CN107957442A - Permanganate index autotitrating method - Google Patents
Permanganate index autotitrating method Download PDFInfo
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- CN107957442A CN107957442A CN201711444876.5A CN201711444876A CN107957442A CN 107957442 A CN107957442 A CN 107957442A CN 201711444876 A CN201711444876 A CN 201711444876A CN 107957442 A CN107957442 A CN 107957442A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
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Abstract
The invention discloses a kind of permanganate index autotitrating method to include the following steps：The stoste voltage V1 of sample after resolution is recorded；Control module controls the quantitative sodium oxalate of the first syringe pump addition；The magnitude of voltage V2 of ORP electrodes output is recorded, control module calculates final voltage value automatically according to empirical equation V end=(V1-V2) * f+V2；Control module controls the second syringe pump that potassium permanganate is added dropwise by the volume of setting, is often added dropwise once, and real-time voltage value V of collection is real, when V is real<V is whole, and titration continues, and when V reality >=V terminal hours, titration stops, being often added dropwise once, and control module records a titration volumes and real-time voltage, sample tests are automatically saved in sample message table；Export voltage change in sample tests and titration process；Titration curve is drawn with voltage change in titration process, whether monitoring sample normally titrates.
Description
Technical field
The present invention relates to the measure field of permanganate index in water, is provided in particular in a kind of both reduced and human subjective is sentenced
The dependence of disconnected titration end-point, also from water sample patterns affect, the permanganate index automatic drip of raising test data accuracy
Determine method.
Background technology
Permanganate index refers under certain condition, with potassium permanganate (KMnO4) it is oxidant, disappeared when handling water sample
The amount of the oxidant of consumption.It is expressed as the mg/litre (O of oxygen2, mg/l).Permanganate index at the specified experimental conditions, can only
Partial oxidation Organic substance in water, is not the scale for reflecting total organic content in water body.International Organization for standardization (ISO) suggests high
Potassium manganate method is only limitted to measure surface water, drinking water and source water, is not suitable for industrial wastewater.
Permanganate index test principle be：The potassium permanganate and sulfuric acid of known quantity are added in sample, in boiling water bath
Resolution 30 minutes, potassium permanganate aoxidize some organic matter and inorganic matter reducing substanceses in sample, are added after reaction excessive
The remaining potassium permanganate of oxalic acid sodium reduction, then the sodium oxalate with potassium permanganate index solution residual titration excess is obtained by calculation
Permanganate index in sample.
During the permanganate index of laboratory test at present, operating personnel judge to drip according to the change of color sample
Determine terminal, the experiment qualification to operating personnel requires high.If having abnormal color after water sample muddiness or water sample resolution, even if
The experimenter of skilled operation, the judgement to titration end-point also can be impacted, easily causes test result to have deviation.Therefore there is an urgent need for
The automatic Titration principle of research energy accurate judgement permanganate index titration end-point, applied to permanganate index automatic Titration system
System.
Therefore, there is an urgent need for a kind of both reduced to judge human subjective the dependence of titration end-point, also from water sample patterns affect,
Improve the permanganate index autotitrating method of test data accuracy.
The content of the invention
The object of the present invention is to provide a kind of both reduced to judge human subjective the dependence of titration end-point, also from water sample
Patterns affect, improves the permanganate index autotitrating method of test data accuracy.
To achieve these goals, technical solution provided by the invention is：A kind of permanganate index automatic Titration is provided
Method, there is provided：Host computer, control module, the first syringe pump, the second syringe pump, ORP electrodes, sodium oxalate, potassium permanganate, sulfuric acid,
Include the following steps：
(1) sample is added into the potassium permanganate of known quantity and sulfuric acid is cleared up, the sample for clearing up completion is placed in titration
Position, is inserted into Suitable depth in sample by ORP electrodes, after control module receives the control signal of seat in the plane, automatically begins to titrate,
The stoste voltage V1 of ORP electrodes output is recorded；
(2) control module controls the quantitative sodium oxalate of the first syringe pump addition；
(3) after sodium oxalate and potassium permanganate fully react, the magnitude of voltage V2 of record ORP electrodes output at this time, controls mould
Block calculates final voltage value automatically according to empirical equation V end=(V1-V2) * f+V2, and wherein correction coefficient f is determined before testing
Good and input control module, titration end-point is captured for precise control；
(4) control module controls the second syringe pump that potassium permanganate is added dropwise by the volume of setting, is often added dropwise once, collection one
Secondary real-time voltage value V is real, when V is real<V is whole, and titration continues, and when V reality >=V terminal hours, titration stops, being often added dropwise once, controls
Module records a titration volumes and real-time voltage, and after the completion of titration, sample tests are automatically saved in sample message table；
(5) voltage change in sample tests and titration process is exported；
(6) voltage change in titration process is used to draw titration curve, whether monitoring sample normally titrates, if curve light
It is sliding without fluctuation, it is and consistent with normal titration curve trend, judge that the automatic test result of the sample is normal, if curve is rough and ripple
It is dynamic bigger, then judge that the automatic test result of the sample is abnormal.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) rule of thumb formula V end=(V1-V2) * f+V2 calculate final voltage value, and V1, V2 are real-time voltage value,
It is not required to gather for a long time, simplifies the process for determining that titration terminates ORP value, dynamic control titration end-point, substantially increases terminal
The flexibility of judgement.
(2) it is not a fixed value that correction coefficient, which is variable, different manufacturers, the adjusted school of ORP electrodes of different model
After positive coefficient, you can adapt to the titration system, the applicable electrode of the titration system is not limited to certain a special electrodes.
(3) it is not required to calibrate electrode after replacing ORP electrodes, correction coefficient need to be only adjusted according to titration situation
It is whole, you can to ensure titration end-point accurate judgement.
(4) to occurring the water sample of abnormal color after turbid water sample and resolution, titration method provided by the invention can accurately be known
Other titration end-point, from the influence of sample state.
It will be become more fully apparent by following description and with reference to attached drawing, the present invention, these attached drawings are used to explain the present invention
Embodiment.
Brief description of the drawings
Fig. 1 is the schematic diagram of permanganate index automatic Titration system.
Fig. 2 is expressed as the schematic diagram of the titration curve of permanganate index autotitrating method of the present invention.
Embodiment
The embodiment of the present invention described referring now to attached drawing, similar element numbers represent similar element in attached drawing.Such as
Upper described, as illustrated in fig. 1 and 2, permanganate index autotitrating method of the present invention is to be based on permanganate index automatic Titration
What system was realized.
As shown in Figure 1, permanganate index automatic Titration system is made of three parts, it is respectively control module, syringe pump
With ORP electrodes.Control module be used for titration system control, including control syringe pump action, gather ORP electrodes voltage,
Titration end-point is judged etc.；Syringe pump has two, is respectively used to the dropwise addition of liquor potassic permanganate and sodium oxalate solution；ORP
Electrode is used for the real-time change for catching voltage in titration process.
Permanganate index autotitrating method of the present invention is introduced with reference to Fig. 2, wherein：Abscissa is to be consumed in titration process
Permanganate solution volume, ordinate is the magnitude of voltage that electrode exports in titration process, when real-time electricity Ya≤V terminal hours, titration
Stop.
(1) sample is added into the potassium permanganate of known quantity and sulfuric acid is cleared up, the sample for clearing up completion is placed in titration
Position, ORP electrodes are inserted into Suitable depth in sample, after control module receives the control signal of seat in the plane, automatically begin to titrate, right
The stoste voltage V1 of ORP electrodes output is recorded；
(2) control module controls the quantitative sodium oxalate of the first syringe pump addition；
(3) after sodium oxalate and potassium permanganate fully react, the magnitude of voltage V2 of record ORP electrodes output at this time, controls mould
Block calculates final voltage value automatically according to empirical equation V end=(V1-V2) * f+V2, and wherein correction coefficient f is determined before testing
Good and input control module, titration end-point is captured for precise control；It should be noted that the determination process of correction coefficient f：
Larger coefficient is inputted in control module, is put into the sample cleared up, automatically begins to titrate, after the completion of titration, export titrated
The magnitude of voltage exported in journey, draws titration curve, liquor potassic permanganate is being added dropwise in titration curve with magnitude of voltage and titration volumes
During trend that is smooth and being declined slightly is presented, be titration end-point when curve is in mutation trend is risen, obtain electric at this time
Pressure value, rule of thumb formula, with reference to the stoste magnitude of voltage V1 and magnitude of voltage V2 for adding sodium oxalate, can be calculated correction coefficient f.
(4) control module controls the second syringe pump that potassium permanganate is added dropwise by the volume of setting, is often added dropwise once, collection one
Secondary real-time voltage value V is real, when V is real<V is whole, and titration continues, and when V reality >=V terminal hours, titration stops, being often added dropwise once, controls
Module records a titration volumes and real-time voltage, and after the completion of titration, sample tests are automatically saved in sample message table；
(5) voltage change in sample tests and titration process is exported；
(6) voltage change in titration process is used to draw titration curve, whether monitoring sample normally titrates, if curve light
It is sliding that without fluctuation, and consistent with normal titration curve trend, the automatic test result of the judgement sample is normal, if curve it is rough and
Fluctuate bigger, then judge that the automatic test result of the sample is abnormal.
It should be noted that how many sodium oxalate added every time, it is well known to those skilled in the art and has standard to look into
's.
The first syringe pump and the second syringe pump are introduced, the present invention uses two syringe pumps, and the first syringe pump is used to drip
Add sodium oxalate solution, the second syringe pump is used to liquor potassic permanganate be added dropwise.Each syringe pump pump is respectively connected with two valve positions, is denoted as
A and B, wherein the valve position A of the first syringe pump and the second syringe pump is all connected with reagent bottle, i.e., as shown in Figure 1, two pumps connect respectively
Sodium oxalate solution and liquor potassic permanganate, B connection sample bottles.
In addition, the particular technique index that syringe pump uses is as follows：
1st, liquid measure accuracy：Error≤1% (during rated travel)；
2nd, liquid measure accuracy：Repeatability error≤0.5% (during rated travel)；
3rd, rated travel (control step number)：60mm (6000 step)；
4th, linear velocity scope：0.05mm/s-50mm/s；
5th, rated travel run time scope：1.2s-1200s；
6th, control resolution：0.01mm (1 step)；
7th, drive mechanism：Ball-screw-transmission；
8th, piston maximum driving force：≥60N；
9th, piston secondary drive power：≥34N；
10th, using specification of syringe：50 μ L, 100 μ L, 250 μ L, 500 μ L, 1mL, 2.5mL, 5mL, 10mL, 25mL (this hair
Bright embodiment uses 10mL syringes)；
11st, valve-type：Standard configuration：3 mouthfuls of 120 ° of valves, may customize：4 mouthfuls of 90 ° of valves, T-shaped 90 ° of valves, 90 ° of distributing valves；
12nd, the valve transposition time：≤ 280ms (adjacent between two mouthfuls)；
13rd, fluid path material：Borosilicate glass, polytetrafluoroethylene (PTFE), polytrifluorochloroethylene；
14th, fluid path maximum pressure-bearing reference value：0.68Mpa；
15th, pipe interface：1/4 " -28 internal thread interface；
16th, syringe interface：1/4 " -28 internal thread interface；
17th, signal inputs：2 road Transistor-Transistor Logic level signal inputs (driving current ＞ 16mA), after controlling static pause instruction
Restarting；
18th, signal output：3 road OC gate signals outputs, for indicating operating status；
19th, communication interface：RS485/RS232 can be set；
20th, traffic rate：9600bps/38400bps can be set；
21st, device parameter is set：6 DIP toggle switch (communication interface, communication speed etc.)；
22nd, appearance and size (length × width × height)：114×65×254(mm)；
23rd, it is applicable in power supply：DC 24V/1.5A；
24th, operating ambient temperature：15 DEG C -40 DEG C (mainly the temperature characterisitic of polytetrafluoroethylene material is determined in by syringe
It is fixed)；
25th, working environment relative humidity：＜ 80%；
26th, weight：2.15kg.
ORP electrodes are introduced, the height of ORP electrodes need to be adjusted according to liquid level in sample bottle, ensure platinum
Ring is soaked in solution.ORP electrodes should be soaked in 3.3M KCl solution when not in use.ORP standards can be used molten when first used
Liquid is corrected electrode.
The particular technique parameter of ORP electrodes is as follows：
1st, ORP testing ranges：±5000mV；
2nd, Applicable temperature scope：0-100℃；
3rd, electrode is pressure-resistant：It is up to 50PSI；
4th, effective measurement region of electrode：Platinum ring (99.99%), the L of 0.25 " O.D. × 0.1 "；
5th, reference system：The double salt bridge designs of Ag/AgCl；
6th, with reference to filling liquid：3.3M (KCl) not refilling type (inner presseds)；
7th, liquid connects material：Glass, platinum and ceramics.
It should be noted that the spare and accessory parts such as syringe pump, syringe, triple valve, ORP electrodes disclosed in the embodiment of the present invention
Concrete model or technical parameter, be all a kind of combination in numerous embodiments, the power of the present invention can not be limited with this
The protection domain that profit requires, can also select the spare and accessory parts of other models to be combined as needed in practical application, still belong to this
The covered scope of invention.
Claims (1)
1. a kind of permanganate index autotitrating method, it is characterised in that provide：Host computer, control module, the first injection
Pump, the second syringe pump, ORP electrodes, sodium oxalate, potassium permanganate, sulfuric acid, include the following steps：
(1) sample is added into the potassium permanganate of known quantity and sulfuric acid is cleared up, the sample for clearing up completion is placed in titration position,
ORP electrodes are inserted into Suitable depth in sample, after control module receives the control signal of seat in the plane, automatically begin to titrate, it is right
The stoste voltage V1 of ORP electrodes output is recorded；
(2) control module controls the quantitative sodium oxalate of the first syringe pump addition；
(3) after sodium oxalate and potassium permanganate fully react, the magnitude of voltage V2 of record ORP electrodes output at this time, control module is certainly
Dynamic rule of thumb formula V end=(V1-V2) * f+V2 calculate final voltage value, and wherein correction coefficient f is determined simultaneously before testing
Input control module, titration end-point is captured for precise control；
(4) control module controls the second syringe pump that potassium permanganate is added dropwise by the volume of setting, is often added dropwise once, and collection is once real
When magnitude of voltage V it is real, when V is real<V is whole, and titration continues, and when V reality >=V terminal hours, titration stops, being often added dropwise once, control module
A titration volumes and real-time voltage are recorded, after the completion of titration, sample tests are automatically saved in sample message table；
(5) voltage change in sample tests and titration process is exported；
(6) use titration process in voltage change draw titration curve, monitoring sample whether normally titrate, if line smoothing without
Fluctuation, and it is consistent with normal titration curve trend, the automatic test result of the judgement sample is normal, if curve is rough and fluctuates
It is bigger, then judge that the automatic test result of the sample is abnormal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711444876.5A CN107957442A (en) | 2017-12-27 | 2017-12-27 | Permanganate index autotitrating method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711444876.5A CN107957442A (en) | 2017-12-27 | 2017-12-27 | Permanganate index autotitrating method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201159728Y (en) * | 2007-11-12 | 2008-12-03 | 江苏绿叶环保科技仪器有限公司 | Automatic detection instrument for permanganate index |
| CN201780281U (en) * | 2010-08-31 | 2011-03-30 | 宇星科技发展(深圳)有限公司 | Online water quality analyzer for permanganate index |
| JP2011183305A (en) * | 2010-03-09 | 2011-09-22 | Taiheiyo Cement Corp | Method of treating incineration ash |
| CN102288667A (en) * | 2011-05-06 | 2011-12-21 | 厦门隆力德环境技术开发有限公司 | Titration endpoint determination method for ORP (oxidation-reduction potential) value of permanganate index type water quality analyzer |
-
2017
- 2017-12-27 CN CN201711444876.5A patent/CN107957442A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201159728Y (en) * | 2007-11-12 | 2008-12-03 | 江苏绿叶环保科技仪器有限公司 | Automatic detection instrument for permanganate index |
| JP2011183305A (en) * | 2010-03-09 | 2011-09-22 | Taiheiyo Cement Corp | Method of treating incineration ash |
| CN201780281U (en) * | 2010-08-31 | 2011-03-30 | 宇星科技发展(深圳)有限公司 | Online water quality analyzer for permanganate index |
| CN102288667A (en) * | 2011-05-06 | 2011-12-21 | 厦门隆力德环境技术开发有限公司 | Titration endpoint determination method for ORP (oxidation-reduction potential) value of permanganate index type water quality analyzer |
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