CN105116098B - A kind of autotitrating method and application - Google Patents
A kind of autotitrating method and application Download PDFInfo
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Abstract
The invention discloses a kind of autotitrating method, comprise the following steps：(1) sampling and sample pretreatment；(2) titrator pre-sets；(3) first stage titration；(4) second stage titration；(5) titrate after speed regulating control amount point；(6) data acquisition.A kind of autotitrating method that the present invention provides, be a kind of can accurately, the method for testing of science judgment titration end-point, by the way of setting speed regulating control point and speed regulating control amount, ensure that becoming more meticulous of titration process, after reaching speed regulating control amount point simultaneously, according to the hysteresis quality of chemical reaction, take the mode that dropwise Deca, time delay judge, such that it is able to effectively ensure the accuracy of titration end-point.The autotitrating method of the present invention, using full automatic mode, it is to avoid the impact to measurement result for the artificial operation, and measurement result accuracy is high, reproducible.Can be used in rinsing performance test.
Description
Technical field
The present invention relates to a kind of autotitrating method and application, belong to household electrical appliance technical field.
Background technology
Rinsing performance, that is, the ability of washing machine removal detergent and residual contaminants, is the important of washing machine performance detection
Project.In existing various countries washing machine standard, the detection method of rinsing performance is different, and its Cleaning Principle substantially can be divided into two
Class：One is using certain component substances of detergent as indicator, detects its change before and after rinsing so that it is determined that washing machine floats
Wash performance.The basicity method using as China and IEC (International Electrotechnical Commission), is the change of detection detergent neutral and alkali material
Change situation.The washing machine standard that the U.S. currently revises is then surfactant (the linear alkylbenzene (LAB) sulphur in detection detergent
Sour sodium, LAS) changes of contents.Two is the particular matter adding certain convenient detection in laundry processes, by it in cleaning mixture
In changes of contents determine washing machine rinse capacity.As in Nippon Standard add sodium chloride, by detect cleaning mixture electrical conductivity Lai
Determine the changes of contents of sodium chloride, thus detecting rinsing performance.Then add 2- benzene in Australia/New Zealand's washing machine standard
Base -5- benzimidazole-sulfonic acid (PBIS) is as indicator substance.Said method cuts both ways, the method operation letter of China and IEC
Single, but data reappearance is poor；American process may face the excessively complicated problem of detection test；Day this method is easily tested
Test the interference with water, and rinse test individually must separate to do with decantation test；Australia/New Zealand's method is not only grasped
Make complexity just can test and it is necessary to carry out pretreatment to standard wash thing.Therefore, find one the simplest, feasible, can
The test method of letter is the emphasis of current industry concern.Basicity method is the standard method of China although there is data redundancy
The problem of difference, but it in operation and is disturbed in degree and has very big advantage compared to additive method.
Presently commercially available titrator is all constant-current titration principle, and the product even being titrated with pH value is also by pH
Value is converted into electrical potential information.The titration process of therefore conventional titration instrument is divided into 2 kinds of modes mostly：1st, a titration end-point is set,
Titrator starts to titrate with a certain initial velocity, and when the closer to this terminal, rate of titration is slower, when reaching this terminal, drips
Fixed termination；2nd, it is not provided with titration end-point, after to each titration, solution potential situation of change is carried out with differential calculation, observe
Catastrophe point (threshold points), finds catastrophe point and records titer now and pH value data now.2nd kind of titration mode is general
For research work, using less in actual production.
Most of titrators adopt the first titration mode, but first kind of way has problems with：(1) this automatic drip
Determine process and be very easy to occur dripping the situation of terminal, because chemical reaction has hysteresis quality, because solution is different, performance is also different,
Often when titrator finds arrival or close to terminal, can be difficult to grasp its speed, so in actual use, such automatic drip
Determine instrument mostly using manual titration function, so-called " automatic Titration " simply ornaments；(2) even if " automatic Titration " is can be real
Existing, also lack unified criterion, that is, the problem how long being judged after reaching home.Additionally, no matter titrator precision is many
Height, be still likely to occur previous drop in terminal before, one drop in the situation after terminal afterwards, titration end-point now equally occur
The problem how to be judged.
For a long time, when carrying out rinsing performance of washing machine test, because different enterprises adopt distinct device (sensor accuracy
Different), the difference such as human users' proficiency, operating habit, lead to rinsing test repeatability poor.To titration when especially testing
Often there is larger difference in the judgement of terminal.Because chemical reaction has a hysteresis quality, the therefore diversity to endpoint, past
Toward leading to test result stability and the reduction of accuracy.Therefore, research a kind of can accurately, the survey of science judgment titration end-point
Method for testing, it appears particularly necessary.
Content of the invention
For solving the deficiencies in the prior art, it is an object of the invention to provide a kind of autotitrating method and application, the party
Method can accurately judge titration end-point, realizes the accuracy of titration results, can be used in rinsing performance test.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that：
A kind of autotitrating method, comprises the following steps：(1) sampling and sample pretreatment；(2) titrator pre-sets；
(3) first stage titration；(4) second stage titration；(5) titrate after speed regulating control amount point；(6) data acquisition.
In aforementioned titration method, specifically include following steps：
(1) sampling and sample pretreatment：Take testing sample solution, through microporous filter membrane filtration, put in dress sample container；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time, delay time, speed 1, speed 2, speed regulating control point pH value, endpoint pH and speed regulating control amount；Described speed regulating control
Amount is speed regulating control amount point pH value with the difference of speed regulating control point pH value accounts for the difference of speed regulating control point pH value and endpoint pH
Ratio；
(3) first stage titration：After test starts, carry out pre- stirring, after pre- stirring terminates, the speed to set for the titrator
1 starts to titrate, until testing sample pH value reaches speed regulating control point pH value；
(4) second stage titration：After sample pH reaches speed regulating control point pH value, titrator is started with the speed 2 setting
Titration, until testing sample pH value reaches speed regulating control amount point pH value；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches speed regulating control amount point pH value, titrator is according to
Little titer is titrated, and often instills 1, waits delay time through later, judges that pH value is not up to endpoint pH and then continues
Instilling next, until judging that pH value meets or exceeds endpoint pH, stopping titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve, judge that pH value reaches endpoint pH and stops titration, directly obtain endpoint titration data；Judge pH value
Exceed endpoint pH and stop titration, interpolation calculation obtains endpoint titration data.
In aforementioned titration method, pre- mixing time is 0.1～10min, and delay time is 1s～100s.
In aforementioned titration method, speed regulating control amount is 1%～99%.
In aforementioned titration method, speed 1 is 0.01～10mL/min, and speed 2 is 0.01～10mL/min, titer
Drip for 0.002mL/～0.008mL/ drips.
Further, in aforementioned titration method, titer drips for 0.005mL/.
Application in rinsing performance test for the autotitrating method.
In aforementioned applications, rinsing performance tests the basicity test for rinsing performance of washing machine.
In aforementioned applications, the basicity test of rinsing performance of washing machine specifically includes following steps：
(1) sampling and sample pretreatment：Take test water and residual rinse liquid respectively, each 3 parts, every part of 300mL, through water
It is 0.45 μm of microporous filter membrane filtration, be respectively put in dress sample container, test respectively as testing sample；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time is 1min, delay time is 10s, speed 1 is 2mL/min, speed 2 is that 0.5mL/min, speed regulating control point pH value are
7.00th, endpoint pH is 4.50 and speed regulating control amount is 30%；
(3) first stage titration：After test starts, carry out pre- stirring 1min, after pre- stirring terminates, titrator is to set
Speed 1 starts to titrate for 2mL/min, until testing sample pH value reaches 7.00；
(4) second stage titration：After sample pH reaches 7.00, titrator is started with the speed 2 setting for 0.5mL/min
Titration, until testing sample pH value reaches 6.25；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches 6.25, titrator is according to titer
0.005mL/ is titrated, and often instills 1, after waiting 10s, judges that not up to 4.5 continuation of pH value instill next and drip, directly
To when judging that pH value is equal to or less than 4.50, stop titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve；Judge that pH value is less than 4.5 and stops titration, carry out interpolation calculation and obtain endpoint titration data, judge
PH value is equal to 4.5 and stops titration, directly obtains endpoint titration data.
(7) calculate：Carry out being calculated the relative basicity of residual rinse liquid by titration end-point data.
The titration method of the present invention can pre-set before titration pre- mixing time, delay time, speed 1, speed 2,
The value of speed regulating control point pH value, endpoint pH and speed regulating control amount.Whole process experiences three titration phase, stirs in advance first
Start after end to titrate, start to be titrated to speed regulating control point pH value from original ph, titrated using speed 1；Secondly, when detecting
After pH value reaches the speed regulating control point pH value setting, titrated using speed 2；Finally when detect pH value reach speed regulating control amount point
During pH value (when reaching speed regulating control amount), titration is carried out using titer until titration terminates.In last stage
Titration process, that is, reach in the titration process after speed regulating control amount point pH value, after system titrates one section of delay time of a wait
Again result pH value is judged, be primarily directed to the hysteresis quality of chemical reaction, be also beneficial to result of the test is compared and (prolong
When the time different, pH value is also different).When occur previous drop in endpoint pH before, afterwards one drop in endpoint pH after
Situation, the method for the present invention is the titer being gone out using interpolation calculation corresponding to titration end-point.
The judgement to speed governing controlled quentity controlled variable point pH value for the system in the present invention, be by the speed regulating control point pH value that pre-sets,
The value of endpoint pH and speed regulating control amount is determined, judge.Speed regulating control amount is speed regulating control amount point pH value and speed governing
The difference of control point pH value accounts for the ratio of the difference of speed regulating control point pH value and endpoint pH.Therefore, speed regulating control amount point pH value
Calculating such as formula (1) shown in：
± | speed regulating control point pH value-titration end-point the pH value | × speed governing of speed regulating control amount point pH value=speed regulating control point pH value
Controlled quentity controlled variable (1)
The solution taking different pH value carries out acid base titration respectively using the inventive method, titration results such as Tables 1 and 2 institute
Show.
Table 1
Table 2
From Tables 1 and 2, the titration method of the present invention goes for acid base titration, and gained titration results are accurately, surely
Fixed, favorable repeatability.
The titration method of the present invention can be applied in rinsing performance test.With the basicity test in rinsing performance of washing machine
As a example the middle application method of the present invention.Take test water and residual rinse liquid first, through 0.45 μm of microporous filter membrane filtration of water system
Afterwards, standby as testing sample, set respectively endpoint pH as 4.50, speed regulating control point pH value as 7.00, delay time as
10s, initial mixing time are 1 minute, speed regulating control amount is that 30%, speed 1 is 2mL/min and speed 2 is 0.5mL/min.Root
According to the difference of the burette selected, titer is different, and in rinsing performance test, titer drips for 0.005mL/.Survey
After runin is begun, first carry out the pre- stirring of 1 minute, automatically begin to after 1 minute titrate, the point pH value from original ph to speed regulating control
7.00 is the first titration phase, is titrated according to 2mL/min speed.When reaching pH=7.00, enter the second titration phase,
Titrated with 0.5mL/min speed, when reaching speed regulating control amount point pH, entered final titration phase.
In the basicity of rinsing performance of washing machine is tested, when speed regulating control amount is set to 30%, speed regulating control amount point pH value
=6.25.When pH value reaches 6.25, with titer 0.005mL/ instillation, often instill one, wait 10s so that molten
It is sufficiently mixed reaction between liquid, be conducive to real-time pH value being measured, such that it is able to accurately judge titration end-point.After 10s, judge now
, there are three kinds of possibility in pH value and the magnitude relationship of endpoint pH 4.50：1) pH value is equal to 4.50, then titration terminates, and directly obtains
Final result；2) pH value is more than 4.50, then continue to instill next, wait 10s, repeat determination step；3) pH value is less than 4.50,
Then combining the test data of upper, carrying out interpolation calculation, thus obtaining the result of endpoint pH 4.50.For example after 1 instills,
Wait 10 seconds, after 10s, pH value is 4.52, now total titer is 2.494mL, then instills 1, waits 10 seconds, after 10s, pH value is
4.47, now total titer is 2.499mL, then according to above-mentioned data, can simulate (calculating according in front and back's data difference), pH value
During for 4.50, total titer is about 2.496mL.After test terminates, test data is converted directly into by test data sheet by software.
Avoid conventional titration instrument personnel copy it may happen that mistake, whole titration data are entered by the way of mean sample simultaneously
Row sampling, takes 21 points (containing Origin And Destination) therein, draw final data form generate tables of data (as shown in table 3) and
Curve (as shown in Figure 1), also allows for carrying out subsequent analysis to test solvent.Data form also can be according to actual titration situation, spirit
The numerical value of setting transverse and longitudinal coordinate of living.Additionally, also providing " once differentiation " and " second differential " of experimental data, contribute to finding to dash forward
Become position, titration process is analysed in depth.After obtaining endpoint titration data, calculated according to formula (2), obtained residual
Stay the basicity that rinsing liquid is relative to test water, wherein, titrated using hydrochloric acid in the basicity test of rinsing performance of washing machine,
In formula (2), Ar is relative basicity, MHClMolar concentration (mol/L) for hydrochloric acid solution, uHClFor titration residual rinsing
The hydrochloric acid consumption (mL) of liquid, υHClFor titrating the hydrochloric acid consumption (mL) of test water, υSVolume for titrated test water
(mL),uPVolume (mL) for titrated residual rinse liquid.
Table 3
| Titration point sampling | Titer (mL) | Solution pH value |
| Initially | 0 | 7.090 |
| 1 | 0.899 | 6.942 |
| 2 | 1.082 | 6.830 |
| 3 | 1.266 | 6.724 |
| 4 | 1.450 | 6.605 |
| 5 | 1.633 | 6.478 |
| 6 | 1.817 | 6.329 |
| 7 | 1.934 | 6.035 |
| 8 | 1.978 | 5.840 |
| 9 | 2.023 | 5.780 |
| 10 | 2.069 | 5.748 |
| 11 | 2.114 | 5.716 |
| 12 | 2.158 | 5.678 |
| 13 | 2.203 | 5.630 |
| 14 | 2.249 | 5.569 |
| 15 | 2.293 | 5.487 |
| 16 | 2.338 | 5.379 |
| 17 | 2.384 | 5.223 |
| 18 | 2.428 | 4.989 |
| 19 | 2.473 | 4.665 |
| End value | 2.496 | 4.50 |
The invention has benefit that：The present invention provide a kind of autotitrating method, be one kind can accurately, science
Judge the method for testing of titration end-point, it is ensured that titration process by the way of set speed regulating control point and speed regulating control amount
Become more meticulous, after reaching speed regulating control amount point, according to the hysteresis quality of chemical reaction, take the side that dropwise Deca, time delay judge simultaneously
Formula, so that titration controls more accurately, can fully be reacted it is therefore prevented that closing on the measurement result of solution ph before terminal between solution
Inaccurate, such that it is able to effectively ensure the accuracy of titration end-point, it is to avoid the shadow that excessive Deca causes to titration results
Ring.The autotitrating method of the present invention, using full automatic mode, efficiently, facilitates, has saved cost of labor, avoiding simultaneously
Manually operate the impact to measurement result, measurement result accuracy is high, reproducible.Can be used in rinsing performance test, especially
It is in the basicity test be applied to rinsing performance of washing machine.
Brief description
Fig. 1 is the test data curve chart of the present invention.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further introduced.
A kind of autotitrating method of embodiment 1, specifically includes following steps：
(1) sampling and sample pretreatment：Take testing sample solution, through microporous filter membrane filtration, put in dress sample container；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time 0.5min, delay time 20s, speed 1 are 1mL/min, speed 2 is 0.1mL/min, speed regulating control point pH value, terminal pH
Value and speed regulating control amount 15%；
(3) first stage titration：After test starts, carry out pre- stirring, after pre- stirring terminates, the speed to set for the titrator
1 starts to titrate, until testing sample pH value reaches speed regulating control point pH value；
(4) second stage titration：After sample pH reaches speed regulating control point pH value, titrator is started with the speed 2 setting
Titration, until testing sample pH value reaches speed regulating control amount point pH value；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches speed regulating control amount point pH value, titrator is according to
Little titer 0.002mL/ is titrated, and often instills 1, waits delay time through later, judges that pH value is not up to terminal
PH value then continues to instill next, until judging that pH value meets or exceeds endpoint pH, stops titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve, judge that pH value reaches endpoint pH and stops titration, directly obtain endpoint titration data；Judge pH value
Exceed endpoint pH and stop titration, interpolation calculation obtains endpoint titration data.
Using the titration method of embodiment 1, titration results are as shown in table 4.
Table 4
| Original ph | Titration end-point | Total titer (mL) |
| 2.52 | PH=9.0 | 10.116 |
| 2.22 | PH=9.0 | 11.775 |
| 2.44 | PH=9.0 | 10.598 |
A kind of autotitrating method of embodiment 2, specifically includes following steps：
(1) sampling and sample pretreatment：Take testing sample solution, through water system microporous filter membrane filtration, put into dress sample and hold
In device；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time 2min, delay time 30s, speed 1 be 3mL/min, speed 2 be 1mL/min, speed regulating control point pH value, endpoint pH with
And speed regulating control amount 50%；
(3) first stage titration：After test starts, carry out pre- stirring, after pre- stirring terminates, the speed to set for the titrator
1 starts to titrate, until testing sample pH value reaches speed regulating control point pH value；
(4) second stage titration：After sample pH reaches speed regulating control point pH value, titrator is started with the speed 2 setting
Titration, until testing sample pH value reaches speed regulating control amount point pH value；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches speed regulating control amount point pH value, titrator is according to
Little titer 0.008mL/ is titrated, and often instills 1, waits delay time through later, judges that pH value is not up to terminal
PH value then continues to instill next, until judging that pH value meets or exceeds endpoint pH, stops titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve, judge that pH value reaches endpoint pH and stops titration, directly obtain endpoint titration data；Judge pH value
Exceed endpoint pH and stop titration, interpolation calculation obtains endpoint titration data.
Using the titration method of embodiment 2, titration results are as shown in table 5.
Table 5
| Original ph | Titration end-point | Total titer (mL) |
| 8.69 | PH=4.0 | 4.372 |
| 8.69 | PH=4.0 | 4.385 |
| 8.69 | PH=4.0 | 4.348 |
A kind of autotitrating method of embodiment 3, specifically includes following steps：
(1) sampling and sample pretreatment：Take testing sample solution, through 0.45 μm of microporous filter membrane filtration of water system, put into
In dress sample container；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time 1min, delay time 10s, speed 1 are 2mL/min, speed 2 is 0.5mL/min, speed regulating control point pH value, endpoint pH
And speed regulating control amount 30%；
(3) first stage titration：After test starts, carry out pre- stirring, after pre- stirring terminates, the speed to set for the titrator
1 starts to titrate, until testing sample pH value reaches speed regulating control point pH value；
(4) second stage titration：After sample pH reaches speed regulating control point pH value, titrator is started with the speed 2 setting
Titration, until testing sample pH value reaches speed regulating control amount point pH value；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches speed regulating control amount point pH value, titrator is according to
Little titer 0.005mL/ is titrated, and often instills 1, waits delay time through later, judges that pH value is not up to terminal
PH value then continues to instill next, until judging that pH value meets or exceeds endpoint pH, stops titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve, judge that pH value reaches endpoint pH and stops titration, directly obtain endpoint titration data；Judge pH value
Exceed endpoint pH and stop titration, interpolation calculation obtains endpoint titration data.
Using the titration method of embodiment 3, titration results are as shown in table 6.
Table 6
| Original ph | Titration end-point | Total titer (mL) |
| 7.89 | PH=4.0 | 3.652 |
| 7.89 | PH=4.0 | 3.649 |
| 7.89 | PH=4.0 | 3.657 |
A kind of autotitrating method of embodiment 4, specifically includes following steps：
(1) sampling and sample pretreatment：Take testing sample solution, through water system microporous filter membrane filtration, put into dress sample and hold
In device；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time 0.1min, delay time 100s, speed 1 are 10mL/min, speed 2 is 0.01mL/min, speed regulating control point pH value, terminal
PH value and speed regulating control amount 1%；
(3) first stage titration：After test starts, carry out pre- stirring, after pre- stirring terminates, the speed to set for the titrator
1 starts to titrate, until testing sample pH value reaches speed regulating control point pH value；
(4) second stage titration：After sample pH reaches speed regulating control point pH value, titrator is started with the speed 2 setting
Titration, until testing sample pH value reaches speed regulating control amount point pH value；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches speed regulating control amount point pH value, titrator is according to
Little titer 0.002mL/ is titrated, and often instills 1, waits delay time through later, judges that pH value is not up to terminal
PH value then continues to instill next, until judging that pH value meets or exceeds endpoint pH, stops titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve, judge that pH value reaches endpoint pH and stops titration, directly obtain endpoint titration data；Judge pH value
Exceed endpoint pH and stop titration, interpolation calculation obtains endpoint titration data.
Using the titration method of embodiment 4, titration results are as shown in table 7.
Table 7
| Original ph | Titration end-point | Total titer (mL) |
| 9.33 | PH=4.5 | 13.021 |
| 9.33 | PH=4.5 | 13.026 |
| 9.33 | PH=4.5 | 13.018 |
A kind of autotitrating method of embodiment 5, specifically includes following steps：
(1) sampling and sample pretreatment：Take testing sample solution, through water system microporous filter membrane filtration, put into dress sample and hold
In device；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time 10min, delay time 1s, speed 1 are 0.01mL/min, speed 2 is 10mL/min, speed regulating control point pH value, terminal pH
Value and speed regulating control amount 99%；
(3) first stage titration：After test starts, carry out pre- stirring, after pre- stirring terminates, the speed to set for the titrator
1 starts to titrate, until testing sample pH value reaches speed regulating control point pH value；
(4) second stage titration：After sample pH reaches speed regulating control point pH value, titrator is started with the speed 2 setting
Titration, until testing sample pH value reaches speed regulating control amount point pH value；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches speed regulating control amount point pH value, titrator is according to
Little titer 0.004mL/ is titrated, and often instills 1, waits delay time through later, judges that pH value is not up to terminal
PH value then continues to instill next, until judging that pH value meets or exceeds endpoint pH, stops titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve, judge that pH value reaches endpoint pH and stops titration, directly obtain endpoint titration data；Judge pH value
Exceed endpoint pH and stop titration, interpolation calculation obtains endpoint titration data.
Using the titration method of embodiment 5, titration results are as shown in table 8.
Table 8
| Original ph | Titration end-point | Total titer (mL) |
| 8.16 | PH=4.5 | 3.982 |
| 8.28 | PH=4.5 | 3.889 |
| 8.58 | PH=4.5 | 3.920 |
A kind of autotitrating method of embodiment 6, specifically includes following steps：
(1) sampling and sample pretreatment：Take testing sample solution, through water system microporous filter membrane filtration, put into dress sample and hold
In device；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time 5min, delay time 50s, speed 1 are 8mL/min, speed 2 is 0.08mL/min, speed regulating control point pH value, endpoint pH
And speed regulating control amount 70%；
(3) first stage titration：After test starts, carry out pre- stirring, after pre- stirring terminates, the speed to set for the titrator
1 starts to titrate, until testing sample pH value reaches speed regulating control point pH value；
(4) second stage titration：After sample pH reaches speed regulating control point pH value, titrator is started with the speed 2 setting
Titration, until testing sample pH value reaches speed regulating control amount point pH value；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches speed regulating control amount point pH value, titrator is according to
Little titer 0.006mL/ is titrated, and often instills 1, waits delay time through later, judges that pH value is not up to terminal
PH value then continues to instill next, until judging that pH value meets or exceeds endpoint pH, stops titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve, judge that pH value reaches endpoint pH and stops titration, directly obtain endpoint titration data；Judge pH value
Exceed endpoint pH and stop titration, interpolation calculation obtains endpoint titration data.
Using the titration method of embodiment 6, titration results are as shown in table 9.
Table 9
| Original ph | Titration end-point | Total titer (mL) |
| 1.44 | PH=9.0 | 33.078 |
| 1.44 | PH=9.0 | 33.084 |
| 1.44 | PH=9.0 | 33.082 |
The titration method of above-described embodiment 1～6 is used equally in rinsing performance test.Embodiment 7 is dripping embodiment 3
The method of determining is applied to the example in the basicity test of rinsing performance of washing machine.
Embodiment 7
The basicity test of rinsing performance of washing machine, specifically includes following steps：
(1) sampling and sample pretreatment：Take test water and residual rinse liquid respectively, each 3 parts, every part of 300mL, through water
After being 0.45 μm of microporous filter membrane filtration, respectively take 100mL to be respectively put in dress sample container, test respectively as testing sample；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- stirring of titrator respectively
Time 1min, delay time 10s, speed 1 are 2mL/min, speed 2 is 0.5mL/min, speed regulating control point pH value is 7.00, whole
Point pH value is 4.50 and speed regulating control amount is 30%；
(3) first stage titration：After test starts, carry out pre- stirring 1min, after pre- stirring terminates, titrator is to set
Speed 1 starts to titrate for 2mL/min, until testing sample pH value reaches 7.00；
(4) second stage titration：After sample pH reaches 7.00, titrator is started with the speed 2 setting for 0.5mL/min
Titration, until testing sample pH value reaches 6.25；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches 6.25, titrator is according to titer
0.005mL/ is titrated, and often instills 1, after waiting 10s, judges that not up to 4.50 continuation of pH value instill next and drip,
Until when judging that pH value is equal to or less than 4.50, stopping titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample,
Generate tables of data and curve；Judge that pH value is less than 4.5 and stops titration, carry out interpolation calculation and obtain endpoint titration data, judge
PH value is equal to 4.5 and stops titration, directly obtains endpoint titration data；
(7) calculate：Carry out being calculated the relative basicity of residual rinse liquid by titration end-point data.According to formulaCalculated, obtained the basicity that residual rinse liquid is relative to test water.Wherein, this enforcement
Titrated using hydrochloric acid in example, Ar is relative basicity, MHClMolar concentration (mol/L) for hydrochloric acid solution, uHClResidual for titrating
Stay three parts of meansigma methodss (mL) of the hydrochloric acid consumption of rinsing liquid, υHClFor titrating three parts of meansigma methodss (mL) of hydrochloric acid consumption of test water,
υSVolume (herein for 100mL) for titrated test water, uPVolume (herein for 100mL) for titrated residual rinse liquid.
Wherein, molar concentration M of the hydrochloric acid solution through demarcatingHClFor 0.1mol/L, titration results are as shown in table 10.
Table 10
It is calculated by data in table 9, relative basicity Ar=7.86 × 10 of residual rinse liquid-4.
Claims (9)
1. a kind of autotitrating method it is characterised in that：Comprise the following steps：
(1) sampling and sample pretreatment：Take testing sample solution, through microporous filter membrane filtration, put in dress sample container；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, respectively during the pre- stirring of setting titrator
Between, delay time, speed 1, speed 2, speed regulating control point pH value, endpoint pH and speed regulating control amount；Described speed regulating control amount
I.e. the difference of speed regulating control amount point pH value and speed regulating control point pH value accounts for the ratio of speed regulating control point pH value and the difference of endpoint pH
Example；
(3) first stage titration：After test starts, carry out pre- stirring, after pre- stirring terminates, titrator is left with the speed 1 setting
Begin to titrate, until testing sample pH value reaches speed regulating control point pH value；
(4) second stage titration：After sample pH reaches speed regulating control point pH value, titrator starts to titrate with the speed 2 setting,
Until testing sample pH value reaches speed regulating control amount point pH value；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches speed regulating control amount point pH value, titrator is according to smallest drop
Quantitation is titrated, and often instills 1, waits delay time through later, judges that pH value is not up to endpoint pH and then continues to instill
Next drips, until judging that pH value meets or exceeds endpoint pH, stops titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample, generate
Tables of data and curve, judge that pH value reaches endpoint pH and stops titration, directly obtain endpoint titration data；Judge that pH value exceedes
Endpoint pH stops titration, and interpolation calculation obtains endpoint titration data.
2. autotitrating method according to claim 1 it is characterised in that：Described pre- mixing time is 0.1～10min,
Delay time is 1～100s.
3. autotitrating method according to claim 1 it is characterised in that：Described speed regulating control amount is 1%～99%.
4. autotitrating method according to claim 1 it is characterised in that：Described speed 1 is 0.01～10mL/min, institute
Stating speed 2 is 0.01～10mL/min, and described titer drips for 0.002mL/～and 0.008mL/ drips.
5. the autotitrating method according to claim 1 or 4 it is characterised in that：Described titer is 0.005mL/
Drip.
6. application in rinsing performance test for the autotitrating method as described in any one of Claims 1 to 5.
7. autotitrating method according to claim 6 application it is characterised in that：Described rinsing performance is tested as laundry
The basicity test of machine rinsing performance.
8. the autotitrating method according to claim 6 or 7 application it is characterised in that：Described rinsing performance test is also
Calculate including step (7)：Carry out being calculated rinsing performance test result according to by titration end-point data.
9. autotitrating method according to claim 8 application it is characterised in that：The alkali of described rinsing performance of washing machine
Degree test, specifically includes following steps：
(1) sampling and sample pretreatment：Take test water and residual rinse liquid respectively, each 3 parts, every part of 300mL, through water system
0.45 μm of microporous filter membrane filtration, is respectively put in dress sample container, tests respectively as testing sample；
(2) titrator pre-sets：After inserting burette and pH probe in dress sample container, set the pre- mixing time of titrator respectively
For 1min, delay time be 10s, speed 1 be 2mL/min, speed 2 be 0.5mL/min, speed regulating control point pH value be 7.00, eventually
Point pH value is 4.50 and speed regulating control amount is 30%；
(3) first stage titration：After test starts, carry out pre- stirring 1min, after pre- stirring terminates, the speed to set for the titrator
1 starts to titrate for 2mL/min, until testing sample pH value reaches 7.00；
(4) second stage titration：After sample pH reaches 7.00, titrator starts to drip with the speed 2 setting for 0.5mL/min
Fixed, until testing sample pH value reaches 6.25；
(5) titrate after speed regulating control amount point：After testing sample pH value reaches 6.25, titrator is according to titer 0.005mL/
Titrated, often instilled 1, after waiting 10s, judged that not up to 4.50 continuation of pH value instill next and drip, until judging
When pH value is equal to or less than 4.50, stop titration；
(6) data acquisition：After stopping titration, whole titration data of record are sampled by the way of mean sample, generate
Tables of data and curve；Judge that pH value is less than 4.5 and stops titration, carry out interpolation calculation and obtain endpoint titration data, judge pH value
Stop titration equal to 4.5, directly obtain endpoint titration data；
(7) calculate：Carry out being calculated the relative basicity of residual rinse liquid by titration end-point data.
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| CN106404775B (en) * | 2016-09-05 | 2019-11-12 | 江苏德林环保技术有限公司 | A kind of the Single wavelength autocontrol method and device of quick photometric titration |
| CN106645134A (en) * | 2017-02-22 | 2017-05-10 | 王飞 | Color measurement instrument for chemical analysis |
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| JPH0660900B2 (en) * | 1988-09-09 | 1994-08-10 | 三井東圧化学株式会社 | COD automatic simple measuring device |
| CN201034942Y (en) * | 2007-04-18 | 2008-03-12 | 南京财经大学 | Food supplies fatty acid values automatic determinator |
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| CN102331479A (en) * | 2010-07-15 | 2012-01-25 | 中国家用电器研究院 | Method for measuring rinsing performance of washing machine |
| CN101975865B (en) * | 2010-10-09 | 2012-09-05 | 中国神华能源股份有限公司 | Automatic titration system for acid or alkali liquor |
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