CN111983135A - Detection method for determining selenium in crude tellurium dioxide - Google Patents
Detection method for determining selenium in crude tellurium dioxide Download PDFInfo
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Abstract
The invention relates to the technical field of analysis and test, in particular to a detection method for measuring selenium in crude tellurium dioxide, in particular to a method for measuring the selenium content of 1.00-10.00% in crude tellurium dioxide, wherein a sample is dissolved by nitric acid, after sulfuric acid smokes, in 6mol/L hydrochloric acid medium, reducing selenium into elemental selenium by using hydroxylamine hydrochloride, separating the elemental selenium from other impurities, dissolving precipitate by using acid, starch is taken as an indicator, potassium iodide is added, sodium thiosulfate standard titration solution is used for titration to determine the selenium content in the crude tellurium dioxide, and the aim is to provide a method for detecting the selenium content in the crude tellurium dioxide, which has the advantages of low cost, rapidness and accuracy and can meet the requirements of production and scientific research, the method for measuring the selenium content in the crude tellurium dioxide has good accuracy and precision, the standard recovery rate is 98.6-101.4%, and the relative standard deviation is 0.38-1.70%.
Description
Technical Field
The invention relates to the technical field of analysis and test, in particular to a detection method for measuring selenium in crude tellurium dioxide.
Background
Enterprises comprehensively recover valuable metals from copper smelting byproducts to obtain good economic benefits, wherein the byproducts comprise byproducts in the copper smelting process, and comprise main elements of tellurium dioxide and impurity elements such as copper, lead, arsenic, antimony, bismuth, selenium and the like, precious metal elements such as gold, silver and the like, and valuable elements are comprehensively recovered from copper anode slime to realize the comprehensive utilization of resources, so that the industrial trend is formed.
Disclosure of Invention
The invention aims to provide a detection method for measuring selenium in crude tellurium dioxide, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a detection method for measuring selenium in crude tellurium dioxide comprises the following steps:
the first step is as follows: decomposing a test material by using nitric acid and sulfuric acid;
the second step is that: reducing in hydrochloric acid medium by hydroxylamine hydrochloride;
the third step: filtering and separating impurities;
the fourth step: and (4) titrating.
Preferably, when the nitric acid and the sulfuric acid are used for decomposing the test material, the test material is weighed and placed in a 500mL conical beaker, 10mL nitric acid is added, the surface dish is covered, the solution is completely dissolved by heating at a low temperature, 5mL sulfuric acid is added, the temperature is heated until white smoke just comes off, the cooling is carried out, the surface dish and the wall of the beaker are flushed by a small amount of water, the heating is continued until the white smoke just comes off, the cooling is carried out, and the surface dish and the wall of the beaker are flushed by a small amount of water.
Preferably, during the reduction process of hydroxylamine hydrochloride in hydrochloric acid medium, 100mL (1+20) of hydrochloric acid is added, the mixture is heated to slight boiling to dissolve salts, 1 g-2 g of tartaric acid is added, 2 g-4 g of hydroxylamine hydrochloride is slowly added, and the solution is shaken while adding until the salts are dissolved. Heating at low temperature to keep the solution slightly boiling, and keeping the temperature for 1.5-2 h.
Preferably, in the process of filtering to separate impurities, after the precipitate is completely blackened and coagulated, the precipitate is filtered by slow filter paper, the beaker and the precipitate are washed 5 times each by (1+20) hydrochloric acid, and the precipitate is washed by water about 10 times. And transferring the precipitate and filter paper into an original beaker, adding 15mL of hydrochloric acid and 0.5 mL-1 mL of nitric acid, covering a surface dish, placing on a water bath at 60-70 ℃ for heating and dissolving, taking down after the precipitate is completely dissolved, adding 100mL of boiling water and 2g of urea, boiling for 3min, taking down, and cooling to room temperature.
Preferably, during the titration operation, phenolphthalein ethanol solution is used as an indicator, sodium hydroxide solution is used for neutralization to make the solution alkaline, 20mL (1+1) sulfuric acid is added, cooling is carried out, sodium thiosulfate standard solution is used for titration for about 4mL, 3mL starch solution and 2 drops potassium iodide solution are added under full stirring, sodium thiosulfate standard solution is used for titration until the blue color disappears, a few drops of potassium iodide solution are added, titration is carried out until the blue color disappears, and the steps are repeated until the blue color of the solution does not change after the potassium iodide solution is added, namely the end point.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention aims to provide a method for detecting the selenium content in the crude tellurium dioxide, which has the advantages of low cost, rapidness and accuracy and can meet the requirements of production and scientific research;
2. in the invention, the method for measuring the selenium content in the crude tellurium dioxide has good accuracy and precision, the standard recovery rate is 98.6-101.4%, and the relative standard deviation is 0.38-1.70%.
Drawings
FIG. 1 is a process of analyzing the selenium content in crude tellurium dioxide according to the present invention;
FIG. 2 is a table of the results of the sample analysis experiments of the present invention.
Detailed Description
Referring to fig. 1 and fig. 2, the present invention provides a technical solution:
a detection method for measuring selenium in crude tellurium dioxide,
1. sodium thiosulfate standard titration solution calibration
Weighing accurate three parts of 0.10g of potassium dichromate which is dried to constant weight at 120 +/-2 ℃, placing the potassium dichromate in a 250mL iodine flask, dissolving the potassium dichromate in 25mL of water, adding 2g of potassium iodide and 20mL of sulfuric acid solution, uniformly mixing, placing the mixture in a dark place for 10min, adding 150mL of water (15 ℃ -20 ℃), titrating the mixture by using a sodium thiosulfate standard titration solution, adding 2 drops of a starch solution (2.3.11) when the endpoint is approached, continuously titrating the mixture until the solution is changed from blue to bright green, and simultaneously carrying out a blank test.
The actual concentration of the sodium thiosulfate standard titration solution was calculated according to formula (1):
C＝(m×1000)/((V_1-V_2)×M)------------(1)
in the formula:
c-the mass concentration of the standard solution of sodium thiosulfate, moL/L;
m-weighing the mass of potassium dichromate, g;
v1-volume of standard solution of sodium thiosulfate consumed by titration, mL;
v2-volume of sodium thiosulfate standard solution consumed in blank experiment, mL;
m-molar mass of potassium dichromate, g/moL, is [ M (1/6K2Cr2O7) ═ 49.031 ].
2. Analysis of
Weighing a test material, placing the test material in a 500mL conical beaker, adding 10mL nitric acid, covering a watch glass, heating at low temperature to completely dissolve the test material, adding 5mL sulfuric acid, heating until white smoke just emits, taking down the test material to cool, blowing and washing the watch glass and the wall of the glass by using a small amount of water, continuing heating until white smoke just emits, taking down the test material to cool, and blowing and washing the watch glass and the wall of the glass by using a small amount of water.
Adding 100mL (1+20) of hydrochloric acid, heating to slightly boil to dissolve salts, taking down and adding 1 g-2 g of tartaric acid, slowly adding 2 g-4 g of hydroxylamine hydrochloride, and shaking the solution while adding until the solution is dissolved. Then adding a little paper pulp, placing the paper pulp at the low temperature of an electric heating plate, heating the paper pulp to slightly boil, preserving the heat for 1.5 to 2 hours at the temperature of between 80 and 90 ℃, standing and clarifying the paper pulp after the precipitate is condensed, and filtering the paper pulp by using slow-speed filter paper.
The beaker and the precipitate were washed 5 times each with (1+20) hydrochloric acid and the precipitate was washed with water about 10 times.
And transferring the precipitate and filter paper into an original beaker, adding 15mL of hydrochloric acid and 0.5 mL-1 mL of nitric acid, covering a surface dish, placing on a water bath at 60-70 ℃ for heating and dissolving, taking down after the precipitate is completely dissolved, adding 100mL of boiling water and 2g of urea, boiling for 3min, taking down, and cooling to room temperature.
Taking phenolphthalein ethanol solution as an indicator, neutralizing with sodium hydroxide solution to make the solution alkaline, adding 20mL (1+1) of sulfuric acid, cooling, dripping about 4mL of sodium thiosulfate standard solution, uniformly stirring, adding 3mL of starch solution and 2 drops of potassium iodide solution, continuously titrating with the sodium thiosulfate standard solution until the blue color disappears, adding a few drops of potassium iodide solution, continuously titrating until the blue color disappears, and repeating the steps until the solution does not change into the blue color after the potassium iodide solution is added, namely the end point.
Note: the amount of the sodium thiosulfate standard solution added for the first time depends on the selenium content of the sample.
3. Presentation of analytical results
The mass fraction of selenium is in omega and the value% is expressed, and the content is calculated according to the formula (2):
ω(Se)＝(C×(V_3-V_0)×78.96)/(m×4)×10^(-3)×100(2)
in the formula:
c, the quantity concentration of substances of the sodium thiosulfate standard solution is expressed in moL per liter (moL/L);
v3-at the time of titration, the sample consumed the volume of sodium thiosulfate standard solution in milliliters (mL);
v0 — blank consumption of volume of sodium thiosulfate standard solution in milliliters (mL) for titration;
78.96-molar mass of selenium in gram moles (g/moL);
m is the mass of the sample in grams g.
The calculation result is expressed to the last two decimal places.
Example 1:
selecting a crude tellurium dioxide sample in the copper smelting process of a certain plant, performing standard addition recovery and a precision test according to a proposed analysis method, wherein the experimental analysis results are 1.79%, 1.80%, 1.87%, 1.86%, 1.85%, 1.86% and 1.84%, the relative standard deviation of the sample determination is 1.70%, when the selenium content is 5mg, the selenium content is 5.07mg, the selenium recovery rate is 101.4%, when the selenium content is 10.00mg, the selenium content is 10.13mg, and the selenium recovery rate is 101.3%.
Example 2:
selecting a crude tellurium dioxide sample in the copper smelting process of a certain plant, and performing standard addition recovery and precision test according to a proposed analysis method, wherein the experimental analysis results are 3.13%, 3.12%, 3.19%, 3.18%, 3.17%, 3.23% and 3.19%, the relative standard deviation of the sample determination is 3.17%, and the deviation is large.
Example 3:
selecting a crude tellurium dioxide sample in the copper smelting process of a certain plant, performing standard addition recovery and a precision test according to a proposed analysis method, wherein the experimental analysis results are 4.64%, 4.63%, 4.68%, 4.72%, 4.69% and 4.70%, the relative standard deviation of the sample determination is 0.69%, when the selenium content is 5mg, the selenium content is 4.93mg, the selenium recovery rate is 98.6%, when the selenium content is 10.00mg, the selenium content is 9.99mg, and the selenium recovery rate is 99.9%.
Example 4:
selecting a crude tellurium dioxide sample in the copper smelting process of a certain plant, and performing standard addition recovery and precision test according to a proposed analysis method, wherein the experimental analysis results are 5.51%, 5.52%, 5.49%, 5.47%, 5.53% and 5.52%, the relative standard deviation of the sample determination is 5.50%, and the deviation is large.
Example 5:
selecting a crude tellurium dioxide sample in the copper smelting process of a certain plant, performing standard addition recovery and a precision test according to a proposed analysis method, wherein the experimental analysis results are 6.98%, 7.00%, 6.99%, 7.02%, 7.00%, 7.02% and 7.06%, the relative standard deviation of the sample determination is 0.38%, when the selenium content is 5mg, the selenium content is 5.00mg, the selenium recovery rate is 100.0%, when the selenium content is 10.00mg, the selenium content is 10.06mg and the selenium recovery rate is 100.6%.
The result shows that the relative standard deviation of the sample measurement is between 0.38% and 1.70%, and the sample standard addition recovery rate is between 98.6% and 101.4%. The method has high result accuracy and good precision, and meets the analysis requirements.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. The foregoing is only a preferred embodiment of the present invention, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present invention, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (5)
1. A detection method for measuring selenium in crude tellurium dioxide is characterized by comprising the following steps:
the first step is as follows: decomposing a test material by using nitric acid and sulfuric acid;
the second step is that: reducing in hydrochloric acid medium by hydroxylamine hydrochloride;
the third step: filtering and separating impurities;
the fourth step: and (4) titrating.
2. The detection method for detecting selenium in crude tellurium dioxide as claimed in claim 1, wherein: when the nitric acid and the sulfuric acid are used for decomposing the test material, weighing the test material, placing the test material in a 500mL conical beaker, adding 10mL nitric acid, covering a surface dish, heating at a low temperature until the test material is completely dissolved, adding 5mL sulfuric acid, heating until white smoke just appears, taking down and cooling, purging the surface dish and the wall of the beaker with a small amount of water, continuing heating until the white smoke just appears, taking down and cooling, and purging the surface dish and the wall of the beaker with a small amount of water.
3. The detection method for detecting selenium in crude tellurium dioxide as claimed in claim 1, wherein: in a hydrochloric acid medium, in the process of reducing by hydroxylamine hydrochloride, adding 100mL (1+20) of hydrochloric acid, heating to slight boiling to dissolve salts, taking down, adding 1 g-2 g of tartaric acid, slowly adding 2 g-4 g of hydroxylamine hydrochloride, shaking the solution while adding until the salts are dissolved, heating at low temperature to keep the solution slight boiling, and preserving heat for 1.5 h-2 h.
4. The detection method for detecting selenium in crude tellurium dioxide as claimed in claim 1, wherein: in the process of filtering and separating impurities, after the precipitate is completely blackened and coagulated, filtering by using slow filter paper, washing the beaker and the precipitate by using (1+20) hydrochloric acid for 5 times respectively, and washing the precipitate by using water for about 10 times. And transferring the precipitate and filter paper into an original beaker, adding 15mL of hydrochloric acid and 0.5 mL-1 mL of nitric acid, covering a surface dish, placing on a water bath at 60-70 ℃ for heating and dissolving, taking down after the precipitate is completely dissolved, adding 100mL of boiling water and 2g of urea, boiling for 3min, taking down, and cooling to room temperature.
5. The detection method for detecting selenium in crude tellurium dioxide as claimed in claim 1, wherein: during titration, phenolphthalein ethanol solution is used as an indicator, sodium hydroxide solution is used for neutralization to make the solution alkaline, 20mL (1+1) of sulfuric acid is added, cooling is carried out, sodium thiosulfate standard solution is used for titration of about 4mL, 3mL of starch solution and 2 drops of potassium iodide solution are added under full stirring, sodium thiosulfate standard solution is continuously used for titration until blue color disappears, a few drops of potassium iodide solution are added, titration is continued until blue color disappears, and the steps are repeated until the solution does not change to blue color after the potassium iodide solution is added, namely the end point.
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