CN107101905B - Method for measuring selenium content in crude selenium - Google Patents
Method for measuring selenium content in crude selenium Download PDFInfo
- Publication number
- CN107101905B CN107101905B CN201710270326.XA CN201710270326A CN107101905B CN 107101905 B CN107101905 B CN 107101905B CN 201710270326 A CN201710270326 A CN 201710270326A CN 107101905 B CN107101905 B CN 107101905B
- Authority
- CN
- China
- Prior art keywords
- selenium
- precipitate
- crude
- reaction
- content
- 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.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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)
- Manufacture And Refinement Of Metals (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for measuring selenium content in crude selenium, which comprises the following steps: A) mixing and heating crude selenium and water, and adding a reducing agent for reaction to obtain a precipitate; B) dissolving the precipitate with acid, and adding an oxidant to perform oxidation reaction, wherein the oxidant is selected from a composite oxidant formed by perchloric acid and hydrogen peroxide, potassium permanganate or potassium dichromate; C) salifying the oxidation product obtained in the step B), adding a precipitator into the oxidation product to react to obtain precipitate, and calculating the selenium content in the crude selenium according to the mass of the precipitate, wherein the precipitator is selected from barium nitrate or barium chloride. The method for measuring the selenium content in the crude selenium provided by the invention is simple, short in flow, accurate in result and easy to master by operators. The reagent used in the method is cheap and easy to obtain, and multi-method instruments such as an ICP spectrometer and the like are avoided, so that the assay and analysis cost is reduced. The method is suitable for detection and analysis of crude selenium production, and is favorable for guiding production. And also applicable to trade settlement analysis.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and particularly relates to a method for measuring selenium content in crude selenium.
Background
Selenium is a non-metallic chemical element and the chemical symbol is Se. Selenium is an important industrial raw material and can be used as a photosensitive material, a catalyst in the electrolytic manganese industry and the like. Has wide application.
At present, 90% of primary selenium is mainly generated in anode mud of copper electrolysis, and a crude product is the crude selenium. In the process of producing cathode copper by electrolysis, the produced copper anode mud is smelted by a pyrogenic process to produce selenium-containing flue gas, and the flue gas is treated by a purification system and reduced by a reducing agent such as sodium sulfite and the like to produce crude selenium. Wherein the selenium content is approximately 80-99%.
Crude selenium is an important byproduct in copper smelting, and selenium is the most important element in the copper smelting. The determination of selenium has great guiding significance for the control index of the production process and trade settlement.
At present, no standard analysis method for performing the determination of selenium in crude selenium is published, and part of the methods can refer to a chemical analysis method of selenium with higher purity, an analysis method of selenium dioxide, a determination method of crude selenium reported in part of documents, a sodium thiosulfate titration method, a hydroxylamine hydrochloride reduction gravimetric method and the like.
Specifically disclosed in the nonferrous metals industry YST 226.12-2009 of the people's republic of China is a selenization chemical analysis method-part 12-selenium content determination-sodium thiosulfate volumetric method (determination range 98.0-99.0%), which comprises the following steps: after the sample is decomposed with hydrochloric acid and nitric acid, the titration is carried out in a sulfuric acid medium by using a standard titration solution of sodium thiosulfate. And adding potassium iodide when the end point is approached, continuously titrating the iodine separated out by the reaction by using a sodium thiosulfate standard titration solution by using starch as an indicator, and titrating until the blue color disappears as the end point. And calculating the content of the selenium in the sample. The method is mainly suitable for measuring the selenium content in the selenium with higher purity, and the measuring range is 98.0-99.0%. Compared with crude selenium, the selenium substance has simple matrix components, and can be titrated by sodium thiosulfate after a sample is simply dissolved. The crude selenium has complex matrix components and contains more impurity elements, and the titration directly by sodium thiosulfate has larger error.
The specific method of the sodium thiosulfate titration method comprises the following steps: decomposing a sample by nitric acid and sulfuric acid, reducing and separating out monomer selenium by using hydroxylamine hydrochloride in 6moL/L hydrochloric acid solution containing tartaric acid, filtering and separating from other elements, dissolving the monomer selenium by using acid, and titrating by using a sodium thiosulfate standard titration solution in a sulfuric acid medium. And adding potassium iodide when the end point is approached, continuously titrating the iodine separated out by the reaction by using a sodium thiosulfate standard titration solution by using starch as an indicator, and titrating until the blue color disappears as the end point. According to the method, because the sodium thiosulfate is added in the early stage to react with most of selenium, and the potassium iodide is added near the end point, the approximate content of the selenium in the sample needs to be known in advance, and the measurement is inconvenient for a crude selenium sample with unknown content. In addition, because the reaction speed of potassium iodide and selenium is not very fast, when the reaction end point is approached, after the sodium thiosulfate and the generated iodine react, the blue color disappears, and the end point is reached, but the newly generated iodine generated by the reaction of potassium iodide and selenium can turn the color of the solution, so that repeated titration is needed, the process is complicated, the end point judgment is difficult, and the error is large. Meanwhile, if the reaction solution is left for a long time, a small amount of iodide ions in the solution are oxidized to cause color reversion, and the titration error is increased.
The standard YS/T1084.3 crude selenium chemical analysis method-part 3-determination of selenium content discloses a hydroxylamine hydrochloride reduction gravimetric method, which comprises the following specific steps: dissolving a sample by aqua regia, reducing selenium into a simple substance state by hydroxylamine hydrochloride in a hydrochloric acid medium of 3-4 mol/L, separating the simple substance state from other impurities, filtering by a glass sand core crucible, washing precipitates by water and ethanol, weighing after constant weight. The filtrate was collected, and the amount of selenium remaining in the filtrate was measured by ICP-OES method to correct the residual selenium.
A chinese patent with application number 201310545957.X discloses a method for analyzing selenium content in crude selenium, specifically comprising: dissolving the sample by using nitric acid and hydrochloric acid, filtering, and separating acid-insoluble element interference; hydrazine hydrate reduction, filtration and separation of part of interference elements; dissolving the precipitate with acid, measuring tellurium with ICP spectrometer, and removing main interference elements; the content of selenium in the filtrate is measured by a spectrometer, and the analysis result is corrected.
However, in the two methods, hydroxylamine hydrochloride or hydrazine hydrate is needed to reduce selenium in the crude selenium into elemental selenium precipitate, most of selenium in the solution before reduction is oxidized and dissolved by acid, and the reduction reaction time is long. In addition, impurities such as tellurium, copper, lead, bismuth, arsenic, iron and the like in the solution are reduced to a certain degree in the reduction reaction to form coprecipitation. Repeated rinsing is sometimes required many times. This effect is even more pronounced if the crude selenium sample has a higher content of impurities, which can reach a ratio of 0.05-0.1% at high levels. Affecting the accuracy of the assay result. It is sometimes necessary to subtract the measured impurity content by ICP-OES. In addition, the Chinese patent with the application number of 201310545957.X adopts different reducing agents, namely hydrazine hydrate, but the reducing effect is different, and more impurities are introduced into the precipitate. The amount of selenium remaining in the filtrate must be corrected by measuring ICP-OES, and the amount of tellurium in the precipitate must be subtracted by measuring ICP-OES. The measurement process is more cumbersome.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide a method for determining selenium content in crude selenium, which is simple, short in process and accurate in result.
The invention provides a method for measuring selenium content in crude selenium, which comprises the following steps:
A) mixing and heating crude selenium and water, and adding a reducing agent for reaction to obtain a precipitate;
B) dissolving the precipitate with acid, and adding an oxidant selected from one or more of (perchloric acid and hydrogen peroxide), potassium permanganate and potassium dichromate to perform an oxidation reaction;
C) salifying the oxidation product obtained in the step B), adding a precipitator into the oxidation product to react to obtain precipitate, and calculating the selenium content in the crude selenium according to the mass of the precipitate, wherein the precipitator is selected from barium nitrate or barium chloride.
Preferably, the oxidant is selected from a composite oxidant formed by perchloric acid and hydrogen peroxide, and the volume ratio of the perchloric acid to the hydrogen peroxide in the composite oxidant is (4-6): (4-6).
Preferably, the reducing agent is selected from hydroxylamine hydrochloride, hydrazine sulfate, hydrazine hydrate or tin dichloride.
Preferably, the acid is selected from nitric acid or hydrochloric acid.
Preferably, the oxidation product of step B) is salified by mixing with sodium hydroxide, potassium hydroxide or sodium carbonate.
Preferably, the precipitating agent is selected from barium nitrate.
Preferably, the reaction temperature of the step A) is about 90-100 ℃, and the reaction time is 30-60 minutes;
the temperature of the oxidation reaction in the step B) is 90-100 ℃, and the time is 20-40 minutes;
the reaction temperature of the step C) is 90-100 ℃, and the reaction time is 1.5-2 hours.
Preferably, the method comprises the following steps:
mixing and heating the crude selenium and water, and then adding hydroxylamine hydrochloride for reaction to obtain a precipitate;
dissolving the precipitate with acid, and adding perchloric acid and hydrogen peroxide for oxidation reaction;
and (3) reacting the oxidation product with sodium hydroxide and barium nitrate in sequence to obtain a precipitate, and calculating the content of selenium in the crude selenium according to the mass of the precipitate.
Preferably, the calculation formula is shown in formula (I):
in the formula (I), w is the percentage content of selenium in the crude selenium,
m1in order to be able to measure the quality of the precipitate,
m0the mass of the crude selenium is.
Preferably, the crude selenium comprises selenium and impurity components, and main impurity elements in the impurity components comprise Pb, S, Cu, Te, Fe, As and Sb.
Compared with the prior art, the invention provides a method for measuring the selenium content in crude selenium, which comprises the following steps: A) mixing and heating crude selenium and water, and adding a reducing agent for reaction to obtain a precipitate; B) dissolving the precipitate with acid, and adding an oxidant to perform oxidation reaction, wherein the oxidant is selected from a composite oxidant formed by perchloric acid and hydrogen peroxide, potassium permanganate or potassium dichromate; C) salifying the oxidation product obtained in the step B), adding a precipitator into the oxidation product to react to obtain precipitate, and calculating the selenium content in the crude selenium according to the mass of the precipitate, wherein the precipitator is selected from barium nitrate or barium chloride. The method for measuring the selenium content in the crude selenium provided by the invention is simple, short in flow, accurate in result and easy to master by operators. The reagent used in the method is cheap and easy to obtain, and multi-method instruments such as an ICP spectrometer and the like are avoided, so that the assay and analysis cost is reduced. The method is suitable for detection and analysis of crude selenium production, and is favorable for guiding production. And also applicable to trade settlement analysis.
Detailed Description
The invention provides a method for measuring selenium content in crude selenium, which comprises the following steps:
A) mixing and heating crude selenium and water, and adding a reducing agent for reaction to obtain a precipitate;
B) dissolving the precipitate with acid, and adding an oxidant to perform oxidation reaction, wherein the oxidant is selected from a composite oxidant formed by perchloric acid and hydrogen peroxide, potassium permanganate or potassium dichromate;
C) salifying the oxidation product obtained in the step B), adding a precipitator into the oxidation product to react to obtain precipitate, and calculating the selenium content in the crude selenium according to the mass of the precipitate, wherein the precipitator is selected from barium nitrate or barium chloride.
The invention firstly mixes and heats crude selenium and water, and then adds a reducing agent for reaction to obtain a precipitate. The crude selenium is generated by purifying the smelting flue gas of the copper anode slime, and is a selenium material with the selenium content of about 80-99 wt%. In the invention, the crude selenium comprises selenium and impurity components, the selenium content in the crude selenium is 80 wt% -99 wt%, and the main impurity elements in the impurity components comprise Pb, S, Cu, Te, Fe, As and Sb. The content of the impurity elements in the crude selenium is as follows by mass percent: pb: 0.001 wt% -2 wt%; s: 0.01 wt% -3 wt%; cu: 0.001 wt% -1 wt%; te: 0.001 wt% -1 wt%; fe: 0.001 wt% -0.5 wt%; as: 0.001 wt% -0.05 wt%; sb: 0.001 wt% -0.05 wt%.
The crude selenium and water are mixed and heated, the heating temperature is preferably 90-100 ℃, and after the crude selenium and water are heated to be slightly boiled, a reducing agent is added for reaction to obtain a precipitate. The reducing agent is selected from hydroxylamine hydrochloride, hydrazine sulfate, hydrazine hydrate and tin dichloride, and is preferably hydroxylamine hydrochloride. The reaction temperature is preferably 90-100 ℃, the slight boiling is kept, and the reaction time is 30-60 minutes.
After obtaining a precipitate, the precipitate was filtered and washed. The washed precipitate is then dissolved with an acid. Among them, the acid is preferably nitric acid or hydrochloric acid, and more preferably nitric acid. The dissolving temperature is preferably 90-100 ℃.
After the precipitate is completely dissolved, adding an oxidant to perform oxidation reaction, wherein the oxidant is selected from a composite oxidant formed by perchloric acid and hydrogen peroxide, potassium permanganate or potassium dichromate, preferably the composite oxidant formed by perchloric acid and hydrogen peroxide, and the volume ratio of the perchloric acid to the hydrogen peroxide in the composite oxidant is (4-6): (4-6), preferably 5: 5. The temperature of the oxidation reaction is preferably 90-100 ℃, and the time is preferably 20-40 minutes.
Then, the oxidation product is salinized, and the salinization method comprises the following specific steps: the above oxidation product is mixed with sodium hydroxide, potassium hydroxide or sodium carbonate to perform salinization, and preferably, the above oxidation product is mixed with sodium hydroxide to perform salinization.
And finally, adding a precipitator for reaction to obtain precipitate, and calculating the selenium content in the crude selenium according to the mass of the precipitate, wherein the precipitator is selected from barium nitrate or barium chloride. In the present invention, the precipitant is selected from barium nitrate or barium chloride, preferably barium nitrate. The reaction temperature is preferably 90-100 ℃, the slight boiling is kept, and the time is preferably 1.5-2 h. And calculating the content of selenium in the crude selenium according to the mass of the dried precipitate.
In the invention, the mass ratio of the crude selenium to the reducing agent is preferably 1 (6-10), more preferably 1: (7-9). The mass-to-volume ratio of crude selenium to acid is preferably 1 g: (30-50) ml, more preferably 1 g: (35-45) ml.
The mass volume ratio of the crude selenium to the oxidant is 1 g: (16-24) ml, preferably 1 g: (18-22) ml;
the mass-to-volume ratio of crude selenium to the aqueous solution of the substance salifying the oxidation product is preferably 1 g: (70-90) ml, more preferably 1 g: (75-85) ml, wherein the concentration of the aqueous solution of the substance for salinizing the oxidation product is 180-220 g/L;
the mass volume ratio of the crude selenium to the aqueous solution of the precipitant is 1 g: (36-50) ml, preferably 1 g: (40-45) ml, and the concentration of the aqueous solution of the precipitator is 130-170 g/L.
In some embodiments of the present invention, the method for determining the selenium content in crude selenium comprises the following steps:
mixing and heating the crude selenium and water, and then adding hydroxylamine hydrochloride for reaction to obtain a precipitate;
dissolving the precipitate with acid, and adding perchloric acid and hydrogen peroxide for oxidation reaction;
and (3) reacting the oxidation product with sodium hydroxide and barium nitrate in sequence to obtain a precipitate, and calculating the content of selenium in the crude selenium according to the mass of the precipitate.
Wherein, the calculation formula is shown as formula (I):
in the formula (I), w is the percentage content of selenium in the crude selenium,
m1in order to be able to measure the quality of the precipitate,
m0the mass of the crude selenium is the mass of the crude selenium,
0.2817 is coefficient, 0.2817 is 78.96/280.3, 78.96 is molecular weight of Se, 280.3 is BaSeO4Molecular weight of (2).
The method for measuring the selenium content in the crude selenium provided by the invention is simple, short in flow, accurate in result and easy to master by operators. The reagent used in the method is cheap and easy to obtain, and multi-method instruments such as an ICP spectrometer and the like are avoided, so that the assay and analysis cost is reduced. The method is suitable for detection and analysis of crude selenium production, and is favorable for guiding production. And also applicable to trade settlement analysis.
For further understanding of the present invention, the method for determining selenium content in crude selenium provided by the present invention is described below with reference to the following examples, and the scope of the present invention is not limited by the following examples.
The crude selenium sample used in the following examples was produced by purifying flue gas from copper anode slime smelting, and the selenium content was approximately 80 wt% to 99 wt%, and the main impurity elements in the impurity components other than selenium included Pb, S, Cu, Te, Fe, As, and Sb. The content of the impurity elements in the crude selenium is as follows by mass percent: pb: 0.001 wt% -2 wt%; s: 0.01 wt% -3 wt%; cu: 0.001 wt% -1 wt%; te: 0.001 wt% -1 wt%; fe: 0.001 wt% -0.5 wt%; as: 0.001 wt% -0.05 wt%; sb: 0.001 wt% -0.05 wt%.
Example 1
Weighing 0.5022g (m) of crude selenium sample0) And placed in a 250mL Erlenmeyer flask. About 100mL of water was added, the mixture was boiled slightly under heating, and 4g of hydroxylamine hydrochloride was added. And (4) heating at a low temperature. Filter with slow quantitative filter paper. The pellet and beaker were washed 3 times with water. Transferring the precipitate into a beaker, adding 19mLHNO3Heating on an electric heating plate at low temperature, taking down after brown smoke is exhausted, and cooling. 4.5mL of hydrogen peroxide and 4mL of perchloric acid were added and the reaction was heated to completion at low temperature. Taken off, about 40mL of sodium hydroxide (200g/L) was slowly added to adjust the solution to a weak acidSex, heat at low temperature, slightly cool. About 21mL of barium nitrate solution (150g/L) was slowly added dropwise, heated at low temperature until the reaction was complete, and cooled. The precipitate was filtered through slow quantitative filter paper and washed with dilute nitric acid. Drying the precipitate in an electrothermal constant-temperature drying oven at 105 +/-5 ℃ for about 2 hours, cooling and weighing (m)1) And calculating the content of selenium in the sample according to the formula (I).
Example 2
Weighing 0.4981g (m) of crude selenium sample0) And placed in a 250mL Erlenmeyer flask. About 110mL of water was added, the mixture was boiled slightly under heating, and 3.5g of hydroxylamine hydrochloride was added. And (4) heating at a low temperature. Filter with slow quantitative filter paper. The pellet and beaker were washed 3 times with water. Transferring the precipitate into an original beaker, adding 22mL hydrochloric acid, heating on an electric heating plate at low temperature, taking down after brown smoke is exhausted, and cooling. 5mL of hydrogen peroxide and 5mL of perchloric acid were added and the reaction was heated to completion at low temperature. After removal, about 45mL of potassium hydroxide (220g/L) was slowly added to adjust the solution to weak acidity, and the solution was heated at low temperature and slightly cooled. About 23mL of barium nitrate solution (150g/L) was slowly added dropwise, heated at low temperature until the reaction was complete, and cooled. The precipitate was filtered through slow quantitative filter paper and washed with dilute nitric acid. Drying the precipitate in an electrothermal constant-temperature drying oven at 105 +/-5 ℃ for about 2 hours, cooling and weighing (m)1) And calculating the content of selenium in the sample according to the formula (I).
Example 3
Weighing 0.5009g (m) of crude selenium sample0) And placed in a 250mL Erlenmeyer flask. About 100mL of water was added, the mixture was boiled slightly and 5g of hydrazine hydrate was added. And (4) heating at a low temperature. Filter with slow quantitative filter paper. The pellet and beaker were washed 3 times with water. Transferring the precipitate into a beaker, adding 20mLHNO3Heating on an electric heating plate at low temperature, taking down after brown smoke is exhausted, and cooling. 6g of potassium permanganate is added, and the reaction is heated at low temperature until the reaction is complete. Taking off, slowly adding about 42mL sodium hydroxide (200g/L), adjusting the solution to weak acidity, heating at low temperature, and slightly cooling. About 20mL of barium chloride solution (170g/L) was slowly added dropwise, heated at low temperature until the reaction was complete, and cooled. The precipitate was filtered through slow quantitative filter paper and washed with dilute nitric acid. Drying the precipitate in an electrothermal constant-temperature drying oven at 105 +/-5 ℃ for about 2 hours, cooling and weighing (m)1) And calculating the content of selenium in the sample according to the formula (I).
Example 4 precision experiments
The amount of selenium in two different crude selenium samples was measured in parallel 4 times using the method of example 1 and then the relative standard deviation of the measurements was calculated. The results are shown in Table 1.
TABLE 1 precision test results
Example 5 recovery experiment
A crude selenium sample (background Se content: 85.01%) was taken, the selenium content was determined by the method of example 1, and a spiking recovery experiment was performed by quantitatively adding pure selenium (Se ≥ 99.99%), and the experimental results are shown in Table 2.
TABLE 2 recovery of sample by addition of standard
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A method for measuring the selenium content in crude selenium is characterized by comprising the following steps:
A) mixing and heating crude selenium and water, adding a reducing agent for reaction to obtain a precipitate,
the reducing agent is selected from hydroxylamine hydrochloride, hydrazine sulfate, hydrazine hydrate or tin dichloride;
B) dissolving the precipitate with acid, and then adding an oxidant to perform an oxidation reaction, wherein the oxidant is selected from the following components in a volume ratio of (4-6): (4-6) a complex oxidant of perchloric acid and hydrogen peroxide, wherein the acid is selected from nitric acid or hydrochloric acid;
C) mixing the oxidation product obtained in the step B) with sodium hydroxide, potassium hydroxide or sodium carbonate, salinizing, adding a precipitator to react to obtain precipitate, and calculating the selenium content in the crude selenium according to the mass of the precipitate, wherein the precipitator is selected from barium nitrate or barium chloride;
the formula for calculating the selenium content in the crude selenium is shown as the formula (I):
in the formula (I), w is the percentage content of selenium in the crude selenium,
m1in order to be able to measure the quality of the precipitate,
m0the mass of the crude selenium is.
2. The method according to claim 1, wherein the reaction temperature in the step A) is 90-100 ℃, and the reaction time is 30-60 minutes;
the temperature of the oxidation reaction in the step B) is 90-100 ℃, and the time is 20-40 minutes;
the reaction temperature of the step C) is 90-100 ℃, and the reaction time is 1.5-2 hours.
3. The method of claim 1, comprising the steps of:
mixing and heating the crude selenium and water, and then adding hydroxylamine hydrochloride for reaction to obtain a precipitate;
dissolving the precipitate with acid, and adding perchloric acid and hydrogen peroxide for oxidation reaction;
and (3) reacting the oxidation product with sodium hydroxide and barium nitrate in sequence to obtain a precipitate, and calculating the content of selenium in the crude selenium according to the mass of the precipitate.
4. The method of claim 1, wherein the crude selenium comprises selenium and impurity components, and main impurity elements in the impurity components comprise Pb, S, Cu, Te, Fe, As and Sb.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710270326.XA CN107101905B (en) | 2017-04-24 | 2017-04-24 | Method for measuring selenium content in crude selenium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710270326.XA CN107101905B (en) | 2017-04-24 | 2017-04-24 | Method for measuring selenium content in crude selenium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107101905A CN107101905A (en) | 2017-08-29 |
| CN107101905B true CN107101905B (en) | 2020-03-24 |
Family
ID=59657196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710270326.XA Active CN107101905B (en) | 2017-04-24 | 2017-04-24 | Method for measuring selenium content in crude selenium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107101905B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111983135A (en) * | 2020-07-04 | 2020-11-24 | 福建紫金矿冶测试技术有限公司 | Detection method for determining selenium in crude tellurium dioxide |
Family Cites Families (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02254339A (en) * | 1989-03-29 | 1990-10-15 | Mitsubishi Metal Corp | Apparatus for estimating evaporation residue in volatilizing refined material |
| US6942782B2 (en) * | 2000-03-07 | 2005-09-13 | Nalco Company | Method and apparatus for measuring deposit forming capacity of fluids using an electrochemically controlled pH change in the fluid proximate to a piezoelectric microbalance |
| CN100577559C (en) * | 2007-10-31 | 2010-01-06 | 清远先导稀有材料有限公司 | Method for producing barium selenate |
| CN101149357B (en) * | 2007-11-06 | 2010-11-24 | 苏州大学 | Selenium content detection method |
| AU2009230806B2 (en) * | 2008-10-31 | 2012-12-20 | Elanco New Zealand | Improved medicament formulation |
| CN101492181B (en) * | 2009-02-20 | 2011-07-27 | 中南大学 | Method for removing tungsten, vanadium, phosphor and arsenic from molybdate solution by deposition |
| CN101792167A (en) * | 2010-01-29 | 2010-08-04 | 张颖 | Method for preparing modified micro-barium sulfate |
| CN102086029B (en) * | 2010-12-04 | 2012-09-26 | 金川集团有限公司 | Method for extracting selenium from selenium-contained material |
| CN102175673A (en) * | 2011-01-18 | 2011-09-07 | 安徽泰格生物技术股份有限公司 | Method for detecting total selenium content |
| CN103588181B (en) * | 2013-10-30 | 2015-04-22 | 四川鑫龙碲业科技开发有限责任公司 | Wet method for preparing low-sulfur refined selenium |
| CN103592197B (en) * | 2013-11-07 | 2015-09-16 | 铜陵有色金属集团股份有限公司 | A kind of method analyzing Se content in thick selenium |
| CN103645165B (en) * | 2013-11-26 | 2016-04-06 | 金堆城钼业股份有限公司 | Measure the method for Se content in molybdenum and molybdenum product |
| CN104911358B (en) * | 2015-06-10 | 2017-07-14 | 中南大学 | A kind of method that arsenic and selenium are separated in the alkaline leaching liquid from copper anode mud |
| CN105000537B (en) * | 2015-06-29 | 2017-07-14 | 中南大学 | A kind of method for separating selenium in alkaline leaching liquid |
| CN106323933B (en) * | 2016-08-12 | 2017-07-21 | 浙江大学 | A kind of assay method of simple substance Se content |
| CN106542506A (en) * | 2016-12-08 | 2017-03-29 | 湖南水口山有色金属集团有限公司 | A kind of method that selenium is reclaimed from heavy tellurium waste liquid |
-
2017
- 2017-04-24 CN CN201710270326.XA patent/CN107101905B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107101905A (en) | 2017-08-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wu et al. | The kinetics of leaching galena concentrates with ferric methanesulfonate solution | |
| CN114487263B (en) | Method for measuring nickel cobalt manganese content in nickel cobalt manganese-containing waste | |
| CN107101905B (en) | Method for measuring selenium content in crude selenium | |
| CN108300859A (en) | A kind of method to dechlorinate in zinc electrolyte | |
| Tang et al. | Synergistic extraction of zinc from ammoniacal/ammonia sulfate solution by a mixture of β-diketone and 2-hydroxy-5-nonylacetophenone oxime | |
| Cooke et al. | Application of Lead Reductor to Determination of Uranium | |
| CN110361441B (en) | Method for detecting trace impurity elements in tungsten carbide powder | |
| JP7392393B2 (en) | Tungsten and element evaluation method | |
| CN115452807A (en) | Method for recovering rhodium and ruthenium in waste residues and method for detecting rhodium and ruthenium in waste residues | |
| CN104402068A (en) | Method for preparing high-purity rhodium trichloride from carbonyl-synthetic-reaction waste rhodium catalyst degradation solution | |
| CN104561579A (en) | Method for efficiently recovering rare and noble metals by composite reduction | |
| CN115166136A (en) | Method for measuring total sulfur content in sodium hydrosulfide | |
| CN114324736A (en) | Method for measuring content of elemental iron in reduced ilmenite powder | |
| JP6141668B2 (en) | Determination of selenium by chemical form | |
| CN111965123A (en) | Method for measuring trace heavy metal lead by inhibition kinetics photometry | |
| CN110850026A (en) | Method for analyzing COD (chemical oxygen demand) of high-chloride acidic uranium solution | |
| JP4961600B2 (en) | Processing method of zinc concentrate | |
| CN110907593A (en) | Chemical analysis method for determining nickel in nickel catalyst by changing complex anions | |
| CN117191507B (en) | Method for separating nickel in different object phases in laterite-nickel ore | |
| JP2020193939A (en) | Method for preparing sample for quantification and method for manufacturing silver chloride | |
| KR101225288B1 (en) | M-fe analysis method in reduced iron | |
| Marchenko et al. | Analysis of the Possibility of Using Carbamide for Separation of U and Pu in Extractive Processing of SNF | |
| CN110412208B (en) | Method for measuring bromine content in soot product | |
| CN107385229A (en) | The method of iron in a kind of pressurize oxygen-enriched air oxidation removal iron content, zinc solution | |
| CN112379039A (en) | Chemical analysis test method for determining zinc in high-cadmium, high-lead and high-zinc material |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wan Shuang Inventor after: Li Xianhe Inventor after: Zhao Jiuke Inventor after: Jiang Hong Inventor after: Qi Yuehua Inventor before: Wan Shuang Inventor before: Li Xianhe Inventor before: Zhao Jiuke Inventor before: Jiang Hong Inventor before: Qi Yuehua |