CN213023009U - Water quality permanganate index on-line analyzer - Google Patents
Water quality permanganate index on-line analyzer Download PDFInfo
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- CN213023009U CN213023009U CN202021501792.8U CN202021501792U CN213023009U CN 213023009 U CN213023009 U CN 213023009U CN 202021501792 U CN202021501792 U CN 202021501792U CN 213023009 U CN213023009 U CN 213023009U
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000006243 chemical reaction Methods 0.000 claims abstract description 62
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 238000004448 titration Methods 0.000 claims abstract description 30
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 62
- 239000010453 quartz Substances 0.000 claims description 48
- 230000002572 peristaltic effect Effects 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000002347 injection Methods 0.000 claims description 14
- 239000007924 injection Substances 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 8
- 229920001971 elastomer Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical class [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 229910000371 mercury(I) sulfate Inorganic materials 0.000 claims description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 2
- OQVYMXCRDHDTTH-UHFFFAOYSA-N 4-(diethoxyphosphorylmethyl)-2-[4-(diethoxyphosphorylmethyl)pyridin-2-yl]pyridine Chemical compound CCOP(=O)(OCC)CC1=CC=NC(C=2N=CC=C(CP(=O)(OCC)OCC)C=2)=C1 OQVYMXCRDHDTTH-UHFFFAOYSA-N 0.000 claims 1
- 239000004809 Teflon Substances 0.000 claims 1
- 229920006362 Teflon® Polymers 0.000 claims 1
- 238000005070 sampling Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 13
- 238000004458 analytical method Methods 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 4
- 230000007774 longterm Effects 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 31
- 238000003825 pressing Methods 0.000 description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 16
- 239000004033 plastic Substances 0.000 description 11
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 11
- 229940039790 sodium oxalate Drugs 0.000 description 11
- -1 polytetrafluoroethylene Polymers 0.000 description 6
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000012496 blank sample Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
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- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
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Abstract
The utility model provides a quality of water permanganate index on-line analyzer, the analyzer includes: potassium permanganate reagent measures subassembly, reagent measurement subassembly, advances kind subassembly, titration reaction subassembly, flowing back subassembly and singlechip, potassium permanganate reagent measurement subassembly and detect reagent measurement subassembly pass through liquid delivery channel and are connected with titration reaction subassembly, advance kind subassembly and pass through liquid delivery channel and are connected with titration reaction subassembly, the flowing back subassembly passes through liquid delivery channel and is connected with titration reaction subassembly, the singlechip is arranged in being connected with electronic components in each subassembly. The utility model provides a structure can realize automatic, quick, the accurate analysis to the permanganate index content in the water, has advantages such as measurement accuracy, stability are good, provide reliable guarantee for the long-term accurate monitoring of quality of water permanganate index.
Description
Technical Field
The utility model belongs to the technical field of quality of water on-line monitoring, concretely relates to quality of water permanganate index on-line analyzer.
Background
Chemical Oxygen Demand (COD) refers to the amount of strong oxidant consumed to oxidize reducing substances in 1L of a water sample under certain conditions, expressed as the amount of oxygen consumed to oxidize these substances (mg/L). The COD directly reflects the pollution degree of the water body by the reducing substances. In the prior art, the permanganate index is usually measured by taking a water sample on site and sending the water sample to a laboratory, then pretreating and digesting the water sample, and manually titrating the water sample, so that the efficiency is low, the operation is complex, and the consistency is poor. The water quality permanganate index on-line analyzer can overcome the defects and is widely applied to various levels of water quality monitoring stations at present.
For a water quality permanganate index on-line analyzer, accurate judgment of a titration end point is the key of the analyzer, and the prior analyzer has the defects that: the automation degree is not high, the precision is poor, and particularly for water samples with large turbidity and chromaticity, misjudgment is easily caused when the titration end point is judged, so that the analysis result is inaccurate. In addition, most of the existing instruments adopt metering modes such as a peristaltic pump or an injection pump and the like during reagent metering, and the result is inaccurate during long-term metering, so that the measurement error is large.
SUMMERY OF THE UTILITY MODEL
In order to solve the problem, the utility model discloses a quality of water permanganate index on-line analyzer can avoid water sample colourity and turbidity to COD testing result's interference, reagent measurement reliable and stable, provides reliable guarantee for the long-term accurate monitoring of quality of water permanganate index.
In order to achieve the above object, the utility model provides a following technical scheme:
a water quality permanganate index on-line analyzer comprises: the device comprises a potassium permanganate reagent metering component, a detection reagent metering component, a sample introduction component, a titration reaction component, a liquid discharge component and a single chip microcomputer, wherein the potassium permanganate reagent metering component and the detection reagent metering component are connected with the titration reaction component through a liquid conveying channel;
the potassium permanganate reagent metering assembly comprises an injection pump, a three-way joint and an electromagnetic pressure pipe valve which are sequentially connected, one side of the electromagnetic pressure pipe valve is connected with the potassium permanganate reagent and is connected to the injection pump through a liquid conveying channel, and the other side of the electromagnetic pressure pipe valve is connected to the titration reaction assembly through a liquid conveying channel;
the reagent metering assembly comprises two transparent metering tubes, the lower end of each transparent metering tube is connected with a corresponding electromagnetic tube pressing valve through a three-way joint, the upper end of each transparent metering tube is connected with a corresponding three-way electromagnetic air valve, each three-way electromagnetic air valve is connected with a first peristaltic pump, one side channel of each electromagnetic tube pressing valve is respectively connected into two reagent bottles through a pipeline, and the other side channel of each electromagnetic tube pressing valve is connected to a titration reaction tank through a liquid conveying channel;
the sample feeding assembly comprises a second peristaltic pump, two three-way joints and two electromagnetic pressure pipe valves, the two electromagnetic pressure pipe valves are positioned on two sides of the second peristaltic pump, the two three-way joints are respectively positioned between the two electromagnetic pressure pipe valves and the second peristaltic pump, and the sample feeding assembly is used for conveying a water sample and distilled water to the titration reaction tank through a liquid conveying channel;
the titration reaction component comprises a quartz reaction tank, a heating element arranged outside the quartz reaction tank, a temperature sensor for measuring the temperature of a solution in the quartz reaction tank, an indicating electrode extending into the tank and a reference electrode forming a loop with the indicating electrode;
the liquid discharge assembly comprises a third peristaltic pump, a three-way joint and an electromagnetic pipe pressing valve which are sequentially connected;
the single chip microcomputer is connected with all electronic elements in the analyzer.
Furthermore, the singlechip is connected with the injection pump, each peristaltic pump, each electromagnetic pipe pressing valve, the temperature sensor, each electrode, the motor and the heating element.
Furthermore, a pair of photoelectric switches are respectively arranged on two sides of the spherical cavity of each metering tube, each photoelectric switch outputs signals to a three-way electromagnetic air valve corresponding to the upper end of the quartz metering tube to control the opening and closing of the electromagnetic pipe pressing valve channel, and the singlechip is connected with each photoelectric switch.
Furthermore, a spherical cavity is arranged on the transparent metering tube and is positioned between the two photoelectric switches on the metering tube.
Furthermore, a quartz glass tube is sleeved outside the temperature sensor, and a heat-conducting medium is filled in the gap in the tube.
Furthermore, the reference electrode is connected to the reaction tank through a saturated potassium sulfate liquid storage tank, a rubber tube and a quartz glass tube.
Further, the indicating electrode is a platinum wire electrode, and the reference electrode is a mercury-mercurous sulfate electrode.
Further, the magnetic stirring system comprises a motor, a magnet and a polytetrafluoroethylene magneton, wherein the magnet is fixed on the direct current speed reduction motor, and the polytetrafluoroethylene magneton is placed in the reaction tank.
Furthermore, a heat-insulating layer is arranged outside the heating element, and a protective shell is arranged outside the heat-insulating layer.
Furthermore, the heating element is a flexible heating sheet and is wrapped on the outer surface of the quartz reaction tank.
Compared with the prior art, the utility model has the advantages of as follows and beneficial effect:
1. the utility model provides a permanganate index on-line analyzer will advance kind, reagent measurement, clear up and return step full automatization such as titrating, can realize automatic, quick and accurate analysis to COD content in the water sample.
2. The reagent metering volume can be adjusted by adjusting the inner diameter of the metering tube or the position of the photoelectric switch, the metering precision is high, and the stability is good.
3. The quartz metering tube is corrosion-resistant and oxidation-resistant, and the defects of large metering error, high maintenance cost and the like caused by aging and deformation of the pump tube in the metering mode of the peristaltic pump are overcome.
4. The rubber tube and the slender quartz glass tube are used for connecting the reference electrode, so that the problems that the service life of the electrode is greatly shortened when the reference electrode is directly inserted into reaction liquid and mercury vapor is volatilized can be avoided. The reference electrode is inserted into the saturated potassium sulfate liquid storage tank, and the reference electrode is equivalent to be used for measurement at room temperature, so that the service life can be prolonged.
Drawings
Figure 1 is the structure schematic diagram of the water quality permanganate index on-line analyzer provided by the utility model.
Fig. 2 is a connection block diagram of the electric elements of the water quality permanganate index on-line analyzer provided by the utility model.
Description of reference numerals:
P1-P3: first to third peristaltic pumps; b-precision syringe pump; C1-C6: first to sixth three-way plastic joints; D1-D6: first to sixth electromagnetic pinch valves; S1-S2: first to second quartz metering tubes; G1-G4: first to fourth photoelectric switches; r1: a potassium permanganate reagent bottle; r2 is a sulfuric acid reagent bottle; r3: a sodium oxalate reagent bottle; f1: a quartz reaction tank; f2: a temperature sensor; f3: an indicator electrode; f4: a reference electrode; f5: a liquid storage tank; f6: an elongated quartz glass tube; f7: a quartz glass sleeve; f8: a polytetrafluoroethylene magneton; f9: a magnet; f10: a DC deceleration electrode; f11: a heating plate; f12: a heat-insulating layer; f13: and (4) protecting the shell.
Detailed Description
The technical solutions provided by the present invention will be described in detail with reference to specific embodiments, and it should be understood that the following specific embodiments are only used for illustrating the present invention and are not used for limiting the scope of the present invention.
The utility model provides a quality of water permanganate index on-line analyzer, as shown in figure 1, figure 2, include: the device comprises a potassium permanganate reagent metering component, a detection reagent metering component, a sample introduction component, a titration reaction component, a liquid discharge component and a single chip microcomputer, wherein the potassium permanganate reagent metering component and the detection reagent metering component are connected with the titration reaction component through a liquid conveying channel, the sample introduction component is connected with the titration reaction component through the liquid conveying channel, and the sample introduction component is used for conveying a water sample and distilled water; the liquid discharge assembly is connected with the titration reaction assembly through a liquid conveying channel, and the single chip microcomputer is connected with the electronic components in each assembly and controls the electronic components to work. The single-chip microcomputer is not shown in the figure.
The potassium permanganate reagent metering assembly comprises an injection pump B, a first three-way plastic connector C1 and a first electromagnetic pressure pipe valve D1 which are sequentially connected, the injection pump B is used for injecting a potassium permanganate reagent, one end of the first three-way plastic connector C1 is connected with the injection pump B, the other two ends of the first three-way plastic connector C1 are communicated to the first electromagnetic pressure pipe valve D1, one side of the first electromagnetic pressure pipe valve D1 is used for conveying the potassium permanganate reagent R1 to a potassium permanganate reagent bottle R1, and the other side of the first electromagnetic pressure pipe valve D1 is connected to the titration reaction assembly through a liquid conveying channel.
The reagent metering assembly comprises a first quartz metering tube S1 and a second quartz metering tube S2, wherein the first quartz metering tube S1 and the second quartz metering tube S2 are both transparent metering tubes and are both provided with spherical cavities. The lower end of the first quartz measuring tube S1 is connected with a second electromagnetic pinch valve D2 through a second three-way plastic joint C2, the upper end of the first quartz measuring tube is connected with a first three-way electromagnetic air valve V1, the first three-way electromagnetic air valve V1 is connected with a first peristaltic pump P1, the upper side and the lower side of a spherical cavity of the first quartz measuring tube S1 are respectively provided with a first photoelectric switch G1 and a second photoelectric switch G2, and the two photoelectric switches output signals to the first three-way electromagnetic air valve V1 corresponding to the upper end of the first quartz measuring tube S1 to control the opening and closing of a channel of the electromagnetic pinch valve. The second electromagnetic pipe-pressing valve D2 has one side channel connected via pipe to the sulfuric acid reagent bottle R2 and the other side connected via pipe to the titration reaction tank. Similarly, the lower end of the second quartz measuring tube S2 is connected with a third electromagnetic pinch valve D3 through a third three-way plastic joint C3, the upper end is connected with a second three-way electromagnetic air valve V2, the second three-way electromagnetic air valve V2 is connected with a first peristaltic pump P1, the upper side and the lower side of the spherical cavity of the second quartz measuring tube S2 are respectively provided with a third photoelectric switch G3 and a fourth photoelectric switch G4, and the two photoelectric switches output signals to the second three-way electromagnetic air valve V2 corresponding to the upper end of the second quartz measuring tube S2 to control the opening and closing of the channel of the electromagnetic pinch valve. The third electromagnetic pipe-pressure valve D3 has one side channel connected to sodium oxalate reagent bottle R3 via pipe and the other side connected to the titration reaction tank via pipe.
The sample feeding assembly comprises a second peristaltic pump P2, a fourth three-way plastic joint C4, a fifth three-way plastic joint C5, a fourth electromagnetic pressure pipe valve D4 and a fifth electromagnetic pressure pipe valve D5, the two electromagnetic pressure pipe valves are respectively positioned on two sides of the second peristaltic pump, and the two three-way plastic joints are respectively positioned between the two electromagnetic pressure pipe valves and the second peristaltic pump and are used for conveying a water sample and distilled water into the titration reaction tank through a liquid conveying channel.
The titration reaction component comprises a quartz reaction cell F1, a heating element, a temperature sensor F2, an indicating electrode F3, a reference electrode F4, a magnetic stirring system, a heat-insulating layer F12 and a protective shell F13, wherein a heating plate F11, the temperature sensor F2, the indicating electrode F3 and the reference electrode are electrically connected with the single chip microcomputer respectively. The quartz reaction tank F1 comprises a liquid outlet and an overflow port, wherein the liquid outlet is positioned at the bottom of the quartz reaction tank, and the overflow port is positioned at the upper end of the quartz reaction tank. The heating element is a flexible heating sheet F11 and is wrapped on the outer surface of the quartz reaction cell F1. The heating element is also provided with a heat preservation layer F12 for heat preservation, and a protective shell F13 is arranged outside the heat preservation layer F12 for protecting the whole structure. The temperature sensor F2 is a thermistor, a quartz glass sleeve F7 is sleeved on the outer surface of the thermistor, and heat-conducting silica gel is filled in the gap in the quartz glass sleeve. The sleeve plays a role in protection. The temperature sensor F2, a sleeve thereof and an indicating electrode F3 extend into the reaction solution in the quartz reaction cell F1, and the indicating electrode F3 is a platinum wire electrode. The reference electrode F4 is a mercury-mercurous sulfate electrode and is connected to the reaction cell through a saturated potassium sulfate liquid storage tank F5, a rubber tube and a slender quartz glass tube F6, and the indicating electrode F3 and the reference electrode F4 form a loop. Because the temperature of the reaction liquid is high, the rubber tube and the slender quartz glass tube are used for connecting the reference electrode, so that the problem that the service life of the electrode is greatly shortened when the reference electrode is directly inserted into the reaction liquid and mercury vapor possibly volatilizes can be avoided. In order to prevent the situation that the saturated potassium sulfate solution is lacked to acquire the sudden change voltage possibly due to evaporation or permeation when the rubber tube and the elongated quartz glass tube are used for a long time, the reference electrode is inserted into the saturated potassium sulfate liquid storage tank through connection of the elongated quartz glass tube and the rubber tube, the reference electrode is equivalent to measurement at room temperature, and the service life can be prolonged. The magnetic stirring system comprises a polytetrafluoroethylene magneton F8, a magnet F9 and a direct-current deceleration electrode F10, wherein the magnet F9 is fixed on a direct-current deceleration motor F10, and the polytetrafluoroethylene magneton F8 is placed in a reaction tank F1.
The liquid discharge assembly comprises a third peristaltic pump P3, a sixth three-way plastic joint C6 and a sixth electromagnetic pipe pressing valve D6, and the third peristaltic pump P3 and the sixth electromagnetic pipe pressing valve D6 are connected through a sixth three-way plastic joint C6. The waste liquid and the rinse liquid are divided by the electromagnetic pinch valve, and the system only recovers the waste liquid, thereby achieving the purpose of reducing the volume of the waste liquid.
The electronic elements in each component, namely the injection pump, each peristaltic pump, each electromagnetic pipe pressing valve, each photoelectric switch, the temperature sensor, each electrode, the motor and the heating element are all connected with the single chip microcomputer.
Example 1: volume metering of sulfuric acid and sodium oxalate
According to the calculation formula of COD, the addition amount of the reagent volume has a large influence on the analysis result in the measurement of the COD content, so that accurate metering is required. For the measurement of sulfuric acid, we designed the quartz measuring tube S1 so that the inner diameter R1 of the spherical chamber portion was 20mm, the inner diameter R2 of the cylindrical portion was 4mm, and the wall thickness was 1.5mm, so that the volume of the spherical chamber portion was 1.5mm
Volume of cylinder part
Wherein h is the distance between two photoelectric switch induction parts, and h theoretical value is:
the distance refers to the distance of the photoelectric switch fixed on the cylinder part, the distance does not contain a spherical part, and the distance can be properly adjusted according to the actual metering condition.
During metering, a channel a of the electromagnetic pressure pipe valve D2 is opened, a channel b is closed, the peristaltic pump P1 rotates clockwise, sulfuric acid solution R2 is pumped to a photoelectric switch G1 at the uppermost end of the quartz metering pipe S1 through the reagent metering assembly, the peristaltic pump P1 stops rotating, then the channel b of the electromagnetic pressure pipe valve D2 is opened, the channel a is closed, the peristaltic pump P1 rotates anticlockwise, the sulfuric acid solution is discharged to a photoelectric switch G2 at the lower end of the quartz metering pipe S1, the peristaltic pump P1 stops rotating, and the volume of the extracted sulfuric acid is 5 mL;
for the measurement of sodium oxalate, we designed the quartz measuring tube S2 so that the inner diameter R1 of the spherical chamber portion was 26mm, the inner diameter R2 of the cylindrical portion was 4mm, and the wall thickness was 1.5mm, so that the volume of the spherical chamber portion was 1.5mm
Volume of cylinder part
Wherein h is the distance between two photoelectric switch induction parts, and h theoretical value is:
the distance refers to the distance of the cylindrical part, the spherical part is not contained, and the distance can be adjusted according to the actual metering requirement.
During metering, a channel a of the electromagnetic pressure pipe valve D3 is opened, a channel b is closed, the peristaltic pump P1 rotates clockwise, sodium oxalate solution R3 is pumped to a photoelectric switch G3 at the uppermost end of the quartz metering pipe S2 through the reagent metering assembly, the peristaltic pump P1 stops rotating, then the electromagnetic pressure pipe valve D3 channel b is opened, the channel a is closed, the peristaltic pump P1 rotates anticlockwise, the sodium oxalate solution R3 is discharged to the photoelectric switch G4 at the lower end of the quartz metering pipe S2, the peristaltic pump P1 stops rotating, and the volume of the extracted sodium oxalate solution is 10.00 mL;
example 2: low COD concentration water sample test (0-8mg/L)
As shown in FIG. 1, when the apparatus is in operation, the saturated potassium sulfate solution is filled in the liquid storage tank F5, and the analysis is carried out according to the following steps:
step 1, pipeline rinsing
A fourth electromagnetic pressure pipe valve D4 and a fifth electromagnetic pressure pipe valve D5 are opened in channel a and closed in channel b, a second peristaltic pump P2 pumps 60mL of water sample to a quartz reaction tank F1, a motor F10 drives a polytetrafluoroethylene magneton F8 to stir for 30s, then a sixth electromagnetic pressure pipe valve D6 is opened in channel b and closed in channel a, and a third peristaltic pump P3 empties a cleaning water sample in the quartz reaction tank F1;
The fourth electromagnetic pipe pressing valve D4 and the fifth electromagnetic pipe pressing valve D5 are opened in channel b and closed in channel a, and the second peristaltic pump P2 pumps 100.0mL of water sample to the quartz reaction tank F1;
step 3, potassium permanganate metering
The channel a of the first electromagnetic pressure pipe valve D1 is opened, the channel B is closed, the injection pump B starts to work to extract a solution (25mmol/L, the same below) in a potassium permanganate reagent bottle R1 of 10.00mL, the channel B of the first electromagnetic pressure pipe valve D1 is opened, the channel a is closed, and the potassium permanganate solution is quantitatively added into a quartz reaction tank F1;
step 4, digestion
The second electromagnetic pipe pressing valve D2 is opened in the channel a and closed in the channel b, the first peristaltic pump P1 rotates clockwise, 5.00mL of sulfuric acid solution (1+3, V/V, the same applies to the metering method in the embodiment 1) is quantitatively added into the quartz reaction cell F1 through the reagent metering assembly, then the flexible heating plate F11 starts to work, the liquid in the quartz reaction cell F1 is continuously heated to 100 ℃ under the stirring of the motor F10, and digestion timing is started, and the digestion time is 30 min;
step 5, metering sodium oxalate
The third electromagnetic pipe-pressing valve D3 is opened at channel a and closed at channel b, the first peristaltic pump P1 rotates clockwise, 10.00mL of sodium oxalate solution (10mmol/L, the same as the metering method in example 1 is adopted below) is quantitatively added into the quartz reaction tank F1 through the reagent metering component, and the color of the solution in the quartz reaction tank F1 changes from purple red to colorless;
step 6, back titration
The channel a of the first electromagnetic pressure pipe valve D1 is opened, the channel B is closed, the injection pump B extracts 10.00mL of potassium permanganate solution, then the channel B of the first electromagnetic pressure pipe valve D1 is opened, the channel a is closed, the injection pump B adds the potassium permanganate solution into the quartz reaction tank F1 along the pipeline at the speed of about 2 drops per second until a loop formed by the indicating electrode F3 and the reference electrode F4 collects a sudden change voltage, the voltage signal is fed back to the injection pump B to stop rotating, the amount of potassium permanganate added into the reaction tank is calculated according to the number of turns of the stepping motor in the injection pump B, and the COD content in the water sample can be calculated by combining the following formula:
in the formula, V1Consuming the volume of the potassium permanganate solution, mL, for step 6;
V2in order to calibrate the volume, mL, of the potassium permanganate solution consumed by the blank sample, the step is manually completed in a laboratory, and the calibration is carried out once when the reagent is replaced each time;
c is the concentration of sodium oxalate standard solution, mol/L
Step 7, waste liquid emptying
After the COD value is measured, a channel a of a sixth electromagnetic pipe pressing valve D6 is opened, a channel b is closed, and a third peristaltic pump P3 empties reaction liquid from a quartz reaction tank F1;
step 8, emptying pipeline
The fourth electromagnetic pipe pressing valve D4 and the fifth electromagnetic pipe pressing valve D5 are opened in channel a and closed in channel b, and the second peristaltic pump P2 rotates clockwise to drain the water sample in the pipeline.
Example 3: high COD concentration water sample test (8-24mg/L)
For the water sample test with high COD concentration, the same as the example 2, the measurement steps are the same except the step 2, and the water sample needs to be diluted in the step 2, which is specifically as follows:
the fourth electromagnetic pipe pressing valve D4 and the fifth electromagnetic pipe pressing valve D5 are opened in the channel b and closed in the channel a, the peristaltic pump P2 pumps 33.0mL of water sample to the quartz reaction tank F1, then the electromagnetic pipe pressing valves D4 and D5 are opened in the channel a and closed in the channel b, and the peristaltic pump P2 pumps 67.0mL of distilled water to the quartz reaction tank F1. In the step, a water sample and distilled water are added according to a certain dilution ratio, so that the total volume of the water sample and the distilled water is ensured to be 100.0 mL.
The COD content was calculated using the following formula:
V0to calibrate the volume of potassium permanganate solution consumed by the blank, mL, this step was done manually in the laboratory, once for each reagent change.
V1Consuming the volume of the potassium permanganate solution, mL, for step 6;
V2in order to calibrate the volume, mL, of the potassium permanganate solution consumed by the blank sample, the step is manually completed in a laboratory, and the calibration is carried out once when the reagent is replaced each time;
V3volume of water sample added for dilution step, mL
C is the concentration of sodium oxalate standard solution, mol/L
f is the proportion of distilled water in 100mL of liquid in the dilution step.
The technical means disclosed by the scheme of the present invention is not limited to the technical means disclosed by the above embodiments, but also includes the technical scheme formed by the arbitrary combination of the above technical features. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications are also considered as the protection scope of the present invention.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021501792.8U CN213023009U (en) | 2020-07-27 | 2020-07-27 | Water quality permanganate index on-line analyzer |
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