CN109358040A - A kind of measuring method of Phenol for Waste Water content and the measurement device used - Google Patents

A kind of measuring method of Phenol for Waste Water content and the measurement device used Download PDF

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Publication number
CN109358040A
CN109358040A CN201810424608.5A CN201810424608A CN109358040A CN 109358040 A CN109358040 A CN 109358040A CN 201810424608 A CN201810424608 A CN 201810424608A CN 109358040 A CN109358040 A CN 109358040A
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China
Prior art keywords
waste water
automatic liquid
measured
liquid feeder
water
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CN201810424608.5A
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Chinese (zh)
Inventor
杜松
王吉坤
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Pingxiang Coal Science Environmental Protection Technology Co Ltd
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Pingxiang Coal Science Environmental Protection Technology Co Ltd
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Priority to CN201810424608.5A priority Critical patent/CN109358040A/en
Publication of CN109358040A publication Critical patent/CN109358040A/en
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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

Abstract

A kind of measuring method of Phenol for Waste Water content and the device used, solve that low determination efficiency, security risk and accuracy are poor, and method includes: that 1. waste water and distilled water to be measured are quantitatively sent into drop reaction pipe;It is reacted 2. control automatic liquid feeder instills reaction solution with waste water to be measured;3. opening light source;4. receiving waste water water sample light beam according to color sensor, by controller automatic liquid feeder, hypo solution is added, and convert optical signals to electric signal in due course;5. controller receives electric signal, controls and hypo solution is added into drop reaction pipe;6. calculating the phenol content of water sample to be measured.The device are as follows: one group of automatic liquid feeder, waste water quantitative water supply to be measured part and distilled water quantitative water supply part with drop reaction tube inlet pipeline connection, while being connect respectively with controller circuitry, and controller is also connected with light source and display output unit control.Beneficial effect is: high degree of automation eliminates safe hidden trouble, as a result accurately.

Description

A kind of measuring method of Phenol for Waste Water content and the measurement device used
Technical field
The present invention relates to a kind of water analyzing detecting method and the equipment used, especially a kind of measurement of Phenol for Waste Water content Method and the measurement device used.
Background technique
In the prior art, the waste water usually by concentration containing phenol higher than 1000mg/L is known as high-concentration phenolic wastewater.Phenol will be contained Waste water of the concentration less than 1000mg/L is known as low concentration phenol wastewater.The chemical company in China includes petrochemical plant, coal gasification Factory, coking of coal factory, plastic molding and processing plant, pharmaceutical factory, paper mill etc. can generate a large amount of high-concentration phenolic wastewater.But because production purpose, The difference such as process flow causes Phenol for Waste Water type and content to have very big difference.
Phenolic substances is a kind of prototype matter poisonous substance, and to all toxic effect of various bions, and phenolic substances is to water Body water source, aquatile, crops can also produce serious influence, be Environmental Protection Agency (EPA) list 129 in priority acccess control One of pollutant, in China, phenol wastewater is also listed in one of the harmful waste water of emphasis solution, China in water pollution control Environmental regulation provides that the volatile phenol first discharge standard of trade effluent is 0.5mg/L;The volatile phenol content of Drinking Water must be small In 0.002mg/L.
At present in the determination method of Phenol for Waste Water content, National Standard Method (HJ503-2009) point is can be used in volatile phenol Analysis, and the measurement of difficult volatile phenol and total phenol content can only be using the method for titration.Titration method has the disadvantage that
1. operating personnel's large labor intensity, operating efficiency are low.
2. being that can not carry out in closed glass container with titration process, the poisonous and harmful chemical reagent of volatilization can be to reality It tests the healthy and safe of personnel and causes certain threat.
3. the color change situation of color indicator can only be felt to judge by operator to color, but every Individual has nothing in common with each other to the vision of color, so will cause when measuring same wastewater sample, measurement result has biggish Deviation.
4. testing procedure is cumbersome, the detection scale of automation, mass cannot achieve.
Summary of the invention
To overcome in the prior art, there is the above deficiency in the titration method that the measurement of difficult volatile phenol and total phenol content uses, The measurement device that the present invention discloses a kind of measuring method of Phenol for Waste Water content and uses.
The scheme that the present invention realizes that the goal of the invention of measuring method uses is: this method is realized by following steps:
Step 1., by the distilled water of the waste water to be measured of wastewater trough and distillation sink, is quantitatively sent into drop reaction pipe in the ratio of setting It is interior;
Step 2. controls automatic liquid feeder, sulfuric acid automatic liquid feeder, bromine standard liquid automatic liquid feeder, potassium iodide automatic liquid-feeding Timing instills sulfuric acid, bromine standard liquid and potassium iodide into drop reaction pipe to device respectively, and sulfuric acid, bromine standard liquid and potassium iodide are anti-in titration It is reacted in should managing with the water-reducible waste water to be measured of distillation;
Step 3. after reaction, opens light source;
Step 4. color sensor is received by waste water water sample light beam to be measured, by controller automatic liquid feeder, to drop Determine that hypo solution is added in reaction tube, and converts optical signals to electric signal in due course;
Step 5. controller receives electric signal, and is compared with the preset value of electric signal, if electric signal reaches setting value, controls Automatic liquid feeder processed stops that hypo solution is added into drop reaction pipe;
Step 6. calculates the phenol content of water sample to be measured according to the additive amount of automatic liquid feeder;
Step 7. controller exports the phenol content information of waste water to be measured by input-output unit.
The scheme that the present invention realizes that the goal of the invention of measurement device uses is:
The device includes: one group of automatic liquid feeder, drop reaction pipe, light source, controller, display output unit, waste water to be measured Quantitative water supply part and distilled water quantitative water supply part;
One group of automatic liquid feeder, waste water quantitative water supply to be measured part and the distilled water quantitative water supply part respectively with titration The connection of reaction tube entrance pipe, while being connect with controller circuitry, controller is also connected with light source and display output unit control;
The automatic liquid feeder include: rack, quantity tube, quantity tube piston rod, piston rod control slide plate, control motor, Lead screw, travelling nut and quantity tube efferent duct;
The quantity tube is fixed on the rack, and quantity tube piston rod is connect with piston rod control slide plate, and piston rod controls slide plate With rack constitute can opposite sliding be flexibly connected, be fixedly connected with travelling nut on piston rod control slide plate, travelling nut with Threads of lead screw connection, lead screw one end are rotatablely installed on the rack, and the other end is connect with control motor, and control motor is mounted on rack On, quantity tube efferent duct is connected to quantity tube one end.
The beneficial effects of the present invention are:
1. now can be realized automatically through the invention by the mode of operation that solution, stirring, color judgement is originally manually added dropwise, drop The low operation intensity of operating personnel.
2. titration process carries out in closed glass container, poisonous and harmful chemical reagent is avoided to experimenter's body Injury.
3. avoiding difference of the experimenter because of colour vision, analysis precision is improved.
4. automatic sampling apparatus of the invention is, it can be achieved that waste water phenol content is full-automatic, mass detection work is (disposable It can carry out 16 sample detections).
5. the configuration of the present invention is simple, small in size, performance is stablized, and laboratory and scene is suitble to do industry.
6. color sensor is contactless, lossless with titer reagent in the detection process, without current potential in potentiometric titration Maintenance, guarantee and the loss supplement of electrode.
7. color sensor changes suitable for various colors, signal stabilization, the titration of all colours indicator method can be applied to The judgement of terminal.
Detailed description of the invention
Present invention is described with reference to the accompanying drawing.
Attached drawing 1 is the assay device structures schematic diagram that the present invention uses.
Attached drawing 2 is automatic liquid feeder structural schematic diagram of the present invention.
In attached drawing: 1 automatic liquid feeder, 1.1 racks, 1.2 quantity tubes, 1.3 quantity tube piston rods, the control of 1.4 piston rods Slide plate, 1.5 control motors, 1.6 lead screws, 1.7 travelling nuts, 1.8 quantity tube efferent ducts,
2 drop reaction pipes, 3 light sources, 4 controllers, 5 display output units, 6 waste water quantitative water supply to be measured parts, 7 distilled water are quantitative Water supply part.
Specific embodiment
A kind of measuring method of Phenol for Waste Water content, this method are realized by following steps:
Step 1., by the distilled water of the waste water to be measured of wastewater trough and distillation sink, is quantitatively sent into drop reaction pipe in the ratio of setting It is interior;
Step 2. controls automatic liquid feeder, sulfuric acid automatic liquid feeder, bromine standard liquid automatic liquid feeder, potassium iodide automatic liquid-feeding Timing instills sulfuric acid, bromine standard liquid and potassium iodide into drop reaction pipe to device respectively, and sulfuric acid, bromine standard liquid and potassium iodide are anti-in titration It is reacted in should managing with the water-reducible waste water to be measured of distillation;
Step 3. after reaction, opens light source;
Step 4. color sensor is received by waste water water sample light beam to be measured, by controller automatic liquid feeder, to drop Determine that hypo solution is added in reaction tube, and converts optical signals to electric signal in due course;
Step 5. controller receives electric signal, and is compared with the preset value of electric signal, if electric signal reaches setting value, controls Automatic liquid feeder processed stops that hypo solution is added into drop reaction pipe;
Step 6. calculates the phenol content of water sample to be measured according to the additive amount of automatic liquid feeder;
Step 7. controller exports the phenol content information of waste water to be measured by input-output unit.
A kind of measurement device that the measuring method of Phenol for Waste Water content uses,
The device includes: one group of automatic liquid feeder 1, drop reaction pipe 2, light source 3, controller 4, display output unit 5, to be measured Waste water quantitative water supply part 6 and distilled water quantitative water supply part 7;
One group of automatic liquid feeder 1, waste water quantitative water supply to be measured part 6 and the distilled water quantitative water supply part 7 respectively with 2 entrance pipe of drop reaction pipe connection, while with 4 circuit connection of controller, controller 4 also with light source 3 and display output unit 5 Control connection;
The automatic liquid feeder 1 includes: rack 1.1, quantity tube 1.2, quantity tube piston rod 1.3, piston rod control slide plate 1.4, motor 1.5, lead screw 1.6, travelling nut 1.7 and quantity tube efferent duct 1.8 are controlled;
The quantity tube 1.2 is fixed in rack 1.1, and quantity tube piston rod 1.3 is connect with piston rod control slide plate 1.4, living Stopper rod controls slide plate 1.4 and is flexibly connected with what the composition of rack 1.1 opposite can be slided, is fixedly connected on piston rod control slide plate 1.4 There is travelling nut 1.7, travelling nut 1.7 is threadedly coupled with lead screw 1.6, and 1.6 one end of lead screw is rotatably installed in rack 1.1, separately One end is connect with control motor 1.5, and control motor 1.5 is mounted in rack 1.1, quantity tube efferent duct 1.8 and quantity tube 1.2 1 End connection.
In use, waste water quantitative water supply to be measured part 6 and distilled water quantitative water supply part 7 enter with drop reaction pipe 2 respectively Mouth pipeline connection, quantitatively injects waste water and distilled water to be measured to drop reaction pipe 2.
Automatic liquid feeder 1 quantitatively instills reaction solution to drop reaction pipe 2, and reaction solution of the present invention has: sulfuric acid, bromine Standard liquid and potassium iodide, sulfuric acid, bromine standard liquid and potassium iodide, each reaction solution respectively correspond an automatic liquid feeder 1.
Automatic liquid feeder 1, control motor 1.5 are driven lead screw 1.6 to drive travelling nut 1.7 mobile, travelling nut 1.7 Piston rod control slide plate 1.4 is driven to slide, piston rod control slide plate 1.4 drives quantity tube piston rod 1.3 that will send out in quantity tube 1.2 Thermal response liquid is released quantity tube 1.2 and is entered to drop reaction pipe 2.
Using the present invention according to the requirement of the capacity method titration total phenol of bromination, total phenol content in waste water is detected, The concentration value of measurement device input 0.1mol/L sodium thiosulfate standard solution through the invention, inputs the quality to solubilizer Value, successively are as follows: (1+1) sulfuric acid 10ml, 0.1mol/L bromine standard liquid 25ml, 10%KI solution 10ml, 10g/L starch solution 1ml.So The blank assay of distilled water is carried out afterwards, and addition (1+1) sulfuric acid 10ml, 0.1mol/L bromine standard liquid of successively fixing time 25ml, 10%KI is molten Liquid 10ml, 10g/L starch solution 1ml and buret;0.1mol/L sodium thiosulfate standard solution is then full of quantity tube, and After excluding the bubble in quantity tube.It presses start key to start to detect, after to be detected, display consumption sodium thiosulfate standard is molten The blank value V of liquid0, blank value is inputted instrument, waste water total phenol content is then treated and is detected: successively fix time addition (1+ 1) sulfuric acid 10ml, 0.1mol/L bromine standard liquid 25ml, 10%KI solution 10ml, 10g/L starch solution 1ml, will in buret 0.1mol/L sodium thiosulfate standard solution is full of quantity tube, and excludes the bubble in buret.Start to detect, it is to be detected to finish Afterwards, the blank value V of display consumption sodium thiosulfate standard solution1.The result of waste water total phenol content is most shown on display screen finally W or printer output.
Wherein, the calculation formula of waste water total phenol content: WTotal phenol(mg/L)=0.1*(V1-V0)*15.68*1000*B/V
In formula:
V0: blank assay consumes the volume of sodium thiosulfate standard solution, ml
V1: sample consumes the volume of sodium thiosulfate standard solution, ml
V: sample volume, ml
B: wastewater dilution multiple
0.1: Concentration of Sodium Thiohsulfate Standard Solution, mol/L
15.68: with the comparable phenol content of 1mol sodium thiosulfate, mg
1000: unit conversion has g/L to be scaled mg/L
Volatile phenol content difficult in waste water is examined in the requirement for being titrated difficult volatile phenol according to direct bromination using the present invention It surveys, the concentration value of measurement device input 0.1mol/L sodium thiosulfate standard solution through the invention is inputted to solubilizer Mass value, successively are as follows: (1+1) sulfuric acid 10ml, 0.1mol/L bromine standard liquid 25ml, 10%KI solution 10ml, 10g/L starch solution 1ml.Then the blank assay of distilled water is carried out, successively fix time addition (1+1) sulfuric acid 10ml, 0.1mol/L bromine standard liquid 25ml, 10%KI solution 10ml, 10g/L starch solution 1ml is in buret, by 0.1mol/L sodium thiosulfate standard solution full of quantitative Pipe, and exclude the bubble in buret.Start key is pressed to start to detect, after to be detected, display consumption sodium thiosulfate mark The blank value V of quasi- solution0, blank value is inputted into instrument, waste water difficulty volatile phenol content is then treated and is detected: successively being fixed time (1+1) sulfuric acid 10ml, 0.1mol/L bromine standard liquid 25ml, 10%KI solution 10ml, 10g/L starch solution 1ml is added in buret, 0.1mol/L sodium thiosulfate standard solution is full of quantity tube, and excludes the bubble in buret.Start key is pressed to start to examine It surveys, after to be detected, the blank value V of display consumption sodium thiosulfate standard solution2.Waste water hardly possible is most shown on display screen finally The result W of volatile phenol content or printer output.
Wherein, the calculation formula of waste water difficulty volatile phenol content:
WDifficult volatile phenol(mg/L)=0.1*(V1-V0)*15.68*1000*B/V
In formula:
V0: blank assay consumes the volume of sodium thiosulfate standard solution, ml
V2: sample consumes the volume of sodium thiosulfate standard solution, ml
V: sample volume, ml
B: wastewater dilution multiple
0.1: Concentration of Sodium Thiohsulfate Standard Solution, mol/L
15.68: with the comparable phenol content of 1mol sodium thiosulfate, mg
1000: unit conversion has g/L to be scaled mg/L.

Claims (2)

1. a kind of measuring method of Phenol for Waste Water content, it is characterised in that this method is realized by following steps:
Step 1., by the distilled water of the waste water to be measured of wastewater trough and distillation sink, is quantitatively sent into drop reaction pipe in the ratio of setting It is interior;
Step 2. controls automatic liquid feeder, sulfuric acid automatic liquid feeder, bromine standard liquid automatic liquid feeder, potassium iodide automatic liquid-feeding Timing instills sulfuric acid, bromine standard liquid and potassium iodide into drop reaction pipe to device respectively, and sulfuric acid, bromine standard liquid and potassium iodide are anti-in titration It is reacted in should managing with the water-reducible waste water to be measured of distillation;
Step 3. after reaction, opens light source;
Step 4. color sensor is received by waste water water sample light beam to be measured, by controller automatic liquid feeder, to drop Determine that hypo solution is added in reaction tube, and converts optical signals to electric signal in due course;
Step 5. controller receives electric signal, and is compared with the preset value of electric signal, if electric signal reaches setting value, controls Automatic liquid feeder processed stops that hypo solution is added into drop reaction pipe;
Step 6. calculates the phenol content of water sample to be measured according to the additive amount of automatic liquid feeder;
Step 7. controller exports the phenol content information of waste water to be measured by input-output unit.
2. the measurement device that a kind of measuring method of Phenol for Waste Water content according to claim 1 uses, it is characterised in that:
The device includes: one group of automatic liquid feeder (1), drop reaction pipe (2), light source (3), controller (4), display output list First (5), waste water quantitative water supply to be measured part (6) and distilled water quantitative water supply part (7);
One group of automatic liquid feeder (1), waste water quantitative water supply to be measured part (6) and the distilled water quantitative water supply part (7) Be connected to respectively with drop reaction pipe (2) entrance pipe, at the same with controller (4) circuit connection, controller (4) also with light source (3) It controls and connects with display output unit (5);
The automatic liquid feeder (1) includes: rack (1.1), quantity tube (1.2), quantity tube piston rod (1.3), piston rod Control slide plate (1.4), control motor (1.5), lead screw (1.6), travelling nut (1.7) and quantity tube efferent duct (1.8);
The quantity tube (1.2) is fixed on rack (1.1), quantity tube piston rod (1.3) and piston rod control slide plate (1.4) Connection, piston rod control slide plate (1.4) and are flexibly connected with what rack (1.1) composition opposite can be slided, and piston rod controls slide plate (1.4) it is fixedly connected on travelling nut (1.7), travelling nut (1.7) is threadedly coupled with lead screw (1.6), lead screw (1.6) one end It is rotatably installed on rack (1.1), the other end is connect with control motor (1.5), and control motor (1.5) is mounted on rack (1.1) On, quantity tube efferent duct (1.8) is connected to quantity tube (1.2) one end.
CN201810424608.5A 2018-05-07 2018-05-07 A kind of measuring method of Phenol for Waste Water content and the measurement device used Pending CN109358040A (en)

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Publication number Priority date Publication date Assignee Title
CN111307795A (en) * 2020-04-13 2020-06-19 马学文 Water quality detection device

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Publication number Priority date Publication date Assignee Title
CN111307795A (en) * 2020-04-13 2020-06-19 马学文 Water quality detection device

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