WO2020098361A1 - 双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置 - Google Patents

双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置 Download PDF

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WO2020098361A1
WO2020098361A1 PCT/CN2019/105473 CN2019105473W WO2020098361A1 WO 2020098361 A1 WO2020098361 A1 WO 2020098361A1 CN 2019105473 W CN2019105473 W CN 2019105473W WO 2020098361 A1 WO2020098361 A1 WO 2020098361A1
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module
excitation current
electrode
end point
platinum electrode
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PCT/CN2019/105473
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孙颖奇
卢欣春
罗勇钢
刘冠军
倪亮
雷丽江
杨明鑫
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国电南瑞科技股份有限公司
南瑞集团有限公司
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Publication of WO2020098361A1 publication Critical patent/WO2020098361A1/zh

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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
    • G01N27/416—Systems
    • G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte

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  • the invention relates to the technology of a permanganate index online analyzer, in particular to a double platinum electrode type permanganate index online analyzer titration end indicator device.
  • the potassium permanganate oxidation-titration method is the analysis principle widely used by the online permanganate index water quality analyzer.
  • redox potential (ORP, Oxidation-Reduction Potential) electrode is usually used to monitor the redox potential of the reaction solution. Near the end of the titration, the redox potential of the reaction system will gradually increase and stabilize at a certain value. The judgment of the end point of the titration can be realized by judging the threshold value of the redox potential.
  • the ORP electrode uses platinum as the working electrode, silver chloride as the reference electrode, and the microporous material as the liquid junction.
  • the reference electrode filling solution is usually a saturated potassium chloride solution, which will cause loss at the liquid junction.
  • the potassium permanganate oxidation-titration method is widely used in the online analyzer of permanganate index.
  • the online analyzer in the related art usually uses the ORP electrode to monitor the potential of the reaction system and judge the end point by the threshold voltage.
  • the ORP potential of the reaction system is greater than a certain threshold voltage to indicate the end point of the titration. There is a deviation in the end point indication.
  • the ORP electrode is prone to aging, causing potential drift and requiring regular replacement, which affects the overall performance of the analyzer.
  • the embodiments of the present invention provide a titration end point indicator device of a double platinum electrode type permanganate index online analyzer, which uses a double platinum electrode to determine the end point of the titration.
  • the titration end point indication method used is unique, the end point indication is accurate, and is not affected by the electrode voltage drift.
  • the titration end point indicating device provided by the double platinum electrode type permanganate index online analyzer provided by the embodiment of the present invention includes: a double platinum electrode, an excitation current commutation module, a constant current source module, a signal acquisition module and a microprocessor module.
  • the double platinum electrode is placed in the reaction solution, the constant current source module is connected to two platinum plates of the double platinum electrode through an excitation current commutation module, and the excitation current commutation module is connected to a signal acquisition module.
  • the signal acquisition module is connected with the microprocessor module.
  • the constant current source module includes a reference voltage source, an integrated precision differential amplifier, a high input impedance operational amplifier and a sampling resistor.
  • the reference voltage source is integrated with the sampling resistor and high input impedance through an integrated precision differential amplifier The amplifier is connected.
  • the constant current source module generates a microamp-level excitation current.
  • the double platinum electrode includes two platinum sheets, and the distance between the two platinum sheets is 5-10 mm.
  • the signal acquisition module amplifies and filters the double platinum electrode signal and then inputs it into the microprocessor module through analog-to-digital conversion.
  • the microprocessor module searches for the maximum value according to the collected electrode signal data sequence and gives an indication signal for the end point of the titration.
  • the excitation current commutation module commutes the excitation current at intervals of 12 hours or 24 hours under the control of the microprocessor module.
  • the device applies a small constant current to the double platinum electrode and collects the voltage on the double platinum electrode at the same time.
  • the end point of the titration is indicated by the change of the voltage on the double platinum electrode under constant current excitation.
  • the remarkable feature of this device is that at the end of the titration, the voltage on the double platinum electrode will have a maximum value, through which the end value of the titration can be accurately indicated.
  • the device is also designed with an excitation current commutation module to commutate the excitation current at a certain time interval, which effectively reduces the ion adhesion on the electrode surface and improves the reliability;
  • the embodiment of the present invention uses a double platinum electrode for the titration endpoint Judging that the electrode structure is simple, the maintenance rate is low, and the service life is long.
  • the titration end point indication method adopted by the invention is unique, the end point indication is accurate, and is not affected by the electrode voltage drift.
  • FIG. 1 is a functional block diagram of an endpoint indicating device of a double platinum electrode type permanganate index online analyzer provided by an embodiment of the present invention
  • FIG. 2 is a schematic block diagram of a constant current source module provided by an embodiment of the present invention.
  • FIG. 3 is a graph of a titration voltage provided by an embodiment of the present invention.
  • FIG. 1 is a schematic block diagram of an end point indicating device of a double platinum electrode type permanganate index online analyzer provided by an embodiment of the present invention.
  • a double platinum electrode type permanganate index online analyzer end point indicator The device consists of double platinum electrodes 1, excitation current commutation module 2, constant current source module 3, signal acquisition module 4, and microprocessor module 5.
  • the double platinum electrode 1 is placed in the reaction solution 6, and the constant current source module 3 generates a microampere-level excitation current and is applied to the two platinum electrode through the excitation current commutation module 4
  • the excitation current I flows in from the platinum sheet 1-1, and after flowing through the reaction solution 6, flows out from the platinum sheet 1-2.
  • the excitation current I will flow from the platinum plate 1-2, and after passing through the reaction solution 6, will flow out from the platinum plate 1-1.
  • the distance between the two platinum sheets 1-1 and 1-2 of the double platinum electrode 1 is d, and d is usually selected to be 5-10 mm.
  • the voltage signal generated on the double platinum electrodes 1 is input into the signal acquisition module 4 through the excitation current commutation module 2.
  • the signal acquisition module 4 amplifies and filters the signal of the double platinum electrode 1 and then enters the microprocessor module 5 through analog-to-digital conversion.
  • the microprocessor module 5 searches for the maximum value according to the collected electrode signal data sequence and gives an indication signal for the end point of the titration, and at the same time controls the excitation current commutation module 2 to commutate the excitation current at intervals of 12 hours or 24 hours.
  • the monitoring frequency of the permanganate index is 6 times / day. At this frequency, the excitation current can be commutated at 24-hour intervals. If it is higher than this frequency, the commutation can be performed at 12-hour intervals.
  • FIG. 2 is a functional block diagram of a constant current source module provided by an embodiment of the present invention.
  • the constant current source module 3 adopts a Holland current source structure, which is composed of a reference voltage source 3-1 and an integrated precision differential amplifier 3-2. , Sampling resistance 3-3, high input impedance operational amplifier 3-4.
  • the reference voltage source 3-1 is connected to the sampling resistor 3-3 and the high input impedance operational amplifier 3-4 through an integrated precision differential amplifier 3-2, respectively.
  • the constant current source 3 has good dynamic response characteristics and can provide a constant current in the order of microamperes.
  • the constant current value is determined by the reference voltage source 3-1 and the sampling resistor 3-3.
  • the potassium permanganate solution is dropped into the sodium oxalate solution drop by drop.
  • the reaction process can be described by the following ion reaction equation.
  • the solution contained only the reduced state, and the potassium permanganate solution was gradually dropped into the reaction system to produce the oxidation state.
  • the device provided by the embodiment of the present invention is used to monitor the voltage change on the double platinum electrodes during this process and perform the end point indication.
  • the voltage signal on the double platinum electrode during the titration can be described by the following formula.
  • E is the voltage signal on the double platinum electrode
  • I is the excitation current
  • x is the titration fraction
  • R is the thermodynamic constant
  • T is the thermodynamic temperature
  • n is the number of gain and loss electrons
  • F is the Faraday constant
  • K is the constant
  • FIG. 3 is a voltage curve of a device provided by an embodiment of the present invention during a titration process of a permanganate index online analyzer.
  • the excitation current I When the excitation current I is applied to the double platinum electrodes, there will be an electrolytic effect, which causes the ions in the sample to adhere to the platinum plate in the actual water sample measurement. For this reason, the excitation current I will be commutated at certain intervals to reduce the platinum plate electrode. Ion attachment.
  • the device applies a tiny constant current to the double platinum electrode and collects the voltage on the double platinum electrode at the same time.
  • the titration end point is indicated by the change of the voltage on the double platinum electrode under constant current excitation.
  • the remarkable feature of this device is that at the end of the titration, the voltage on the double platinum electrode will have a maximum value, through which the end value of the titration can be accurately indicated.
  • the device is also designed with an excitation current commutation module to commutate the excitation current at a certain time interval, which effectively reduces the ion adhesion on the electrode surface and improves the reliability.
  • the embodiment of the invention adopts double platinum electrodes to judge the end point of titration, the electrode structure is simple, the maintenance rate is low, and the service life is long.
  • the titration end point indication method adopted in the embodiment of the present invention is unique, the end point indication is accurate, and is not affected by electrode voltage drift.

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Abstract

一种双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置，包括双铂电极（1）、激励电流换向模块（2）、恒流源模块（3）、信号采集模块（4）和微处理器模块（5），该双铂电极（1）置于反应溶液（6）中，该恒流源模块（3）经过激励电流换向模块（2）与双铂电极（1）的两个铂片（1-1，1-2）相连接，该激励电流换向模块（2）与信号采集模块（4）相连接，该信号采集模块（4）与微处理器模块（5）相连接。

Description

双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置
相关申请的交叉引用
本申请基于申请号为201811346457.2、申请日为2018年11月13日的中国专利申请提出，并要求该中国专利申请的优先权，该中国专利申请的全部内容在此引入本申请作为参考。
技术领域
本发明涉及高锰酸盐指数在线分析仪技术，尤其涉及一种双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置。
背景技术
高锰酸钾氧化-滴定法是高锰酸盐指数水质在线分析仪所广泛采用的分析原理。在滴定过程中，通常采用氧化还原电位(ORP，Oxidation-Reduction Potential)电极来监测反应溶液的氧化还原电位，在滴定终点附近，反应体系氧化还原电位会逐渐升高，并稳定于某一值，通过对氧化还原电位的阈值判断即可实现对滴定终点的判断。ORP电极以铂为工作电极，氯化银为参比电极，以微孔材质作为液接界，参比电极填充液通常为饱和氯化钾溶液，会在液接界处产生损耗，一方面会干扰测量，另一方面会导致电极电位漂移，从而影响滴定终点判断的准确度，降低分析仪性能表现。为此，高锰酸盐指数在线分析仪的ORP电极需定期维护、定期更换，提高了运维成本。
高锰酸钾氧化-滴定法在高锰酸盐指数在线分析仪中得到了广泛应有。在滴定过程中，相关技术中的在线分析仪通常采用ORP电极来监测反应体系电位并通过阈值电压来进行终点判断，以反应体系ORP电位大于某一阈值电压来指示滴定终点，终点指示存在偏差。在使用过程中ORP电极容易 老化，产生电位漂移，需要定期更换，影响了分析仪的整体性能表现。
发明内容
为克服相关技术的缺陷，本发明实施例提供一种双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置，采用双铂电极进行滴定终点判断，电极结构简单，维护率低，使用寿命长，采用的滴定终点指示方式具有唯一性，终点指示准确，且不受电极电压漂移影响。
本发明实施例提供的双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置，包括：双铂电极、激励电流换向模块、恒流源模块、信号采集模块和微处理器模块，所述双铂电极置于反应溶液中，所述恒流源模块经过激励电流换向模块与双铂电极的两个铂片相连接，所述激励电流换向模块与信号采集模块相连接，所述信号采集模块与微处理器模块相连接。
上述方案中，所述恒流源模块包括基准电压源、集成精密差动放大器、高输入阻抗运算放大器和取样电阻，所述基准电压源通过集成精密差动放大器分别与取样电阻和高输入阻抗运算放大器相连接。
上述方案中，所述恒流源模块产生微安量级激励电流。
上述方案中，所述双铂电极包括两个铂片，两个铂片之间的间距为5～10mm。
上述方案中，所述信号采集模块将双铂电极信号放大滤波后经过模数转换输入微处理器模块中。
上述方案中，所述微处理器模块根据采集到的电极信号数据序列寻找最大值并给出滴定终点指示信号。
上述方案中，所述激励电流换向模块在微处理器模块控制下以12小时或24小时的时间间隔对激励电流进行换向。
应用本发明实施例具备以下有益技术效果：
该装置在滴定过程中在双铂电极上施加微小的恒定电流并同时采集双 铂电极上的电压，通过恒定电流激励下双铂电极上电压的变化来指示滴定终点。该装置的显著特点是在滴定终点处，双铂电极上的电压会有极大值，通过该极大值可以准确指示滴定终点。同时该装置内还设计有激励电流换向模块，以一定的时间间隔对激励电流进行换向，有效降低了电极表面的离子附着，提升了可靠性；本发明实施例采用双铂电极进行滴定终点判断，电极结构简单，维护率低，使用寿命长。本发明采用的滴定终点指示方式具有唯一性，终点指示准确，且不受电极电压漂移影响。
附图说明
图1为本发明实施例提供的双铂电极式高锰酸盐指数在线分析仪终点指示装置的原理框图；
图2为本发明实施例提供的恒流源模块的原理框图；
图3为本发明实施例提供的滴定电压曲线图。
具体实施方式
下面结合附图对本发明作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
图1为本发明实施例提供的双铂电极式高锰酸盐指数在线分析仪终点指示装置的原理框图，如图1所示，一种双铂电极式高锰酸盐指数在线分析仪终点指示装置，由双铂电极1，激励电流换向模块2，恒流源模块3，信号采集模块4，微处理器模块5组成。在高锰酸盐指数在线分析仪滴定过程中，双铂电极1置于反应溶液6中，恒流源模块3产生微安量级激励电流经过激励电流换向模块4施加到双铂电极的两个铂片1-1、1-2上。在图1所示的激励电流换向模块2状态下，激励电流I从铂片1-1上流入，经过反应溶液6后，从铂片1-2上流出。当激励电流换向模块2切换至另一种状态时，激励电流I将从铂片1-2上流入，经过反应溶液6后，从铂片1-1上 流出。双铂电极1的两个铂片1-1、1-2之间的间距为d，d通常可选为5～10mm。激励电流I流过反应溶液6时会在铂片1-1、1-2上产生电势差，形成电压信号。双铂电极1上产生的电压信号经过激励电流换向模块2输入信号采集模块4中。信号采集模块4将双铂电极1信号放大滤波后经过模数转换输入微处理器模块5中。微处理器模块5根据采集到的电极信号数据序列寻找最大值并给出滴定终点指示信号，同时控制激励电流换向模块2以12小时或24小时的时间间隔对激励电流进行换向。通常情况高锰酸盐指数的监测频次为6次/天，在此频次下可以24小时的时间间隔对激励电流换向，若高于此频次，则可以12小时的时间间隔进行换向。
图2为本发明实施例提供的恒流源模块的原理框图，如图2所示，恒流源模块3采用Holland电流源结构，由基准电压源3-1、集成精密差动放大器3-2、取样电阻3-3、高输入阻抗运算放大器3-4组成。基准电压源3-1通过集成精密差动放大器3-2分别与取样电阻3-3和高输入阻抗运算放大器3-4相连接。恒流源3具有良好的动态响应特性，可以提供微安量级的恒定电流，恒流值由基准电压源3-1与取样电阻3-3决定。
高锰酸盐指数分析仪在滴定过程中，高锰酸钾溶液逐滴滴入到草酸钠溶液中，反应过程可由如下离子反应方程式描述。
Figure PCTCN2019105473-appb-000001
在滴定开始前，溶液中只含有还原态，随着高锰酸钾溶液的滴入反应体系中逐渐产生氧化态。本发明实施例提供的装置用于监测这一过程中双铂电极上的电压变化，并进行终点指示。滴定过程中双铂电极上的电压信号可由下式描述。
Figure PCTCN2019105473-appb-000002
式中E为双铂电极上的电压信号；I为激励电流；x为滴定分数；R为热力学常数；T为热力学温度；n为得失电子数；F为法拉第常数；K为常 数；C为滴定开始前还原物质的浓度。由公式可得，在一定的溶液环境中，在滴定终点处(x＝1)，双铂电极上的电压信号会有极大值，通过该极大值即可指示滴定终点。相较于ORP电极以大于阈值电压来判断滴定终点，本发明所述装置的滴定终点判定具有唯一性，且维护性显著优于ORP电极终点指示装置。图3为本发明实施例提供的装置在高锰酸盐指数在线分析仪滴定过程中的电压曲线。
激励电流I施加到双铂电极上，会产生电解效应，造成在实际水样测量中样品中的离子在铂片上附着，为此激励电流I将以一定时间间隔进行换向以降低铂片电极上的离子附着。
该装置在滴定过程中在双铂电极上施加微小的恒定电流并同时采集双铂电极上的电压，通过恒定电流激励下双铂电极上电压的变化来指示滴定终点。该装置的显著特点是在滴定终点处，双铂电极上的电压会有极大值，通过该极大值可以准确指示滴定终点。同时该装置内还设计有激励电流换向模块，以一定的时间间隔对激励电流进行换向，有效降低了电极表面的离子附着，提升了可靠性。本发明实施例采用双铂电极进行滴定终点判断，电极结构简单，维护率低，使用寿命长。本发明实施例采用的滴定终点指示方式具有唯一性，终点指示准确，且不受电极电压漂移影响。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变形，这些改进和变形也应视为本发明的保护范围。

Claims (7)

  1. 一种双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置，包括：
    双铂电极、激励电流换向模块、恒流源模块、信号采集模块和微处理器模块，所述双铂电极置于反应溶液中，所述恒流源模块经过激励电流换向模块与双铂电极的两个铂片相连接，所述激励电流换向模块与信号采集模块相连接，所述信号采集模块与微处理器模块相连接。
  2. 根据权利要求1所述的装置，其中，所述恒流源模块包括基准电压源、集成精密差动放大器、高输入阻抗运算放大器和取样电阻，所述基准电压源通过集成精密差动放大器分别与取样电阻和高输入阻抗运算放大器相连接。
  3. 根据权利要求1所述的装置，其中，所述恒流源模块产生微安量级激励电流。
  4. 根据权利要求1所述的装置，其中，所述双铂电极包括两个铂片，两个铂片之间的间距为5～10mm。
  5. 根据权利要求1所述的装置，其中，所述信号采集模块将双铂电极信号放大滤波后经过模数转换输入微处理器模块中。
  6. 根据权利要求1所述的装置，其中，所述微处理器模块根据采集到的电极信号数据序列寻找最大值并给出滴定终点指示信号。
  7. 根据权利要求1所述的装置，其中，所述激励电流换向模块在微处理器模块控制下以12小时或24小时的时间间隔对激励电流进行换向。
PCT/CN2019/105473 2018-11-13 2019-09-11 双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置 WO2020098361A1 (zh)

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CN109521077A (zh) * 2018-11-13 2019-03-26 国电南瑞科技股份有限公司 一种双铂电极式高锰酸盐指数在线分析仪滴定终点指示装置
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