CN113916868A - Method for measuring copper content in copper ash of copper alloy smelting furnace - Google Patents
Method for measuring copper content in copper ash of copper alloy smelting furnace Download PDFInfo
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- CN113916868A CN113916868A CN202010663701.9A CN202010663701A CN113916868A CN 113916868 A CN113916868 A CN 113916868A CN 202010663701 A CN202010663701 A CN 202010663701A CN 113916868 A CN113916868 A CN 113916868A
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- 239000010949 copper Substances 0.000 title claims abstract description 113
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000003723 Smelting Methods 0.000 title claims abstract description 20
- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 11
- 239000002893 slag Substances 0.000 claims abstract description 47
- 238000004458 analytical method Methods 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims description 46
- 239000004927 clay Substances 0.000 claims description 25
- 238000001816 cooling Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000011521 glass Substances 0.000 claims description 18
- 239000012086 standard solution Substances 0.000 claims description 16
- 238000005485 electric heating Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 14
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 6
- 239000005695 Ammonium acetate Substances 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 229940043376 ammonium acetate Drugs 0.000 claims description 6
- 235000019257 ammonium acetate Nutrition 0.000 claims description 6
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical class [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 6
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- 238000010025 steaming Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical class N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910001610 cryolite Inorganic materials 0.000 claims description 3
- 125000001153 fluoro group Chemical class F* 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- -1 saturated ammonium hydride Chemical class 0.000 claims description 3
- 239000000779 smoke Substances 0.000 claims description 3
- 238000009736 wetting Methods 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 239000012047 saturated solution Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000005070 sampling Methods 0.000 abstract description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- 241000784732 Lycaena phlaeas Species 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000126 substance Substances 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/72—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
A method for measuring the copper content in copper ash of a copper alloy smelting furnace comprises the following process steps: pretreatment of a sample, analysis of a copper ingot, analysis of molten slag, analysis of screened ash and calculation of a result; the method comprises the steps of pretreating a sample by adopting a pyrometallurgical smelting mode, extracting metal copper in the sample, simultaneously crushing screened ash and smelting slag, finally converting a copper ash sample with complex and uneven components into three single and even components, analyzing the three components respectively by using a conventional analysis means, calculating the copper content of the sample according to the weight occupied by each component, and solving the problems of complex components, uneven components and poor sampling representativeness of the copper ash sample.
Description
Technical Field
The invention relates to the field of chemical analysis, in particular to a method for measuring copper content in copper ash of a copper alloy smelting furnace.
Background
In the casting link of copper processing enterprises, a large amount of copper ash can be generated in the slagging-off and ash-removing processes of each smelting furnace, and the copper ash has high copper content and high recoverable value. China is deficient in copper resources and needs to be imported from foreign countries in a large amount every year. A copper processing enterprise with 10 ten thousand tons of annual output can generate more than 1000 tons of copper ash every year, and the value is about 2000 ten thousand yuan.
The copper ash contains complex components, such as smelting slag, metallic copper, refractory bricks, charcoal and other impurities, and the metallic copper contains different components, such as brass, red copper, cupronickel and the like. Due to the complexity of components and the nonuniformity of samples, the accurate determination of the copper content in the copper ash becomes very difficult, and the accurate detection result cannot be used for guiding the transaction of the copper ash.
The method for measuring the copper content in the copper ash of the copper alloy smelting furnace is not reported at present. Meanwhile, due to the complexity of copper ash samples and poor sampling representativeness, several common copper content determination methods are not suitable at present, and how to accurately and reliably determine the copper content is beneficial to guiding the treatment of the copper ash, so that the recycling of resources is promoted, and the problem which is difficult to solve for a long time is formed.
In view of the above, a method for determining the copper content in the copper ash of a copper alloy smelting furnace has been developed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for measuring the copper content in copper ash of a copper alloy smelting furnace, wherein a sample is pretreated by adopting a pyrogenic smelting mode, metal copper in the sample is extracted, screened ash and smelting slag are crushed simultaneously, the copper ash sample with complex and uneven components is converted into three single and even components, the three components are respectively analyzed by using a conventional analysis means, the copper content of the sample is calculated according to the weight occupied by each component, and the problems of complex components, uneven components and poor sampling representativeness of the copper ash sample are solved.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for measuring the copper content in copper ash of a copper alloy smelting furnace comprises the following process steps: pretreatment of a sample, analysis of a copper ingot, analysis of molten slag, analysis of screened ash and calculation of a result.
Firstly, pretreating a sample: after a sample is divided according to a quartering method, 900g to 1100g of sample is taken, the sample is sieved by a 80-mesh sieve after being crushed, the ash under the sieve of the sample is weighed and reserved for analysis, the residual sample on the sieve is divided into two 300 ml clay crucibles into which 50g of anhydrous borax is added in advance, then the clay crucibles are put into a box-type resistance furnace, the temperature is raised to 850-950 ℃, the clay crucibles are taken out when the sample in the clay crucibles is in a semi-molten state, then the clay crucibles are covered by 80g to 120g of anhydrous borax and 5g to 15g of cryolite, the clay crucibles are continuously put into the box-type resistance furnace, the temperature is slowly raised to 1100-1150 ℃, the clay crucibles are taken out and shaken during the period, the materials in the clay crucibles are uniformly melted until the melting is completed, the melted solution is cooled to obtain smooth copper ingots, the slag is collected, the weights of the smooth copper ingots and the slag are respectively weighed, the slag is crushed to be not less than 80 meshes, reserving a sample for analysis;
and step two, analyzing the copper ingot: weighing 0.30 g of scrap sample of a smooth copper ingot, placing the scrap sample in a 250mL beaker, slowly adding 5mL of nitric acid along the wall of the beaker, covering a watch glass of the beaker, placing the beaker on an electric heating plate after the severe reaction of the scrap sample and the nitric acid is stopped, heating at low temperature to completely dissolve the scrap sample, continuously steaming at low temperature until the solution in the beaker is oily, taking the beaker filled with the solution from the electric heating plate, washing the wall of the beaker with water and diluting the solution in the beaker, diluting the solution to 25-35mL, shaking the diluted solution uniformly, cooling to room temperature, neutralizing the diluted solution with ammonia water until blue precipitate appears, adding 3mL of glacial acetic acid and 1mL of saturated ammonium bifluoride solution, shaking uniformly, titrating with a pre-calibrated sodium thiosulfate standard solution with the molar concentration of 0.1mol/L, recording the consumption volume of the sodium thiosulfate standard solution, and calculating the content of copper.
Thirdly, analyzing the slag: weighing 0.10g of slag sample, placing the slag sample in a 150mL glass beaker, adding 3-5 drops of hydrofluoric acid, 10mL of hydrochloric acid and 5mL of nitric acid, dissolving at low temperature, adding 3mL of perchloric acid after the slag sample is dissolved, placing the slag sample on an electric heating plate, heating until dense smoke is emitted for 2-3min, taking down the slag sample, cooling to room temperature, adding 10mL of hydrochloric acid, heating to dissolve salt precipitated in the glass beaker, taking down and cooling to room temperature, fixing the volume of the solution with water after the salt is dissolved to 100mL, and measuring the copper content by adopting a flame atomic absorption spectrometer or an ICP-OES standard working curve method;
fourthly, analyzing screened ash: weighing 0.40g of a test material of screened ash, placing the test material of the screened ash in a 500mL triangular flask, wetting the test material of the screened ash with water, adding 10mL of hydrochloric acid, placing the test material on an electric heating plate, heating at a low temperature for 3-5min, taking down, cooling for 4-6min, adding 5mL of nitric acid and 1mL of liquid bromine, covering a watch glass of the triangular flask, uniformly mixing, heating at a low temperature, taking down and cooling after the test material in the triangular flask is completely decomposed, washing the watch glass of the triangular flask with water, continuously heating and steaming until the solution in the triangular flask is less than or equal to 2mL, taking down and cooling, adding 30mL of water into the triangular flask after cooling, washing the cup wall and the watch glass, placing the triangular flask on the electric heating plate for boiling, dissolving salts separated out in the triangular flask, taking down and cooling to room temperature, dropwise adding an ammonium acetate solution until the solution in the triangular flask is red, adding 3-5mL of an ammonium acetate solution when the solution in the triangular flask is not deepened any more, dropwise adding a saturated ammonium fluoride solution, dropwise adding a saturated ammonium hydrogen fluoride saturated solution until the red color disappears in the triangular flask, and adding 1mL of the saturated fluorine Adding 2-3g of potassium iodide into saturated ammonium hydride solution, titrating with a pre-calibrated sodium thiosulfate standard solution with the molar concentration of 0.04mol/L, recording the consumption volume of the sodium thiosulfate standard solution, and calculating the copper content;
and fifthly, calculating a result: substituting the copper content measured by the three components in the steps into the following calculation formula to obtain the percentage content of copper in the copper ash:
in the above formula: m1 is the weight of ash under sieve, in g; m2 is the weight of the copper ingot and the unit is g; m3 is the weight of slag in g; m0 is the total weight of the sample in g; w1 is the percentage of copper in the screen dust; w2 is the percentage content of copper in the copper ingot; w3 is the percentage of copper in the slag.
The invention has the beneficial effects that: the invention provides a method for measuring copper in copper ash of a smelting furnace, which comprises the steps of pretreating a sample by adopting a pyrogenic smelting mode, extracting metal copper in the sample, crushing screened ash and smelting slag simultaneously, finally converting a copper ash sample with complex and uneven components into three single and even components, respectively analyzing the three components by using a conventional analysis means, and calculating the copper content of the sample according to the weight occupied by each component.
Detailed Description
The present invention will be described in further detail with reference to the following examples and embodiments:
example 1
Firstly, pretreating a sample: dividing a sample by a quartering method, taking 1010.46g of sample, crushing the sample by a crusher, sieving the crushed sample by an 80-mesh sieve, weighing 456.03g of sieved ash of the sample, subpackaging the rest of the sample on the sieve into two 300 ml clay crucibles into which 50g of anhydrous borax is added in advance, then putting the clay crucibles into a box type resistance furnace, heating to 900 ℃, taking out the clay crucibles when the samples in the clay crucibles are in a semi-molten state, adding 100g of anhydrous borax and 10g of cryolite for covering, continuing to put the clay crucibles into the box type resistance furnace, slowly heating to 1150 ℃, taking out the clay crucibles, shaking the clay crucibles until the materials in the clay crucibles are molten uniformly until the materials are molten, taking out the clay crucibles and cooling to room temperature, obtaining copper ingots after the solution is cooled, breaking the slag outside the copper ingots to obtain smooth copper ingots, collecting the molten slag, weighing the weights of the smooth copper ingots and the molten slag respectively, wherein the weight of the smooth copper ingots is 357.86g, the weight of the molten slag is 431.20g, the molten slag is crushed to be not less than 80 meshes, and a sample is reserved for analysis;
and step two, analyzing the copper ingot: weighing 0.3004 g of scrap sample of a smooth copper ingot, placing the scrap sample in a 250mL beaker, slowly adding 5mL of nitric acid along the wall of the beaker, covering a watch glass of the beaker, placing the beaker on an electric heating plate after the severe reaction of the scrap sample and the nitric acid is stopped, heating at low temperature to completely dissolve the scrap sample, continuously steaming at low temperature until the solution in the beaker is oily, taking the beaker off from the electric heating plate, washing the wall of the beaker with water, diluting the solution in the beaker to 30mL, shaking the diluted solution uniformly, cooling to room temperature, neutralizing the diluted solution with ammonia water until blue precipitate appears, adding 3mL of glacial acetic acid and 1mL of saturated ammonium bifluoride solution, shaking uniformly, titrating to an end point with a pre-calibrated sodium thiosulfate standard solution with a molar concentration of 0.1003mol/L, consuming 38.60mL of the sodium thiosulfate standard solution altogether, and calculating the copper content in the smooth copper ingot according to the formula:
in the above formula: c is the molar concentration of the standard solution of sodium thiosulfate in units: mol/L; v is the volume of sodium sulfate consumed standard solution at titration, unit: mL; m is the molar mass of copper, 63.55 g/mol; m is the sample weighing of the copper ingot, and the unit is as follows: g;
the copper content in the smooth copper ingot is 81.90 percent by calculation;
thirdly, analyzing the slag: weighing 0.1002g of slag sample, placing the slag sample in a 150mL glass beaker, adding 3-5 drops of hydrofluoric acid, 10mL of hydrochloric acid and 5mL of nitric acid, dissolving at low temperature, adding 3mL of perchloric acid after the slag sample is dissolved, placing the slag sample on an electric heating plate, heating the slag sample until dense smoke is emitted for 2-3min, taking down the slag sample, cooling the slag sample to room temperature, adding 10mL of hydrochloric acid, heating and dissolving salts precipitated in the glass beaker, taking down the slag and cooling the slag to room temperature, fixing the volume of the solution with water after the salts are dissolved to 100mL, measuring the copper content by adopting an ICP-OES standard working curve method, drawing a working curve by six standard points with the configured Cu concentrations of 0.0, 2.0, 4.0, 6.0, 8.0 and 10.0mg/L respectively, and measuring the copper content of the slag to be 0.66%;
fourthly, analyzing screened ash: weighing 0.4006g of a sample of the screened ash, placing the sample of the screened ash in a 500mL triangular flask, wetting the sample of the screened ash with water, adding 10mL of hydrochloric acid, placing the sample on an electric heating plate for low-temperature heating for 3-5min, taking down and cooling for 4-6min, adding 5mL of nitric acid and 1mL of liquid bromine, covering a watch glass of the triangular flask, uniformly mixing, heating at low temperature, taking down and cooling after the sample in the triangular flask is completely decomposed, washing the watch glass of the triangular flask with water, continuously heating and steaming until the solution in the triangular flask is less than or equal to 2mL, taking down and cooling, adding 30mL of water into the triangular flask after cooling, washing the cup wall and the watch glass, placing the triangular flask on the electric heating plate for boiling, dissolving salts separated out from the triangular flask, taking down and cooling to room temperature, dropwise adding an ammonium acetate solution until the solution in the triangular flask is red, adding 3-5mL of an ammonium acetate solution after the solution in the triangular flask is not deepened any more, dropwise adding a saturated ammonium hydrogen fluoride solution until the red saturated ammonium hydrogen fluoride in the triangular flask disappears, and then adding 1mL of the saturated fluorine Adding 2-3g of potassium iodide into saturated ammonium hydride solution, titrating by using a sodium thiosulfate standard solution with the molar concentration of 0.04mol/L to totally consume 20.17mL of the sodium thiosulfate standard solution, and calculating the content of copper in screened ash according to a formula:
in the above formula: c is the molar concentration of the standard solution of sodium thiosulfate in units: mol/L; v is the volume of sodium sulfate consumed standard solution at titration, unit: mL; m is the molar mass of copper, 63.55 g/mol; m is the sample weighing of the screened ash, unit: g;
and fifthly, calculating a result: substituting the copper content measured by the three components in the steps into the following calculation formula to obtain the percentage content of copper in the copper ash:
in the above formula: m1 is the ash weight under sieve, unit: g; m2 is the weight of the copper ingot, unit: g; m3 is the weight of slag, unit: g; m0 is the total weight of the sample, in units: g; w1 is the percentage copper in the undersize ash; w2 is the percentage of copper in the copper ingot; w3 is the percentage content of copper in the slag;
the copper content in the copper ash sample was 35.11%.
Claims (3)
1. A method for measuring the copper content in copper ash of a copper alloy smelting furnace is characterized by comprising the following steps: the process comprises the following steps: pretreatment of a sample, analysis of a copper ingot, analysis of molten slag, analysis of screened ash and calculation of a result.
2. The method for measuring the copper content in the copper ash of the copper alloy smelting furnace according to claim 1, characterized by comprising the following steps:
firstly, pretreating a sample: after a sample is divided according to a quartering method, 900g to 1100g of sample is taken, the sample is sieved by a 80-mesh sieve after being crushed, the ash under the sieve of the sample is weighed and reserved for analysis, the residual sample on the sieve is divided into two 300 ml clay crucibles into which 50g of anhydrous borax is added in advance, then the clay crucibles are put into a box-type resistance furnace, the temperature is raised to 850-950 ℃, the clay crucibles are taken out when the sample in the clay crucibles is in a semi-molten state, then the clay crucibles are covered by 80g to 120g of anhydrous borax and 5g to 15g of cryolite, the clay crucibles are continuously put into the box-type resistance furnace, the temperature is slowly raised to 1100-1150 ℃, the clay crucibles are taken out and shaken during the period, the materials in the clay crucibles are uniformly melted until the melting is completed, the melted solution is cooled to obtain smooth copper ingots, the slag is collected, the weights of the smooth copper ingots and the slag are respectively weighed, the slag is crushed to be not less than 80 meshes, reserving a sample for analysis;
and step two, analyzing the copper ingot: weighing 0.30 g of scrap sample of a smooth copper ingot, placing the scrap sample in a 250mL beaker, slowly adding 5mL of nitric acid along the wall of the beaker, covering a watch glass of the beaker, placing the beaker on an electric heating plate after the severe reaction of the scrap sample and the nitric acid is stopped, heating at low temperature to completely dissolve the scrap sample, continuously steaming at low temperature until the solution in the beaker is oily, taking the beaker filled with the solution from the electric heating plate, washing the wall of the beaker with water and diluting the solution in the beaker, diluting the solution to 25-35mL, shaking the diluted solution uniformly, cooling to room temperature, neutralizing the diluted solution with ammonia water until blue precipitate appears, adding 3mL of glacial acetic acid and 1mL of saturated ammonium bifluoride solution, shaking uniformly, titrating with a pre-calibrated sodium thiosulfate standard solution with the molar concentration of 0.1mol/L, recording the consumption volume of the sodium thiosulfate standard solution, and calculating the content of copper.
3. The method for measuring the copper content in the copper ash of the copper alloy smelting furnace according to claim 1, characterized by comprising the following steps:
thirdly, analyzing the slag: weighing 0.10g of slag sample, placing the slag sample in a 150mL glass beaker, adding 3-5 drops of hydrofluoric acid, 10mL of hydrochloric acid and 5mL of nitric acid, dissolving at low temperature, adding 3mL of perchloric acid after the slag sample is dissolved, placing the slag sample on an electric heating plate, heating until dense smoke is emitted for 2-3min, taking down the slag sample, cooling to room temperature, adding 10mL of hydrochloric acid, heating to dissolve salt precipitated in the glass beaker, taking down and cooling to room temperature, fixing the volume of the solution with water after the salt is dissolved to 100mL, and measuring the copper content by adopting a flame atomic absorption spectrometer or an ICP-OES standard working curve method;
fourthly, analyzing screened ash: weighing 0.40g of a test material of screened ash, placing the test material of the screened ash in a 500mL triangular flask, wetting the test material of the screened ash with water, adding 10mL of hydrochloric acid, placing the test material on an electric heating plate, heating at a low temperature for 3-5min, taking down, cooling for 4-6min, adding 5mL of nitric acid and 1mL of liquid bromine, covering a watch glass of the triangular flask, uniformly mixing, heating at a low temperature, taking down and cooling after the test material in the triangular flask is completely decomposed, washing the watch glass of the triangular flask with water, continuously heating and steaming until the solution in the triangular flask is less than or equal to 2mL, taking down and cooling, adding 30mL of water into the triangular flask after cooling, washing the cup wall and the watch glass, placing the triangular flask on the electric heating plate for boiling, dissolving salts separated out in the triangular flask, taking down and cooling to room temperature, dropwise adding an ammonium acetate solution until the solution in the triangular flask is red, adding 3-5mL of an ammonium acetate solution when the solution in the triangular flask is not deepened any more, dropwise adding a saturated ammonium fluoride solution, dropwise adding a saturated ammonium hydrogen fluoride saturated solution until the red color disappears in the triangular flask, and adding 1mL of the saturated fluorine Adding 2-3g of potassium iodide into saturated ammonium hydride solution, titrating with a pre-calibrated sodium thiosulfate standard solution with the molar concentration of 0.04mol/L, recording the consumption volume of the sodium thiosulfate standard solution, and calculating the copper content;
and fifthly, calculating a result: substituting the copper content measured by the three components in the steps into the following calculation formula to obtain the percentage content of copper in the copper ash:
in the above formula: m1 is the weight of ash under sieve, in g; m2 is the weight of the copper ingot and the unit is g; m3 is the weight of slag in g; m0 is the total weight of the sample in g; w1 is the percentage of copper in the screen dust; w2 is the percentage content of copper in the copper ingot; w3 is the percentage of copper in the slag.
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