Assisted ejection agent is based on more particularly to one kind
Cobalt internal standard XRF analysis sheet glass preparation method.
Background technique
In the melting preparation process of XRF analysis glass sheet sample, due to melt have adherency or infiltration platinum crucible or
The tendency of mold is adhered to sheet glass on crucible or mold, is not readily separated, to influence the uniform of XRF analysis sheet glass
Property.Therefore, it is necessary to using release agent so that sheet glass is removed from crucible or mold.Currently, release agent only has iodide and bromine
Compound.Release agent is one layer of halide membrane layer that halide is formed on the surface of molten mass, for obstructing melt to platinum earthenware
The infiltration of crucible.Since membrane layer is very thin, so the dosage of release agent should be seldom, generally 20~50mg.But due to halogen family member
Element has very strong volatility at high temperature, causes the dosage of release agent to increase, while being influenced by melting temperature and time.Generally
The volatility of iodine and iodide is bigger than bromine, so the dosage of iodide is bigger.Existing document report shows that bromide takes off
The dosage of mould agent is 30~100mg, and the dosage that iodide make release agent is 300~1000mg.
XRF analysis shows that bromide and iodide can all generate different degrees of influence to measurement, therefore should control dosage
It is interfered with evading.When making release agent using bromide, volatile matter bromine vapor has a strong foul smell, during human body sucking can generate
Poison.In addition the specific gravity of bromine is larger, is usually all difficult to pump drainage with exhausting system, easily causes interior and gathers.Iodide pyrolysis is common
In the purifying of high pure metal, showing that a large amount of iodide exist will increase the loss of coherent element in melting process.
There are problems to be for state of the art: 1, with bromide release agent can Toxic volatilization and aggregation, prepare environment
Difference；2, iodide dosage is big, it is at high cost, 3, iodide dosage great Yi cause the loss of tested component, accuracy of analysis is low.
Summary of the invention
The present invention is directed to overcome prior art defect, it is therefore an objective to provide it is a kind of prepare it is environmental-friendly, at low cost and preparation week
The preparation method of the phase short cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, with this method preparation based on assisted ejection
The cobalt internal standard XRF analysis of agent is high with the accuracy that sheet glass is analyzed.
To achieve the above object, the step of the technical solution adopted by the present invention is:
Step 1: weighing helping for the cobalt sesquioxide of 0.1000g, the lithium tetraborate of 6.0000~7.0000g and 0.1000g
Release agent mixes, obtains the lithium tetraborate containing cobalt and assisted ejection agent.
Step 2: weighing the lithium carbonate of 1.0000g, the assisted ejection agent of 0.1500~0.2000g, 0.0500~0.0800g
Iodide and 0.5000g sample, mix, obtain the lithium carbonate containing iodine and assisted ejection agent.
Step 3: the lithium tetraborate containing cobalt and assisted ejection agent described in 5.0000~6.0000g is placed in platinum crucible, then
The lithium carbonate containing iodine and assisted ejection agent is placed on the lithium tetraborate containing cobalt and assisted ejection agent, then with remaining institute
It states containing cobalt and the covering of the lithium tetraborate of assisted ejection agent.
Step 4: the lithium tetraborate containing cobalt and assisted ejection agent and the lithium carbonate containing iodine and assisted ejection agent are known as mixing
Close object.
It will be placed in high temperature furnace equipped with the platinum crucible of the mixture, pre-oxidize 15 under the conditions of 680~720 DEG C~
20min takes out the platinum crucible equipped with pre-oxidation mixture.
Step 5: the platinum crucible equipped with pre-oxidation mixture is moved in another high temperature furnace, at 980~1050 DEG C
Under the conditions of melt 15~25min；The platinum crucible that molten mixture is housed is taken out, natural cooling is removed, and demoulding is based on
The cobalt internal standard XRF analysis sheet glass of assisted ejection agent.
The purity of the cobalt sesquioxide is to analyze pure grade or more.
The purity of the lithium tetraborate is to analyze pure grade or more.
The assisted ejection agent is one or more of soluble starch, citric acid and triethanolamine；The assisted ejection agent it is pure
Degree is pure to analyze.
The purity of the lithium carbonate is to analyze pure grade or more.
The iodide are one of potassium iodide, sodium iodide and ammonium iodide；The purity of the iodide is to analyze pure grade
More than.
The platinum crucible material is platinum alloy, in which: platinum 95wt%, gold are 5wt%；The platinum alloy it is pure
Degree > 99.99wt%.
Due to the adoption of the above technical scheme, compared with prior art, the present invention having following good effect:
The present invention uses iodide as release agent under demolding aids effect, does not use bromide, avoids Toxic
Volatilization and aggregation, improve the melting preparation condition of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, environmental-friendly.
The present invention reduces the dosage of iodide using assisted ejection agent, not only reduces the cobalt internal standard based on assisted ejection agent
The preparation cost of XRF analysis sheet glass, and can be shortened the production cycle.
The present invention reduces the dosage of iodide using assisted ejection agent, and the iodide reduced in melting preparation process are waved
Hair, improves the accuracy of analysis of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent.
Therefore, the present invention has the characteristics that environmental-friendly, the at low cost and period is short, with this method preparation based on assisted ejection
The cobalt internal standard XRF analysis of agent is high with the accuracy that sheet glass is analyzed.
Specific embodiment
The present invention is described further With reference to embodiment, not to the limitation of its protection scope.
To avoid repeating, the material Unify legislation for being first related to present embodiment is as follows, repeats no more in embodiment:
The purity of the cobalt sesquioxide is to analyze pure grade or more.
The purity of the lithium tetraborate is to analyze pure grade or more.
The purity of the assisted ejection agent is that analysis is pure.
The purity of the lithium carbonate is to analyze pure grade or more.
The purity of the iodide is to analyze pure grade or more.
The platinum crucible material is platinum alloy, in which: platinum 95wt%, gold are 5wt%；The platinum alloy it is pure
Degree > 99.99wt%.
Embodiment 1
A kind of preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent.Preparation side described in the present embodiment
The step of method, is:
Step 1: weighing helping for the cobalt sesquioxide of 0.1000g, the lithium tetraborate of 6.0000~6.4000g and 0.1000g
Release agent mixes, obtains the lithium tetraborate containing cobalt and assisted ejection agent.
Step 2: weighing the lithium carbonate of 1.0000g, the assisted ejection agent of 0.1500~0.1800g, 0.0500~0.0600g
Iodide and 0.5000g sample, mix, obtain the lithium carbonate containing iodine and assisted ejection agent.
Step 3: the lithium tetraborate containing cobalt and assisted ejection agent described in 5.0000~5.4000g is placed in platinum crucible, then
The lithium carbonate containing iodine and assisted ejection agent is placed on the lithium tetraborate containing cobalt and assisted ejection agent, then with remaining institute
It states containing cobalt and the covering of the lithium tetraborate of assisted ejection agent.
Step 4: the lithium tetraborate containing cobalt and assisted ejection agent and the lithium carbonate containing iodine and assisted ejection agent are known as mixing
Close object.
It will be placed in high temperature furnace equipped with the platinum crucible of the mixture, pre-oxidize 17 under the conditions of 680~700 DEG C~
20min takes out the platinum crucible equipped with pre-oxidation mixture.
Step 5: the platinum crucible equipped with pre-oxidation mixture is moved in another high temperature furnace, at 980~1010 DEG C
Under the conditions of melt 21~25min；The platinum crucible that molten mixture is housed is taken out, natural cooling is removed, and demoulding is based on
The cobalt internal standard XRF analysis sheet glass of assisted ejection agent.
In the present embodiment: the assisted ejection agent is one of soluble starch, citric acid and triethanolamine；The iodide
For potassium iodide.
Embodiment 2
A kind of preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent.Preparation side described in the present embodiment
The step of method, is:
Step 1: weighing helping for the cobalt sesquioxide of 0.1000g, the lithium tetraborate of 6.4000~6.7000g and 0.1000g
Release agent mixes, obtains the lithium tetraborate containing cobalt and assisted ejection agent.
Step 2: weighing the lithium carbonate of 1.0000g, the assisted ejection agent of 0.1600~0.1900g, 0.0600~0.0700g
Iodide and 0.5000g sample, mix, obtain the lithium carbonate containing iodine and assisted ejection agent.
Step 3: the lithium tetraborate containing cobalt and assisted ejection agent described in 5.4000~5.7000g is placed in platinum crucible, then
The lithium carbonate containing iodine and assisted ejection agent is placed on the lithium tetraborate containing cobalt and assisted ejection agent, then with remaining institute
It states containing cobalt and the covering of the lithium tetraborate of assisted ejection agent.
Step 4: the lithium tetraborate containing cobalt and assisted ejection agent and the lithium carbonate containing iodine and assisted ejection agent are known as mixing
Close object.
It will be placed in high temperature furnace equipped with the platinum crucible of the mixture, pre-oxidize 16 under the conditions of 690~710 DEG C~
19min takes out the platinum crucible equipped with pre-oxidation mixture.
Step 5: the platinum crucible equipped with pre-oxidation mixture is moved in another high temperature furnace, 1000~1030
18~22min is melted under the conditions of DEG C；The platinum crucible that molten mixture is housed is taken out, natural cooling is removed, and demoulding obtains base
In the cobalt internal standard XRF analysis sheet glass of assisted ejection agent.
In the present embodiment: the assisted ejection agent is the mixing of two kinds of substances in soluble starch, citric acid and triethanolamine
Object；The iodide are sodium iodide.
Embodiment 3
A kind of preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent.Preparation side described in the present embodiment
The step of method, is:
Step 1: weighing helping for the cobalt sesquioxide of 0.1000g, the lithium tetraborate of 6.7000~7.0000g and 0.1000g
Release agent mixes, obtains the lithium tetraborate containing cobalt and assisted ejection agent.
Step 2: weighing the lithium carbonate of 1.0000g, the assisted ejection agent of 0.1700~0.2000g, 0.0700~0.0800g
Iodide and 0.5000g sample, mix, obtain the lithium carbonate containing iodine and assisted ejection agent.
Step 3: the lithium tetraborate containing cobalt and assisted ejection agent described in 5.7000~6.0000g is placed in platinum crucible, then
The lithium carbonate containing iodine and assisted ejection agent is placed on the lithium tetraborate containing cobalt and assisted ejection agent, then with remaining institute
It states containing cobalt and the covering of the lithium tetraborate of assisted ejection agent.
Step 4: the lithium tetraborate containing cobalt and assisted ejection agent and the lithium carbonate containing iodine and assisted ejection agent are known as mixing
Close object.
It will be placed in high temperature furnace equipped with the platinum crucible of the mixture, pre-oxidize 15 under the conditions of 700~720 DEG C~
18min takes out the platinum crucible equipped with pre-oxidation mixture.
Step 5: the platinum crucible equipped with pre-oxidation mixture is moved in another high temperature furnace, 1020~1050
15~19min is melted under the conditions of DEG C；The platinum crucible that molten mixture is housed is taken out, natural cooling is removed, and demoulding obtains base
In the cobalt internal standard XRF analysis sheet glass of assisted ejection agent.
In the present embodiment: the assisted ejection agent is the mixture of soluble starch, citric acid and triethanolamine；The iodide
For ammonium iodide.
Present embodiment compared with prior art, has following good effect:
Present embodiment uses iodide as release agent under demolding aids effect, does not use bromide, avoids
The volatilization and aggregation of Toxic improve the melting preparation condition of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, ring
Border is friendly.
Present embodiment reduces the dosage of iodide using assisted ejection agent, not only reduces based on assisted ejection agent
The preparation cost of cobalt internal standard XRF analysis sheet glass, and can be shortened the production cycle.
Present embodiment reduces the dosage of iodide using assisted ejection agent, reduces the iodine in melting preparation process
Compound volatilization, improves the accuracy of analysis of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent.
Therefore, present embodiment has the characteristics that environmental-friendly, the at low cost and period is short, the base prepared with this method
In assisted ejection agent cobalt internal standard XRF analysis sheet glass it is with high accuracy.
Claims (7)
1. a kind of preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, it is characterised in that the preparation side
The step of method, is:
Step 1: weighing the assisted ejection of the cobalt sesquioxide of 0.1000g, the lithium tetraborate of 6.0000~7.0000g and 0.1000g
Agent mixes, obtains the lithium tetraborate containing cobalt and assisted ejection agent；
Step 2: weighing the iodine of the lithium carbonate of 1.0000g, the assisted ejection agent of 0.1500~0.2000g, 0.0500~0.0800g
The sample of compound and 0.5000g mixes, obtains the lithium carbonate containing iodine and assisted ejection agent；
Step 3: the lithium tetraborate containing cobalt and assisted ejection agent described in 5.0000~6.0000g is placed in platinum crucible, then by institute
It states the lithium carbonate containing iodine and assisted ejection agent to be placed on the lithium tetraborate containing cobalt and assisted ejection agent, then described be contained with remaining
Cobalt and the covering of the lithium tetraborate of assisted ejection agent；
Step 4: the lithium tetraborate containing cobalt and assisted ejection agent and the lithium carbonate containing iodine and assisted ejection agent are known as mixing
Object；
Platinum crucible equipped with the mixture is placed in high temperature furnace, 15~20min is pre-oxidized under the conditions of 680~720 DEG C,
Take out the platinum crucible equipped with pre-oxidation mixture；
Step 5: the platinum crucible equipped with pre-oxidation mixture is moved in another high temperature furnace, in 980~1050 DEG C of conditions
15~25min of lower melting；The platinum crucible that molten mixture is housed is taken out, natural cooling is removed, demoulding, is obtained de- based on helping
The cobalt internal standard XRF analysis sheet glass of mould agent.
2. the preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, feature exist according to claim 1
In the purity of the cobalt sesquioxide be to analyze pure grade or more.
3. the preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, feature exist according to claim 1
In the purity of the lithium tetraborate be to analyze pure grade or more.
4. the preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, feature exist according to claim 1
In the assisted ejection agent be one or more of soluble starch, citric acid and triethanolamine；The purity of the assisted ejection agent is point
It analyses pure.
5. the preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, feature exist according to claim 1
In the purity of the lithium carbonate be to analyze pure grade or more.
6. the preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, feature exist according to claim 1
In the iodide be one of potassium iodide, sodium iodide and ammonium iodide；The purity of the iodide is to analyze pure grade or more.
7. the preparation method of the cobalt internal standard XRF analysis sheet glass based on assisted ejection agent, feature exist according to claim 1
In the platinum crucible material be platinum alloy, in which: platinum 95wt%, gold be 5wt%；The purity of the platinum alloy >
99.99wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810876639.4A CN108982562B (en) | 2018-08-03 | 2018-08-03 | Preparation method of cobalt internal standard XRF (X-ray fluorescence) analysis glass sheet based on release assisting agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810876639.4A CN108982562B (en) | 2018-08-03 | 2018-08-03 | Preparation method of cobalt internal standard XRF (X-ray fluorescence) analysis glass sheet based on release assisting agent |
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| CN108982562A true CN108982562A (en) | 2018-12-11 |
| CN108982562B CN108982562B (en) | 2021-02-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115452871A (en) * | 2022-08-08 | 2022-12-09 | 武汉科技大学 | Preparation of glass sheet for XRF analysis of iron ore and correction method of measurement result |
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| CN108982562B (en) | 2021-02-19 |
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