CN111650192A - Method for removing lead in lead-bismuth alloy and method for measuring tellurium in lead-bismuth alloy - Google Patents
Method for removing lead in lead-bismuth alloy and method for measuring tellurium in lead-bismuth alloy Download PDFInfo
- Publication number
- CN111650192A CN111650192A CN202010548113.0A CN202010548113A CN111650192A CN 111650192 A CN111650192 A CN 111650192A CN 202010548113 A CN202010548113 A CN 202010548113A CN 111650192 A CN111650192 A CN 111650192A
- Authority
- CN
- China
- Prior art keywords
- lead
- solution
- tellurium
- bismuth alloy
- measuring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 151
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 229910001152 Bi alloy Inorganic materials 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 79
- 238000005259 measurement Methods 0.000 claims abstract description 60
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000203 mixture Substances 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 48
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002244 precipitate Substances 0.000 claims abstract description 37
- 239000012488 sample solution Substances 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims description 124
- 238000002835 absorbance Methods 0.000 claims description 33
- 150000002500 ions Chemical class 0.000 claims description 26
- 239000012086 standard solution Substances 0.000 claims description 20
- -1 tellurium ions Chemical class 0.000 claims description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 12
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 12
- 239000001119 stannous chloride Substances 0.000 claims description 12
- 235000011150 stannous chloride Nutrition 0.000 claims description 12
- 230000001376 precipitating effect Effects 0.000 claims description 8
- 239000012490 blank solution Substances 0.000 claims description 7
- 150000003497 tellurium Chemical class 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000002826 coolant Substances 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 2
- 238000003723 Smelting Methods 0.000 abstract 1
- 229910052797 bismuth Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 238000003908 quality control method Methods 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 3
- 238000002798 spectrophotometry method Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000012470 diluted sample Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A method for removing lead in a lead-bismuth alloy and a method for measuring tellurium in the lead-bismuth alloy are disclosed, wherein the method for removing lead in the lead-bismuth alloy comprises the following steps: a dissolving step; removing: adding a hydrochloric acid solution to the sample solution to cause the sample solution to generate a lead ion precipitate to obtain a solid-liquid mixture, and obtaining a lead ion-removed solution from the solid-liquid mixture. The method for measuring tellurium in lead-bismuth alloy comprises the following steps: obtaining a lead ion removal solution as a measurement solution; and detecting the content of tellurium in the measured solution. Because the lead removal efficiency is high and the loss rate of tellurium is low, the serious interference of lead to the tellurium measurement result can be effectively eliminated, and the accuracy of the tellurium measurement result can be ensured. The method for removing the lead is simple and rapid to operate, the method for measuring the tellurium is high in analysis sensitivity, short in time and wide in application prospect, and meets the requirements on quality control of the lead-bismuth alloy in scientific research and production in aspects such as measurement of tellurium in raw materials and products of a lead-bismuth alloy smelting technology, measurement of tellurium in a lead-bismuth stack coolant, measurement of tellurium in raw materials of a lead storage battery and the like.
Description
Technical Field
The invention relates to the technical field of alloy component analysis, in particular to a method for removing lead in a lead-bismuth alloy and a method for measuring tellurium in the lead-bismuth alloy.
Background
With the continuous progress of the technology, the application fields of the lead bismuth alloy are more and more extensive, such as metal metallurgy, lead plates for medical use, storage batteries for ordinary use, spallation target and coolant in an accelerator driven subcritical system (ADS), reactor coolant and the like.
Some impurity elements, such as tellurium, inevitably occur in the lead bismuth alloy. The impurity elements can greatly influence the properties of the lead bismuth alloy, so that the use of the lead bismuth alloy is influenced, the content of the impurity elements needs to be accurately measured, the quality of the lead bismuth alloy can be strictly controlled, and the use requirements of the lead bismuth alloy in different fields are met.
The existing methods for measuring the content of impurity elements in the lead-bismuth alloy mainly comprise a spectrophotometry method, an atomic absorption spectrometry method, an inductively coupled plasma mass spectrometry method and the like. In the existing measurement technology, a large amount of diluted sample solution and a labeling method are adopted, the detection limit is greatly reduced due to the interference of lead ions, the accurate measurement of impurity elements is seriously influenced, and even if an expensive ICP-MS (inductively coupled plasma mass spectrometry) detection technology is adopted, the detection limit of the impurity elements is also larger than 1 mug/mL, namely 1 mug/g, for the lead-bismuth alloy sample solution with the concentration of 1 g/mL. Therefore, the method for removing the lead in the lead-bismuth alloy has very important significance for accurately measuring trace impurities.
The quality of the lead-bismuth alloy can be ensured only by controlling the content of tellurium in the lead-bismuth alloy at a low level, and the use requirements of the lead-bismuth alloy in multiple fields are met, but the prior art cannot meet the accurate measurement requirements of impurity elements, particularly tellurium, in the lead-bismuth alloy.
Therefore, the method has important significance for removing lead in the lead-bismuth alloy and simply, quickly and accurately measuring the content of tellurium in the lead-bismuth alloy. However, the prior art does not have a method for effectively removing lead in the lead-bismuth alloy and a method for simply, rapidly and accurately measuring the trace tellurium content in the lead-bismuth alloy.
Disclosure of Invention
In view of the above problems, the present invention has been made to provide a method for removing lead from a lead bismuth alloy and a method for measuring tellurium thereof, which overcome or at least partially solve the above problems.
According to one aspect of the invention, a method for removing lead in a lead-bismuth alloy is provided, wherein the method comprises the following steps: a dissolving step: dissolving the lead-bismuth alloy to obtain a sample solution containing lead ions; removing: adding a hydrochloric acid solution to the sample solution to cause lead ions in the sample solution to generate lead ion precipitates, thereby obtaining a solid-liquid mixture containing the lead ion precipitates, and obtaining a lead ion removal solution according to the solid-liquid mixture.
Optionally, the dissolving step comprises: and dissolving the lead-bismuth alloy by using nitric acid.
Optionally, the concentration of the hydrochloric acid solution is 1.5M to 6.0M, and the volume ratio of the hydrochloric acid solution to the sample solution is 3 to 8.
Optionally, obtaining the lead ion removal solution from the solid-liquid mixture comprises: and after the solid-liquid mixture is mixed more uniformly, placing the mixture for a first time threshold value to precipitate lead ion precipitates in the solid-liquid mixture, and taking supernatant of the solid-liquid mixture to obtain the lead ion removal solution.
Optionally, precipitating the lead ion precipitate in the solid-liquid mixture comprises: and precipitating the lead ion precipitate in the solid-liquid mixture through centrifugal operation, wherein the rotating speed of the centrifugal operation is 4000r/min to 5000 r/min.
Optionally, the first time threshold is 20 minutes to 40 minutes.
According to another aspect of the present invention, there is also provided a method for measuring tellurium in a lead bismuth alloy, including: obtaining a measuring solution: obtaining the lead ion removal solution obtained by the method for removing lead from the lead-bismuth alloy as a measurement solution; a measurement step: and detecting the content of tellurium in the measuring solution.
Optionally, the measuring step comprises: and detecting the absorbance of the series of tellurium standard solutions by taking the blank solution as a reference, obtaining a standard curve of the tellurium concentration and the absorbance, detecting the absorbance of the measurement solution, and obtaining the content of tellurium in the measurement solution according to the standard curve and the absorbance of the measurement solution.
Optionally, detecting the absorbance of the measurement solution comprises: and reducing the tellurium ions in the measuring solution into a tellurium simple substance through a reducing solution, and then detecting the absorbance of the measuring solution.
Optionally, the reducing of the tellurium ions in the measurement solution to elemental tellurium by a reduction solution comprises: reacting the reducing solution with the measuring solution at a set temperature for a second time threshold.
Optionally, the reducing solution is a stannous chloride solution of 0.1g/ml to 0.3 g/ml.
Optionally, the set temperature is 10 ℃ to 30 ℃ and the second time threshold is 5 minutes to 10 minutes.
Optionally, the absorbance of the series of tellurium standard solutions and the absorbance of the measurement solution are measured at a wavelength of 410 nm to 460 nm.
Compared with the prior art, the method for removing lead in the lead-bismuth alloy has the following beneficial effects:
the hydrochloric acid solution is added into the sample solution, so that lead ions in the sample solution generate lead ion precipitates, a solid-liquid mixture of the lead ion precipitates is obtained, the lead ion removing solution is obtained according to the solid-liquid mixture, the lead removing efficiency in the lead-bismuth alloy is improved, the tellurium ion precipitates can be avoided, and the low loss rate of tellurium is ensured.
The lead bismuth alloy can be dissolved by nitric acid, the dissolving effect of the lead bismuth alloy can be ensured, the concentration of the hydrochloric acid solution is set to be 1.5-6.0M, and the volume ratio of the hydrochloric acid solution to the sample solution is 3-8, so that a large amount of lead ions can be ensured to generate lead ion precipitates, and the removal efficiency of lead in the lead bismuth alloy is further improved.
The solid-liquid mixture is mixed more uniformly and then placed for a first time threshold value, lead ion precipitates in the solid-liquid mixture are precipitated, the first time threshold value is 20 minutes to 40 minutes, the lead ion precipitates in the solid-liquid mixture are precipitated through centrifugal operation, and the rotating speed of the centrifugal operation is 4000r/min to 5000r/min, so that a large amount of precipitates of the lead ion precipitates can be guaranteed, and lead can be effectively removed.
And the method for removing lead in the lead-bismuth alloy is simple, convenient, rapid and effective to operate.
Compared with the prior art, the method for measuring tellurium in the lead-bismuth alloy not only has the beneficial effects of the method for removing lead in the lead-bismuth alloy, but also has the following beneficial effects:
because the existence of lead seriously affects the accurate measurement of tellurium, the method for measuring tellurium in the lead-bismuth alloy provided by the invention removes a large amount of lead in the lead-bismuth alloy, has high lead removal efficiency and low tellurium loss rate, thereby improving the accuracy of the measurement result of tellurium and greatly eliminating the interference of lead ions on the accurate measurement of tellurium.
The tellurium in the lead bismuth alloy can greatly influence the properties of the lead bismuth alloy, so that the use of the lead bismuth alloy is influenced, the quality of the lead bismuth alloy can be effectively controlled by accurately measuring the content of the tellurium, and the use requirements of the lead bismuth alloy in multiple fields are met. And because the content of tellurium in the lead bismuth alloy needs to be controlled at a low level, the quality of the lead bismuth alloy can be ensured, and the method for measuring tellurium in the lead bismuth alloy provided by the invention is particularly suitable for measuring tellurium of which the content needs to be controlled at a low level, and is particularly suitable for accurately measuring trace tellurium.
Therefore, in order to accurately measure the content of tellurium in the lead-bismuth alloy and eliminate the serious interference of a large amount of lead to the measurement of tellurium, the invention provides a method for simply, quickly and efficiently removing lead and a method for measuring tellurium, so that the removal rate of lead is more than 97 percent, the loss rate of tellurium is not more than 4 percent, the detection limit of tellurium reaches 0.02 mu g/mL, the correlation coefficient of a standard curve is more than 0.999, the relative standard deviation is less than 5 percent, and the measurement requirement of tellurium in the lead-bismuth alloy is met.
The method utilizes different chemical properties of lead and tellurium, and adopts a simple and rapid method to remove a large amount of lead ions in the solution, thereby greatly eliminating the interference of the lead ions on the accurate measurement of the tellurium. The tellurium ions are reduced into the elemental tellurium through the stannous chloride of 0.1g/ml to 0.3g/ml, the solution is changed from colorless to black, the generation efficiency of the elemental tellurium can be ensured by setting the values of the temperature and the second time threshold, the accuracy of the measurement result is improved, the content of the trace tellurium is measured by adopting a simple, convenient, rapid and accurate spectrophotometry, and the method has important practical value.
Drawings
Other objects and advantages of the present invention will become apparent from the following description of the invention which refers to the accompanying drawings, and may assist in a comprehensive understanding of the invention.
FIG. 1 is a schematic diagram of a method for removing lead from a lead bismuth alloy according to one embodiment of the invention;
FIG. 2 is a schematic diagram of a method of measuring tellurium in a lead bismuth alloy in accordance with one embodiment of the present invention;
fig. 3 is a standard curve of tellurium in the method for measuring tellurium in a lead bismuth alloy according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention. It should be apparent that the described embodiment is one embodiment of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
This embodiment first provides a method for removing lead from a lead-bismuth alloy, and fig. 1 is a schematic diagram of the method for removing lead from a lead-bismuth alloy according to an embodiment of the present invention. The method for removing lead in the lead-bismuth alloy comprises the following steps:
s102, a dissolving step: and dissolving the lead-bismuth alloy to obtain a sample solution containing lead ions. It will be appreciated by those skilled in the art that there will also be impurity ions, such as tellurium ions, in the sample solution.
The dissolving step may include dissolving the lead bismuth alloy with nitric acid. The dissolving effect of the lead-bismuth alloy can be ensured by dissolving the lead-bismuth alloy with nitric acid. In some embodiments, the lead bismuth alloy may be dissolved with 3.5mol/L to 4.5mol/L nitric acid. For example, 3.5mol/L nitric acid, 3.8mol/L nitric acid, 4.0mol/L nitric acid, 4.2mol/L nitric acid, 4.5mol/L nitric acid, etc. can be used, and nitric acid in the concentration range has a good effect of dissolving the lead bismuth alloy, and can ensure complete dissolution of the lead bismuth alloy.
S104, removing: adding a hydrochloric acid solution to the sample solution to cause lead ions in the sample solution to generate a lead ion precipitate, thereby obtaining a solid-liquid mixture containing the lead ion precipitate, and obtaining a lead ion-removed solution from the solid-liquid mixture.
The method for removing lead in the lead-bismuth alloy improves the removal efficiency of lead in the lead-bismuth alloy and can also avoid tellurium ion precipitation, thereby ensuring that the loss rate of tellurium is low. And the method for removing lead in the lead-bismuth alloy is simple, convenient, rapid and effective to operate.
In some embodiments, the concentration of the hydrochloric acid solution may be 1.5M to 6.0M, for example, the concentration of the hydrochloric acid solution is 1.5M, 2.0M, 2.5M, 3.0M, 3.5M, 4.0M, 4.5M, 5.0M, 5.5M, 6.0M, and the like. The volume ratio of the hydrochloric acid solution to the sample solution may be 3 to 8, for example, the volume ratio of the hydrochloric acid solution to the sample solution is 3, 4, 5, 6, 7, 8, and the like. Therefore, a large amount of lead ions can be ensured to generate lead ion precipitates, wherein the lead ion precipitates comprise lead chloride, and the removal efficiency of lead in the lead-bismuth alloy is further improved.
In some embodiments, obtaining the lead ion removal solution from the solid-liquid mixture may include: and (3) after the solid-liquid mixture is mixed more uniformly, placing the mixture for a first time threshold value to precipitate lead ion precipitates in the solid-liquid mixture, and taking the supernatant of the solid-liquid mixture to obtain a lead ion removal solution.
Wherein, can make solid-liquid mixture mix more evenly through the mode of stirring. The first time threshold may be 20 minutes to 40 minutes, for example, the first time threshold may be 20 minutes, 25 minutes, 30 minutes, 35 minutes, 40 minutes, etc., and the first time threshold in this range may ensure the efficiency of the removal process while ensuring the precipitation effect.
Precipitating the lead ion precipitate in the solid-liquid mixture may include: the lead ion precipitate in the solid-liquid mixture is precipitated by centrifugation, and the rotation speed of the centrifugation may be 4000r/min to 5000r/min, for example, 4000r/min, 4100r/min, 4200r/min, 4300r/min, 4400r/min, 4500r/min, 4600r/min, 4700r/min, 4800r/min, 4900r/min, 5000r/min, or the like.
The lead ion precipitate in the solid-liquid mixture is precipitated through centrifugal operation, and the arrangement of the rotating speed of the centrifugal operation can ensure that the lead ion precipitate is precipitated in large quantity, so that lead is effectively removed.
The method for removing lead from the lead-bismuth alloy has the advantages of high lead removal efficiency, low tellurium loss rate, capability of effectively eliminating the serious interference of lead on the tellurium measurement result, capability of ensuring the accuracy of the tellurium measurement result, simplicity and convenience in operation and short required time.
This embodiment also provides a method for measuring tellurium in a lead bismuth alloy, and fig. 2 is a schematic diagram of the method for measuring tellurium in a lead bismuth alloy according to an embodiment of the present invention. The method for measuring tellurium in lead-bismuth alloy comprises the following steps:
s202, a step of obtaining a measurement solution: obtaining a lead ion removal solution obtained by any one of the methods for removing lead from a lead-bismuth alloy as a measurement solution;
s204, a measurement step: and detecting the content of tellurium in the measured solution.
The measuring step may include: and detecting the absorbance of the series of tellurium standard solutions by taking the blank solution as a reference, obtaining a standard curve of the tellurium concentration and the absorbance, detecting the absorbance of the measured solution, and obtaining the content of tellurium in the measured solution according to the standard curve and the absorbance of the measured solution.
Detecting the absorbance of the measurement solution may include: and (3) reducing the tellurium ions in the measuring solution into a tellurium simple substance through the reducing solution, and then detecting the absorbance of the measuring solution. The reducing solution may be a stannous chloride solution of 0.1g/ml to 0.3g/ml, for example, a stannous chloride solution of 0.1g/ml, a stannous chloride solution of 0.2g/ml, a stannous chloride solution of 0.3g/ml, or the like.
Reducing the tellurium ions in the measurement solution to elemental tellurium by the reducing solution may include: the reducing solution is reacted with the measurement solution at the set temperature for a second time threshold. Specifically, the set temperature may be 10 ℃ to 30 ℃, for example, the set temperature is 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃ or the like, and the second time threshold may be 5 minutes to 10 minutes, for example, the second time threshold is 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes or the like. The set temperature and the second time threshold can ensure the generation efficiency of the tellurium simple substance, thereby improving the accuracy of the measurement result.
Detecting the absorbance of the measurement solution may include: in some embodiments, the absorbance of the series of tellurium standard solutions is detected and the absorbance of the solutions is measured at wavelengths of 410 nm to 460 nm, e.g., wavelengths of 410 nm, 420 nm, 430 nm, 440 nm, 450 nm, 460 nm, etc.
Specifically, a series of tellurium standard solutions were prepared by diluting a tellurium standard solution with a measurement solution containing no tellurium. Accurately transferring 2.5mL of series tellurium standard solution, measuring solution and 0.3mL of 0.1-0.3g/mL stannous chloride solution, adding the solutions into a cuvette, uniformly mixing, reacting for 5-10 minutes at the temperature of 10-30 ℃, taking a blank solution without tellurium as a reference, measuring the absorbance of the series tellurium standard solution and the measuring solution in the wavelength range of 410-460 nanometers, taking the concentration of tellurium in the series tellurium standard solution as a horizontal coordinate and the corresponding absorbance as a vertical coordinate, drawing a standard curve, and taking a standard curve graph of tellurium in the method for measuring tellurium in the lead-bismuth alloy according to one embodiment of the invention as shown in FIG. 3. The tellurium content can be obtained by calculation.
Because the existence of lead seriously affects the accurate measurement of tellurium, the method for measuring tellurium in the lead-bismuth alloy provided by the embodiment removes a large amount of lead in the lead-bismuth alloy, has high lead removal efficiency and low tellurium loss rate, improves the accuracy of the measurement result of tellurium, and greatly eliminates the interference of lead ions on the accurate measurement of tellurium.
The tellurium in the lead bismuth alloy can greatly influence the properties of the lead bismuth alloy, so that the use of the lead bismuth alloy is influenced, the quality of the lead bismuth alloy can be effectively controlled by accurately measuring the content of the tellurium, and the use requirements of the lead bismuth alloy in multiple fields are met. And because the content of tellurium in the lead bismuth alloy needs to be controlled at a low level, the quality of the lead bismuth alloy can be ensured, and the method for measuring tellurium in the lead bismuth alloy provided by the embodiment is particularly suitable for measuring tellurium of which the content needs to be controlled at a low level, and is particularly suitable for accurately measuring trace tellurium.
Therefore, in order to accurately measure the content of tellurium in the lead-bismuth alloy and eliminate the serious interference of a large amount of lead on the measurement of tellurium, the embodiment provides a simple, rapid and efficient method for removing lead and a method for measuring tellurium, so that the removal rate of lead is more than 97%, the loss rate of tellurium is not more than 4%, the detection limit of tellurium reaches 0.02 μ g/mL, the correlation coefficient of a standard curve is more than 0.999, the relative standard deviation is less than 5%, and the measurement requirement of tellurium in the lead-bismuth alloy is met.
In the embodiment, a large amount of lead ions in the solution are removed by a simple and rapid method by utilizing different chemical properties of lead and tellurium, so that the interference of the lead ions on the accurate measurement of tellurium is greatly eliminated. The tellurium ions are reduced into the elemental tellurium through the stannous chloride of 0.1g/ml to 0.3g/ml, the solution is changed from colorless to black, the generation efficiency of the elemental tellurium can be ensured by setting the values of the temperature and the second time threshold, the accuracy of the measurement result is improved, the content of the trace tellurium is measured by adopting a simple, convenient, rapid and accurate spectrophotometry, and the method has important practical value.
The following are the operational procedures and experimental results of each embodiment:
example 1
The method comprises the following specific steps:
s102, a dissolving step: dissolving the lead-bismuth alloy by using 3.5mol/L nitric acid to obtain a sample solution containing lead ions. It will be understood by those skilled in the art that there will also be tellurium ions in the sample solution.
S104, removing: adding a hydrochloric acid solution with the concentration of 1.5M into the sample solution, wherein the volume ratio of the hydrochloric acid solution to the sample solution is 3, so that lead ions in the sample solution generate lead ion precipitates, thus obtaining a solid-liquid mixture containing the lead ion precipitates, standing the solid-liquid mixture for 20 minutes after the solid-liquid mixture is mixed more uniformly, precipitating the lead ion precipitates in the solid-liquid mixture through centrifugal operation at the rotating speed of 4000r/min, and taking the supernatant of the solid-liquid mixture to obtain the lead ion removal solution.
S202, a step of obtaining a measurement solution: obtaining a lead ion removal solution obtained in the method for removing lead from the lead-bismuth alloy as a measurement solution;
s204, a measurement step: accurately transferring 2.5mL of series tellurium standard solution, measuring solution and 0.3mL of 0.1g/mL stannous chloride solution, adding the solutions into a cuvette, uniformly mixing, reacting at 10 ℃ for 10 minutes, taking a blank solution without tellurium as a reference, measuring the absorbance of the series tellurium standard solution and the measuring solution at 410 nm, taking the concentration of tellurium in the series tellurium standard solution as an abscissa and the corresponding absorbance as an ordinate, drawing a standard curve, and obtaining the standard curve as shown in figure 3, wherein a linear equation is that y is 0.051x +0.012, r (correlation coefficient of the standard curve) is 0.9997, and the detection limit is 0.02 mu g/mL. And calculating to obtain the content of tellurium.
The experimental results of example 1 are shown in the following table:
| ion type | Content before experiment | Content after experiment | Removal/loss ratio (%) |
| Lead ion (mg/mL) | 100.0 | 1.1 | 98.9 |
| Tellurium ion (μ g/mL) | 1.000 | 0.998 | 0.2 |
Example 2
The method comprises the following specific steps:
s102, a dissolving step: dissolving the lead-bismuth alloy by using 4.0mol/L nitric acid to obtain a sample solution containing lead ions. It will be understood by those skilled in the art that there will also be tellurium ions in the sample solution.
S104, removing: adding a hydrochloric acid solution with the concentration of 3.5M into the sample solution, wherein the volume ratio of the hydrochloric acid solution to the sample solution is 5, so that lead ions in the sample solution generate lead ion precipitates, thus obtaining a solid-liquid mixture containing the lead ion precipitates, standing the solid-liquid mixture for 30 minutes after the solid-liquid mixture is mixed more uniformly, precipitating the lead ion precipitates in the solid-liquid mixture through a centrifugal operation at the rotating speed of 4500r/min, and taking the supernatant of the solid-liquid mixture to obtain a lead ion removal solution.
S202, a step of obtaining a measurement solution: obtaining a lead ion removal solution obtained in the method for removing lead from the lead-bismuth alloy as a measurement solution;
s204, a measurement step: accurately transferring 2.5mL of series tellurium standard solution, measuring solution and 0.3mL of 0.2g/mL stannous chloride solution, adding the solutions into a cuvette, uniformly mixing, reacting at 20 ℃ for 7 minutes, taking a blank solution without tellurium as a reference, measuring the absorbance of the series tellurium standard solution and the measuring solution at 435 nm, taking the concentration of tellurium in the series tellurium standard solution as an abscissa and the corresponding absorbance as an ordinate, drawing a standard curve, and obtaining the standard curve as shown in figure 3, wherein the linear equation is that y is 0.051x +0.012, r (the correlation coefficient of the standard curve) is 0.9997, and the detection limit is 0.02 mu g/mL. And calculating to obtain the content of tellurium.
The experimental results of example 2 are shown in the following table:
| ion type | Content before experiment | Content after experiment | Removal/loss ratio (%) |
| Lead ion (mg/mL) | 100.0 | 2.2 | 97.8 |
| Tellurium ion (μ g/mL) | 0.050 | 0.048 | 4.0 |
Example 3
The method comprises the following specific steps:
s102, a dissolving step: dissolving the lead bismuth alloy by using 4.5mol/L nitric acid to obtain a sample solution containing lead ions. It will be understood by those skilled in the art that there will also be tellurium ions in the sample solution.
S104, removing: adding a hydrochloric acid solution with the concentration of 6.0M into the sample solution, wherein the volume ratio of the hydrochloric acid solution to the sample solution is 8, so that lead ions in the sample solution generate lead ion precipitates, thus obtaining a solid-liquid mixture containing the lead ion precipitates, standing the solid-liquid mixture for 40 minutes after the solid-liquid mixture is mixed more uniformly, precipitating the lead ion precipitates in the solid-liquid mixture through centrifugal operation at the rotating speed of 5000r/min, and taking the supernatant of the solid-liquid mixture to obtain the lead ion removal solution.
S202, a step of obtaining a measurement solution: obtaining a lead ion removal solution obtained in the method for removing lead from the lead-bismuth alloy as a measurement solution;
s204, a measurement step: accurately transferring 2.5mL of series tellurium standard solution, measuring solution and 0.3mL of 0.3g/mL stannous chloride solution, adding the solutions into a cuvette, uniformly mixing, reacting for 5 minutes at 30 ℃, taking a blank solution without tellurium as a reference, measuring the absorbance of the series tellurium standard solution and the measuring solution at 460 nanometers, taking the concentration of tellurium in the series tellurium standard solution as an abscissa and the corresponding absorbance as an ordinate, drawing a standard curve, and obtaining the standard curve as shown in figure 3, wherein a linear equation is that y is 0.051x +0.012, r (correlation coefficient of the standard curve) is 0.9997, and the detection limit is 0.02 mu g/mL. And calculating to obtain the content of tellurium.
The experimental results of example 3 are shown in the following table:
| ion type | Content before experiment | Content after experiment | Removal/loss ratio (%) |
| Lead ion (mg/mL) | 100.0 | 1.8 | 98.2 |
| Tellurium ion (μ g/mL) | 0.050 | 0.049 | 2.0 |
As can be seen from the experimental results of the above embodiment 1, embodiment 2 and embodiment 3, the method for removing lead from the lead-bismuth alloy provided by this embodiment has high lead removal efficiency, the lead removal rate is greater than 97%, the serious interference of lead on the tellurium measurement result can be effectively eliminated, and the tellurium loss rate is not greater than 4%, so as to ensure the accuracy of the tellurium measurement result.
It should also be noted that, in the case of the embodiments of the present invention, features of the embodiments and examples may be combined with each other to obtain a new embodiment without conflict.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and the scope of the present invention is subject to the scope of the claims.
Claims (13)
1. A method for removing lead in a lead-bismuth alloy comprises the following steps:
a dissolving step: dissolving the lead-bismuth alloy to obtain a sample solution containing lead ions;
removing: adding a hydrochloric acid solution to the sample solution to cause lead ions in the sample solution to generate lead ion precipitates, thereby obtaining a solid-liquid mixture containing the lead ion precipitates, and obtaining a lead ion removal solution according to the solid-liquid mixture.
2. The method for removing lead from a lead-bismuth alloy according to claim 1, wherein the dissolving step comprises:
and dissolving the lead-bismuth alloy by using nitric acid.
3. The method for removing lead from a lead-bismuth alloy according to claim 2,
the concentration of the hydrochloric acid solution is 1.5M to 6.0M, and the volume ratio of the hydrochloric acid solution to the sample solution is 3 to 8.
4. The method for removing lead from a lead-bismuth alloy according to claim 3, wherein obtaining the lead ion removal solution from the solid-liquid mixture comprises:
and after the solid-liquid mixture is mixed more uniformly, placing the mixture for a first time threshold value to precipitate lead ion precipitates in the solid-liquid mixture, and taking supernatant of the solid-liquid mixture to obtain the lead ion removal solution.
5. The method for removing lead from a lead-bismuth alloy according to claim 4, wherein precipitating the lead ion precipitate in the solid-liquid mixture comprises:
and precipitating the lead ion precipitate in the solid-liquid mixture through centrifugal operation, wherein the rotating speed of the centrifugal operation is 4000r/min to 5000 r/min.
6. The method for removing lead from a lead-bismuth alloy according to claim 5,
the first time threshold is 20 minutes to 40 minutes.
7. A method for measuring tellurium in a lead bismuth alloy comprises the following steps:
obtaining a measuring solution: obtaining the lead ion removal solution obtained in the method for removing lead from a lead-bismuth alloy according to any one of claims 1 to 6 as a measurement solution;
a measurement step: and detecting the content of tellurium in the measuring solution.
8. The method for measuring tellurium in a lead bismuth alloy as claimed in claim 7, wherein the measuring step comprises:
and detecting the absorbance of the series of tellurium standard solutions by taking the blank solution as a reference, obtaining a standard curve of the tellurium concentration and the absorbance, detecting the absorbance of the measurement solution, and obtaining the content of tellurium in the measurement solution according to the standard curve and the absorbance of the measurement solution.
9. The method for measuring tellurium in lead-bismuth alloy according to claim 8, wherein detecting the absorbance of the measurement solution comprises:
and reducing the tellurium ions in the measuring solution into a tellurium simple substance through a reducing solution, and then detecting the absorbance of the measuring solution.
10. The method for measuring tellurium in a lead bismuth alloy as claimed in claim 9, wherein the reduction of tellurium ions in the measuring solution to elemental tellurium by a reducing solution comprises:
reacting the reducing solution with the measuring solution at a set temperature for a second time threshold.
11. The method for measuring Te in a lead-bismuth alloy according to claim 10, wherein,
the reducing solution is a stannous chloride solution of 0.1g/ml to 0.3 g/ml.
12. The method for measuring Te in a lead-bismuth alloy according to claim 11, wherein,
the set temperature is 10 ℃ to 30 ℃, and the second time threshold is 5 minutes to 10 minutes.
13. The method for measuring Te in a lead-bismuth alloy according to claim 12, wherein,
detecting the absorbance of the series of tellurium standard solutions and the absorbance of the measurement solution at a wavelength of 410 nm to 460 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010548113.0A CN111650192A (en) | 2020-06-16 | 2020-06-16 | Method for removing lead in lead-bismuth alloy and method for measuring tellurium in lead-bismuth alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010548113.0A CN111650192A (en) | 2020-06-16 | 2020-06-16 | Method for removing lead in lead-bismuth alloy and method for measuring tellurium in lead-bismuth alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111650192A true CN111650192A (en) | 2020-09-11 |
Family
ID=72349362
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010548113.0A Pending CN111650192A (en) | 2020-06-16 | 2020-06-16 | Method for removing lead in lead-bismuth alloy and method for measuring tellurium in lead-bismuth alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111650192A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113304535A (en) * | 2021-05-26 | 2021-08-27 | 中国原子能科学研究院 | Filtering component for lead-bismuth cooling reactor purifying device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102841068A (en) * | 2012-09-19 | 2012-12-26 | 白银有色集团股份有限公司 | Method for analyzing and determining bismuth content in pure lead |
| CN103088218A (en) * | 2013-01-16 | 2013-05-08 | 西北师范大学 | Method for extracting silver and lead from smelting slag generated by pyrogenic process treatment of copper anode mud |
| CN105347315A (en) * | 2015-11-18 | 2016-02-24 | 金川集团股份有限公司 | Method for extracting crude tellurium from tellurium-containing smelting waste residue |
| KR101911062B1 (en) * | 2016-11-03 | 2018-10-23 | 전남대학교산학협력단 | Electrode active material, method for manufacturing the material, carbon anode comprising the material and Pb/C battery |
-
2020
- 2020-06-16 CN CN202010548113.0A patent/CN111650192A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102841068A (en) * | 2012-09-19 | 2012-12-26 | 白银有色集团股份有限公司 | Method for analyzing and determining bismuth content in pure lead |
| CN103088218A (en) * | 2013-01-16 | 2013-05-08 | 西北师范大学 | Method for extracting silver and lead from smelting slag generated by pyrogenic process treatment of copper anode mud |
| CN105347315A (en) * | 2015-11-18 | 2016-02-24 | 金川集团股份有限公司 | Method for extracting crude tellurium from tellurium-containing smelting waste residue |
| KR101911062B1 (en) * | 2016-11-03 | 2018-10-23 | 전남대학교산학협력단 | Electrode active material, method for manufacturing the material, carbon anode comprising the material and Pb/C battery |
Non-Patent Citations (3)
| Title |
|---|
| 廖立夫等: "《分析化学》", 31 August 2015, 华中科技大学出版社 * |
| 杨丽娟等: "《铅锌质量技术监督手册》", 30 April 2002, 冶金工业出版社 * |
| 马钦科: "《元素的分光光度测定》", 31 July 1983, 地质出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113304535A (en) * | 2021-05-26 | 2021-08-27 | 中国原子能科学研究院 | Filtering component for lead-bismuth cooling reactor purifying device |
| CN113304535B (en) * | 2021-05-26 | 2022-05-13 | 中国原子能科学研究院 | Filtering component for lead-bismuth cooling reactor purifying device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Horton et al. | Separation of uranium by solvent extraction with tri-n-octylphosphine oxide. Direct colorimetric determination with dibenzoylmethane | |
| CN101995385B (en) | Ultraviolet quantitative determination method for concentration of vanadium battery positive electrolyte and application thereof | |
| CN1904097A (en) | Technology of preparing fluorine less niobium oxide by oxalic acid system extraction method | |
| CN111650192A (en) | Method for removing lead in lead-bismuth alloy and method for measuring tellurium in lead-bismuth alloy | |
| Fu et al. | Determination of metal impurity elements in lithium hexafluorophosphate using inductively coupled plasma tandem mass spectrometry based on reaction gas mixtures | |
| CN102539362B (en) | Ultraviolet quantitative determination method for concentration of electrolyte of positive electrode of vanadium battery and application thereof | |
| CN102323377A (en) | Measurement method for uranium content in ammonium diuranate | |
| CN110726790A (en) | Method for measuring chloride ions in fluorine-containing lithium salt | |
| CN101055252A (en) | Method for determining minim plumbum of aluminium ingot | |
| CN107055613A (en) | One kind is without substrate niobium pentoxide nano chip arrays negative material and its preparation method and application | |
| CN114062188B (en) | Method for measuring lithium elution amount of ternary cathode material crystal lattice | |
| CN111504924A (en) | Method for removing lead and bismuth in lead-bismuth alloy and method for measuring cadmium in lead-bismuth alloy | |
| CN112179894A (en) | Method for detecting free iron in lithium iron phosphate anode slurry of lithium ion battery | |
| CN115448280A (en) | Method for preparing lithium manganese iron phosphate from lithium iron phosphate | |
| CN112268980A (en) | Method for testing lithium type rate of nuclear-grade lithium type cation exchange resin | |
| CN111504751A (en) | Sample pretreatment method for determining total iron content | |
| CN107298449A (en) | A kind of method that liquid phase prepares nano-lithium fluoride | |
| CN117214283B (en) | Method for measuring cadmium element in hafnium and hafnium alloy | |
| CN112129753B (en) | Method for detecting chloride content in electrolyte for lithium ion battery | |
| CN116754349B (en) | ICP-OES-based digestion method for lithium sulfide impurity elements and content determination method thereof | |
| CN116338057B (en) | Detection and analysis method of difluoro sodium phosphate | |
| CN116297410A (en) | Interference shielding method for testing sulfur content in carbonate | |
| Raju et al. | Study on the effect of free acidity and entrained TBP in UNPS on the quality of ADU powder | |
| CN113072096A (en) | Preparation method of thorium-based molten salt reactor oxygen-free zirconium tetrafluoride applied to nuclear fission energy | |
| CN118083937A (en) | Manganese iron phosphate precursor, manganese iron lithium phosphate positive electrode material, preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200911 |
|
| RJ01 | Rejection of invention patent application after publication |