CN114371143A - Method for measuring trace sulfur in cathode copper - Google Patents
Method for measuring trace sulfur in cathode copper Download PDFInfo
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- CN114371143A CN114371143A CN202210038697.6A CN202210038697A CN114371143A CN 114371143 A CN114371143 A CN 114371143A CN 202210038697 A CN202210038697 A CN 202210038697A CN 114371143 A CN114371143 A CN 114371143A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000011593 sulfur Substances 0.000 title claims abstract description 72
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 72
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910052802 copper Inorganic materials 0.000 claims abstract description 34
- 239000010949 copper Substances 0.000 claims abstract description 34
- 238000004458 analytical method Methods 0.000 claims abstract description 24
- 230000003595 spectral effect Effects 0.000 claims abstract description 19
- 238000011088 calibration curve Methods 0.000 claims abstract description 16
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 150000003568 thioethers Chemical class 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 6
- 238000007865 diluting Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 75
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000012086 standard solution Substances 0.000 claims description 24
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 238000005868 electrolysis reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 11
- 238000001704 evaporation Methods 0.000 claims description 10
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 39
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 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
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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Abstract
The invention relates to the technical field of spectrochemical analysis and test, in particular to a method for measuring trace sulfur in cathode copper, which comprises the following steps: s1: preparing a solution; s2: electrolyzing to remove copper and enrich trace sulfur; s3: establishing a calibration curve; s4: the samples were tested. The method comprises the steps of dissolving a sample by using nitric acid, oxidizing by using potassium permanganate to convert all sulfides in the sample into sulfate ions, electrolyzing by using a constant-current electrolyzer to remove copper, concentrating and diluting the solution to a certain volume after the solution is faded, fixing the volume, selecting an analysis wavelength of 180.731nm when an analysis spectral line is selected on a spectrometer, avoiding spectral interference of coexisting elements on sulfur, simultaneously deducting a background at a proper position, measuring the relative spectral intensity of the sulfur, calculating the mass fraction of the sulfur on a working curve, and further realizing determination of trace sulfur.
Description
Technical Field
The invention relates to the technical field of spectrochemical analysis and test, in particular to a method for measuring trace sulfur in cathode copper.
Background
Copper is one of nonferrous metals with excellent comprehensive application performance, and is widely applied to the fields of electric power, electronics, energy, petrifaction, machinery, metallurgy, traffic, light industry, emerging industry and the like, in recent years, along with the requirement of new energy and communication industry on high conductivity of pure copper, the total amount of impurities contained in cathode copper as a raw material is required to be not more than one ten thousandth, and when the mass fraction of sulfur in the cathode copper is 0.0004%, a proper method with high precision and good accuracy does not exist at present, the accurate detection requirement cannot be met, and improvement is needed.
Chinese patent No. CN105784696A discloses an analytical determination method for sulfur in each valence state in sodium aluminate solution, in the method, sulfur in each valence state in the solution is independently determined, so that mutual interference among sulfur in each valence state is avoided, the determination effect is good, the error is small, and meanwhile, the method performs analysis in modes of titration, filtration, precipitation and the like, is simple, rapid and accurate in operation, has the beneficial effects of good determination effect, small error, simplicity and rapidness in operation, rapidness and accuracy, but does not relate to determination of trace sulfur when the mass fraction of sulfur in cathode copper is 0.0004%, and can not meet the current accurate detection requirement.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for measuring trace sulfur in cathode copper.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for measuring trace sulfur in cathode copper comprises the following steps:
s1: solution preparation: weighing cathode copper, adding potassium permanganate to quantitatively convert sulfides in a sample into sulfate ions, and adding a depolarizer ammonium chloride to eliminate the influence of nitrous acid on electrolytic copper removal;
s2: electrolytic copper removal and trace sulfur enrichment: controlling the electrolytic current to electrolyze and remove copper, heating and concentrating the solution after copper removal, and fixing the volume to a certain volume;
s3: establishing a calibration curve: preparing a series of standard solutions according to the concentration range of sulfur after the solution is concentrated;
s4: and (3) determining a sample: selecting the analysis spectral line and background deduction position of sulfur, establishing an analysis method and measuring on a computer.
In order to ensure that the sulfide in the sample is completely oxidized, the improvement of the invention is that 5.0000g of the sample is weighed in a 250mL high glass beaker in S1, 35mL of nitric acid (1+1) is added to be dissolved at low temperature and evaporated, the sample is taken down and cooled, ammonium chloride solution is added to 150mL, about 4mL of potassium permanganate solution is added dropwise and continuously stirred, so that the solution is changed from blue to dark purple, and all sulfides in the oxidized sample are sulfate ions.
In order to ensure that all sulfide in a sample is converted into sulfate ions, the invention improves the method, evaporation is needed in the evaporation process until the cup wall is oily for 8-10 minutes, the concentration of the ammonium chloride solution is set to be 0.02g/L, and the mass fraction of the potassium permanganate solution is 2%.
In order to improve the treatment effect of removing copper and enriching trace sulfur by electrolysis, the invention improves the steps that a magnetic stirring rod is placed in a beaker in S2, the beaker is placed on a tray of an electrolyzer, a stirring device is started to stir the solution uniformly, a platinum anode and a platinum cathode are arranged on the electrolyzer, a cathode net is immersed in the solution, two half watch glasses are used for covering a high-type beaker, and the surface of the cathode is about 2.0A/dm2Stirring and electrolyzing under the current density of (1) until the solution is colorless, washing the watch glass, the cup wall and the electrolytic rod with water, and reducing the current density to 1.0A/dm2And continuing electrolysis, if the newly immersed electrode part has no copper precipitation, the electrolysis is complete.
In order to ensure the copper removal effect and improve the accuracy of a detection result, the improvement of the invention is that after the electrolysis is completed, the power supply is not cut off, the electrode is slowly lifted, the electrode is rinsed by water, the washing solution and the solution after the copper is resolved by electricity are combined, evaporated at a low temperature to be less than 50mL in volume, cooled, then moved into a 50mL volumetric flask, diluted by water to scale and mixed uniformly, and a blank test is carried out along with a sample.
In order to ensure the smooth establishment of the calibration curve, the invention improves that in the process of establishing the calibration curve in the S3, 0mL, 1.00mL, 5.00mL and 10.00mL of sulfur standard solutions and 5.00mL of sulfur standard solutions are added into a group of 100mL volumetric flasks, 5mL of nitric acid (1+1) is respectively added, the volumetric flasks are diluted to the scale with water and are uniformly mixed, and the concentration of the solution in each volumetric flask is 0ug/mL, 0.10ug/mL, 0.50ug/mL, 1.00ug/mL and 5.00 ug/mL.
In order to ensure the concentration of the solution in each volumetric flask, the invention improves that the concentration of the added 0mL, 1.00mL, 5.00mL and 10.00mL sulfur standard solution is 10ug/mL, and the concentration of the added 5.00mL sulfur standard solution is 100 ug/mL.
In order to ensure the smooth operation of the measured sample, the invention improves the method that the instrument is opened when the sample is measured in the S4, after the instrument is stabilized, the analysis spectral line is selected, the content of sulfur element in the standard solution is input into the equipment analysis software, and the standard solution is sucked one by one to establish a calibration curve equation.
In order to improve the accuracy of the sample, the invention improves that the linear correlation coefficient of the curve equation is not lower than 0.999, and the wavelength of the spectral line is selected to be 180.731 nm.
In order to further ensure the accuracy of the whole analysis process, the invention improves that the water used in the determination analysis process is distilled water or water with equivalent purity.
Compared with the prior art, the invention has the advantages and positive effects that:
in the invention, a sample is dissolved by nitric acid, sulfides in the sample are completely converted into sulfate ions by potassium permanganate oxidation, copper is removed by electrolysis by a constant current electrolyzer, the solution is concentrated and diluted to a certain volume after being faded, the volume is fixed, the analysis wavelength is selected to be 180.731nm when an analysis spectral line is selected on a spectrometer, the spectral interference of coexisting elements to sulfur is avoided, the background is deducted at a proper position, the relative spectral intensity of sulfur is measured, the mass fraction of sulfur is calculated on a working curve, and then the determination of trace sulfur is realized.
Drawings
FIG. 1 is a schematic diagram of a preparation process of a method for measuring trace sulfur in cathode copper according to the present invention;
FIG. 2 is a schematic diagram of the result of the precision measurement in the embodiment of the method for measuring trace sulfur in cathode copper according to the present invention;
FIG. 3 is a graph showing the experimental results of the spiking recovery rate experiment in the embodiment of the method for measuring trace sulfur in cathode copper according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1, the present invention provides a technical solution: a method for measuring trace sulfur in cathode copper comprises the following steps:
s1: solution preparation: weighing cathode copper, adding potassium permanganate to quantitatively convert sulfides in a sample into sulfate ions, and adding a depolarizer ammonium chloride to eliminate the influence of nitrous acid on electrolytic copper removal;
s2: electrolytic copper removal and trace sulfur enrichment: controlling the electrolytic current to electrolyze and remove copper, heating and concentrating the solution after copper removal, and fixing the volume to a certain volume;
s3: establishing a calibration curve: preparing a series of standard solutions according to the concentration range of sulfur after the solution is concentrated;
s4: and (3) determining a sample: selecting the analysis spectral line and background deduction position of sulfur, establishing an analysis method and measuring on a computer.
Weighing 5.0000g of a sample in S1, placing the sample in a 250mL high-strength glass beaker, adding 35mL of nitric acid (1+1) for low-temperature dissolution and evaporation, taking down and cooling, adding an ammonium chloride solution to 150mL, dropwise adding about 4mL of a potassium permanganate solution, continuously stirring to change the solution from blue to dark purple, wherein all sulfides in the oxidized sample are sulfate ions, the sulfide in the sample can be completely oxidized, the evaporation is required in the evaporation process until the cup wall appears oily for 8-10 minutes, the concentration of the ammonium chloride solution is set to be 0.02g/L, the mass fraction of the potassium permanganate solution is 2%, and the sulfide in the sample can be further ensured to be completely converted into the sulfate ions.
S2, putting a magnetic stirring rod into the beaker, putting the beaker on a tray of an electrolyzer, starting a stirring device to stir the solution uniformly, installing a platinum anode and a platinum cathode on the electrolyzer to immerse a cathode net in the solution, covering the beaker with two half-pieces of watch glass, and covering the surface of the cathode with a high-type beaker, wherein the surface of the cathode is about 2.0A/dm2Stirring and electrolyzing under the current density of (1) until the solution is colorless, washing the watch glass, the cup wall and the electrolytic rod with water, and reducing the current density to 1.0A/dm2And continuing electrolysis, if no copper is separated out from the newly immersed electrode part, indicating that the electrolysis is complete, greatly improving the treatment effect of removing copper by electrolysis and enriching trace sulfur, slowly lifting the electrode without cutting off the power supply after the electrolysis is complete, rinsing the electrode with water, combining the washing solution and the solution after copper is electrolyzed, evaporating the solution at a low temperature to a volume below 50mL, cooling, transferring the solution into a 50mL volumetric flask, diluting the solution with water to scale, mixing the solution uniformly, carrying out a blank test along with the sample, and ensuring the smooth operation of the blank test along with the sample.
In the process of establishing the calibration curve in S3, 0mL, 1.00mL, 5.00mL, 10.00mL of sulfur standard solution and 5.00mL of sulfur standard solution are added into a group of 100mL volumetric flasks, 5mL of nitric acid (1+1) is respectively added, the solutions are diluted to the scales with water and mixed uniformly, the concentrations of the solutions in the volumetric flasks are 0ug/mL, 0.10ug/mL, 0.50ug/mL, 1.00ug/mL and 5.00ug/mL, the concentrations of the solutions in the volumetric flasks are 10ug/mL, and the concentration of the solution in the 5.00mL of sulfur standard solution is 100ug/mL, so that the concentration of the solution in each volumetric flask can be ensured, and the smooth establishment of the calibration curve is further ensured.
And (S4) opening the instrument when the sample is measured, selecting an analysis spectral line after the instrument is stabilized, inputting the content of sulfur elements in the standard solution into equipment analysis software, sucking the standard solution one by one to establish a calibration curve equation, wherein the linear correlation coefficient of the curve equation is not less than 0.999, and the wavelength of the spectral line is selected to be 180.731nm, so that the spectral interference of coexisting elements on sulfur can be avoided, and the data accuracy of the measured sample is ensured.
Distilled water or water with equivalent purity is adopted in the water used in the determination and analysis process, and the distilled water or the water with equivalent purity is utilized, so that the error can be greatly reduced, and the accuracy of the whole analysis process is further ensured.
Examples
Referring to FIGS. 1-3, the actual sample of cathode copper sample number SYD2001 was tested as follows:
s1: solution preparation: sample dissolution: weighing 5.0000g of sample in a 250mL high glass beaker, adding 35mL of nitric acid (1+1) for low-temperature dissolution, evaporating until the wall of the beaker is oily for 8-10 minutes, taking down and cooling, adding ammonium chloride solution (0.02g/L) to 150mL, dropwise adding about 4mL of potassium permanganate (2%) solution, continuously stirring to change the solution from blue to dark purple, oxidizing all sulfides in the sample into sulfate ions, and carrying out a blank experiment along with the sample;
s2: electrolytic copper removal and trace sulfur enrichment: putting a magnetic stirring rod into the beaker, putting the beaker on a tray of an electrolyzer, starting a stirring device to uniformly stir the solution, installing a platinum anode and a platinum cathode on the electrolyzer, immersing a cathode net in the solution, covering the high-type beaker with two half watch glasses, and covering the surface of the cathode by about 2.0A/dm2Stirring and electrolyzing under the current density of (1) until the solution is colorless, washing the watch glass, the cup wall and the electrolytic rod with water, and reducing the current density to 1.0A/dm2And continuing electrolysis, if the newly immersed electrode part has no copper precipitation, indicating that the electrolysis is complete, not cutting off the power supply, slowly lifting the electrode, and rinsing the electrode by using water. Combining the washing solution and the solution after copper is electrically separated out, evaporating at low temperature until the volume is below 50mL, cooling, transferring the solution with the mass fraction of 0.0004-0.005% into a 50mL volumetric flask, diluting with water to scale, and mixing uniformly;
s3: establishing a calibration curve: opening the instrument, selecting an analysis spectral line after the instrument automatically completes system initialization, inputting the concentrations of 0, 0.1ug/ml, 0.5ug/ml, 1.0ug/ml and 5.0ug/ml sulfur standard solutions into equipment analysis software, and sucking the standard solutions one by one to establish a calibration curve equation to obtain a calibration curve;
s4: and (3) determining a sample: inputting the mass of a sample into instrument operation software, carrying out sulfur element intensity measurement on a sample solution and a reagent blank after electrolytic copper removal concentration, carrying out spectrogram superposition on each point of a working curve and the sample, selecting a spectral line without interference and a flat background position to subtract the background, automatically calculating the content of sulfur elements in the reagent blank and the sample by an instrument, selecting a standard substance close to the content of the element to be measured of the sample as a control sample after the sample is measured, verifying the accuracy of the result, carrying out 7 times of sulfur content measurement on a cathode copper SYD2001 sample, wherein the relative standard deviation is the precision;
and (3) parallelly processing cathode copper SYD2001 sample solutions to perform a standard recovery rate experiment, respectively adding 2.0ml of sulfur standard solution (10ug/ml), which is equivalent to 20ug of sulfur, measuring a standard addition amount, and calculating the standard recovery rate.
The working principle is as follows: firstly, solution preparation is carried out, cathode copper is weighed, potassium permanganate is added to enable sulfide in a sample to be quantitatively converted into sulfate ions, a depolarizer ammonium chloride is added to eliminate nitrous acid influence, then electrolytic copper removal is carried out to enrich trace sulfur, electrolytic copper removal is carried out under the condition of controlling the electrolytic current, the solution after copper removal is heated and concentrated, the constant volume is set to a certain volume, a calibration curve is established, a series of standard solutions are prepared according to the concentration range of sulfur after solution concentration, finally, a sample is measured, an analysis spectral line and a background position of sulfur are selected, and the analysis method is established for on-machine measurement.
Although the present invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The method for measuring trace sulfur in cathode copper is characterized by comprising the following steps of:
s1: solution preparation: weighing cathode copper, adding potassium permanganate to quantitatively convert sulfides in a sample into sulfate ions, and adding a depolarizer ammonium chloride to eliminate the influence of nitrous acid on electrolytic copper removal;
s2: electrolytic copper removal and trace sulfur enrichment: controlling the electrolytic current to electrolyze and remove copper, heating and concentrating the solution after copper removal, and fixing the volume to a certain volume;
s3: establishing a calibration curve: preparing a series of standard solutions according to the concentration range of sulfur after the solution is concentrated;
s4: and (3) determining a sample: selecting the analysis spectral line and background deduction position of sulfur, establishing an analysis method and measuring on a computer.
2. The method for measuring trace sulfur in cathode copper according to claim 1, wherein: weighing 5.0000g of a sample in the S1, putting the sample in a 250mL high glass beaker, adding 35mL of nitric acid (1+1) to dissolve at a low temperature and evaporate, taking down and cooling, adding an ammonium chloride solution to 150mL, dropwise adding about 4mL of a potassium permanganate solution, and continuously stirring to change the solution from blue to dark purple, wherein all sulfides in the oxidized sample are sulfate ions.
3. The method for measuring trace sulfur in cathode copper according to claim 2, wherein: in the evaporation process, the solution needs to be evaporated until the cup wall appears oily for 8-10 minutes, the concentration of the ammonium chloride solution is set to be 0.02g/L, and the mass fraction of the potassium permanganate solution is 2%.
4. The method for measuring trace sulfur in cathode copper according to claim 1, wherein: in the process of removing copper and enriching trace sulfur by electrolysis in S2, a magnetic stirring rod is placed in a beaker and placed on an electrolyzer tray, a stirring device is started to stir the solution uniformly, a platinum anode and a platinum cathode are installed on the electrolyzer to immerse a cathode net in the solution, and two half watchwares are covered with a high watch plateBeaker, about 2.0A/dm on cathode surface2Stirring and electrolyzing under the current density of (1) until the solution is colorless, washing the watch glass, the cup wall and the electrolytic rod with water, and reducing the current density to 1.0A/dm2And continuing electrolysis, if the newly immersed electrode part has no copper precipitation, the electrolysis is complete.
5. The method for measuring trace sulfur in cathode copper according to claim 4, wherein: and after the electrolysis is completed, slowly lifting the electrode without cutting off a power supply, rinsing the electrode with water, combining a washing solution with the solution after copper is electrolyzed out, evaporating the solution to a volume of below 50mL at a low temperature, cooling the solution, transferring the solution into a 50mL volumetric flask, diluting the solution with water to scale, and uniformly mixing the solution and the sample to perform a blank test.
6. The method for measuring trace sulfur in cathode copper according to claim 1, wherein: in the process of establishing the calibration curve in the S3, adding 0mL, 1.00mL, 5.00mL and 10.00mL sulfur standard solutions and 5.00mL sulfur standard solutions into a group of 100mL volumetric flasks, respectively adding 5mL nitric acid (1+1), diluting with water to scale, and uniformly mixing, wherein the concentration of the solution in each volumetric flask is 0ug/mL, 0.10ug/mL, 0.50ug/mL, 1.00ug/mL and 5.00 ug/mL.
7. The method for measuring trace sulfur in cathode copper according to claim 6, wherein: the concentrations of the added 0mL, 1.00mL, 5.00mL and 10.00mL sulfur standard solutions are 10ug/mL, and the concentration of the added 5.00mL sulfur standard solution is 100 ug/mL.
8. The method for measuring trace sulfur in cathode copper according to claim 1, wherein: and (4) opening the instrument when the sample is measured in the S4, selecting an analysis spectral line after the instrument is stabilized, inputting the content of sulfur elements in the standard solution into the equipment analysis software, and sucking the standard solution one by one to establish a calibration curve equation.
9. The method for measuring trace sulfur in cathode copper according to claim 8, wherein: the linear correlation coefficient of the curve equation should not be lower than 0.999, and the wavelength of the spectral line is selected to be 180.731 nm.
10. The method for measuring trace sulfur in cathode copper according to claim 1, wherein: distilled water or water with equivalent purity is adopted as water used in the determination analysis process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210038697.6A CN114371143A (en) | 2022-01-13 | 2022-01-13 | Method for measuring trace sulfur in cathode copper |
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| CN202210038697.6A CN114371143A (en) | 2022-01-13 | 2022-01-13 | Method for measuring trace sulfur in cathode copper |
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- 2022-01-13 CN CN202210038697.6A patent/CN114371143A/en not_active Withdrawn
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