CN108982562B - Preparation method of cobalt internal standard XRF (X-ray fluorescence) analysis glass sheet based on release assisting agent - Google Patents
Preparation method of cobalt internal standard XRF (X-ray fluorescence) analysis glass sheet based on release assisting agent Download PDFInfo
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- 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 invention relates to a preparation method of a cobalt internal standard XRF (X-ray fluorescence) analysis glass sheet based on an assistant release agent. The scheme is as follows: and (3) uniformly mixing 0.1g of cobaltous oxide, 6-7 g of lithium tetraborate and 0.1g of demolding aid to obtain the lithium tetraborate containing cobalt and the demolding aid, which is called a mixture I for short. And uniformly mixing 1g of lithium carbonate, 0.15-0.2 g of release aid agent, 0.05-0.08 g of iodide and 0.5g of sample to obtain lithium carbonate containing iodine and release aid agent, which is called a mixture II for short. 5-6 g of the mixture I is placed in a platinum crucible, and then the mixture II is placed and covered with the rest of the mixture I. Placing the platinum crucible filled with the mixture I and the mixture II in a high-temperature furnace, pre-oxidizing at 680-720 ℃, taking out, transferring to another high-temperature furnace, and melting at 980-1050 ℃; and taking out, naturally cooling, stripping and demolding to obtain the co internal standard XRF analysis glass sheet based on the release assisting agent. The invention has the advantages of environmental protection, low cost, short period and high accuracy of analysis by using the prepared product.
Description
Technical Field
The invention belongs to the technical field of preparation of glass sheets for XRF analysis of cobalt internal standard. In particular to a preparation method of a cobalt internal standard XRF (X-ray fluorescence) analysis glass sheet based on an assistant release agent.
Background
During the melting preparation process of the glass sheet sample for XRF analysis, the melt has a tendency to adhere to or infiltrate the platinum crucible or the mold, so that the glass sheet is adhered to the crucible or the mold and is not easy to separate, thereby affecting the uniformity of the glass sheet for XRF analysis. Therefore, a release agent must be used to peel the glass sheet from the crucible or mold. Currently, the only mold release agents are iodide and bromide. The release agent is a halide diaphragm layer formed on the surface of the molten mass by halide and used for preventing the platinum crucible from being infiltrated by the molten mass. Because the membrane layer is very thin, the amount of the release agent used is small, and is generally 20-50 mg. However, the halogen element has strong volatility at high temperature, so that the dosage of the release agent is increased, and the influence of melting temperature and time is also caused. Iodine and iodide are generally more volatile than bromine and so iodide is used in greater amounts. The existing literature reports show that the dosage of bromide used as a mold release agent is 30-100 mg, and the dosage of iodide used as a mold release agent is 300-1000 mg.
XRF analysis shows that both bromide and iodide affect the measurements to varying degrees, so dosage should be controlled and interference avoided. When bromide is used as the release agent, the volatile bromine vapor has strong foul smell, and poisoning can be caused when a human body inhales the bromine vapor. In addition, the bromine has a large specific gravity, and is difficult to pump and exhaust by a general air pumping system, so that indoor accumulation is easily caused. Iodide pyrolysis is commonly used for the purification of high purity metals, indicating that the presence of large amounts of iodide increases the loss of the relevant elements during the melting process.
The prior art in the field has the problems that: 1. the bromide release agent can volatilize and gather toxic substances, and the preparation environment is poor; 2. the use amount of the iodide is large, the cost is high, 3, the loss of the measured component is easily caused by the large use amount of the iodide, and the analysis accuracy is low.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide the preparation method for the assistant release agent-based glass sheet for the cobalt internal standard XRF analysis, which is environment-friendly, low in cost and short in preparation period.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
weighing 0.1000g of cobaltous oxide, 6.0000-7.0000 g of lithium tetraborate and 0.1000g of release aid agent, and uniformly mixing to obtain the lithium tetraborate containing cobalt and the release aid agent.
Weighing 1.0000g of lithium carbonate, 0.1500-0.2000 g of release aid agent, 0.0500-0.0800 g of iodide and 0.5000g of sample, and uniformly mixing to obtain the lithium carbonate containing the iodine and the release aid agent.
And thirdly, 5.0000-6.0000 g of lithium tetraborate containing cobalt and an assistant release agent is placed in a platinum crucible, lithium carbonate containing iodine and the assistant release agent is placed on the lithium tetraborate containing cobalt and the assistant release agent, and then the lithium tetraborate containing cobalt and the assistant release agent is covered with the rest lithium tetraborate containing cobalt and the assistant release agent.
Step four, the lithium tetraborate containing cobalt and the release aid and the lithium carbonate containing iodine and the release aid are called a mixture.
And (3) placing the platinum crucible filled with the mixture into a high-temperature furnace, pre-oxidizing for 15-20 min at 680-720 ℃, and taking out the platinum crucible filled with the pre-oxidized mixture.
Fifthly, moving the platinum crucible filled with the pre-oxidation mixture into another high-temperature furnace, and melting for 15-25 min at 980-1050 ℃; and taking out the platinum crucible filled with the molten mixture, naturally cooling, stripping and demolding to obtain the cobalt internal standard XRF analysis glass sheet based on the release assisting agent.
The purity of the cobaltous oxide is more than analytical grade.
The purity of the lithium tetraborate is above analytical grade.
The release aid is more than one of soluble starch, citric acid and triethanolamine; the purity of the release aid is analytically pure.
The purity of the lithium carbonate is more than analytical grade.
The iodide is one of potassium iodide, sodium iodide and ammonium iodide; the purity of the iodide is more than analytical grade.
The platinum crucible is made of platinum alloy, wherein: 95wt% of platinum and 5wt% of gold; the purity of the platinum alloy is more than 99.99 wt%.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
according to the invention, iodide is used as the release agent under the action of the release aid, bromide is not used, volatilization and aggregation of toxic substances are avoided, the melting preparation condition of the cobalt internal standard XRF analysis glass sheet based on the release aid is improved, and the environment is friendly.
According to the invention, the usage amount of iodide is reduced by using the release aid, so that the preparation cost of the cobalt internal standard XRF analysis glass sheet based on the release aid is reduced, and the production period can be shortened.
According to the invention, the usage amount of iodide is reduced by using the release aid, the volatilization of iodide in the melting preparation process is reduced, and the analysis accuracy of the cobalt internal standard XRF analysis glass sheet based on the release aid is improved.
Therefore, the glass sheet for the XRF analysis based on the cobalt internal standard prepared by the method has the characteristics of environmental friendliness, low cost and short period, and the accuracy of the glass sheet for the XRF analysis based on the cobalt internal standard prepared by the method is high.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
In order to avoid repetition, the materials related to this embodiment are described in a unified manner, and are not described in the embodiments again:
the purity of the cobaltous oxide is more than analytical grade.
The purity of the lithium tetraborate is above analytical grade.
The purity of the release aid is analytically pure.
The purity of the lithium carbonate is more than analytical grade.
The purity of the iodide is more than analytical grade.
The platinum crucible is made of platinum alloy, wherein: 95wt% of platinum and 5wt% of gold; the purity of the platinum alloy is more than 99.99 wt%.
Example 1
A preparation method of a cobalt internal standard XRF analysis glass sheet based on an assistant release agent. The preparation method of the embodiment comprises the following steps:
weighing 0.1000g of cobaltous oxide, 6.0000-6.4000 g of lithium tetraborate and 0.1000g of release aid agent, and uniformly mixing to obtain the lithium tetraborate containing cobalt and the release aid agent.
Weighing 1.0000g of lithium carbonate, 0.1500-0.1800 g of release aid agent, 0.0500-0.0600 g of iodide and 0.5000g of sample, and uniformly mixing to obtain the lithium carbonate containing the iodine and the release aid agent.
And thirdly, 5.0000-5.4000 g of lithium tetraborate containing cobalt and an assistant release agent is placed in a platinum crucible, lithium carbonate containing iodine and the assistant release agent is placed on the lithium tetraborate containing cobalt and the assistant release agent, and then the lithium tetraborate containing cobalt and the assistant release agent is covered with the rest lithium tetraborate containing cobalt and the assistant release agent.
Step four, the lithium tetraborate containing cobalt and the release aid and the lithium carbonate containing iodine and the release aid are called a mixture.
And (3) placing the platinum crucible filled with the mixture into a high-temperature furnace, pre-oxidizing for 17-20 min at 680-700 ℃, and taking out the platinum crucible filled with the pre-oxidized mixture.
Fifthly, moving the platinum crucible filled with the pre-oxidation mixture into another high-temperature furnace, and melting for 21-25 min at 980-1010 ℃; and taking out the platinum crucible filled with the molten mixture, naturally cooling, stripping and demolding to obtain the cobalt internal standard XRF analysis glass sheet based on the release assisting agent.
In this embodiment: the release aid is one of soluble starch, citric acid and triethanolamine; the iodide is potassium iodide.
Example 2
A preparation method of a cobalt internal standard XRF analysis glass sheet based on an assistant release agent. The preparation method of the embodiment comprises the following steps:
weighing 0.1000g of cobaltous oxide, 6.4000-6.7000 g of lithium tetraborate and 0.1000g of release aid agent, and uniformly mixing to obtain the lithium tetraborate containing cobalt and the release aid agent.
Weighing 1.0000g of lithium carbonate, 0.1600-0.1900 g of release aid agent, 0.0600-0.0700 g of iodide and 0.5000g of sample, and uniformly mixing to obtain the lithium carbonate containing the iodine and the release aid agent.
And thirdly, 5.4000-5.7000 g of lithium tetraborate containing cobalt and an assistant release agent is placed in a platinum crucible, lithium carbonate containing iodine and the assistant release agent is placed on the lithium tetraborate containing cobalt and the assistant release agent, and then the lithium tetraborate containing cobalt and the assistant release agent is covered with the rest lithium tetraborate containing cobalt and the assistant release agent.
Step four, the lithium tetraborate containing cobalt and the release aid and the lithium carbonate containing iodine and the release aid are called a mixture.
And (3) placing the platinum crucible filled with the mixture into a high-temperature furnace, pre-oxidizing for 16-19 min at the temperature of 690-710 ℃, and taking out the platinum crucible filled with the pre-oxidized mixture.
Fifthly, moving the platinum crucible filled with the pre-oxidation mixture into another high-temperature furnace, and melting for 18-22 min at 1000-1030 ℃; and taking out the platinum crucible filled with the molten mixture, naturally cooling, stripping and demolding to obtain the cobalt internal standard XRF analysis glass sheet based on the release assisting agent.
In this embodiment: the auxiliary release agent is a mixture of two substances of soluble starch, citric acid and triethanolamine; the iodide is sodium iodide.
Example 3
A preparation method of a cobalt internal standard XRF analysis glass sheet based on an assistant release agent. The preparation method of the embodiment comprises the following steps:
weighing 0.1000g of cobaltous oxide, 6.7000-7.0000 g of lithium tetraborate and 0.1000g of release aid agent, and uniformly mixing to obtain the lithium tetraborate containing cobalt and the release aid agent.
Weighing 1.0000g of lithium carbonate, 0.1700-0.2000 g of release aid agent, 0.0700-0.0800 g of iodide and 0.5000g of sample, and uniformly mixing to obtain the lithium carbonate containing the iodine and the release aid agent.
And thirdly, 5.7000-6.0000 g of lithium tetraborate containing cobalt and an assistant release agent is placed in a platinum crucible, lithium carbonate containing iodine and the assistant release agent is placed on the lithium tetraborate containing cobalt and the assistant release agent, and then the lithium tetraborate containing cobalt and the assistant release agent is covered with the rest lithium tetraborate containing cobalt and the assistant release agent.
Step four, the lithium tetraborate containing cobalt and the release aid and the lithium carbonate containing iodine and the release aid are called a mixture.
And (3) placing the platinum crucible filled with the mixture into a high-temperature furnace, pre-oxidizing for 15-18 min at 700-720 ℃, and taking out the platinum crucible filled with the pre-oxidized mixture.
Fifthly, moving the platinum crucible filled with the pre-oxidation mixture into another high-temperature furnace, and melting for 15-19 min at 1020-1050 ℃; and taking out the platinum crucible filled with the molten mixture, naturally cooling, stripping and demolding to obtain the cobalt internal standard XRF analysis glass sheet based on the release assisting agent.
In this embodiment: the auxiliary release agent is a mixture of soluble starch, citric acid and triethanolamine; the iodide is ammonium iodide.
Compared with the prior art, the specific implementation mode has the following positive effects:
according to the specific embodiment, iodide is used as the release agent under the action of the release aid, bromide is not used, volatilization and aggregation of toxic substances are avoided, the melting preparation condition of the cobalt internal standard XRF analysis glass sheet based on the release aid is improved, and the environment is protected.
According to the embodiment, the use amount of iodide is reduced by using the assistant release agent, so that the preparation cost of the cobalt internal standard XRF analysis glass sheet based on the assistant release agent is reduced, and the production period can be shortened.
According to the specific embodiment, the auxiliary release agent is utilized to reduce the dosage of iodide, reduce the volatilization of iodide in the melting preparation process, and improve the analysis accuracy of the cobalt internal standard XRF analysis glass sheet based on the auxiliary release agent.
Therefore, the specific embodiment has the characteristics of environmental friendliness, low cost and short period, and the assistant release agent-based cobalt internal standard XRF analysis glass sheet prepared by the method has high analysis accuracy.
Claims (6)
1. A preparation method of a co-release agent-based glass sheet for XRF analysis of a cobalt internal standard is characterized by comprising the following steps:
weighing 0.1000g of cobaltous oxide, 6.0000-7.0000 g of lithium tetraborate and 0.1000g of demolding aid, and uniformly mixing to obtain lithium tetraborate containing cobalt and the demolding aid;
weighing 1.0000g of lithium carbonate, 0.1500-0.2000 g of release aid agent, 0.0500-0.0800 g of iodide and 0.5000g of sample, and uniformly mixing to obtain lithium carbonate containing iodine and the release aid agent;
placing 5.0000-6.0000 g of lithium tetraborate containing cobalt and an assistant release agent into a platinum crucible, placing lithium carbonate containing iodine and the assistant release agent on the lithium tetraborate containing cobalt and the assistant release agent, and covering with the rest lithium tetraborate containing cobalt and the assistant release agent;
step four, the lithium tetraborate containing cobalt and the release aid and the lithium carbonate containing iodine and the release aid are called mixtures;
placing the platinum crucible filled with the mixture in a high-temperature furnace, pre-oxidizing for 15-20 min at 680-720 ℃, and taking out the platinum crucible filled with the pre-oxidized mixture;
fifthly, moving the platinum crucible filled with the pre-oxidation mixture into another high-temperature furnace, and melting for 15-25 min at 980-1050 ℃; taking out the platinum crucible filled with the molten mixture, naturally cooling, stripping and demolding to obtain a cobalt internal standard XRF (X-ray fluorescence) analysis glass sheet based on the release assisting agent;
the release aid is more than one of soluble starch, citric acid and triethanolamine; the purity of the release aid is analytically pure.
2. The method of claim 1, wherein the purity of the cobaltous oxide is analytically pure or greater.
3. The method of making an assistant release agent-based cobalt internal standard XRF analysis glass sheet according to claim 1, wherein the purity of lithium tetraborate is analytically pure or higher.
4. The method of claim 1, wherein said lithium carbonate is of purity greater than analytical grade.
5. The method for preparing an XRF analysis glass sheet based on cobalt internal standard of assistant release agent as claimed in claim 1, characterized in that the iodide is one of potassium iodide, sodium iodide and ammonium iodide; the purity of the iodide is more than analytical grade.
6. The method for preparing the assistant release agent-based cobalt internal standard XRF analysis glass sheet according to claim 1, characterized in that the platinum crucible material is platinum alloy, wherein: 95wt% of platinum and 5wt% of gold; the purity of the platinum alloy is more than 99.99 wt%.
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