CN114062590A - Method for measuring content of lead element in rhenium-rich slag and leaching slag generated by extracting rhenium - Google Patents
Method for measuring content of lead element in rhenium-rich slag and leaching slag generated by extracting rhenium Download PDFInfo
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- CN114062590A CN114062590A CN202111241581.4A CN202111241581A CN114062590A CN 114062590 A CN114062590 A CN 114062590A CN 202111241581 A CN202111241581 A CN 202111241581A CN 114062590 A CN114062590 A CN 114062590A
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- rhenium
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- sulfuric acid
- lead
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- 239000002893 slag Substances 0.000 title claims abstract description 189
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 title claims abstract description 176
- 229910052702 rhenium Inorganic materials 0.000 title claims abstract description 175
- 238000002386 leaching Methods 0.000 title claims abstract description 96
- 238000000034 method Methods 0.000 title claims abstract description 67
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 169
- 239000000243 solution Substances 0.000 claims abstract description 114
- 238000004448 titration Methods 0.000 claims abstract description 110
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000007864 aqueous solution Substances 0.000 claims abstract description 46
- 239000002244 precipitate Substances 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 30
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011975 tartaric acid Substances 0.000 claims abstract description 22
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 22
- 238000009835 boiling Methods 0.000 claims abstract description 20
- 238000001704 evaporation Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000007853 buffer solution Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 claims abstract description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 241000220317 Rosa Species 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 238000002474 experimental method Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 4
- 238000009776 industrial production Methods 0.000 abstract description 8
- 238000005259 measurement Methods 0.000 abstract description 6
- 239000011133 lead Substances 0.000 description 100
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 19
- 238000012360 testing method Methods 0.000 description 13
- 238000011084 recovery Methods 0.000 description 12
- 239000012086 standard solution Substances 0.000 description 12
- 239000007974 sodium acetate buffer Substances 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 10
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000002699 waste material Substances 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 5
- 230000000873 masking effect Effects 0.000 description 5
- 229910052787 antimony Inorganic materials 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000011343 solid material Substances 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 3
- 230000002452 interceptive effect Effects 0.000 description 3
- 239000006210 lotion Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- QSHYGLAZPRJAEZ-UHFFFAOYSA-N 4-(chloromethyl)-2-(2-methylphenyl)-1,3-thiazole Chemical compound CC1=CC=CC=C1C1=NC(CCl)=CS1 QSHYGLAZPRJAEZ-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 239000012490 blank solution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
- G01N31/166—Continuous titration of flowing liquids
-
- 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
-
- 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
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
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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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
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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
- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
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Abstract
The invention discloses a method for measuring the content of lead in rhenium-rich slag and leaching slag generated by extracting rhenium, which comprises the following steps: adding hydrochloric acid into rhenium-rich slag or leaching slag samples in a container and heating until the rhenium-rich slag or the leaching slag samples are dissolved; adding mixed nitric-sulfuric acid, heating and evaporating to dryness, adding sulfuric acid aqueous solution, heating and evaporating to dryness; adding sulfuric acid water solution and tartaric acid water solution, boiling; adding absolute ethyl alcohol, filtering, washing the precipitate and the container with sulfuric acid washing liquor, and putting the precipitate and the filter paper back to the original container; adding a buffer solution, boiling, adding water and a xylenol orange indicator, titrating by using an EDTA standard titration solution, taking the titration end point that the solution is changed from rosy to bright yellow, and obtaining the content of the lead element in the rhenium-rich slag or the leaching slag according to the consumption of the volume of the EDTA standard titration solution at the titration end point. The method provided by the invention has the advantages of higher accuracy, better precision and wide measurement range, can meet the requirements of industrial production, and fills the blank of the rhenium-rich slag produced by extracting rhenium and the method for analyzing and determining the content of lead in the leaching slag.
Description
Technical Field
The invention relates to the field of analysis and test of ore samples, in particular to a method for measuring the content of lead elements in rhenium-rich slag and leaching slag generated by extracting rhenium.
Background
In the process of extracting and preparing products such as perrhenic acid, ammonium perrhenate, rhenium powder and the like by a metallurgical wet method, the content of produced resource wastes is complex, wherein rhenium-rich slag and leaching slag are most representative. The rhenium-rich slag is a material obtained by precipitating rhenium from waste acid obtained by pyrometallurgical smelting of copper concentrate, and the leaching slag is a solid material left after leaching rhenium components from ores, copper concentrate or other solid materials by using a leaching agent. Aiming at the secondary resource waste, in order to be thoroughly utilized, impurity elements contained in the secondary resource waste need to be analyzed, and are removed and recovered in a targeted manner, so that the maximum utilization rate is achieved.
At present, no relevant analysis and determination method exists in China for determining the content of lead in the rhenium-rich slag and the leaching slag. When the content of lead in other materials is analyzed daily, an Atomic Absorption Spectroscopy (AAS) method, an inductively coupled plasma emission spectroscopy (ICP-AES) method and an EDTA volumetric method can be used for the determination method, and although the Atomic Absorption Spectroscopy (AAS) method and the inductively coupled plasma emission spectroscopy (ICP-AES) method are high in accuracy and analysis speed, the method can only be used for determining trace lead, cannot meet the requirements of industrial production, and is high in detection cost; the existing EDTA volumetric method affects the accuracy of the measurement result due to the problems of incomplete dissolution of a sample with complex components, incomplete lead sulfate precipitation, long filtration time, large influence of interfering elements, unobvious color change of a titration end point and the like.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a method for measuring the content of lead in rhenium-rich slag and leaching slag generated by extracting rhenium, and aims to solve the problem that no method for analyzing and measuring the content of lead in rhenium-rich slag and leaching slag generated by extracting rhenium exists in the prior art.
The technical scheme of the invention is as follows:
the invention provides a method for measuring the content of lead in rhenium-rich slag and leaching slag generated by extracting rhenium, which comprises the following steps:
(1) putting rhenium-rich slag or leaching slag samples generated by extracting rhenium into a container, adding hydrochloric acid, and heating until the rhenium-rich slag or the leaching slag samples generated by extracting rhenium are dissolved;
(2) adding mixed acid of nitric acid and sulfuric acid, heating and evaporating to dryness, adding aqueous solution of sulfuric acid, heating and evaporating to dryness;
(3) adding sulfuric acid water solution and tartaric acid water solution, boiling;
(4) adding anhydrous ethanol, standing, and filtering with filter paper;
(5) washing the precipitate and the container with sulfuric acid washing liquid, and returning the precipitate and the filter paper to the original container;
(6) adding a buffer solution into an original container, boiling, adding water, adding a xylenol orange indicator, titrating by using an EDTA standard titration solution, and taking the titration end point that the solution is changed from rose red to bright yellow;
(7) carrying out a blank experiment along with a rhenium-rich slag or leaching slag sample generated by extracting rhenium;
(8) and obtaining the content of lead elements in the rhenium-rich slag or leaching slag generated by extracting rhenium according to the volume of the EDTA standard titration solution consumed at the titration end point.
Optionally, the method for determining the content of lead in the rhenium-rich slag and the leaching slag, which are produced by extracting rhenium, specifically comprises the following steps:
(1) putting 0.2-0.4 g of rhenium-rich slag or leaching slag sample generated by extracting rhenium into a container, adding 5-10 mL of hydrochloric acid, and heating until the rhenium-rich slag or the leaching slag sample generated by extracting rhenium is dissolved;
(2) adding 5-15 mL of mixed nitric-sulfuric acid, heating and evaporating to dryness, adding 5-10 mL of sulfuric acid aqueous solution, heating and evaporating to dryness;
(3) adding 5-10 mL of sulfuric acid aqueous solution and 5mL of tartaric acid aqueous solution, and boiling;
(4) adding 5-10 mL of absolute ethyl alcohol, standing for 2-4 h, and filtering with filter paper to obtain a precipitate;
(5) washing the precipitate and the container with sulfuric acid washing liquid, and returning the precipitate and the filter paper to the original container;
(6) adding 10-40 mL of buffer solution into an original container, boiling, adding 80-120 mL of water, adding 0.1-0.5 g of ascorbic acid, adding a xylenol orange indicator, titrating by using an EDTA standard titration solution, and taking the titration end point that the solution is changed from rose red to bright yellow;
(7) carrying out a blank experiment along with a rhenium-rich slag or leaching slag sample generated by extracting rhenium;
(8) and obtaining the content of lead elements in the rhenium-rich slag or leaching slag generated by extracting rhenium according to the volume of the EDTA standard titration solution consumed at the titration end point.
Optionally, the step (1) further includes: hydrofluoric acid is added.
Optionally, in the step (2), the volume ratio of nitric acid to sulfuric acid in the mixed nitric-sulfuric acid is 7: 3; and/or the volume ratio of the sulfuric acid to the water in the sulfuric acid aqueous solution is 1: 1.
Optionally, in the step (3), the volume ratio of sulfuric acid to water in the sulfuric acid aqueous solution is 1: 1; and/or the concentration of tartaric acid in the tartaric acid aqueous solution is 150 g/mL.
Optionally, in the step (5), the volume ratio of sulfuric acid to water in the sulfuric acid washing solution is 1: 50.
Optionally, in the step (6), the buffer solution is prepared by the following method: 150g of anhydrous sodium acetate was dissolved in water, 50mL of acetic acid was added, and diluted to 1000mL with water.
Optionally, in the step (6), the xylenol orange indicator is a xylenol orange aqueous solution, and the concentration of xylenol orange in the xylenol orange aqueous solution is 5 g/L.
Optionally, in the step (6), the EDTA standard titration solution is prepared by the following method: 40g of disodium ethylene diamine tetraacetate is dissolved in a 10L reagent bottle, diluted to the scale with water and mixed evenly.
Optionally, the filter paper is a quantitative filter paper.
Has the advantages that: the invention provides a method for measuring the content of lead in rhenium-rich slag and leaching slag generated by extracting rhenium, which comprises the steps of firstly dissolving the rhenium-rich slag or leaching slag sample generated by extracting rhenium by hydrochloric acid, then forming lead sulfate precipitate by lead in the solution by using nitric-sulfuric acid mixed acid and sulfuric acid aqueous solution, further adding sulfuric acid aqueous solution to reduce the solubility of lead sulfate, eliminating the influence of interference elements Sb and Bi on a titration end point by using tartaric acid aqueous solution as a masking agent, titrating the lead sulfate precipitate in a buffer solution by using EDTA standard titration solution after filtering and separating the lead sulfate precipitate, and titrating by using xylenol orange as an indicator, wherein when the solution is changed from red to bright yellow, the titration end point is adopted.
The EDTA analysis and determination method provided by the invention has the advantages of high selectivity, high accuracy, good precision, wide measurement range and low cost, can be used for determining the rhenium-rich slag or leaching slag sample produced by extracting rhenium with the lead mass content of more than 1%, and can meet the requirements of industrial production. Compared with the existing instrument methods (AAS method and ICP-AES method) for measuring the lead content in other materials, the method can measure the rhenium-rich slag or leaching slag sample produced by extracting rhenium with the lead content of more than 1 percent, has low input cost, convenient and quick operation, can realize batch operation of the sample, can improve the working efficiency and can meet the requirement of industrial production; compared with the EDTA volumetric method adopted by the existing determination of the lead content in other materials, the method has the advantages of complete dissolution of the sample, complete generation of lead sulfate precipitate, short filtering time, small influence of interference elements, obvious color change of the titration end point and accurate determination result. The determination method provided by the invention makes up the blank of the rhenium-rich slag generated by extracting rhenium and the method for analyzing and determining the lead content in the leaching slag, and provides a reference standard for determining the rhenium-rich slag generated by extracting rhenium and the lead content in the leaching slag.
Detailed Description
The invention provides a method for measuring the content of lead in rhenium-rich slag and leaching slag generated by extracting rhenium, and the invention is further explained in detail below in order to make the purpose, technical scheme and effect of the invention clearer and more clear. 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 process of extracting and preparing products such as perrhenic acid, ammonium perrhenate, rhenium powder and the like by a metallurgical wet method, the content of produced resource wastes is complex, wherein rhenium-rich slag and leaching slag are most representative. The rhenium-rich slag is a material obtained by precipitating rhenium from waste acid obtained by pyrometallurgical smelting of copper concentrate, and the leaching slag is a solid material left after leaching rhenium components from ores, copper concentrate or other solid materials by using a leaching agent. Aiming at the secondary resource waste, in order to be thoroughly utilized, impurity elements contained in the secondary resource waste need to be analyzed, and are removed and recovered in a targeted manner, so that the maximum utilization rate is achieved. However, for the determination of the lead content in the rhenium-rich slag and the leaching slag, no relevant analysis and determination method exists at home at present, and based on this, the embodiment of the invention provides a method for determining the lead content in the rhenium-rich slag and the leaching slag produced by extracting rhenium, wherein the method comprises the following steps:
(1) putting rhenium-rich slag or leaching slag samples generated by extracting rhenium into a container, adding hydrochloric acid, and heating until the rhenium-rich slag or the leaching slag samples generated by extracting rhenium are dissolved;
(2) adding mixed acid of nitric acid and sulfuric acid, heating and evaporating to dryness, adding aqueous solution of sulfuric acid, heating and evaporating to dryness;
(3) adding sulfuric acid water solution and tartaric acid water solution, boiling;
(4) adding anhydrous ethanol, standing, and filtering with filter paper;
(5) washing the precipitate and the container with sulfuric acid washing liquid, and returning the precipitate and the filter paper to the original container;
(6) adding a buffer solution into an original container, boiling, adding water, adding a xylenol orange indicator, titrating by using an EDTA standard titration solution, and taking the titration end point that the solution is changed from rose red to bright yellow;
(7) carrying out a blank experiment along with a rhenium-rich slag or leaching slag sample generated by extracting rhenium;
(8) and obtaining the content of lead elements in the rhenium-rich slag or leaching slag generated by extracting rhenium according to the volume of the EDTA standard titration solution consumed at the titration end point.
In the embodiment, rhenium-rich slag or leaching slag produced by extracting rhenium contains copper, arsenic, lead, zinc, iron and the like, data errors are reduced by adopting a mode of multiple precipitation, adding a sulfuric acid aqueous solution and a masking agent, separating impurities, removing interference of coexisting substances and the like, specifically, firstly, hydrochloric acid is adopted to dissolve rhenium-rich slag or leaching slag sample produced by extracting rhenium to form a solution, then, mixed nitric-sulfuric acid and sulfuric acid aqueous solution are added to enable lead in the solution to form lead sulfate precipitate while soluble sulfates such as copper, zinc, iron and the like in the solution are not precipitated, further, sulfuric acid aqueous solution is added to reduce the solubility of lead sulfate, tartaric acid aqueous solution is used as the masking agent to eliminate the influence of interference elements Sb and Bi on a titration end point, after the lead sulfate precipitate is filtered and separated, the lead sulfate precipitate is titrated in a buffer solution through EDTA standard solution and xylenol orange is used as an indicator, when the solution is changed from rose red to brilliant yellow as the titration end point, recording the volume of the EDTA standard titration solution consumed at the titration end point, carrying out a blank experiment along with the rhenium-rich slag or leaching slag sample for correction, and calculating the lead content of the rhenium-rich slag or leaching slag sample generated by extracting rhenium according to the consumed volume of the EDTA standard titration solution at the titration end point, wherein the specific calculation process is as follows:
1) and determining the titration coefficient of the EDTA standard titration solution to lead:
the titration coefficient of EDTA standard titration solution to lead is the quality of lead equivalent to each milliliter of EDTA standard titration solution, and the specific test steps and the calculation method are as follows: parallelly sucking 4 parts of lead standard solution, adding 10-40 mL of acetic acid-sodium acetate buffer solution, 80-120 mL of water and 2-3 drops of xylenol orange indicator, and titrating by using an EDTA standard titration solution until the solution is changed from rose red to bright yellow, namely the end point. Recording volume V of lead standard solution removed2And the volume V of EDTA standard titration solution consumed at the end of the titration1. Then, the titration coefficient of the EDTA standard titration solution for lead is:
in the formula (1), the mass concentration of lead in the rho-lead standard solution is g/mL;
V2-removing the volume of lead standard solution, mL;
V1-consumption of volume of EDTA standard titration solution at titration endpoint, mL;
the titration coefficient of the F-EDTA standard titration solution to lead, g/mL.
The final titration factor was averaged over 4 groups.
2) Calculating the lead content omega in the rhenium-rich slag or leaching slag sample generated by extracting rhenium:
in the formula:
omega-mass fraction of lead in rhenium-rich slag or leaching slag samples produced by extracting rhenium;
the titration coefficient of the F-EDTA standard titration solution to lead, g/mL;
v, consuming the volume of EDTA standard titration solution (mL) when extracting rhenium-rich slag or leaching slag samples generated by rhenium by titration;
V0-the volume of EDTA standard titration solution consumed in titrating the blank solution, mL;
m-mass of rhenium-rich slag or leaching slag sample produced by extracting rhenium, g.
The EDTA analysis method provided by the embodiment has the advantages of high selectivity, high accuracy, high precision, wide measurement range and low cost, can be used for measuring rhenium-rich slag or leaching slag samples produced by extracting rhenium with lead content of more than 1%, and can meet the requirements of industrial production. Compared with the existing instrument method for measuring the lead content in other materials, the method can measure the rhenium-rich slag or leaching slag sample produced by extracting rhenium, the lead content of which is more than 1 percent, has the advantages of low input cost, convenient and quick operation, realization of batch operation of the sample, improvement of the working efficiency and adaptability to the industrial production requirement; compared with the EDTA volumetric method adopted by the existing determination of the lead content in other materials, the method has the advantages of complete dissolution of the sample, complete generation of lead sulfate precipitate, short filtering time, small interfering elements, obvious color change of the titration end point and accurate determination result. The determination method provided by the invention makes up the blank of the rhenium-rich slag generated by extracting rhenium and the method for analyzing and determining the lead content in the leaching slag, and provides a reference standard for determining the rhenium-rich slag generated by extracting rhenium and the lead content in the leaching slag.
In one embodiment, the method for determining the content of lead in the rhenium-rich slag and leaching slag produced by extracting rhenium specifically comprises the following steps:
(1) putting 0.2-0.4 g of rhenium-rich slag or leaching slag sample generated by extracting rhenium into a container, adding 5-10 mL of hydrochloric acid, and heating until the rhenium-rich slag or the leaching slag sample generated by extracting rhenium is dissolved;
(2) adding 5-15 mL of mixed nitric-sulfuric acid, heating and evaporating to dryness, adding 5-10 mL of sulfuric acid aqueous solution, heating and evaporating to dryness;
(3) adding 5-10 mL of sulfuric acid aqueous solution and 5mL of tartaric acid aqueous solution, and boiling;
(4) adding 5-10 mL of absolute ethyl alcohol, standing for 2-4 h, and filtering with filter paper to obtain a precipitate;
(5) washing the precipitate and the container with sulfuric acid washing liquid, and returning the precipitate and the filter paper to the original container;
(6) adding 10-40 mL of buffer solution into an original container, boiling, adding 80-120 mL of water, adding 0.1-0.5 g of ascorbic acid, adding a xylenol orange indicator, titrating by using an EDTA standard titration solution, and taking the titration end point that the solution is changed from rose red to bright yellow;
(7) carrying out a blank experiment along with a rhenium-rich slag or leaching slag sample generated by extracting rhenium;
(8) and obtaining the content of lead elements in the rhenium-rich slag or leaching slag generated by extracting rhenium according to the volume of the EDTA standard titration solution consumed at the titration end point.
In the step (1), the hydrochloric acid can be concentrated hydrochloric acid which is commercially available.
In one embodiment, in the step (1), the container may be a beaker, but is not limited thereto.
In one embodiment, the step (1) further comprises: hydrofluoric acid is added. When the silicon content of the rhenium-rich slag or leaching slag sample generated by extracting rhenium is higher, a little hydrofluoric acid is added.
In one embodiment, in the step (2), the mixed nitric-sulfuric acid is prepared by mixing concentrated nitric acid and concentrated sulfuric acid, and the volume ratio of nitric acid to sulfuric acid in the mixed nitric-sulfuric acid is 7: 3.
In one embodiment, in the step (2), the volume ratio of sulfuric acid to water in the aqueous sulfuric acid solution is 1: 1.
In one embodiment, in the step (2), the volume ratio of nitric acid to sulfuric acid in the mixed nitric-sulfuric acid is 7:3, and the volume ratio of sulfuric acid to water in the sulfuric acid aqueous solution is 1: 1. The preparation of the aqueous solution of sulfuric acid with the volume ratio can lead to complete precipitation of lead because of the passivation phenomenon of lead in concentrated sulfuric acid.
In one embodiment, in the step (3), the volume ratio of sulfuric acid to water in the aqueous sulfuric acid solution is 1: 1.
In one embodiment, in step (3), the concentration of tartaric acid in the aqueous tartaric acid solution is 150 g/mL.
In one embodiment, in the step (3), the volume ratio of sulfuric acid to water in the sulfuric acid aqueous solution is 1:1, and the concentration of tartaric acid in the tartaric acid aqueous solution is 150 g/mL. The sulfuric acid aqueous solution with the volume ratio can better reduce the solubility of lead sulfate, and the tartaric acid aqueous solution with the concentration can be used as a masking agent to better eliminate the influence of Sb and Bi, so that the measurement result is more accurate.
The purpose of adding absolute ethyl alcohol in the step (4) is to reduce the solubility of lead sulfate.
In one embodiment, in the step (4), the filter paper is quantitative filter paper.
In a specific embodiment, in the step (4), the filter paper is a chronic quantitative filter paper or a medium-speed quantitative filter paper, and in this embodiment, the filter paper can be selected according to actual needs.
In one embodiment, in step (5), the volume ratio of sulfuric acid to water in the sulfuric acid wash is 1: 50. The sulfuric acid washing liquor with the proportion can not only wash out the precipitate and impurities in the container, but also avoid the dissolution of lead sulfate.
In one embodiment, in the step (6), the buffer is added to reduce the variation range of the solution pH, so that the test result is more accurate. The ascorbic acid is added to mask the effect of iron ions on lead ions.
The preparation method of the buffer solution comprises the following steps: 150g of anhydrous sodium acetate was dissolved in water, 50mL of acetic acid was added, and diluted to 1000mL with water.
In one embodiment, the xylenol orange indicator is an aqueous xylenol orange solution, and the concentration of xylenol orange in the aqueous xylenol orange solution is 5 g/L.
In one embodiment, the EDTA standard titration solution is formulated as follows: 40g of disodium ethylene diamine tetraacetate is dissolved in a 10L reagent bottle, diluted to the scale with water and mixed evenly.
The invention is further illustrated by the following specific examples.
Example 1
a. Preparation of acetic acid-sodium acetate buffer:
150g of anhydrous sodium acetate was dissolved in water, 50mL of acetic acid was added, and the solution was diluted to 1000mL with water to obtain an acetic acid-sodium acetate buffer.
b. Preparation of EDTA standard titration solution:
dissolving 40g of disodium ethylene diamine tetraacetate in a 10L reagent bottle, diluting the solution to a scale with water, uniformly mixing the solution, and calibrating the solution after the solution is placed.
c. Calculation of the lead content omega in the rhenium-rich slag samples:
1) and determining the titration coefficient of the EDTA standard titration solution to lead:
sucking 4 parts of lead standard solution (with the concentration of 0.002g/mL) in parallel, adding 10mL of the acetic acid-sodium acetate buffer solution, 80mL of water and 2 drops of xylenol orange indicator with the concentration of 5g/L, and titrating by using the EDTA standard titration solution until the solution is changed from rose red to bright yellow, namely the end point. Recording volume V of lead standard solution removed2And the volume V of EDTA standard titration solution consumed at the end of the titration1. Then, the titration coefficient of the EDTA standard titration solution for lead is:
in the formula (1), the mass concentration of rho-lead is g/mL;
V2-removing the volume of lead standard solution, mL;
V1-consumption of volume of EDTA standard titration solution at titration endpoint, mL;
the titration coefficient of the F-EDTA standard titration solution to lead, g/mL.
The final titration factor was averaged over 4 groups.
2) And calculating the lead content omega in the rhenium-rich slag sample:
in the formula:
mass fraction of lead,%, in the omega-rhenium-rich slag sample;
the titration coefficient of the F-EDTA standard titration solution to lead, g/mL;
v, consuming the volume of EDTA standard titration solution mL when titrating the rhenium-rich slag sample;
V0-the volume of EDTA standard titration solution consumed in titrating the blank solution, mL;
m-mass of rhenium-rich slag or leaching slag sample, g.
d. And (3) measuring the lead content in the rhenium-rich slag sample:
(1) weighing 0.3g of rhenium-rich slag sample, placing the rhenium-rich slag sample in a beaker, adding 5mL of hydrochloric acid and 0.5mL of hydrofluoric acid, and heating until the sample is dissolved;
(2) adding 5mL of mixed nitric-sulfuric acid (the volume ratio of nitric acid to sulfuric acid is 7:3), heating and evaporating to dryness, adding 5mL of sulfuric acid aqueous solution (the volume ratio of sulfuric acid to water is 1:1), heating and evaporating to dryness;
(3) adding 5mL of sulfuric acid aqueous solution (volume ratio of sulfuric acid to water is 1:1) and 5mL of tartaric acid aqueous solution with concentration of 150g/mL, and boiling for 2 min;
(4) adding 5mL of absolute ethyl alcohol, and standing for 2 h;
(5) filtering with slow quantitative filter paper, washing precipitate and beaker with sulfuric acid lotion (volume ratio of sulfuric acid to water is 1:50), and returning precipitate and slow quantitative filter paper to original beaker;
(6) adding 10mL of the acetic acid-sodium acetate buffer solution into an original beaker, boiling, adding 80mL of water, adding 0.1g of ascorbic acid and 2 drops of a xylenol orange indicator with the concentration of 5g/L, titrating by using the EDTA standard titration solution, and recording the volume V of the EDTA standard titration solution at the titration end point when the solution is changed from rosy to bright yellow;
(7) carrying out blank experiments along with the samples;
(8) the lead content ω is calculated according to the above equations (1) and (2).
And (4) performing precision and three concentration level standard addition recovery tests according to the steps for measuring the lead content of the rhenium-rich slag sample. Wherein, the precision level is 9; the spiked recovery test levels were 3, 3 for each level. The results of the lead recovery and the precision are shown in tables 1 and 2.
As can be seen from tables 1 and 2, the lead precision was 0.89%, which was much lower than 5%. The recovery rate is 97.32-103.19% in total, which shows that the determination method of the invention has better precision and recovery rate.
TABLE 1 precision test results for lead in rhenium-rich slag samples
TABLE 2 results of lead recovery test in rhenium-rich slag
Example 2
a. The preparation of acetic acid-sodium acetate buffer solution, b, EDTA standard titration solution is the same as example 1, and is not repeated here.
c. Calculation of the lead content omega in the rhenium-rich slag samples:
1) and determining the titration coefficient of the EDTA standard titration solution to lead:
sucking 4 parts of lead standard solution (with the concentration of 0.002g/mL) in parallel, adding 20mL of the acetic acid-sodium acetate buffer solution, 100mL of water and 2 drops of xylenol orange indicator with the concentration of 5g/L, and titrating by using EDTA standard titration solution until the solution is changed from rose red to bright yellow, namely the end point. Recording volume V of lead standard solution removed2And the volume V of EDTA standard titration solution consumed at the end of the titration1. The formula for calculating the titration coefficient of EDTA standard titration solution to lead is the same as that in example 1.
2) And calculating the lead content omega in the leaching residue sample in the same way as in the example 1.
d. And (3) measuring the lead content in the leaching residue sample:
(1) weighing 0.3g of leaching residue sample, placing the sample in a beaker, adding 10mL of hydrochloric acid and 0.8mL of hydrofluoric acid, and heating until the sample is dissolved;
(2) adding 10mL of mixed nitric-sulfuric acid (the volume ratio of nitric acid to sulfuric acid is 7:3), heating and evaporating to dryness, adding 10mL of sulfuric acid aqueous solution (the volume ratio of sulfuric acid to water is 1:1), and evaporating to near dryness;
(3) adding 5mL of sulfuric acid aqueous solution (volume ratio of sulfuric acid to water is 1:1) and 5mL of tartaric acid aqueous solution with concentration of 150g/mL, and boiling for 3 min;
(4) adding 8mL of absolute ethyl alcohol, and standing for 3 h;
(5) filtering with medium-speed quantitative filter paper, washing precipitate and beaker with sulfuric acid lotion (volume ratio of sulfuric acid to water is 1:50), and placing precipitate and slow-speed quantitative filter paper into original beaker;
(6) adding 20mL of the acetic acid-sodium acetate buffer solution into an original beaker, boiling, adding 100mL of water, adding 0.25g of ascorbic acid and 2 drops of 5g/L xylenol orange indicator, titrating by using the EDTA standard titration solution, and recording the volume V of the EDTA standard titration solution at the titration end point when the solution is changed from rose red to bright yellow;
(7) carrying out blank experiments along with the samples;
(8) the lead content ω is calculated according to the above equations (1) and (2).
And (4) performing precision and three concentration level standard addition recovery tests according to the steps for measuring the lead content of the leaching residue sample. Wherein, the precision level is 9; the spiked recovery test levels were 3, 3 for each level. The results of the lead recovery and the precision are shown in tables 3 and 4.
As can be seen from tables 3 and 4, the lead precision was 1.01%, which was far below 5%. The recovery rate is between 97.42 and 100.92 percent, which shows that the determination method of the invention has better precision and recovery rate.
TABLE 3 precision test results of lead in leached residues
TABLE 4 test results of lead recovery from leached residues
Example 3
a. The preparation of sodium acetate buffer solution, b, EDTA standard titration solution is the same as example 1, and the details are not repeated here.
c. Calculating the lead content omega in the rhenium-rich slag and leaching slag samples:
1) and determining the titration coefficient of the EDTA standard titration solution to lead:
parallelly sucking 4 parts of lead standard solution (concentration is 0.002g/mL), adding 40mL of the above acetic acid-sodium acetate buffer solution, 120mL of water and 3 drops of xylenol orange indicator with concentration of 5g/L, and titrating with EDTA standard titration solution until the solution turns from rose red to bright yellow, which is the end point. Recording volume V of lead standard solution removed2And the volume V of EDTA standard titration solution consumed at the end of the titration1. The formula for calculating the titration coefficient of EDTA standard titration solution to lead is the same as that in example 1.
2) Calculating the lead content omega in the rhenium-rich slag and the leaching slag samples in the same way as in the example 1
d. And (3) determining the lead content in the rhenium-rich slag and leaching slag samples:
(1) respectively weighing 0.4g of rhenium-rich slag and leaching slag samples, placing the samples in a beaker, adding 10mL of hydrochloric acid and 1.0mL of hydrofluoric acid, and heating until the samples are dissolved;
(2) adding 15mL of mixed nitric-sulfuric acid (the volume ratio of nitric acid to sulfuric acid is 7:3), heating and evaporating to dryness, adding 10mL of sulfuric acid aqueous solution (the volume ratio of sulfuric acid to water is 1:1), and evaporating to near dryness;
(3) adding 10mL sulfuric acid water solution (volume ratio of sulfuric acid to water is 1:1) and 5mL tartaric acid water solution with concentration of 150g/mL, boiling for 3 min;
(4) adding 10mL of absolute ethyl alcohol, and standing for 4 h;
(5) filtering with medium-speed quantitative filter paper, washing precipitate and beaker with sulfuric acid lotion (volume ratio of sulfuric acid to water is 1:50), and placing precipitate and slow-speed quantitative filter paper into original beaker;
(6) adding 40mL of the acetic acid-sodium acetate buffer solution into an original beaker, boiling, adding 120mL of water, adding 0.5g of ascorbic acid and 3 drops of a xylenol orange indicator with the concentration of 5g/L, titrating by using the EDTA standard titration solution, and recording the volume V of the EDTA standard titration solution at the titration end point when the solution is changed from rose red to bright yellow;
(7) carrying out blank experiments along with the samples;
(8) the lead content ω is calculated according to the above equations (1) and (2).
Different analysis testers analyze and measure the content of lead element in the rhenium-rich slag and the leaching slag at different time according to the testing steps of the rhenium-rich slag and the leaching slag samples, and the measured data is shown in table 5. The relative standard deviation among different analysis testers is lower than 5 percent, and the testing method provided by the invention is proved to be good in accuracy and high in reliability.
TABLE 5 Experimental results of different analysis testers for determining the content of lead in rhenium-rich slag and leached slag
In summary, the invention provides a method for determining rhenium-rich slag produced by extracting rhenium and the content of lead elements in leaching slag, which comprises the steps of firstly adopting hydrochloric acid to dissolve the rhenium-rich slag produced by extracting rhenium or a leaching slag sample to form a solution, then adding mixed nitric acid and sulfuric acid aqueous solution to ensure that lead in the solution forms lead sulfate precipitate while soluble sulfates such as copper, zinc, iron and the like in the solution are not precipitated, further adding sulfuric acid aqueous solution to reduce the solubility of lead sulfate, using tartaric acid aqueous solution as a masking agent to eliminate the influence of interference elements Sb and Bi on a titration end point, filtering and separating the lead sulfate precipitate, then titrating the lead sulfate precipitate in a buffer solution by using EDTA standard titration solution and using xylenol orange as an indicator, and when the solution is changed from red to bright yellow, taking the titration end point as the titration end point.
The EDTA analysis method provided by the invention has the advantages of high selectivity, high accuracy, good precision, wide measurement range and low cost, can be used for measuring the rhenium-rich slag or leaching slag sample produced by extracting rhenium with the lead mass content of more than 1%, and can meet the requirements of industrial production. Compared with the existing instrument method for measuring the content of lead in other materials, the method can measure the rhenium-rich slag or leaching slag sample with the lead content of more than 1 percent and output by extracting rhenium, has the advantages of low input cost, convenient and quick operation, capability of realizing batch operation of the sample, capability of improving the working efficiency and suitability for industrial production requirements. Compared with the EDTA volumetric method adopted by the existing determination of the lead content in other materials, the method has the advantages of thorough dissolution of the sample, complete generation of lead sulfate precipitate, short filtering time, small interfering elements, obvious color change of the titration end point and accurate determination result; the determination method provided by the invention makes up the blank of the rhenium-rich slag generated by extracting rhenium and the method for analyzing and determining the lead content in the leaching slag, and provides a reference standard for determining the rhenium-rich slag generated by extracting rhenium and the lead content in the leaching slag.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for measuring the content of lead in rhenium-rich slag and leaching slag generated by extracting rhenium is characterized by comprising the following steps:
(1) putting rhenium-rich slag or leaching slag samples generated by extracting rhenium into a container, adding hydrochloric acid, and heating until the rhenium-rich slag or the leaching slag samples generated by extracting rhenium are dissolved;
(2) adding mixed acid of nitric acid and sulfuric acid, heating and evaporating to dryness, adding aqueous solution of sulfuric acid, heating and evaporating to dryness;
(3) adding sulfuric acid water solution and tartaric acid water solution, boiling;
(4) adding anhydrous ethanol, standing, and filtering with filter paper;
(5) washing the precipitate and the container with sulfuric acid washing liquid, and returning the precipitate and the filter paper to the original container;
(6) adding a buffer solution into an original container, boiling, adding water, adding a xylenol orange indicator, titrating by using an EDTA standard titration solution, and taking the titration end point that the solution is changed from rose red to bright yellow;
(7) carrying out a blank experiment along with a rhenium-rich slag or leaching slag sample generated by extracting rhenium;
(8) and obtaining the content of lead elements in the rhenium-rich slag or leaching slag generated by extracting rhenium according to the volume of the EDTA standard titration solution consumed at the titration end point.
2. The method for determining the content of lead in the rhenium-rich slag and the leaching slag generated by extracting rhenium according to claim 1, wherein the method for determining the content of lead in the rhenium-rich slag and the leaching slag generated by extracting rhenium specifically comprises the following steps:
(1) putting 0.2-0.4 g of rhenium-rich slag or leaching slag sample generated by extracting rhenium into a container, adding 5-10 mL of hydrochloric acid, and heating until the rhenium-rich slag or the leaching slag sample generated by extracting rhenium is dissolved;
(2) adding 5-15 mL of mixed nitric-sulfuric acid, heating and evaporating to dryness, adding 5-10 mL of sulfuric acid aqueous solution, heating and evaporating to dryness;
(3) adding 5-10 mL of sulfuric acid aqueous solution and 5mL of tartaric acid aqueous solution, and boiling;
(4) adding 5-10 mL of absolute ethyl alcohol, standing for 2-4 h, and filtering with filter paper to obtain a precipitate;
(5) washing the precipitate and the container with sulfuric acid washing liquid, and returning the precipitate and the filter paper to the original container;
(6) adding 10-40 mL of buffer solution into an original container, boiling, adding 80-120 mL of water, adding 0.1-0.5 g of ascorbic acid, adding a xylenol orange indicator, titrating by using an EDTA standard titration solution, and taking the titration end point that the solution is changed from rose red to bright yellow;
(7) carrying out a blank experiment along with a rhenium-rich slag or leaching slag sample generated by extracting rhenium;
(8) and obtaining the content of lead elements in the rhenium-rich slag or leaching slag generated by extracting rhenium according to the volume of the EDTA standard titration solution consumed at the titration end point.
3. The method for determining the content of lead element in rhenium-rich slag and leaching slag generated by extracting rhenium according to claim 1 or 2, characterized in that the step (1) further comprises the following steps: hydrofluoric acid is added.
4. The method for determining the content of lead in the rhenium-rich slag and the leaching slag generated by extracting rhenium according to the claim 1 or the claim 2, characterized in that in the step (2), the volume ratio of nitric acid to sulfuric acid in the mixed acid of nitric and sulfuric acid is 7: 3; and/or the volume ratio of the sulfuric acid to the water in the sulfuric acid aqueous solution is 1: 1.
5. The method for measuring the content of lead element in rhenium-rich slag and leaching slag generated by extracting rhenium according to claim 1 or 2, characterized in that in the step (3), the volume ratio of sulfuric acid to water in the sulfuric acid aqueous solution is 1: 1; and/or the concentration of tartaric acid in the tartaric acid aqueous solution is 150 g/mL.
6. The method for determining the content of lead element in rhenium-rich slag and leaching slag produced by extracting rhenium according to claim 1 or 2, characterized in that in the step (5), the volume ratio of sulfuric acid to water in the sulfuric acid washing solution is 1: 50.
7. The method for determining the content of lead element in rhenium-rich slag and leaching slag produced by extracting rhenium according to claim 1 or 2, characterized in that in the step (6), the preparation method of the buffer solution is as follows: 150g of anhydrous sodium acetate was dissolved in water, 50mL of acetic acid was added, and diluted to 1000mL with water.
8. The method for determining the content of lead element in rhenium-rich slag and leaching slag generated by extracting rhenium according to claim 1 or 2, wherein in the step (6), the xylenol orange indicator is a xylenol orange aqueous solution, and the concentration of xylenol orange in the xylenol orange aqueous solution is 5 g/L.
9. The method for determining the content of lead element in rhenium-rich slag and leaching slag produced by extracting rhenium according to claim 1 or 2, wherein in the step (6), the preparation method of the EDTA standard titration solution is as follows: 40g of disodium ethylene diamine tetraacetate is dissolved in a 10L reagent bottle, diluted to the scale with water and mixed evenly.
10. The method for determining the content of lead in rhenium-rich slag and leaching slag produced by extracting rhenium according to claim 1 or 2, characterized in that the filter paper is quantitative filter paper.
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