CN116297742A - Analysis method for directly measuring fluorine ion content in rare earth carbonate by fluorine ion electrode method - Google Patents
Analysis method for directly measuring fluorine ion content in rare earth carbonate by fluorine ion electrode method Download PDFInfo
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- -1 rare earth carbonate Chemical class 0.000 title claims abstract description 83
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 71
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 52
- 238000004458 analytical method Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 51
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 15
- 239000012086 standard solution Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 8
- 239000001509 sodium citrate Substances 0.000 claims description 8
- 239000004677 Nylon Substances 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 6
- 229920001778 nylon Polymers 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- XJRPTMORGOIMMI-UHFFFAOYSA-N ethyl 2-amino-4-(trifluoromethyl)-1,3-thiazole-5-carboxylate Chemical compound CCOC(=O)C=1SC(N)=NC=1C(F)(F)F XJRPTMORGOIMMI-UHFFFAOYSA-N 0.000 claims description 3
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims 1
- 150000001768 cations Chemical class 0.000 abstract description 15
- 150000002910 rare earth metals Chemical class 0.000 abstract description 4
- 230000007935 neutral effect Effects 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 229910052731 fluorine Inorganic materials 0.000 description 14
- 239000011737 fluorine Substances 0.000 description 14
- 238000005259 measurement Methods 0.000 description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 6
- 239000007853 buffer solution Substances 0.000 description 4
- 230000002452 interceptive effect Effects 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 3
- 239000012085 test solution Substances 0.000 description 3
- 238000007605 air drying Methods 0.000 description 2
- 229940075397 calomel Drugs 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 229960000999 sodium citrate dihydrate Drugs 0.000 description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000047703 Nonion Species 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
-
- 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
-
- 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
Abstract
The invention discloses an analysis method for directly measuring the content of fluoride ions in rare earth carbonate by a fluoride ion electrode method, which relates to the technical field of rare earth fluoride ion detection and comprises the following steps: s1, taking a rare earth carbonate sample, drying to remove foreign matters in the rare earth carbonate sample, grinding, sieving, and uniformly mixing to obtain a sample A, wherein the sample A is used for pretreatment and impurity removal of the rare earth carbonate sample; s2, respectively weighing the sample A and the solid NaOH, mixing, heating and cooling, and adding boiled deionized water into the mixture to leach the mixture until the mixture is completely dissolved to obtain a solution B; according to the analysis method for directly measuring the content of fluoride ions in the rare earth carbonate by using the fluoride ion electrode method, after impurity removal and grinding of a rare earth carbonate sample, mixing with powder of solid NaOH, heating and melting, adding water and adjusting the pH value to be neutral by using hydrochloric acid, so that most of interference cations in the sample are precipitated, the interference cations are conveniently removed, and the experimental result is more accurate.
Description
Technical Field
The invention relates to the technical field of rare earth fluoride ion detection, in particular to an analysis method for directly determining the content of fluoride ions in rare earth carbonate by a fluoride ion electrode method.
Background
The content of fluorine ions in the rare earth directly influences the extraction and separation effects of the rare earth, and the accurate determination of the fluorine ions plays a significant role in production.
According to the analysis method for directly measuring the content of fluorine ions in rare earth carbonate by using a fluorine ion electrode method, the invention is based on the aspects of analyzing the effect of perchloric acid in the distillation process, the property of fluorine ions, the measurement principle of a fluorine ion selective electrode and the like, and the method is carried out by taking the influence of aspects of matrix concentration, sample dissolution mode and the like on the measurement of fluorine ions as the experimental direction, so that the perchloric acid distillation link can be removed, the explosion potential safety hazard caused by perchloric acid and a small amount of organic P507 carried in the rare earth carbonate is eliminated, the analysis efficiency is greatly improved, the analysis cost is reduced, and the analysis process is stable, rapid, safe and environment-friendly.
However, the patent only selects sodium citrate to react with interfering cations in rare earth carbonate to release fluorine ions when detecting the concentration of fluorine ions in the rare earth carbonate, but the interfering cations cannot be removed, which can have a certain influence on the accuracy of measurement and analysis.
Disclosure of Invention
The invention aims to provide an analysis method for directly measuring the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method, so as to solve the defects in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions: the analysis method for directly determining the content of fluorine ions in the rare earth carbonate by using a fluorine ion electrode method comprises the following steps:
s1, taking a rare earth carbonate sample, drying, namely, air-drying the rare earth carbonate sample and a ventilated and light-proof indoor environment, or oven-drying the rare earth carbonate sample to remove foreign matters such as sand, animal and plant limbs and the like, grinding, sieving, and uniformly mixing the rare earth carbonate sample, wherein the drying can be used for preprocessing the rare earth carbonate sample, removing impurities and obtaining a sample A;
s2, respectively weighing the sample A and the solid NaOH, mixing, heating and cooling, and adding boiled deionized water into the mixture to leach the mixture until the mixture is completely dissolved to obtain a solution B;
s3, adding the solution B into a volumetric flask, adding hydrochloric acid into the volumetric flask, shaking uniformly, adding deionized water to fix the volume to the scale after cooling, shaking uniformly, and standing until the solution is clear, so thatCation precipitation with interfering action in solution B, cations with interfering action such as Cu 2+ 、Fe 3+ 、Al 3+ Etc., which can form stable complexes with fluoride ions, reduce the concentration and activity of fluoride ions, so that the measurement result is lower, and the existence of cations per se also reduces the measurement accuracy, the principle of cation precipitation is that the complex forms a complex with hydroxide (OH) in solution - ) Forming a precipitate of water-insoluble oxyhydrogen compound;
s4, taking supernatant, adding sodium citrate and a TISAB solution, wherein the TISAB solution is fully called a TISAB total ionic strength buffer solution for improving ionic strength, selecting sodium citrate dihydrate as the total ionic strength buffer solution, adjusting the pH value of the solution to 5-6 by hydrochloric acid, diluting to a scale by deionized water in a volumetric flask, and shaking uniformly to obtain a solution C;
s5, sequentially taking a fluoride ion standard solution with gradually increased volume, adding sodium citrate and a TISAB solution, diluting to a scale with deionized water, then transferring into a polyethylene cup, inserting a fluoride ion selection electrode and a saturated calomel electrode, continuously stirring by using a magnetic stirrer, respectively measuring potential values in balance, and drawing a fluoride ion solution standard curve which takes the logarithm of nonionic concentration as an abscissa and the potential of the electrode as an ordinate and has the concentration range of (1-100) mug/mL;
s6, placing the solution in a polyethylene beaker, inserting a fluoride ion selective electrode and a saturated calomel electrode, stirring by using a magnetic stirrer, reading a reading potential E1 after stopping, adding a fluoride ion standard solution, stirring by using the magnetic stirrer, and reading a potential E2 after stopping;
and S7, calculating the fluorine ion content according to a formula.
Further, the specific steps of grinding, grinding and sieving in the step S1 are as follows: grinding, primarily screening the rare earth carbonate sample by using a 20-40-mesh nylon screen, grinding the primarily screened rear rare earth carbonate sample, and finely screening by using an 80-100-mesh nylon screen.
Further, when the S2 is heated, the mixed sample A and the solid NaOH are heated to 550-580 ℃ for 15-20min, and are kept warm for 15-20min.
Further, the volumetric flask is 100mL, and the hydrochloric acid is 1:1 hydrochloric acid.
Further, 2-3 drops of bromocresol purple indicator and hydrochloric acid are added into the supernatant before the pH value is regulated in the step S4, and the hydrochloric acid is stopped to be added until the pH value of the solution becomes yellow and reaches 5-6.
Further, the fluoride ion standard solution is 1000. Mu.g/mL.
Further, when the fluoride ion selective electrode and the saturated calomel electrode are inserted, waiting for 3-4min for reading, so as to reduce the hysteresis reaction displayed by the calomel electrode when the temperature changes; the potential value at the time of balancing means that the electrode potential variation is less than 0.1mV within 20 seconds.
Furthermore, the fluoride ion selective electrode is selected from fluoride ion selective electrodes with the potential change of 55-60mV when the fluoride ion concentration is changed by 10 times at room temperature, and the fluoride ion selective electrode is used for ensuring that the selected fluoride ion selective electrode has good performance; the fluoride ion-selective electrode is soaked in NaF solution for 1-1.5 hours before insertion until the blank potential value in pure water is greater than 350mV.
Furthermore, before the fluoride ion selective electrode and the saturated calomel electrode are continuously used, the polishing belt is used for polishing, deionized water is used for washing, and qualitative filter paper is used for absorbing water, so that impurities on the surface of the electrode are prevented, and the effect of the electrode is prevented from being influenced.
1. Compared with the prior art, the analysis method for directly measuring the content of fluoride ions in the rare earth carbonate by using the fluoride ion electrode method provided by the invention has the advantages that the rare earth carbonate sample is mixed with the powder of solid NaOH after impurity removal and grinding, and then is heated and melted, water is added, and the pH value is adjusted to be neutral by using hydrochloric acid, so that most of interference cations in the sample are precipitated, the interference cations are conveniently removed, and the experimental result is more accurate.
2. Compared with the prior art, the analysis method for directly measuring the content of the fluoride ions in the rare earth carbonate by the fluoride ion electrode method provided by the invention has the advantages that sodium citrate and a TISAB solution are added into the solution after the interference cations are removed, the solution is further combined with the residual interference cations in the solution, so that the fluoride ions are released, the ionic strength is improved by the TISAB solution, and the accuracy of experimental calculation results is further improved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to these drawings for a person having ordinary skill in the art.
Fig. 1 is a method step diagram provided in an embodiment of the present invention.
Detailed Description
In order to make the technical scheme of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more of the described features. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise. Furthermore, the terms "mounted," "connected," "coupled," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Referring to fig. 1, the analysis method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method comprises the following steps:
s1, taking a rare earth carbonate sample, drying, namely, air-drying the rare earth carbonate sample and a ventilated and light-proof indoor environment, or oven-drying the rare earth carbonate sample to remove foreign matters such as sand, animal and plant limbs and the like, grinding, sieving, and uniformly mixing the rare earth carbonate sample, wherein the drying can be used for preprocessing the rare earth carbonate sample, removing impurities and obtaining a sample A; wherein the concrete steps of grinding, grinding and sieving are as follows: grinding and primarily screening rare earth carbonate samples by using a 20-40-mesh nylon screen, grinding the primarily screened rear rare earth carbonate samples, finely screening by using an 80-100-mesh nylon screen, and uniformly mixing the finely screened rear rare earth carbonate samples.
S2, respectively weighing the sample A and the solid NaOH, mixing, heating and cooling, and adding boiled deionized water into the mixture to leach the mixture until the mixture is completely dissolved to obtain a solution B; when heating, the mixed sample A and the solid NaOH are heated to 550-580 ℃ for 15-20min, and the temperature is kept for 15-20min, and the sample A and the solid NaOH are slowly heated to ensure full melting.
S3, adding the solution B into a volumetric flask, adding hydrochloric acid into the volumetric flask, regulating the pH value to be neutral, shaking uniformly, adding deionized water to a scale after cooling, preferably selecting 45-55 ℃ deionized water, shaking uniformly, and standing until the solution B is clear, so that cations with interference effects in the solution B are precipitated, and cations with interference effects such as Cu 2+ 、Fe 3+ 、Al 3+ Etc., which can form stable complexes with fluoride ions, reduce the concentration and activity of fluoride ions, so that the measurement result is lower, and the existence of cations per se also reduces the measurement accuracy, the principle of cation precipitation is that the complex forms a complex with hydroxide (OH) in solution - ) Forming water-insoluble oxyhydrogen compound precipitate, wherein the volumetric flask is 100mL, hydrochloric acid is 1:1 hydrochloric acid, the volumetric flask is 100mL, and the hydrochloric acid is 100mL1:1, hydrochloric acid;
s4, taking 1-5mL of supernatant, adding 0.1-0.3g of sodium citrate and 0.1-0.3mL of TISAB solution, fully weighing TISAB total ionic strength buffer solution for improving ionic strength, optionally taking sodium citrate dihydrate as the total ionic strength buffer solution, adding 2-3 drops of bromocresol purple indicator into the supernatant, adding hydrochloric acid until the solution turns yellow to indicate that the pH value of the solution reaches 5-6, or directly using a pH meter to detect that the pH value of the solution is within the range of 5-6 when the pH value of the solution is displayed by the pH meter, stopping adding hydrochloric acid, diluting to a scale by deionized water in a volumetric flask, and shaking uniformly to obtain solution C;
s5, sequentially taking a fluoride ion standard solution with gradually increased volume, wherein the selected fluoride ion standard solution is 1000 mug/mL, adding 0.1-0.3g of sodium citrate and 0.1-0.3mL of TISAB solution, diluting to a scale with deionized water, then transferring into a polyethylene cup, inserting a fluoride ion selection electrode and a saturated calomel electrode, continuously stirring by a magnetic stirrer, respectively measuring potential values in balance, and drawing a fluoride ion solution standard curve with non-ion concentration logarithm as an abscissa, electrode potential as an ordinate and concentration range of (1-100) mug/mL;
when the fluoride ion selective electrode and the saturated calomel electrode are inserted, the reading is carried out after waiting for 3-4min, so that the hysteresis reaction displayed when the calomel electrode is in temperature change is reduced, and when an electromagnetic stirrer is used for stirring, the stirring time is too long, the temperature of the solution is increased, so that the measurement result is inaccurate, the stirring time is too short, and a larger error can be caused by the memory effect of the electrode; the potential value at the time of balance means that the electrode potential variation is less than 0.1mV in 20 seconds; the fluoride ion selective electrode is selected from the fluoride ion selective electrode with the potential change of 55-60mV when the fluoride ion concentration is changed by 10 times at room temperature, and the fluoride ion selective electrode is used for ensuring that the selected fluoride ion selective electrode has good performance; the fluoride ion selective electrode is soaked in NaF solution for 1 to 1.5 hours before insertion until the blank potential value of the fluoride ion selective electrode in pure water is more than 350mV; before the fluoride ion selective electrode and the saturated calomel electrode are continuously used, the polishing belt is used for polishing, deionized water is used for washing, and qualitative filter paper is used for absorbing water, so that impurities on the surface of the electrode are prevented from being generated, and the effect of the electrode is prevented from being influenced.
S6, placing the solution in a polyethylene beaker, inserting a fluoride ion selective electrode and a saturated calomel electrode, stirring for 2-5min by using a magnetic stirrer, stopping waiting for 2-5min to read a potential reading E1, adding 1-5mL of fluoride ion standard solution, stopping stirring for the same time by using the magnetic stirrer, and waiting for the same time to read a potential reading E2;
s7, calculating the fluorine ion content according to a formula, wherein the formula is as follows:
wherein, the liquid crystal display device comprises a liquid crystal display device,
F is the molar mass of fluorine; v (V) b The addition amount of the fluorine standard solution is as follows; c (C) b Is the concentration of fluorine standard solution; v (V) 0 Taking the volume of a fluorine liquid sample; v (V) 1 Preparing a fluorine solution sample into the volume of a test solution; v (V) 2 To from V 1 Taking the volume of the test solution; e2 is the instrument potential reading after the standard solution is added with fluorine; e1 is the instrument potential reading after the test solution is added; k is the fluoride ion selective electrode slope.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that modifications may be made to the described embodiments in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive of the scope of the invention, which is defined by the appended claims.
Claims (9)
1. The analysis method for directly determining the content of fluoride ions in the rare earth carbonate by using a fluoride ion electrode method is characterized by comprising the following steps of: the method comprises the following steps:
s1, taking a rare earth carbonate sample, drying to remove foreign matters in the rare earth carbonate sample, grinding, sieving, and uniformly mixing to obtain a sample A, wherein the sample A is used for pretreatment and impurity removal of the rare earth carbonate sample;
s2, respectively weighing the sample A and the solid NaOH, mixing, heating and cooling, and adding boiled deionized water into the mixture to leach the mixture until the mixture is completely dissolved to obtain a solution B;
s3, adding the solution B into a volumetric flask, adding hydrochloric acid into the volumetric flask, shaking uniformly, adding deionized water to fix the volume to a scale after cooling, shaking uniformly, and standing until the solution B is clear, so that positive ions with interference effect in the solution B are precipitated;
s4, taking supernatant, adding sodium citrate and TISAB solution, regulating the pH value of the solution to 5-6 by using hydrochloric acid, diluting to scale by using deionized water in a volumetric flask, and shaking uniformly to obtain solution C;
s5, sequentially taking a fluoride ion standard solution with gradually increased volume, adding sodium citrate and a TISAB solution, diluting to a scale with deionized water, then transferring into a polyethylene cup, inserting a fluoride ion selection electrode and a saturated calomel electrode, continuously stirring by using a magnetic stirrer, respectively measuring potential values in balance, and drawing a fluoride ion solution standard curve which takes the logarithm of nonionic concentration as an abscissa and the potential of the electrode as an ordinate and has the concentration range of (1-100) mug/mL;
s6, placing the solution in a polyethylene beaker, inserting a fluoride ion selective electrode and a saturated calomel electrode, stirring by using a magnetic stirrer, reading a reading potential E1 after stopping, adding a fluoride ion standard solution, stirring by using the magnetic stirrer, and reading a potential E2 after stopping;
and S7, calculating the fluorine ion content according to a formula.
2. The analytical method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method according to claim 1, wherein the analytical method comprises the following steps: the concrete steps of grinding, grinding and sieving in the step S1 are as follows: grinding, primarily screening the rare earth carbonate sample by using a 20-40-mesh nylon screen, grinding the primarily screened rear rare earth carbonate sample, and finely screening by using an 80-100-mesh nylon screen.
3. The analytical method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method according to claim 1, wherein the analytical method comprises the following steps: and when the S2 is heated, the mixed sample A and the solid NaOH are heated to 550-580 ℃ for 15-20min, and the temperature is kept for 15-20min.
4. The analytical method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method according to claim 1, wherein the analytical method comprises the following steps: the volumetric flask is 100mL, and the hydrochloric acid is 1:1 hydrochloric acid.
5. The analytical method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method according to claim 1, wherein the analytical method comprises the following steps: and before the pH value is regulated in the step S4, adding 2-3 drops of bromocresol purple indicator into the supernatant, and then adding hydrochloric acid until the solution turns yellow, and stopping adding the hydrochloric acid until the pH value of the solution reaches 5-6.
6. The analytical method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method according to claim 1, wherein the analytical method comprises the following steps: the fluoride ion standard solution is 1000 mug/mL.
7. The analytical method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method according to claim 1, wherein the analytical method comprises the following steps: when the fluoride ion selective electrode and the saturated calomel electrode are inserted, waiting for 3-4min and then reading; the potential value at the time of balancing means that the electrode potential variation is less than 0.1mV within 20 seconds.
8. The analytical method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method according to claim 1, wherein the analytical method comprises the following steps: the fluoride ion selective electrode is selected from fluoride ion selective electrodes with the potential change of 55-60mV when the fluoride ion concentration is changed by 10 times at room temperature; the fluoride ion-selective electrode is soaked in NaF solution for 1-1.5 hours before insertion until the blank potential value in pure water is greater than 350mV.
9. The analytical method for directly determining the content of fluoride ions in rare earth carbonate by using a fluoride ion electrode method according to claim 1, wherein the analytical method comprises the following steps: before the fluoride ion selective electrode and the saturated calomel electrode are continuously used, the fluoride ion selective electrode and the saturated calomel electrode are polished by a polishing belt, are washed by deionized water and are sucked by qualitative filter paper.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103592288A (en) * | 2012-08-15 | 2014-02-19 | 北新集团建材股份有限公司 | Analysis method for migration of modified starch water-soluble salts in plasterboard |
| CN103792269A (en) * | 2014-01-23 | 2014-05-14 | 包头华美稀土高科有限公司 | Analytical method for directly measuring fluorine ion content in carbonic acid rare earth by using fluorine ion electrode method |
| CN110510625A (en) * | 2019-09-20 | 2019-11-29 | 四川师范大学 | The method and potassium fluoborate of the fluorine-containing aqueous slkali separation fluorine of bastnaesite and application |
| CN111189893A (en) * | 2019-12-31 | 2020-05-22 | 江苏康达检测技术股份有限公司 | Soil fluoride biological effectiveness determination method |
| CN212575934U (en) * | 2020-05-28 | 2021-02-23 | 四川沃耐稀新材料科技有限公司 | Waste gas treatment system in rare earth metal smelting |
| CN113073195A (en) * | 2021-03-19 | 2021-07-06 | 四川师范大学 | Microwave chemical method for completely extracting fluorine and rare earth in bastnaesite concentrate |
-
2023
- 2023-05-24 CN CN202310590300.9A patent/CN116297742A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103592288A (en) * | 2012-08-15 | 2014-02-19 | 北新集团建材股份有限公司 | Analysis method for migration of modified starch water-soluble salts in plasterboard |
| CN103792269A (en) * | 2014-01-23 | 2014-05-14 | 包头华美稀土高科有限公司 | Analytical method for directly measuring fluorine ion content in carbonic acid rare earth by using fluorine ion electrode method |
| CN110510625A (en) * | 2019-09-20 | 2019-11-29 | 四川师范大学 | The method and potassium fluoborate of the fluorine-containing aqueous slkali separation fluorine of bastnaesite and application |
| CN111189893A (en) * | 2019-12-31 | 2020-05-22 | 江苏康达检测技术股份有限公司 | Soil fluoride biological effectiveness determination method |
| CN212575934U (en) * | 2020-05-28 | 2021-02-23 | 四川沃耐稀新材料科技有限公司 | Waste gas treatment system in rare earth metal smelting |
| CN113073195A (en) * | 2021-03-19 | 2021-07-06 | 四川师范大学 | Microwave chemical method for completely extracting fluorine and rare earth in bastnaesite concentrate |
Non-Patent Citations (2)
| Title |
|---|
| 王卫忠等: "氟离子选择电极法测定土壤中氟化物含量", 《宁夏农林科技》, pages 66 - 69 * |
| 王文华;郭丽;宋丽平;曾庆平;钟可?;张燕萍;: "氟离子选择性电极法测定钕铁硼废料中氟含量", 化学工程与装备, no. 06, pages 141 - 146 * |
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