CN112630374A - Automatic potentiometric titration detection method for analyzing content of effective calcium oxide in lime - Google Patents
Automatic potentiometric titration detection method for analyzing content of effective calcium oxide in lime Download PDFInfo
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Abstract
The invention belongs to the technical field of quality detection of content determination of effective calcium oxide in lime used in the production process of aluminum oxide, and particularly relates to an automatic potentiometric titration detection method for content analysis of effective calcium oxide in lime, which mainly solves the technical problems of poor detection result accuracy, high reagent consumption, low detection efficiency, complicated operation process and the like of an artificial titration analysis method adopted by the existing detection method for the content of effective calcium oxide in lime. According to the method, the reaction principle in the process of detecting the content of the effective calcium oxide in the lime is acid-base neutralization reaction, the pH value in a reaction cup can change along with the continuation of the reaction process, the corresponding pH value indication titration end point is identified through the electrode potential change on an automatic potentiometric titrator, and the detection and analysis of the content of the effective calcium oxide in the lime are realized. The detection result of the invention eliminates the poor accuracy of the detection result of manual titration, and has the advantages of simple operation, low reagent consumption and high detection efficiency, and can accurately and rapidly realize the detection and analysis of the content of the effective calcium oxide in the lime.
Description
Technical Field
The invention belongs to the technical field of alumina production quality detection, and particularly relates to an automatic potentiometric titration detection method for analyzing the content of effective calcium oxide in lime. The titration end point is indicated based on that the electrode potential on an automatic potentiometric titrator changes along with the change of the environment in a reaction cup, the reaction principle is acid-base neutralization reaction in the process of detecting the content of effective calcium oxide in lime, the pH value in the reaction cup changes along with the continuous reaction process, and the corresponding pH value indication titration end point is identified through the change of the electrode potential on the automatic potentiometric titrator.
Background
A large amount of lime is used in the process of producing alumina by the alkali Bayer process, and the quality of the lime is measured mainly by the content of effective calcium oxide in the lime. The settlement between the company and the external supply lime manufacturer mainly takes the effective calcium oxide content as the settlement basis, and the economic benefit of the company is directly influenced by the accuracy of the effective calcium content detected in the detection workshop.
At present, a manual titration method is adopted in a detection workshop, and the content of effective calcium oxide in lime is determined by visually observing the color change of an indicator to determine a titration end point. The method has the problems of non-uniform color difference between people, relatively low precision and accuracy of detection results, lower manual titration working efficiency compared with automatic potentiometric titration, high reagent consumption and complicated operation process, and needs to be improved. Therefore, it is necessary to provide an automatic potentiometric titration detection method for analyzing the content of effective calcium oxide in lime, which is used for solving the technical problems of relatively low accuracy of a measurement result, low working efficiency, high reagent consumption, complicated operation process and the like caused by non-uniform color difference between people.
Disclosure of Invention
The invention provides an automatic potentiometric titration detection method for analyzing the content of effective calcium oxide in lime, aiming at the problems of relatively poor detection result accuracy, high reagent consumption, low detection efficiency and complicated operation process of a manual titration analysis method.
In order to solve the technical problems, the invention adopts the technical scheme that:
an automatic potentiometric titration detection method for analyzing the content of effective calcium oxide in lime is based on that the electrode potential on an automatic potentiometric titrator can change along with the change of the environment in a reaction cup to indicate a titration end point, and the method is characterized in that a dynamic titration method (DET method) is selectively established in Wantong timao2.5 titration software, experimental result acquisition is carried out on parameters in a WAIT command, parameters in an STIR command and parameters in a DET-pH command in a continuous adjustment method, the purpose that the absolute difference between the acquisition result and an artificial titration result is less than or equal to 0.3 percent is achieved, the optimal parameters in the command are selected, the content of the optimal parameters is analyzed and detected, the pH value in the reaction cup can change along with the continuation of the reaction process according to the reaction principle in the detection process of the content of the effective calcium oxide in lime, the corresponding pH value indication titration end point is accurately identified through the electrode potential change on the automatic potentiometric, the content of the effective calcium oxide in the lime is detected and analyzed by automatic potentiometric titration instead of manual titration, and a result matched with a manual titration result is obtained.
Further, the electrode potential change indication titration end point on the automatic potentiometric titrator is based on the fact that a lime sample added with excessive sucrose solution and a hydrochloric acid standard solution (titrant) are subjected to acid-base neutralization reaction, the electrode potential can be changed along with the continuous reaction process, the pH value of the set end point is identified to indicate the titration end point through the electrode potential change inserted into the sample reaction cup, and the purpose that the automatic potentiometric titration method can detect the content of effective calcium oxide in lime is achieved.
Further, the automatic potentiometric titration detection method for analyzing the content of the effective calcium oxide in the lime is based on the indication of titration end point of the change of the electrode potential on an automatic potentiometric titrator, and the method comprises the steps of weighing a certain amount of lime sample, adding excessive sucrose water with a certain concentration, reacting sucrose with calcium oxide to generate sucrose calcium with high solubility, completing titration by using the automatic potentiometric titrator filled with a standard titrant, selectively establishing a dynamic titration method (DET method) in Wantong timao2.5 titration software, and collecting experimental results by continuously adjusting parameters in a WAIT command, parameters in a STIR command and parameters in a DET-pH command in the method, wherein the analysis and detection specifically comprises the following steps:
step one, selectively establishing a dynamic titration method DET method in Wantong timao2.5 titration software;
secondly, adjusting the waiting time of the WAIT command in the dynamic titration method to be 7 min; stirring speed in STIR command "10"; signal drift in the start condition in DET-pH command is "off", signal drift in the titration parameter is "off", measurement point density is "0", stop measurement pH in stop condition is "8.5", measurement value (pH) window in potential evaluation is evaluated as "upper limit 9, lower limit 5", fixed equivalence point evaluation measurement value in additional break point is "pH 8.7"; variable select "FP (1)" in CALC command;
thirdly, weighing 0.0990-0.1010g lime sample in a reaction cup of 100 mL;
fourthly, adding 30-40mL of 8% sucrose water, and placing on a 855 automatic potentiometric titrator sample rack;
fifthly, calling the adjusted dynamic titration method in the second step, and inputting the sample weight;
and sixthly, executing titration, finishing the titration and recording the result.
Compared with the prior art, the invention has the following advantages:
the method has the advantages of high automation degree, high accuracy of detection results, high analysis efficiency, low reagent consumption and simple operation.
Drawings
FIG. 1 is a schematic diagram of a detection method after completion of creation;
FIG. 2 is a schematic view of a stirring speed setting;
FIG. 3 is a schematic illustration of the stir wait time setting;
FIG. 4 is a schematic diagram of a start condition parameter set-up;
FIG. 5 is a schematic view of titration parameter settings;
FIG. 6 is a schematic view of a stop condition parameter set;
FIG. 7 is a schematic diagram of potential evaluation parameter settings;
FIG. 8 is an additional schematic view of a breakpoint parameter set;
FIG. 9 is a schematic diagram of calculation formula settings;
FIG. 10 is a schematic view of a dynamic titration curve.
Detailed Description
Example 1
The automatic potentiometric titration detection method for analyzing the content of the effective calcium oxide in the lime in the implementation is based on that the electrode potential on an automatic potentiometric titrator changes along with the continuous reaction process in a reaction cup to indicate the titration end point, and the method is to selectively establish a dynamic titration method (DET method) in Wantong timao2.5 titration software, determine the optimal parameters by continuously adjusting the parameters in a WAIT command, the parameters in an STIR command and the parameters in a DET-pH command in the method, and execute the analysis and detection task. Weighing a certain amount of lime sample, adding excessive sucrose water with a certain concentration, calling a detection method after adjustment to control the whole titration process to be automatically completed, identifying a titration end point by using an automatic potentiometric titration upper electrode, completing the acquisition of an experimental result, and requiring that the absolute difference between the acquisition result and a manual titration result is less than or equal to 0.3%. The method comprises the following steps:
in the first step, a dynamic titration method (DET method) was selectively created within the Wantong timao2.5 titration software.
Secondly, adjusting the waiting time of the WAIT command in the titration method to be 7 min; stirring speed in STIR command "10"; signal drift in the start condition in DET-pH command is "off", signal drift in the titration parameter is "off", measurement point density is "0", stop measurement pH in stop condition is "8.5", measurement value (pH) window in potential evaluation is evaluated as "upper limit 9, lower limit 5", fixed equivalence point evaluation measurement value in additional break point is "pH 8.7"; the variable in the CALC command selects "FP (1)".
Third, weigh "0.0990-0.1010 g lime sample into a 100mL reaction cup.
And fourthly, adding 30-40mL of 8% sucrose water, and placing on a 855 sample holder of an automatic potentiometric titrator.
And fifthly, calling the adjusted dynamic titration method in the software, and inputting the sample weight.
And sixthly, executing titration, finishing the titration and recording the result.
Example 2
The same sample is analyzed and detected by an artificial titration method and an automatic potentiometric titration method respectively, absolute difference comparison is carried out on the detection results, whether the absolute difference between the automatic potentiometric titration result and the artificial titration result is controlled within a required range or not is verified, and the absolute difference comparison is shown in table 1.
Table 1: absolute difference comparison table
As can be seen from Table 1: the absolute difference between the automatic potentiometric titration result and the manual titration result meets the required range, the operation is simple, the reagent consumption is low, the detection efficiency is high, and the manual titration method can be replaced.
Those skilled in the art will appreciate that the invention may be practiced without these specific details. Although illustrative embodiments of the present invention have been described above to facilitate the understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, and various changes may be made apparent to those skilled in the art as long as they are within the spirit and scope of the present invention as defined and defined by the appended claims, and all matters of the invention which utilize the inventive concepts are protected.
Claims (3)
1. The automatic potentiometric titration detection method for analyzing the content of the effective calcium oxide in the lime is characterized by comprising the following steps of: the automatic potentiometric titration detection method for analyzing the content of the effective calcium oxide in the lime is based on the indication of titration end point of the electrode potential change on an automatic potentiometric titrator, and the method is characterized in that a dynamic titration method DET method is selectively established in Wantong timao2.5 titration software, the optimal parameters are determined by continuously adjusting parameters in a WAIT command, parameters in an STIR command and parameters in a DET-pH command in the method, an analysis detection task is executed, the detection method after the adjustment is finished controls the whole titration process to be automatically finished, the titration end point is identified by using the electrode on the automatic potentiometric titration, the acquisition of an experimental result is finished, and the absolute difference between the acquisition result and an artificial titration result is less than or equal to 0.3%.
2. The automatic potentiometric titration method for analyzing the content of available calcium oxide in lime according to claim 1, wherein: the electrode potential change indication titration end point on the automatic potentiometric titrator is based on the fact that a sample added with excessive sucrose solution reacts with a hydrochloric acid standard solution, the electrode potential changes along with the continuous reaction process, and the set end point pH value indication titration end point is identified through the electrode potential change inserted into a sample reaction cup.
3. The automatic potentiometric titration method for analyzing the content of available calcium oxide in lime according to claim 2, wherein: the automatic potentiometric titration detection method for analyzing the content of the effective calcium oxide in the lime is based on the indication of titration end point of the change of the electrode potential on an automatic potentiometric titrator, and the method comprises the following specific steps of weighing a certain amount of lime sample, adding excessive sucrose water with a certain concentration, reacting sucrose with calcium oxide to generate sucrose calcium with high solubility, completing titration by using the automatic potentiometric titrator filled with a standard titrant, selectively establishing a dynamic titration method DET method in Wantong timao2.5 titration software, and collecting experimental results by continuously adjusting parameters in a WAIT command, parameters in an STIR command and parameters in a DET-pH command in the method, wherein the specific steps of analysis and detection are as follows:
step one, selectively establishing a dynamic titration method DET method in Wantong timao2.5 titration software;
secondly, adjusting the waiting time of the WAIT command in the dynamic titration method to be 7 min; stirring speed in STIR command "10"; in the DET-pH command, the signal drift in the start condition is "off", the signal drift in the titration parameter is "off", the measurement point density is "0", the stop measurement pH in the stop condition is "8.5", the window with measurement pH in the potential evaluation is evaluated as "upper limit 9, lower limit 5", the fixed equivalence point in the additional break point is evaluated as "pH ═ 8.7"; the argument selects "FP-1" in the CALC command;
thirdly, weighing 0.0990-0.1010g lime sample in a reaction cup of 100 mL;
fourthly, adding 30-40mL of 8% sucrose water, and placing on a 855 automatic potentiometric titrator sample rack;
fifthly, calling the adjusted dynamic titration method in the second step, and inputting the sample weight;
and sixthly, executing titration, finishing the titration and recording the result.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113640454A (en) * | 2021-07-30 | 2021-11-12 | 华能国际电力股份有限公司上海石洞口第一电厂 | Method for rapidly testing content of calcium oxide in limestone |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101968451A (en) * | 2010-10-13 | 2011-02-09 | 中国石油化工股份有限公司 | Method for measuring acid values of oil and products by using greening solvent based on potential jump |
| CN102590318A (en) * | 2012-02-24 | 2012-07-18 | 深圳市特种设备安全检验研究院 | Method and device for continuously analyzing pH value, phenolphthalein end-point alkalinity, total alkalinity and chloridion concentration |
| CN202453323U (en) * | 2012-02-24 | 2012-09-26 | 深圳市特种设备安全检验研究院 | Device for continuously analyzing pH (potential of hydrogen) value, phenolphthalein alkalinity, total alkalinity and chlorine ion concentration |
| CN103033550A (en) * | 2011-09-29 | 2013-04-10 | 鞍钢股份有限公司 | Method for simultaneously determining total calcium, sulfate calcium and calcium sulfite in desulfurized fly ash |
| CN104101722A (en) * | 2014-07-15 | 2014-10-15 | 广州特种承压设备检测研究院 | Multi-object continuous automatic analysis device and method for industrial boiler water quality detection |
| CN104876968A (en) * | 2015-04-28 | 2015-09-02 | 同济大学 | Polypyridine chiral ruthenium (II) complex and preparation method and application thereof |
| CN105067756A (en) * | 2015-08-03 | 2015-11-18 | 广西中烟工业有限责任公司 | Potentiometric titration determining method of boric acid in water-based adhesive |
| CN105954341A (en) * | 2016-04-26 | 2016-09-21 | 中国冶金地质总局山东局测试中心 | Method for continuous analysis determination of calcium oxide and magnesium oxide in limestone |
| CN106680420A (en) * | 2016-12-31 | 2017-05-17 | 攀枝花东方钛业有限公司 | Detection method for effective calcium oxide content in quick lime |
| CN107119311A (en) * | 2017-06-29 | 2017-09-01 | 昆山福仕电子材料工业有限公司 | The quick clean online plating solution negative pressure evaporation reuse method of electronickelling production line and equipment |
| CN109917070A (en) * | 2019-03-26 | 2019-06-21 | 东莞东阳光科研发有限公司 | The detection method of free lithium content is remained in tertiary cathode material |
| CN110726803A (en) * | 2019-11-01 | 2020-01-24 | 江苏扬农化工集团有限公司 | Method for determining amino value by automatic potentiometric titration |
| CN211970457U (en) * | 2020-03-02 | 2020-11-20 | 山西华兴铝业有限公司 | Electrolytic aluminum oxide bin |
-
2020
- 2020-12-30 CN CN202011614952.4A patent/CN112630374A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101968451A (en) * | 2010-10-13 | 2011-02-09 | 中国石油化工股份有限公司 | Method for measuring acid values of oil and products by using greening solvent based on potential jump |
| CN103033550A (en) * | 2011-09-29 | 2013-04-10 | 鞍钢股份有限公司 | Method for simultaneously determining total calcium, sulfate calcium and calcium sulfite in desulfurized fly ash |
| CN102590318A (en) * | 2012-02-24 | 2012-07-18 | 深圳市特种设备安全检验研究院 | Method and device for continuously analyzing pH value, phenolphthalein end-point alkalinity, total alkalinity and chloridion concentration |
| CN202453323U (en) * | 2012-02-24 | 2012-09-26 | 深圳市特种设备安全检验研究院 | Device for continuously analyzing pH (potential of hydrogen) value, phenolphthalein alkalinity, total alkalinity and chlorine ion concentration |
| CN104101722A (en) * | 2014-07-15 | 2014-10-15 | 广州特种承压设备检测研究院 | Multi-object continuous automatic analysis device and method for industrial boiler water quality detection |
| CN104876968A (en) * | 2015-04-28 | 2015-09-02 | 同济大学 | Polypyridine chiral ruthenium (II) complex and preparation method and application thereof |
| CN105067756A (en) * | 2015-08-03 | 2015-11-18 | 广西中烟工业有限责任公司 | Potentiometric titration determining method of boric acid in water-based adhesive |
| CN105954341A (en) * | 2016-04-26 | 2016-09-21 | 中国冶金地质总局山东局测试中心 | Method for continuous analysis determination of calcium oxide and magnesium oxide in limestone |
| CN106680420A (en) * | 2016-12-31 | 2017-05-17 | 攀枝花东方钛业有限公司 | Detection method for effective calcium oxide content in quick lime |
| CN107119311A (en) * | 2017-06-29 | 2017-09-01 | 昆山福仕电子材料工业有限公司 | The quick clean online plating solution negative pressure evaporation reuse method of electronickelling production line and equipment |
| CN109917070A (en) * | 2019-03-26 | 2019-06-21 | 东莞东阳光科研发有限公司 | The detection method of free lithium content is remained in tertiary cathode material |
| CN110726803A (en) * | 2019-11-01 | 2020-01-24 | 江苏扬农化工集团有限公司 | Method for determining amino value by automatic potentiometric titration |
| CN211970457U (en) * | 2020-03-02 | 2020-11-20 | 山西华兴铝业有限公司 | Electrolytic aluminum oxide bin |
Non-Patent Citations (4)
| Title |
|---|
| 徐风广等: "《无机非金属材料化验与检测实训》", 31 July 2018, 中国建材工业出版社 * |
| 莫允焕等: "自动电位滴定准确检测酱油还原糖含量的研究", 《中 国 调 味 品》 * |
| 谭丽菊等: "《化学海洋实验》", 30 April 2018, 中国海洋大学出版社 * |
| 黄文娴等: "铁矿中水溶性氯化物测定的前处理方法的研究", 《广东化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113640454A (en) * | 2021-07-30 | 2021-11-12 | 华能国际电力股份有限公司上海石洞口第一电厂 | Method for rapidly testing content of calcium oxide in limestone |
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