A device and method for automatically measuring volatile phenol in water

Abstract

The present invention discloses a device and method for automatically measuring volatile phenol in water, including an automatic integrated distiller, multiple collecting bottles, a multi-way valve, a pump, an extraction bottle and a spectrophotometer, wherein the collecting bottle is used to collect the distillate of the integrated distiller, and each collecting bottle leads to a pipeline, which is respectively connected to each interface of the multi-way valve, the central interface of the multi-way valve is connected to the pump, and the extraction bottle is connected to a port of the multi-way valve for extracting the distillate. The pump is used to transport a reaction reagent to the collecting bottle or the extraction bottle, or to transport a distillate and chloroform to the extraction bottle, and the spectrophotometer is used to measure the absorbance of the chloroform in the extraction bottle after the extraction is completed, and the absorbance is proportional to the concentration, so that the concentration of volatile phenol can be calculated. The present invention combines the automatic integrated distiller, and then realizes automatic reagent addition, automatic extraction, automatic measurement and cleaning, and realizes full automation of the detection process according to the standard HJ503-2009 method, and does not require manual intervention during the measurement.

Description

Technical Field

[0001] The invention relates to the technical field of measuring volatile phenols, and in particular to a device and method for automatically measuring volatile phenols in water. Background Art

[0002] Volatile phenol: It is an important indicator for measuring water quality, which refers to phenol that can evaporate with water vapor. The main pollution sources of phenol are industrial wastewater from gas scrubbing, coking, synthetic ammonia, papermaking, wood preservation and chemical industries. The standard method for measuring volatile phenol is 4-aminoantipyrine spectrophotometry (H503-2009).

[0003] Measuring volatile phenol is one of the water quality monitoring items. Manual operation requires adding reagents for distillation, transfer, extraction, separation, measurement and other steps. There are many steps, the measurement precision is not high, and it also involves contact with toxic chloroform, which is harmful to the human body. If the entire detection operation is automated, these problems can be overcome.

[0004] The existing standard method is operated manually throughout the process, which takes a long time to operate. Distillation and extraction are both troublesome pre-treatment tasks, which are not easy to master for operators without operating experience. Moreover, direct contact with toxic chloroform is harmful to the human body. At present, the only method for automatically measuring volatile phenols is flow injection, which is a technology that appeared in the 1980s and was widely used after 2000. Flow injection devices for automatically measuring volatile phenols are relatively common. This device is carried out in a way inherent to flow injection, adding reagents, distillation, and measurement during the flow process, but there is no extraction, which is different from the standard method in my country. Because extraction also has the effect of enrichment, the absorbance of low-concentration water samples is increased to a measurable level, and flow injection is difficult to achieve the entire process of automatic distillation and automatic extraction, so only the direct photometric method of integrating the absorbance of distilled water samples can be used. Summary of the invention

[0005] The purpose of the present invention is to provide a device and method for automatically measuring volatile phenol in water to solve the problems existing in the above-mentioned prior art. In combination with an automatic distiller, automatic reagent addition, automatic extraction, automatic measurement and cleaning are realized. According to the HJ 503-2009 standard, the detection process is fully automated without the need for manual intervention.

[0006] To achieve the above-mentioned purpose, the present invention provides the following scheme: The present invention provides a device for automatically measuring volatile phenols in water, comprising an automatic integrated distiller, a plurality of collecting bottles, a multi-way valve, a pump, an extraction bottle and a spectrophotometer, wherein the collecting bottle is used to collect the distillate of the integrated distiller, a pipeline is led out from each collecting bottle and respectively connected to each interface of the multi-way valve, the central interface of the multi-way valve is connected to the pump, and the extraction bottle is connected to one port of the multi-way valve; the pump is used to transport reaction reagents to the collecting bottle or the extraction bottle, or to transport distillate and chloroform to the extraction bottle; the spectrophotometer is used to measure the absorbance of chloroform in the extraction bottle after the extraction is completed, and the absorbance is proportional to the concentration, so that the concentration of volatile phenols in water can be calculated.

[0007] Preferably, a plurality of the collecting bottles are placed on an electronic balance respectively, and the value of the distillate weighed by the electronic balance is 250g; when the weight of the distillate in the collecting bottle reaches 250g, the electronic balance feeds back information to the integrated distiller, and the controller of the integrated distiller stops the heating distillation of the distiller.

[0008] Preferably, the multi-way valve has a central interface, and the central interface can be communicated with any one of the multiple interfaces of the valve.

[0009] Preferably, the pump is a peristaltic pump or a syringe pump or a metering pump, and the pump is connected to the central interface of the multi-way valve, and each interface of the multi-way valve is used to connect the distillate, the buffer, the oxidant, the developer and the chloroform respectively.

[0010] Preferably, among the multiple interfaces of the multi-way valve, one interface is connected to the inlet of the extraction bottle.

[0011] Preferably, an electric extractor is provided in the extraction bottle.

[0012] Preferably, the cuvette of the spectrophotometer is connected to an interface of the multi-way valve.

[0013] The present invention also provides a method for automatically measuring volatile phenol in water, which is applied to the above-mentioned device for automatically measuring volatile phenol in water, and comprises the following steps:

[0014] 1) Water sample distillation: the water samples are respectively placed in the distillation bottles of the integrated distillation apparatus, an appropriate amount of phosphoric acid is added, the distillation is heated and distilled, and the distillate is collected in the collection bottle; when the electronic balance measures that the weight of the solution in the collection bottle reaches 250g, the heating of the distillation apparatus is automatically stopped; a pipeline is led out of the collection bottle and connected to one port of the multi-way valve;

[0015] 2) Add reagents for reaction: the pump starts to work, and the pump sequentially adds a buffer, an oxidant and a developer to each collection bottle through the multi-way valve, and reacts for 10 minutes to generate an orange-red antipyrine dye;

[0016] 3) Transferring samples: After the reaction in step 2) is completed, the pump automatically transfers the reacted solution in the collection bottle to the extraction bottle through the multi-way valve;

[0017] 4) Extraction by adding chloroform: Use a pump to accurately add 10 ml of chloroform to the extraction bottle, start the extractor, extract the solution in the extraction bottle, and then let it stand to allow the chloroform and water to separate;

[0018] 5) Measurement: Since chloroform has a greater specific gravity than water and sinks below the solution, the pump transfers the chloroform below the extraction bottle to the cuvette of the spectrophotometer to measure the absorbance. The absorbance is proportional to the concentration, so the concentration of volatile phenols in the water can be calculated.

[0019] Compared with the prior art, the present invention has achieved the following technical effects:

[0020] 1. The device and method for automatically measuring volatile phenol in water of the present invention combines the existing integrated automatic distillation instrument with a multi-way valve to realize automatic reagent addition, automatic extraction and automatic measurement of volatile phenol in water, and realizes full automation.

[0021] 2. The basic structure of the collecting bottle on the integrated distiller remains unchanged and is still placed on the automatic balance. An outlet pipeline is drawn out from the bottom of the bottle. The outlet of each bottle is connected to a port of the multi-way valve, so that each distillate reaches the extraction bottle through the multi-way valve. When the weight of the distilled distillate reaches 250 grams, the instrument automatically performs operations such as adding reagents, transfer, extraction, and detection.

[0022] 3. Through the multi-way valve, the three reagents can be automatically added to each distillate for reaction. After the reaction, the solution is automatically transferred to the extraction bottle for extraction by a pump, and then transferred to the spectrophotometer cuvette for measurement. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0024] Figure 1 This is a schematic diagram of the overall structure of a device for automatically measuring volatile phenols in water;

[0025] Among them, 1 integrated distillation apparatus; 2 collecting bottle; 3 multi-way valve; 4 pump; 5 extraction bottle; 6 spectrophotometer; 7 multi-way valve; 8 various reagents. DETAILED DESCRIPTION

[0026] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] The purpose of the present invention is to provide a device and method for automatically measuring volatile phenols in water to solve the problems existing in the above-mentioned prior art. In combination with an automatic distiller, automatic reagent addition, automatic extraction, automatic measurement and cleaning are realized. According to the standard HJ503-2009 method, the detection process is fully automated and does not require human intervention.

[0028] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0029] like Figure 1 As shown, the present invention provides a device for automatically measuring volatile phenol in water, comprising an automatic integrated distiller 1, a plurality of collecting bottles 2, a multi-way valve 3, a pump 4, an extraction bottle 5, a spectrophotometer 6, a multi-way valve 7 and various reagents 8. The plurality of collecting bottles 2 are used to collect the distillate of the integrated distiller 1, a pipeline connected to a certain interface of the multi-way valve 3 is led out from the bottom of each collecting bottle 2, the central interface of the multi-way valve 3 is connected to the pump 4 through a pipeline, the extraction bottle 5 is connected to the multi-way valve 7 through a pipeline, the pump 4 is used to transport the reaction reagents to the collecting bottle 2 and the distillate and chloroform after the reaction is completed to the extraction bottle 5, and the spectrophotometer 6 is used to measure the absorbance of the chloroform below the extraction bottle 5 after the extraction is completed, and the absorbance is proportional to the concentration, so that the concentration of volatile phenol in water can be calculated.

[0030] Specifically, multiple collecting bottles 2 are placed on an electronic balance, and the preset value of the electronic balance is 250g. When the weight of the distillate in the collecting bottle 2 reaches 250g, the electronic balance feeds back information to the controller of the distiller, and the controller controls the integrated distiller 1 to immediately stop heating and distillation.

[0031] Pump 4 is a peristaltic pump or an injection pump or a metering pump. If it is an injection pump, it is connected to the central port of the multi-way valve, and can draw in and out reagents or solutions. If it is a peristaltic pump, it can be turned in both positive and negative directions, and the reagents and solutions connected to the multi-way valve 3 and the multi-way valve 7 can be respectively transported. The multi-way valve can also be replaced by multiple single-way or three-way electromagnetic valves. In this example, the six interfaces of the multi-way valve 3 are respectively connected to six collecting bottles, and one interface is connected to chloroform; the three interfaces of the multi-way valve 7 are respectively connected to the buffer, the oxidant and the developer, one interface is connected to the extraction bottle, and one interface is connected to the colorimetric vessel of the spectrophotometer. Pump 4 pumps the buffer, the oxidant and the developer into the collecting bottle 2 in sequence, and reacts with the distillate in the collecting bottle 2. After the reaction is completed, it is pumped into the extraction bottle 5 by pump 4 for extraction.

[0032] The extraction bottle 5 is provided with an extractor, which can extract by stirring or oscillating to extract the volatile phenols in the distillate into chloroform.

[0033] After extraction and stratification, the chloroform at the bottom of the extraction bottle 5 is transported by pump 4 through multi-way valve 7 to the cuvette of spectrophotometer 6 to measure the absorbance. The absorbance is proportional to the concentration, so the concentration of volatile phenols in water can be calculated.

[0034] The present invention discloses a method for automatically measuring volatile phenol in water, which is applied to the above-mentioned device for automatically measuring volatile phenol in water and comprises the following steps:

[0035] 1) Water sample distillation: The water sample is placed in each distillation bottle, and an appropriate amount of phosphoric acid is added. The distillation is heated and 250 ml of distillate is collected in the collection bottle 2. When 250 ml of distillate is distilled, the process must be stopped, so each collection bottle 2 is placed on an automatic balance. When the weight of the solution reaches 250 grams, the heating of the integrated distiller 1 is stopped. To this end, the present invention leads a pipeline from the bottom of the collection bottle 2 of the existing integrated distiller 1, which is connected to a port of the multi-way valve 3. The reagent is added through this pipeline for reaction, and the distillate after the reaction is transferred to the extraction bottle 5.

[0036] 2) Add reagents for reaction: After the distillation is completed, the pump 4 automatically starts to work, and the buffer, oxidant and developer are added to each collection bottle 2 in turn through the multi-way valve 3, and react for 10 minutes to generate orange-red antipyrine dye.

[0037] 3) Sample transfer: After the reaction in step 2) is completed, the solution in the collection bottle 2 after the reaction is completed is transferred to the extraction bottle 5 through the multi-way valve by using the pump 4.

[0038] 4) Extraction by adding chloroform: Use pump 4 or a syringe pump to accurately add 10 ml of chloroform to the extraction bottle 5, start the extractor, fully extract the solution in the bottle 5, and then let it stand to allow the chloroform and water to separate;

[0039] 5) Measurement: Since chloroform has a greater specific gravity than water and sinks below the solution, the chloroform below the extraction bottle 5 is transferred to the cuvette of the spectrophotometer 6 through a multi-way valve using a pump 4 or a syringe pump to measure the absorbance. The absorbance is proportional to the concentration, so the concentration of volatile phenols in the water can be calculated.

[0040] Previously, only the flow injection method was automated for measuring volatile phenols in water, but it was not a classic method, and most people still used manual operation methods. The integrated distiller 1 automates distillation, but still requires manual operations such as adding reagents, reactions, transfers, and extractions. The present invention automates the entire process of the classic 4-aminopyrine spectrophotometry, improves measurement precision, eliminates the need for manual operation, and avoids harm to humans from chemical reagents.

[0041] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A device for automatically measuring volatile phenols in water, characterized in that: The invention comprises an automatic integrated distiller, a plurality of collecting bottles, a multi-way valve, a pump, an extraction bottle and a spectrophotometer. The collecting bottle is used to collect the distillate of the integrated distiller, and a pipeline is led out from each collecting bottle. The central interface of the multi-way valve is connected to the pump. There are two multi-way valves, the interfaces of the first multi-way valve are respectively connected to the collecting bottles, and one interface is connected to chloroform. The interfaces of the second multi-way valve are respectively connected to a buffer, an oxidant, a color developer, an extraction bottle and a cuvette of the spectrophotometer. The pump is used to transport a reaction reagent to the collecting bottle or the extraction bottle, or to transport a distillate and chloroform to the extraction bottle. The spectrophotometer is used to measure the absorbance of the chloroform in the extraction bottle after the extraction is completed. The absorbance is proportional to the concentration, so that the concentration of volatile phenol in water can be calculated.

2. The device for automatically measuring volatile phenol in water according to claim 1, characterized in that: The plurality of collecting bottles are placed on an electronic balance respectively, and the value of the distillate weighed by the electronic balance is 250g; when the weight of the distillate in the collecting bottle reaches 250g, the electronic balance feeds back the information to the integrated distiller, and the controller of the integrated distiller stops the heating distillation of the distiller.

3. The device for automatically measuring volatile phenol in water according to claim 1, characterized in that: The multi-way valve has a central interface, and the central interface can be communicated with any one of the multiple interfaces of the valve.

4. The device for automatically measuring volatile phenol in water according to claim 1, characterized in that: The pump is a peristaltic pump, a syringe pump or a metering pump.

5. The device for automatically measuring volatile phenol in water according to claim 1, characterized in that: An electric extractor is arranged in the extraction bottle.

6. A method for automatically measuring volatile phenol in water, applied to the device for automatically measuring volatile phenol in water according to any one of claims 1 to 5, characterized in that: The following steps are involved: 1) Water sample distillation: the water samples are respectively placed in the distillation bottles of the integrated distillation apparatus, an appropriate amount of phosphoric acid is added, the distillation is heated and distilled, and the distillate is collected in the collection bottle; when the electronic balance measures that the weight of the solution in the collection bottle reaches 250g, the heating of the distillation apparatus is automatically stopped; a pipeline is led out of the collection bottle and connected to one port of the multi-way valve; 2) Add reagents for reaction: the pump starts to work, and the pump sequentially adds a buffer, an oxidant and a developer to each collection bottle through the multi-way valve, and reacts for 10 minutes to generate an orange-red antipyrine dye; 3) Transferring samples: After the reaction in step 2) is completed, the pump automatically transfers the reacted solution in the collection bottle to the extraction bottle through the multi-way valve; 4) Extraction by adding chloroform: Use a pump to accurately add 10 ml of chloroform to the extraction bottle, start the extractor, extract the solution in the extraction bottle, and then let it stand to allow the chloroform and water to separate; 5) Measurement: Since chloroform has a greater specific gravity than water and sinks below the solution, the pump transfers the chloroform below the extraction bottle to the cuvette of the spectrophotometer to measure the absorbance. The absorbance is proportional to the concentration, so the concentration of volatile phenols in the water can be calculated.

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