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CN105699372B - A kind of method of testing based on water-soluble soda acid test device - Google Patents

A kind of method of testing based on water-soluble soda acid test device Download PDF

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CN105699372B
CN105699372B CN201610058774.9A CN201610058774A CN105699372B CN 105699372 B CN105699372 B CN 105699372B CN 201610058774 A CN201610058774 A CN 201610058774A CN 105699372 B CN105699372 B CN 105699372B
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solenoid valve
indicator
funnel
cuvette
bottle
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CN105699372A (en
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尹玉娟
刘杰
刘鹏
孙伟
孙昭昌
曹晓华
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State Grid Corp of China SGCC
Qingdao Power Supply Co of State Grid Shandong Electric Power Co Ltd
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Qingdao Power Supply Co of State Grid Shandong Electric Power Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G01N21/80Indicating pH value
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/27Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration

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Abstract

本发明提供了一种基于水溶性酸碱测试装置的测试方法,所述测试装置中所述萃取容器的底端通过第一进液管与所述漏斗连通设置,在所述第一进液管上设置有第一流量计和第一电磁阀;所述指示剂瓶通过第二进液管与所述漏斗连通设置,在所述第二进液管上设置有第二流量计和第二电磁阀。本发明所述的测试装置通过上述设置使得下层萃取相和指示剂分别在各自重力的作用下能够连续地落入漏斗中,从而得以在漏斗的底部均匀混合。本发明的测试装置克服了现有的水溶性酸碱测试装置所需组件繁多、不易组装的缺陷,具有结构简单、便于使用和维护的特点。本发明所述的测试方法可实现对水溶性酸碱的即时检测,且测定结果具有很高的准确度和精确度。

The present invention provides a test method based on a water-soluble acid-base test device. In the test device, the bottom end of the extraction vessel communicates with the funnel through a first liquid inlet pipe. A first flowmeter and a first solenoid valve are arranged on the top; the indicator bottle communicates with the funnel through a second liquid inlet pipe, and a second flowmeter and a second electromagnetic valve are arranged on the second liquid inlet pipe. valve. The test device of the present invention enables the lower extraction phase and the indicator to continuously fall into the funnel under the action of their respective gravity through the above arrangement, so as to be evenly mixed at the bottom of the funnel. The test device of the present invention overcomes the defects that the existing water-soluble acid-base test device requires many components and is difficult to assemble, and has the characteristics of simple structure and convenient use and maintenance. The test method of the invention can realize the instant detection of water-soluble acid and alkali, and the determination result has high accuracy and precision.

Description

一种基于水溶性酸碱测试装置的测试方法A kind of test method based on water-soluble acid-base test device

技术领域technical field

本发明涉及一种酸碱测试方法,尤其涉及一种能够对油品中的水溶性酸碱含量进行自动检测的方法,属于测试方法技术领域。The invention relates to an acid-base test method, in particular to a method capable of automatically detecting the water-soluble acid-base content in oil products, and belongs to the technical field of test methods.

技术背景technical background

石油产品的水溶性酸碱多是由于石油馏分在酸碱精制过程中由未清除干净的残余物所形成的可溶于水的矿物酸或碱,其中,矿物酸主要为硫酸及其衍生物,包括磺酸和酸性硫酸酯,矿物碱主要为苛性钠和碳酸钠。这些水溶性酸碱在油品的生产、使用或贮存过程中,一方面会腐蚀与其接触的金属构件,水溶性碱只腐蚀铝,如汽油中的水溶性碱会使汽化器的铝制零件因生成氢氧化铝胶体物质而堵塞油路、滤清器及油嘴,然而,水溶性酸几乎对所有金属都有强烈的腐蚀作用,如变压器油中的水溶性酸值的增加会使固体绝缘材料和金属产生腐蚀,并降低电气设备的绝缘性能,缩短设备的使用寿命;另一方面油品中含有的水溶性酸碱,在大气中的水分、氧气的相互作用及受热情况下,会引起油品的氧化、胶化、老化及分解。因此,加强水溶性酸碱的检测力度对于维护设备的健康稳定运行具有重要意义。The water-soluble acids and bases of petroleum products are mostly water-soluble mineral acids or bases formed from uncleaned residues in the acid-base refining process of petroleum fractions. Among them, the mineral acids are mainly sulfuric acid and its derivatives. Including sulfonic acid and acidic sulfate ester, the mineral bases are mainly caustic soda and sodium carbonate. During the production, use or storage of oil products, these water-soluble acids and bases will corrode the metal components in contact with them on the one hand, and the water-soluble alkalis will only corrode aluminum. However, water-soluble acid has a strong corrosive effect on almost all metals, such as the increase of water-soluble acid value in transformer oil will make solid insulating materials and metal Corrosion will occur, reduce the insulation performance of electrical equipment, and shorten the service life of the equipment; on the other hand, the water-soluble acid and alkali contained in the oil will cause the oil to deteriorate under the interaction of moisture and oxygen in the atmosphere and under the condition of heat. Oxidation, gelling, aging and decomposition. Therefore, strengthening the detection of water-soluble acids and bases is of great significance for maintaining the healthy and stable operation of equipment.

目前,用于测定电力用油中水溶性酸的方法为人工目视比色法,其具体步骤是:将等体积的蒸馏水与油样混合,加热振荡、静置分层后,收集下层水相,加入溴甲酚绿或溴甲酚紫指示剂后转移至比色皿内,与预先配制好的含有溴甲酚绿或溴甲酚紫的pH标准色阶进行人工目视比色,或者使用海力奇比色计进行人工目视比色,以判断pH值。人工目视比色法存在以下缺陷:(1)整个测定过程步骤繁杂,涉及加热、振荡、测温、取样、排液、显色、比色等环节,采用人工操作的方式效率低、费时长;(2)预先配制的标准色阶会受自然环境的影响而逐渐变色或产生絮状沉淀,进而影响比色结果,导致产生系统误差;(3)人眼对颜色判断的差异不可避免会产生主观误差。At present, the method used to determine water-soluble acids in oil for electric power is artificial visual colorimetry, and its specific steps are: mix equal volumes of distilled water and oil samples, heat and oscillate, stand to separate and separate, and collect the lower aqueous phase , after adding bromocresol green or bromocresol purple indicator, transfer it to a cuvette, and perform manual visual color comparison with the pre-prepared pH standard color scale containing bromocresol green or bromocresol purple, or use The Hailiqi colorimeter performs manual visual color comparison to judge the pH value. The manual visual colorimetry method has the following defects: (1) The entire measurement process is complicated and involves steps such as heating, oscillation, temperature measurement, sampling, liquid drainage, color development, and colorimetry, and the manual operation is inefficient and time-consuming ; (2) The pre-prepared standard color scale will gradually change color or produce flocculent precipitation due to the influence of the natural environment, which will affect the colorimetric results and cause systematic errors; (3) The difference in color judgment by human eyes will inevitably cause subjective error.

为解决人工目视比色法所存在的上述缺陷,中国专利文献CN101614674A公开了一种全自动水溶性酸测定仪,包括试杯、试管、清洗剂瓶、蒸馏水瓶、样品瓶、真空泵、废液瓶、指示剂瓶,所述试杯上设有加热器和温度传感器,所述试杯的杯口分别通过输送管路与清洗剂瓶、蒸馏水瓶、样品瓶、真空泵连通,所述试管的管口通过输送管路与指示剂瓶、试杯联通,所述试杯、试管的底部均通过输送管路与废液瓶联通。虽然上述技术在一定程度上提高了对油品中水溶性酸的测定效率及测定结果的准确度,但由于该技术所述的测定仪是由现有的玻璃器皿加工、组装而成,所需的组件繁多并不易于组装,从而造成对上述测定仪的使用、维护困难,无法实现即时检测。因此,研究与开发一种结构简单、使用维护方便、可即时检测的水溶性酸碱测试装置,是本领域尚未解决的技术难题。In order to solve the above-mentioned defects in the artificial visual colorimetry, Chinese patent document CN101614674A discloses a fully automatic water-soluble acid measuring instrument, which includes a test cup, a test tube, a cleaning agent bottle, a distilled water bottle, a sample bottle, a vacuum pump, a waste liquid bottle, indicator bottle, the test cup is provided with a heater and a temperature sensor, and the mouth of the test cup is respectively connected with a cleaning agent bottle, a distilled water bottle, a sample bottle, and a vacuum pump through a delivery pipeline. The port is connected with the indicator bottle and the test cup through the delivery pipeline, and the bottom of the test cup and the test tube are connected with the waste liquid bottle through the delivery pipeline. Although the above-mentioned technology has improved to a certain extent the accuracy of the measurement efficiency and measurement results of water-soluble acids in oil products, because the measuring instrument described in this technology is processed and assembled from existing glassware, the required There are many components and it is not easy to assemble, which makes it difficult to use and maintain the above-mentioned measuring instrument, and cannot realize instant detection. Therefore, it is an unresolved technical problem in the art to research and develop a water-soluble acid-base testing device that is simple in structure, easy to use and maintain, and capable of instant detection.

发明内容Contents of the invention

本发明解决的是现有技术中的水溶性酸碱检测仪因所需的组件繁多、不易于组装而造成的使用维护困难、无法实现即时检测的问题,进而提供一种结构简单、使用维护方便、可即时检测的水溶性酸碱测试装置及测试方法。The invention solves the problem that the water-soluble acid-base detector in the prior art is difficult to use and maintain and cannot realize real-time detection due to the many components required and the difficulty in assembly, and further provides a simple structure and convenient use and maintenance. , A water-soluble acid-base testing device and testing method capable of immediate detection.

本发明实现上述目的的技术方案为:The technical scheme that the present invention realizes above-mentioned purpose is:

一种基于水溶性酸碱测试装置的测试方法,所述水溶性酸碱测试装置包括:A test method based on a water-soluble acid-base testing device, the water-soluble acid-base testing device comprising:

萃取容器,用于萃取出油样中的水溶性酸或碱,所述萃取容器的底端连通设置有第一进液管,在所述第一进液管上设置有第一流量计和第一电磁阀;与所述萃取容器连接设置有振荡器,所述萃取容器和所述振荡器均位于恒温箱的内部,在所述恒温箱内还设置有温度测定装置;The extraction container is used to extract the water-soluble acid or alkali in the oil sample. The bottom end of the extraction container is communicated with a first liquid inlet pipe, and a first flow meter and a second liquid inlet pipe are arranged on the first liquid inlet pipe. A solenoid valve; an oscillator is connected to the extraction container, and both the extraction container and the oscillator are located inside the thermostat, and a temperature measuring device is also arranged in the thermostat;

指示剂瓶,其内装盛有指示剂,在所述指示剂瓶的底端连通设置有第二进液管,在所述第二进液管上设置有第二流量计和第二电磁阀;An indicator bottle, which contains an indicator, and a second liquid inlet pipe is connected to the bottom end of the indicator bottle, and a second flowmeter and a second solenoid valve are arranged on the second liquid inlet pipe;

漏斗,设置在所述萃取容器和所述指示剂瓶的下方,所述漏斗通过所述第一进液管与所述萃取容器相连通,所述漏斗通过所述第二进液管与所述指示剂瓶相连通,所述漏斗适宜于将所述水溶性酸或碱与所述指示剂混合形成待测液;A funnel is arranged below the extraction container and the indicator bottle, the funnel communicates with the extraction container through the first liquid inlet pipe, and the funnel communicates with the extraction container through the second liquid inlet pipe. The indicator bottle is connected, and the funnel is suitable for mixing the water-soluble acid or alkali with the indicator to form a test solution;

光电比色机构,包括比色皿,所述比色皿设置在所述漏斗的下方,用于接收所述待测液;A photoelectric colorimetric mechanism, including a cuvette, the cuvette is arranged below the funnel for receiving the liquid to be tested;

清洗液瓶,所述清洗液瓶通过第三进液管与所述比色皿相连通,在所述第三进液管上设置有第三电磁阀;A cleaning solution bottle, the cleaning solution bottle communicates with the cuvette through a third liquid inlet pipe, and a third electromagnetic valve is arranged on the third liquid inlet pipe;

真空泵,通过排液管与所述比色皿的底端相连通,在所述排液管上设置有排液电磁阀;A vacuum pump communicates with the bottom end of the cuvette through a liquid discharge pipe, and a liquid discharge solenoid valve is arranged on the liquid discharge pipe;

控制单元,所述控制单元用于控制所述振荡器、第一电磁阀、第二电磁阀、第三电磁阀和所述真空泵的动作;所述控制单元适宜于接收所述温度测定装置传递的温度信息以及所述第一流量计和第二流量计传递的流量信息,并根据所述流量信息控制所述第一电磁阀和第二电磁阀的流量,根据所述温度信息控制所述恒温箱的温度以及所述振荡器的开启时机;A control unit, the control unit is used to control the actions of the oscillator, the first solenoid valve, the second solenoid valve, the third solenoid valve and the vacuum pump; the control unit is suitable for receiving the temperature information and the flow information transmitted by the first flow meter and the second flow meter, and control the flow of the first solenoid valve and the second solenoid valve according to the flow information, and control the thermostat box according to the temperature information temperature and the start timing of the oscillator;

所述测试方法包括如下步骤:Described test method comprises the steps:

(1)初始状态下,控制所述第一电磁阀、第二电磁阀、第三电磁阀和所述排液电磁阀均为关闭状态;向所述指示剂瓶中加入所述指示剂,向所述萃取容器中加入蒸馏水与油样的混合液,当所述恒温箱内的温度达到第一温度阈值时,使用所述振荡器对所述萃取容器进行振荡;(1) In the initial state, control the first solenoid valve, the second solenoid valve, the third solenoid valve and the liquid discharge solenoid valve to be closed; add the indicator to the indicator bottle, A mixture of distilled water and oil sample is added to the extraction container, and when the temperature in the incubator reaches a first temperature threshold, the oscillator is used to oscillate the extraction container;

(2)振荡完成后,所述恒温箱进行降温冷却,当所述恒温箱内的温度达到第二温度阈值时,开启所述第一电磁阀和第二电磁阀,所述混合液的下层萃取相以第一流速流入所述漏斗的同时,所述指示剂以第二流速流入所述漏斗从而得到待测液;其中,所述第一流速为所述第二流速的40-50倍;(2) After the oscillation is completed, the incubator is cooled down. When the temperature in the incubator reaches the second temperature threshold, the first electromagnetic valve and the second electromagnetic valve are opened, and the lower layer of the mixed solution is extracted. While the phase flows into the funnel at the first flow rate, the indicator flows into the funnel at the second flow rate to obtain the liquid to be tested; wherein the first flow rate is 40-50 times the second flow rate;

(3)所述待测液进入所述比色皿以对所述比色皿进行润洗,所述润洗的步骤为:开启所述排液电磁阀和真空泵,将前期进入所述比色皿中的所述待测液排出,然后关闭所述排液电磁阀和真空泵;所述光电比色机构对后期进入所述比色皿中的所述待测液进行比色;(3) The liquid to be tested enters the cuvette to rinse the cuvette, and the step of rinsing is: open the drain solenoid valve and the vacuum pump, and put the liquid into the cuvette in the early stage into the cuvette. The liquid to be tested in the dish is discharged, and then the drain solenoid valve and the vacuum pump are closed; the photoelectric colorimetric mechanism performs colorimetry on the liquid to be tested that enters the cuvette later;

(4)比色结束后,开启所述排液电磁阀和真空泵,将完成比色后的废液排出;开启所述第三电磁阀,所述清洗瓶中的清洗液流入所述比色皿并最终由排液管排出,从而完成清洗工序。(4) After the colorimetry ends, open the liquid discharge solenoid valve and vacuum pump to discharge the waste liquid after the colorimetry is completed; open the third solenoid valve, and the cleaning solution in the cleaning bottle flows into the cuvette And finally discharged by the drain pipe, thus completing the cleaning process.

步骤(1)中,所述第一温度阈值为50-70℃,所述振荡的时间为4-8min;所述第二温度阈值为室温。In step (1), the first temperature threshold is 50-70° C., the oscillation time is 4-8 minutes; the second temperature threshold is room temperature.

步骤(1)中,所述指示剂为溴甲酚紫或溴百里酚蓝。In step (1), the indicator is bromocresol purple or bromothymol blue.

所述蒸馏水与油样的体积比为1:1。The volume ratio of the distilled water to the oil sample is 1:1.

本发明所述的水溶性酸碱测试装置中,所述第一电磁阀、第二电磁阀和第三电磁阀为常闭电磁阀,所述排液电磁阀为常开电磁阀;所述指示剂瓶设置有两个,每个所述指示剂瓶均通过一条单独的第二进液管与所述漏斗相连通,在每条所述第二进液管上均安装有第二流量计和第二电磁阀;在所述漏斗中设置有搅拌装置;在位于所述真空泵和所述排液电磁阀之间的所述排液管上设置有废液回收瓶。In the water-soluble acid-base testing device of the present invention, the first solenoid valve, the second solenoid valve and the third solenoid valve are normally closed solenoid valves, and the drain solenoid valve is a normally open solenoid valve; the indication There are two reagent bottles, each of the indicator bottles communicates with the funnel through a separate second liquid inlet pipe, and a second flow meter and a second flowmeter are installed on each of the second liquid inlet pipes. A second solenoid valve; a stirring device is arranged in the funnel; a waste liquid recovery bottle is arranged on the drain pipe between the vacuum pump and the drain solenoid valve.

本发明所述的基于水溶性酸碱测试装置的测试方法,步骤(2)限定所述混合液的下层萃取相以第一流速流入所述漏斗的同时,所述指示剂以第二流速流入所述漏斗,并限定所述第一流速为所述第二流速的40-50倍,所述下层萃取相与所述指示剂同时流入所述漏斗中从而得到待测液;其原因在于,使下层萃取相和指示剂分别在各自重力的作用下连续地落入漏斗中,由于同时进入漏斗中的下层萃取相和指示剂的体积都非常小,二者在漏斗的底部融合时便能得以均匀混合,如此可以使得全部落入漏斗中的下层萃取相与指示剂混合均匀从而得到待测液,并控制下层萃取相的流速为指示剂流速的40-50倍,以使待测液中的下层萃取相的体积为指示剂体积的40-50倍,从而在保证指示剂的变色敏锐性的前提下尽可能地减少测定误差。本发明所述的测定方法在步骤(3)中,采用光电比色机构对所述比色皿中的所述待测液进行光电比色测定,如此不仅可快速得到测定结果,适宜于油品中水溶性酸碱的快速检测,还可有效克服肉眼观察的误差,大大提高测定结果的准确度和精确度。本发明所述的测定方法在步骤(4)中限定了比色结束后,开启所述排液电磁阀和真空泵,将完成比色后的废液排出;再开启所述第三电磁阀,所述清洗瓶中的清洗液流入所述比色皿并最终由排液管排出,从而完成清洗工序;本发明在测定后还进行清洗处理的目的在于,一方面可实现对油品中水溶性酸碱的即时检测,另一方面确保比色皿的清洁,避免废液在比色皿中的长时间停留可能会为之后的测定引入杂质,从而保证测定结果的准确性。In the test method based on the water-soluble acid-base testing device of the present invention, step (2) defines that while the lower extract phase of the mixed solution flows into the funnel with a first flow rate, the indicator flows into the funnel with a second flow rate. Described funnel, and limit described first flow rate to be 40-50 times of described second flow rate, described lower layer extraction phase flows in described funnel simultaneously with described indicator so as to obtain liquid to be tested; Its reason is to make lower layer The extract phase and the indicator fall into the funnel continuously under the action of their own gravity, and because the volume of the lower extract phase and the indicator entering the funnel at the same time is very small, the two can be mixed evenly when they merge at the bottom of the funnel , so that all the lower extraction phase falling into the funnel can be mixed with the indicator evenly to obtain the test solution, and the flow rate of the lower extraction phase is controlled to be 40-50 times the flow rate of the indicator, so that the lower extraction phase in the test solution The volume of the phase is 40-50 times the volume of the indicator, so as to reduce the measurement error as much as possible under the premise of ensuring the color sensitivity of the indicator. In the determination method of the present invention, in step (3), a photoelectric colorimetric mechanism is used to carry out photoelectric colorimetric measurement of the liquid to be tested in the described cuvette, so that not only the measurement results can be obtained quickly, but also suitable for oil products. The rapid detection of water-soluble acids and bases can also effectively overcome the errors of naked eye observation and greatly improve the accuracy and precision of the measurement results. In the assay method of the present invention, after the colorimetry is defined in step (4), the liquid discharge solenoid valve and the vacuum pump are opened to discharge the waste liquid after the colorimetry is completed; then the third solenoid valve is opened, and the The cleaning solution in the cleaning bottle flows into the cuvette and is finally discharged by the drain pipe, thereby completing the cleaning process; the purpose of the cleaning process after the measurement of the present invention is to realize the removal of water-soluble acid in the oil on the one hand. Real-time detection of alkali, on the other hand, ensures the cleanliness of the cuvette, avoiding the waste liquid staying in the cuvette for a long time may introduce impurities into the subsequent determination, so as to ensure the accuracy of the measurement results.

与现有技术中的水溶性酸碱测试装置相比,本发明所述的水溶性酸碱测试装置具有如下优点:Compared with the water-soluble acid-base test device in the prior art, the water-soluble acid-base test device of the present invention has the following advantages:

(1)本发明所述的水溶性酸碱测试装置,包括萃取容器、指示剂瓶、漏斗、光电比色机构、清洗液瓶和真空泵,并限定所述萃取容器的底端连通设置有第一进液管,在所述第一进液管上设置有第一流量计和第一电磁阀;在所述指示剂瓶的底端连通设置有第二进液管,在所述第二进液管上设置有第二流量计和第二电磁阀;所述漏斗位于所述萃取容器和所述指示剂瓶的下方,所述漏斗通过所述第一进液管与所述萃取容器相连通,并通过所述第二进液管与所述指示剂瓶相连通。本发明的测试装置通过上述设置使得下层萃取相和指示剂分别在各自重力的作用下能够连续地落入漏斗中,由于同时进入漏斗中的下层萃取相和指示剂的体积都非常小,二者在漏斗的底部融合时便能得以均匀混合,如此可以使得全部落入漏斗中的下层萃取相与指示剂混合均匀,从而得到待测液。可见,本发明的测试装置克服了现有的水溶性酸碱测试装置所需组件繁多、不易组装的缺陷,具有结构简单、便于使用和维护的特点。(1) The water-soluble acid-base testing device of the present invention includes an extraction container, an indicator bottle, a funnel, a photoelectric colorimetric mechanism, a cleaning solution bottle and a vacuum pump, and the bottom end of the extraction container is defined to communicate with a first The liquid inlet pipe is provided with a first flow meter and a first electromagnetic valve on the first liquid inlet pipe; a second liquid inlet pipe is provided in communication with the bottom end of the indicator bottle, and a second liquid inlet pipe is arranged on the second liquid inlet pipe. A second flow meter and a second solenoid valve are arranged on the tube; the funnel is located below the extraction container and the indicator bottle, and the funnel communicates with the extraction container through the first liquid inlet pipe, And communicate with the indicator bottle through the second liquid inlet pipe. The test device of the present invention makes the lower layer extract phase and the indicator can continuously fall into the funnel respectively under the effect of respective gravity through the above-mentioned setting, because the volume of the lower layer extract phase and the indicator entering in the funnel at the same time is all very small, both When the bottom of the funnel is fused, it can be mixed evenly, so that the lower extract phase and the indicator that all fall into the funnel can be mixed evenly, so as to obtain the liquid to be tested. It can be seen that the test device of the present invention overcomes the defects that the existing water-soluble acid-base test device requires many components and is difficult to assemble, and has the characteristics of simple structure, easy use and maintenance.

(2)本发明所述的水溶性酸碱测试装置,通过采用控制单元控制所述振荡器、第一电磁阀、第二电磁阀、第三电磁阀和所述真空泵的动作,且所述控制单元适宜于接收所述温度测定装置传递的温度信息以及所述第一流量计和第二流量计传递的流量信息,并根据所述流量信息控制所述第一电磁阀和第二电磁阀的流量,根据所述温度信息控制所述恒温箱的温度以及所述振荡器的开启时机;从而使得本发明的测试装置不仅省去了繁杂的人工操作步骤,有效避免了人工测定造成的系统误差和主观性误差,而且有利于实现对油品中水溶性酸碱的快速、即时测定,大大提高了工作效率及测定结果的准确度。(2) The water-soluble acid-base testing device of the present invention controls the actions of the oscillator, the first solenoid valve, the second solenoid valve, the third solenoid valve and the vacuum pump by using a control unit, and the control The unit is adapted to receive the temperature information transmitted by the temperature measuring device and the flow information transmitted by the first flow meter and the second flow meter, and control the flow of the first solenoid valve and the second solenoid valve according to the flow information , according to the temperature information to control the temperature of the incubator and the opening timing of the oscillator; thus, the test device of the present invention not only saves complicated manual operation steps, but also effectively avoids systematic errors and subjective errors caused by manual measurement. It is beneficial to realize the rapid and real-time determination of water-soluble acid and alkali in oil products, which greatly improves the work efficiency and the accuracy of the determination results.

此外,本发明所述的水溶性酸碱测试装置进一步限定指示剂瓶设置有两个,每个所述指示剂瓶均通过一条单独的第二进液管与所述漏斗相连通,在每条所述第二进液管上均安装有第二流量计和第二电磁阀;如此设置的优点在于,使得本发明通过振荡萃取得到的下层萃取相能够分别与酸或碱指示剂进行混合,再经过比色测定,从而不仅能够得到油品的水溶性酸值,还可得到水溶性碱值,也就是说,本发明所述的测试装置通过采用不同类型的酸碱指示剂而达到对油品的水溶性酸或碱含量进行测定的效果。In addition, the water-soluble acid-base testing device of the present invention further defines that there are two indicator bottles, and each of the indicator bottles is connected to the funnel through a separate second liquid inlet pipe. The second flow meter and the second solenoid valve are installed on the second liquid inlet pipe; the advantage of such arrangement is that the lower extraction phase obtained by the vibration extraction of the present invention can be mixed with the acid or alkali indicator respectively, and then Through colorimetric measurement, not only the water-soluble acid value of the oil product can be obtained, but also the water-soluble alkali value can be obtained. The effect of the water-soluble acid or alkali content is determined.

附图说明Description of drawings

图1为本发明所述的水溶性酸碱测试装置的结构示意图;Fig. 1 is the structural representation of water-soluble acid-base testing device of the present invention;

其中,附图标记如下所示:Among them, the reference signs are as follows:

1-萃取容器;2-第一进液管;3-第一流量计;4-第一电磁阀;5-恒温箱;6-指示剂瓶;7-第二进液管;8-第二流量计;9-第二电磁阀;10-漏斗;11-光电比色机构;12-比色皿;13-清洗液瓶;14-第三进液管;15-第三电磁阀;16-真空泵;17-排液管;18-排液电磁阀;19-废液回收瓶。1-extraction container; 2-first liquid inlet pipe; 3-first flow meter; 4-first solenoid valve; 5-incubator; 6-indicator bottle; 7-second liquid inlet pipe; 8-second Flowmeter; 9-Second solenoid valve; 10-Funnel; 11-Photoelectric colorimetric mechanism; 12-Cuvette; 13-Cleaning liquid bottle; 14-Third inlet pipe; 15-Third solenoid valve; Vacuum pump; 17-drain pipe; 18-drain solenoid valve; 19-waste liquid recovery bottle.

具体实施方式Detailed ways

下面结合具体实施例对本发明提供的水溶性酸碱测试装置及测试方法进行详细说明。The water-soluble acid-base testing device and testing method provided by the present invention will be described in detail below in conjunction with specific examples.

实施例1Example 1

本实施例所述的水溶性酸碱测试装置,如图1所示,包括:The water-soluble acid-base testing device described in the present embodiment, as shown in Figure 1, comprises:

萃取容器1,用于萃取出油样中的水溶性酸或碱,所述萃取容器1的底端连通设置有第一进液管2,在所述第一进液管2上设置有第一流量计3和第一电磁阀4;与所述萃取容器1连接设置有振荡器,所述萃取容器1和所述振荡器均位于恒温箱5的内部,在所述恒温箱5内还设置有温度测定装置;The extraction container 1 is used to extract the water-soluble acid or alkali in the oil sample. The bottom end of the extraction container 1 is communicated with a first liquid inlet pipe 2, and a first liquid inlet pipe 2 is arranged on the first liquid inlet pipe 2. A flow meter 3 and a first electromagnetic valve 4; an oscillator is connected to the extraction container 1, and the extraction container 1 and the oscillator are both located inside the thermostat 5, and the thermostat 5 is also provided with temperature measuring device;

指示剂瓶6,其内装盛有指示剂,在所述指示剂瓶6的底端连通设置有第二进液管7,在所述第二进液管7上设置有第二流量计8和第二电磁阀9;The indicator bottle 6 is filled with an indicator, and the bottom end of the indicator bottle 6 is communicated with a second liquid inlet pipe 7, and a second flow meter 8 and a second flow meter 8 are arranged on the second liquid inlet pipe 7. The second solenoid valve 9;

漏斗10,设置在所述萃取容器1和所述指示剂瓶6的下方,所述漏斗10通过所述第一进液管2与所述萃取容器1相连通,所述漏斗10通过所述第二进液管7与所述指示剂瓶6相连通,所述漏斗10适宜于将所述水溶性酸或碱与所述指示剂混合形成待测液;A funnel 10 is arranged below the extraction container 1 and the indicator bottle 6, the funnel 10 communicates with the extraction container 1 through the first liquid inlet pipe 2, and the funnel 10 passes through the first The second liquid inlet pipe 7 is in communication with the indicator bottle 6, and the funnel 10 is suitable for mixing the water-soluble acid or alkali with the indicator to form a liquid to be tested;

光电比色机构11,包括比色皿12,所述比色皿12设置在所述漏斗10的下方,用于接收所述待测液;Photoelectric colorimetric mechanism 11, including cuvette 12, described cuvette 12 is arranged below the described funnel 10, is used to receive described liquid to be tested;

清洗液瓶13,所述清洗液瓶13通过第三进液管14与所述比色皿12相连通,在所述第三进液管14上设置有第三电磁阀15;A cleaning liquid bottle 13, the cleaning liquid bottle 13 communicates with the cuvette 12 through a third liquid inlet pipe 14, and a third electromagnetic valve 15 is arranged on the third liquid inlet pipe 14;

真空泵16,通过排液管17与所述比色皿12的底端相连通,在所述排液管17上设置有排液电磁阀18。The vacuum pump 16 communicates with the bottom end of the cuvette 12 through a liquid discharge pipe 17 , and a liquid discharge solenoid valve 18 is arranged on the liquid discharge pipe 17 .

在本实施例中,所述第一电磁阀4、第二电磁阀9和第三电磁阀15为常闭电磁阀,所述排液电磁阀18为常开电磁阀。In this embodiment, the first solenoid valve 4 , the second solenoid valve 9 and the third solenoid valve 15 are normally closed solenoid valves, and the drain solenoid valve 18 is a normally open solenoid valve.

基于本实施所述的水溶性酸碱测试装置对水溶性酸进行测试的方法,包括如下步骤:The method for testing water-soluble acid based on the water-soluble acid-base testing device described in this implementation may further comprise the steps:

(1)初始状态下,控制所述第一电磁阀、第二电磁阀、第三电磁阀和所述排液电磁阀均为关闭状态;向所述指示剂瓶中加入溴甲酚紫指示剂,向所述萃取容器中加入等体积的蒸馏水与油样的混合液,当所述恒温箱内的温度达到50℃时,使用所述振荡器对所述萃取容器进行振荡8min;(1) In the initial state, control the first solenoid valve, the second solenoid valve, the third solenoid valve and the drain solenoid valve to be closed; add bromocresol purple indicator in the indicator bottle , adding an equal volume of a mixture of distilled water and oil sample to the extraction vessel, and when the temperature in the thermostat reaches 50°C, use the oscillator to vibrate the extraction vessel for 8 minutes;

(2)振荡完成后,所述恒温箱进行降温冷却,当所述恒温箱内的温度达到室温时,开启所述第一电磁阀和第二电磁阀,所述混合液的下层萃取相以第一流速流入所述漏斗的同时,所述溴甲酚紫指示剂以第二流速流入所述漏斗从而得到待测液;其中,所述第一流速为所述第二流速的40倍;(2) After the oscillation is completed, the incubator is cooled down, and when the temperature in the incubator reaches room temperature, the first solenoid valve and the second solenoid valve are opened, and the lower extract phase of the mixed solution is separated by the first When a flow rate flows into the funnel, the bromocresol purple indicator flows into the funnel at a second flow rate to obtain the test solution; wherein the first flow rate is 40 times that of the second flow rate;

(3)所述待测液进入所述比色皿中,所述光电比色机构对所述比色皿中的所述待测液进行比色;(3) the liquid to be tested enters the cuvette, and the photoelectric colorimetric mechanism performs colorimetry on the liquid to be tested in the cuvette;

(4)比色结束后,开启所述排液电磁阀和真空泵,将完成比色后的废液排出;开启所述第三电磁阀,所述清洗瓶中的蒸馏水流入所述比色皿并最终由排液管排出,从而完成清洗工序。(4) After the colorimetry ends, open the liquid discharge solenoid valve and vacuum pump to discharge the waste liquid after the colorimetry is completed; open the third solenoid valve, the distilled water in the cleaning bottle flows into the cuvette and Finally, it is discharged from the drain pipe, thus completing the cleaning process.

实施例2Example 2

本实施例所述的水溶性酸碱测试装置,如图1所示,包括:The water-soluble acid-base testing device described in the present embodiment, as shown in Figure 1, comprises:

萃取容器1,用于萃取出油样中的水溶性酸或碱,所述萃取容器1的底端连通设置有第一进液管2,在所述第一进液管2上设置有第一流量计3和第一电磁阀4;与所述萃取容器1连接设置有振荡器,所述萃取容器1和所述振荡器均位于恒温箱5的内部,在所述恒温箱5内还设置有温度测定装置;The extraction container 1 is used to extract the water-soluble acid or alkali in the oil sample. The bottom end of the extraction container 1 is communicated with a first liquid inlet pipe 2, and a first liquid inlet pipe 2 is arranged on the first liquid inlet pipe 2. A flow meter 3 and a first electromagnetic valve 4; an oscillator is connected to the extraction container 1, and the extraction container 1 and the oscillator are both located inside the thermostat 5, and the thermostat 5 is also provided with temperature measuring device;

指示剂瓶6,其内装盛有指示剂,在所述指示剂瓶6的底端连通设置有第二进液管7,在所述第二进液管7上设置有第二流量计8和第二电磁阀9;The indicator bottle 6 is filled with an indicator, and the bottom end of the indicator bottle 6 is communicated with a second liquid inlet pipe 7, and a second flow meter 8 and a second flow meter 8 are arranged on the second liquid inlet pipe 7. The second solenoid valve 9;

漏斗10,设置在所述萃取容器1和所述指示剂瓶6的下方,所述漏斗10通过所述第一进液管2与所述萃取容器1相连通,所述漏斗10通过所述第二进液管7与所述指示剂瓶6相连通,在所述漏斗10中设置有搅拌装置,本实施例中所述搅拌装置为搅拌子,所述漏斗10适宜于将所述水溶性酸或碱与所述指示剂混合形成待测液;A funnel 10 is arranged below the extraction container 1 and the indicator bottle 6, the funnel 10 communicates with the extraction container 1 through the first liquid inlet pipe 2, and the funnel 10 passes through the first The second liquid inlet pipe 7 communicates with the indicator bottle 6, and a stirring device is arranged in the funnel 10. In this embodiment, the stirring device is a stirring bar, and the funnel 10 is suitable for mixing the water-soluble acid Or the base is mixed with the indicator to form a test solution;

光电比色机构11,包括比色皿12,所述比色皿12设置在所述漏斗10的下方,用于接收所述待测液;Photoelectric colorimetric mechanism 11, including cuvette 12, described cuvette 12 is arranged below the described funnel 10, is used to receive described liquid to be tested;

清洗液瓶13,所述清洗液瓶13通过第三进液管14与所述比色皿12相连通,在所述第三进液管14上设置有第三电磁阀15;A cleaning liquid bottle 13, the cleaning liquid bottle 13 communicates with the cuvette 12 through a third liquid inlet pipe 14, and a third electromagnetic valve 15 is arranged on the third liquid inlet pipe 14;

真空泵16,通过排液管17与所述比色皿12的底端相连通,在所述排液管17上设置有排液电磁阀18;在位于所述真空泵16和所述排液电磁阀18之间的所述排液管17上设置有废液回收瓶19;The vacuum pump 16 communicates with the bottom end of the cuvette 12 through a liquid discharge pipe 17, and a liquid discharge solenoid valve 18 is arranged on the liquid discharge pipe 17; A waste liquid recovery bottle 19 is arranged on the drain pipe 17 between 18;

控制单元,所述控制单元用于控制所述振荡器、第一电磁阀4、第二电磁阀9、第三电磁阀15和所述真空泵16的动作;所述控制单元适宜于接收所述温度测定装置传递的温度信息以及所述第一流量计3和第二流量计8传递的流量信息,并根据所述流量信息控制所述第一电磁阀4和第二电磁阀9的流量,根据所述温度信息控制所述恒温箱5的温度以及所述振荡器的开启时机。a control unit for controlling the actions of the oscillator, the first solenoid valve 4, the second solenoid valve 9, the third solenoid valve 15 and the vacuum pump 16; the control unit is adapted to receive the temperature Measure the temperature information transmitted by the device and the flow information transmitted by the first flow meter 3 and the second flow meter 8, and control the flow of the first electromagnetic valve 4 and the second electromagnetic valve 9 according to the flow information, and according to the flow information The temperature information controls the temperature of the thermostat 5 and the start timing of the oscillator.

在本实施例中,所述第一电磁阀4、第二电磁阀9和第三电磁阀15为常闭电磁阀,所述排液电磁阀18为常开电磁阀。所述指示剂瓶6设置有两个,每个所述指示剂瓶6均通过一条单独的第二进液管7与所述漏斗10相连通,在每条所述第二进液管7上均安装有第二流量计8和第二电磁阀9。In this embodiment, the first solenoid valve 4 , the second solenoid valve 9 and the third solenoid valve 15 are normally closed solenoid valves, and the drain solenoid valve 18 is a normally open solenoid valve. There are two indicator bottles 6, and each indicator bottle 6 communicates with the funnel 10 through a separate second liquid inlet pipe 7, and on each second liquid inlet pipe 7 Both are equipped with a second flowmeter 8 and a second solenoid valve 9 .

基于本实施所述的水溶性酸碱测试装置对水溶性碱进行测试的方法,包括如下步骤:The method for testing water-soluble alkali based on the water-soluble acid-base testing device described in this implementation may further comprise the steps:

(1)初始状态下,控制所述第一电磁阀、第二电磁阀、第三电磁阀和所述排液电磁阀均为关闭状态;向其中一个所述指示剂瓶中加入溴百里酚蓝指示剂,向所述萃取容器中加入等体积的蒸馏水与油样的混合液,当所述恒温箱内的温度达到70℃时,使用所述振荡器对所述萃取容器进行振荡4min;(1) In the initial state, control the first solenoid valve, the second solenoid valve, the third solenoid valve and the drain solenoid valve to be closed; add bromothymol to one of the indicator bottles For the blue indicator, add an equal volume of distilled water and oil sample mixture into the extraction container, and when the temperature in the incubator reaches 70°C, use the oscillator to vibrate the extraction container for 4 minutes;

(2)振荡完成后,所述恒温箱进行降温冷却,当所述恒温箱内的温度达到室温时,开启所述第一电磁阀和第二电磁阀,所述混合液的下层萃取相以第一流速流入所述漏斗的同时,所述溴百里酚蓝指示剂以第二流速流入所述漏斗,搅拌后从而得到待测液;其中,所述第一流速为所述第二流速的50倍;(2) After the oscillation is completed, the incubator is cooled down, and when the temperature in the incubator reaches room temperature, the first solenoid valve and the second solenoid valve are opened, and the lower extract phase of the mixed solution is separated by the first When a flow rate flows into the funnel, the bromothymol blue indicator flows into the funnel at a second flow rate, and after stirring, the test solution is obtained; wherein the first flow rate is 50% of the second flow rate. times;

(3)将部分所述待测液送入所述比色皿中,开启所述排液电磁阀和真空泵排出所述部分待测液;然后关闭所述排液电磁阀和真空泵,另一部分所述待测液进入润洗后的比色皿中,所述光电比色机构对所述润洗后的比色皿中的所述待测液进行比色;(3) Send part of the liquid to be tested into the cuvette, open the drain solenoid valve and vacuum pump to discharge the part of the liquid to be tested; then close the drain solenoid valve and vacuum pump, and the other part of the liquid to be tested The liquid to be tested enters the cuvette after rinsing, and the photoelectric colorimetric mechanism performs colorimetry to the liquid to be tested in the cuvette after the rinsing;

(4)比色结束后,再次开启所述排液电磁阀和真空泵,将完成比色后的废液排出至废液回收瓶中;开启所述第三电磁阀,所述清洗瓶中的蒸馏水流入所述比色皿并最终由排液管排出至废液回收瓶中,从而完成清洗工序。(4) After the colorimetry ends, open the liquid discharge electromagnetic valve and the vacuum pump again, and discharge the waste liquid after the colorimetry to the waste liquid recovery bottle; open the third electromagnetic valve, and the distilled water in the cleaning bottle It flows into the cuvette and is finally discharged into the waste liquid recovery bottle through the drain pipe, thereby completing the cleaning process.

显然,上述实施例仅仅是为清楚地说明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。Apparently, the above-mentioned embodiments are only examples for clear description, rather than limiting the implementation. For those of ordinary skill in the art, on the basis of the above description, other changes or changes in different forms can also be made. It is not necessary and impossible to exhaustively list all the implementation manners here. And the obvious changes or changes derived therefrom are still within the scope of protection of the present invention.

Claims (4)

  1. A kind of 1. method of testing based on water-soluble soda acid test device, it is characterised in that:
    The water-soluble soda acid test device includes:
    Extraction container (1), for extracting water soluble acid or alkali in oil sample, the bottom connection of the extraction container (1) is set There is the first feed tube (2), first flowmeter (3) and the first magnetic valve (4) are provided with first feed tube (2);With institute State extraction container (1) and be connected with oscillator, the extraction container (1) and the oscillator are respectively positioned on the interior of insulating box (5) Portion, temperature measuring apparatus is additionally provided with the insulating box (5);
    Indicator bottle (6), its is built-in to fill indicator, and the second feed tube is provided with and communicated with the bottom of the indicator bottle (6) (7) second flowmeter (8) and second solenoid valve (9), are provided with second feed tube (7);
    Funnel (10), is arranged on the lower section of the extraction container (1) and the indicator bottle (6), and the funnel (10) passes through institute State the first feed tube (2) with the extraction container (1) to be connected, the funnel (10) passes through second feed tube (7) and institute State indicator bottle (6) to be connected, the water soluble acid or alkali are mixed to form prepare liquid by the funnel (10) with the indicator;
    Photoelectric colorimetry mechanism (11), including cuvette (12), the cuvette (12) are arranged on the lower section of the funnel (10), use In the reception prepare liquid;
    Cleaning fluid bottle (13), the cleaning fluid bottle (13) are connected by the 3rd feed tube (14) with the cuvette (12), The 3rd magnetic valve (15) is provided with 3rd feed tube (14);
    Vavuum pump (16), it is connected by discharging tube (17) with the bottom of the cuvette (12), on the discharging tube (17) It is provided with draining solenoid valve (18);
    Control unit, described control unit are used to control the oscillator, the first magnetic valve (4), second solenoid valve (9), the 3rd The action of magnetic valve (15) and the vavuum pump (16);Described control unit receives the temperature letter of the temperature measuring apparatus transmission The flow information that breath and the first flowmeter (3) and second flowmeter (8) are transmitted, and institute is controlled according to the flow information The first magnetic valve (4) and the flow of second solenoid valve (9) are stated, the temperature of the insulating box (5) is controlled according to the temperature information And the unlatching opportunity of the oscillator;
    The method of testing comprises the following steps:
    (1) under original state, control first magnetic valve, second solenoid valve, the 3rd magnetic valve and the draining solenoid valve equal For closed mode;The indicator is added into the indicator bottle, distilled water and oil sample are added into the extraction container Mixed liquor, when the temperature in the insulating box reaches the first temperature threshold, the extraction container is entered using the oscillator Row vibration;
    (2) after the completion of vibrating, the insulating box carries out cooling down, when the temperature in the insulating box reaches second temperature threshold value When, first magnetic valve and second solenoid valve are opened, lower floor's extraction phase of the mixed liquor flows into the leakage with the first flow velocity While bucket, the indicator flows into the funnel so as to obtain prepare liquid with second flow speed;Wherein, first flow velocity is institute State second flow speed 40-50 times;
    (3) prepare liquid enters to carry out rinse to the cuvette in the cuvette, is the step of the rinse:Open The draining solenoid valve and vavuum pump, the prepare liquid that early stage is entered in the cuvette are discharged, and are then shut off the row Liquid electromagnetic valve and vavuum pump;The photoelectric colorimetry mechanism carries out colorimetric to the prepare liquid that the later stage enters in the cuvette;
    (4) after colorimetric terminates, the draining solenoid valve and vavuum pump are opened, the waste liquid after completion colorimetric is discharged;Described in unlatching 3rd magnetic valve, the cleaning fluid in the washer bottle flows into the cuvette and finally discharged by discharging tube, so as to complete to clean Process.
  2. 2. method of testing according to claim 1, it is characterised in that in step (1), first temperature threshold is 50- 70 DEG C, the time of the vibration is 4-8min;The second temperature threshold value is room temperature.
  3. 3. method of testing according to claim 1, it is characterised in that in step (1), the indicator be bromocresol purple or Bromthymol blue.
  4. 4. according to the method for testing described in claim any one of 1-3, it is characterised in that the volume ratio of the distilled water and oil sample For 1:1.
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US10048127B2 (en) * 2015-08-05 2018-08-14 Viavi Solutions Inc. Optical filter and spectrometer
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