CN102323376B - Metering parameter correction method of permanganate index water quality analyzer - Google Patents
Metering parameter correction method of permanganate index water quality analyzer Download PDFInfo
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Abstract
A metering parameter correction method of a permanganate index water quality analyzer of the invention relates to the field of water quality analysis, and comprises the following steps: A. adding a purified water sample of a first standard equivalence, a sulfuric acid solution of a second standard equivalence, and a potassium permanganate solution of 20%-80% of a third standard equivalence into the permanganate index water quality analyzer by a metering pump, heating and keeping a constant temperature for a certain period by a temperature control member; B. adding a sodium oxalate solution of105% of the third standard equivalence into the permanganate index water quality analyzer by the metering pump; C. performing titration of the potassium permanganate solution by the metering pump of the permanganate index water quality analyzer to reach a titration end point, recording the accumulated titration metering value of the potassium permanganate solution; D. subtracting a metering valueof 5% of the third standard equivalence value from the sum of the metering value of the potassium permanganate solution added in step A and the accumulated titration metering value of the potassium permanganate solution in step C to obtain a corrected standard equivalence of the potassium permanganate solution, and performing metering parameter correction of the potassium permanganate solution metering pump of the permanganate index water quality analyzer by the corrected standard equivalence of the potassium permanganate solution.
Description
Technical field
The present invention relates to the permanganate index Water Test Kits in water analysis field, relate in particular to the measuring parameter modification method of permanganate index Water Test Kits.
Background technology
Because permanganate index can reflect the water pollution situation of potable water, source water and the day water to a certain extent in the water quality.Therefore, permanganate index is the reflection cleaning and cleans the common counter that organic and inorganic oxidizable substance pollutes in the water body.Reducing inorganic things such as the nitrite in the water, ferrous salt, sulfide and organism that with this understanding can be oxidized, all can consume potassium permanganate, therefore permanganate index often is used as the overall target that surface water is subjected to organic contaminant and reducing inorganic thing pollution level, this standard adopts some organism and the inorganic oxidizable substance in the potassium permanganate oxidation water sample, calculates suitable oxygen amount by the potassium permanganate amount that consumes.
The permanganate index Water Test Kits is exactly the instrument that detects permanganate index in the water quality.The measuring process of permanganate index Water Test Kits divides following 3 stages to carry out: 1. get quantitative water sample (100mL, this is the standard of general measure, is particular value, down together), add quantitative liquor potassic permanganate (10mL) and sulfuric acid (10mL); Heated at constant temperature is 30 minutes then.2. add quantitative sodium oxalate solution (10mL) then.3. again with the liquor potassic permanganate titration up to titration end-point occurring and measure the consumption of potassium permanganate in the titration process, titration end-point judges that general what adopt is optical method or ORP electrode method; At last, calculate permanganate index with potassium permanganate consumption in the titration process.
According to the analysis of the testing process of permanganate index Water Test Kits, the factor that influences the permanganate index detected value mainly is that the measuring accuracy of reagent, titration end-point are judged, the accuracy of reagent configuration.Can overcome by some patented technologies or technological means about the accuracy that titration end-point is judged and reagent disposes.Can select for use the higher relatively volume pump of measuring accuracy to solve about the measuring accuracy of reagent, measure as employing pulsed self-priming volume pump etc.
Therefore, in the measuring process of permanganate index Water Test Kits, will directly influence the precision of The ultimate results to the measuring accuracy of reagent.But no matter adopt the higher volume pump of precision to realize that reagent quantitatively pumps into, the permanganate index Water Test Kits is after the use of experience a period of time, and the potassium permanganate volume pump can make measuring accuracy deviation occur because of the problem of precipitation fouling.Sodium oxalate volume pump, sulfuric acid volume pump and other volume pumps then this problem can not occur basically.The mete-wand errors potassium permanganate volume pump and other volume pumps (that is non-equivalent) will cause the error of measurement result; Especially permanganate index is calculated with potassium permanganate consumption in the titration process, and the accuracy of the metering of potassium permanganate volume pump is most important.Therefore, in prior art, no matter the metering of reagent takes any metering method, after instrument uses certain hour, its measuring parameter all can change to some extent, thereby cause Instrument measuring precision to descend and even measure mistake, above-mentioned situation appears and after conventional way need to look after and guide again instrument (mainly being the measuring parameter of adjustment instrument) exactly, just can avoid measuring error to take place.
In addition, the permanganate index Water Test Kits need be calibrated zero point (with distilled water as detected water sample to carry out zero point correction) or measure the situation of small concentration water sample.Because the water sample cleanliness under these 2 kinds of measurement situations are very high, when the phase one, water sample is very little to the consumption of potassium permanganate, can consume few potassium permanganate during phase III titration in the end, and namely titration end-point occurs very early.After when if the permanganate index Water Test Kits is long-time, the measuring parameter of potassium permanganate volume pump is inaccurate, the potassium permanganate metering of phase one adding is inaccurate so (for example sets the potassium permanganate volume pump and adds the 10mL liquor potassic permanganate, and in fact the potassium permanganate volume pump pumps into the 12mL liquor potassic permanganate), and the sodium oxalate solution of subordinate phase still pumps into 10mL, be exactly titration end-point after will causing the phase III to splash into one, and in fact because the liquor potassic permanganate of phase one adding excess, phase III also not titration just more than the titration end-point decision condition, finally cause alignment error, and measure mistake.
In addition, perhaps because liquor potassic permanganate reagent configuration inaccurate (it is a lot of that reagent disposes inaccurate reason, here no longer described in detail), for example liquor potassic permanganate concentration is higher, when calibrating zero point, even the potassium permanganate that the phase one adds metering is out of question, the just situation more than the titration end-point decision condition of not titration also can appear also during its titration phase III, equally finally can cause alignment error.
Summary of the invention
Therefore, the present invention is directed to above-mentioned problem, a kind of measuring parameter modification method of permanganate index Water Test Kits is proposed, the measuring parameter of the potassium permanganate volume pump of correct permanganate index Water Test Kits is set automatically, guarantees that instrument is in normally (non-metering error) measurement state.Also can adapt to simultaneously the reagent concentration configuration and occur under the situation of deviation, guarantee that instrument can be through behind the zero point correction accurately, at normal (non-metering error) measurement state.
The present invention adopts following technical scheme:
The measuring parameter modification method of permanganate index Water Test Kits comprises step:
A. the permanganate index Water Test Kits add by volume pump pure water sample, second standardization equivalent of first standardization equivalent sulfuric acid solution, 20%-80% the 3rd standardization equivalent liquor potassic permanganate and by temperature control member heated constant temperature certain hour;
B. the permanganate index Water Test Kits adds the sodium oxalate solution of 105% 3rd standardization equivalent by volume pump;
C. the permanganate index Water Test Kits carries out the liquor potassic permanganate titration extremely to titration end-point by volume pump, and the accumulation titrimeter value of record liquor potassic permanganate;
D. the variable of the liquor potassic permanganate that adds in the steps A is added that variable that the summation of the accumulation titrimeter value of liquor potassic permanganate among the step C deducts 5% 3rd standardization equivalent value again is the standardization equivalent of the liquor potassic permanganate revised, and with the standardization equivalent of this liquor potassic permanganate of revising the liquor potassic permanganate volume pump of permanganate index Water Test Kits is carried out the measuring parameter correction.
Preferably, the permanganate index Water Test Kits adds the liquor potassic permanganate of 60% 3rd standardization equivalent in the steps A by volume pump.
The measuring parameter modification method of permanganate index Water Test Kits of the present invention is exactly to add in the phase one and lacks than standardization equivalent that (addition is the 20%-80% of standardization equivalent, preferably 60%) liquor potassic permanganate, with the sodium oxalate solution that adds in subordinate phase a little more than standardization equivalent (addition be standardization equivalent 105%), can guarantee not can be because of metering before the instrument correction inaccurate or the configuration of liquor potassic permanganate reagent is inaccurate and cause can't really judging titration end-point in the phase III like this.And according to not consuming potassium permanganate in the pure water sample, then potassium permanganate is that identical equivalent carries out complete reaction with sodium oxalate, just can utilize the volume pump of the sodium oxalate of accurate measurement for the benchmark measuring parameter measuring parameter of the volume pump of potassium permanganate to be revised.Like this, measuring parameter modification method by permanganate index Water Test Kits of the present invention, can come to arrange automatically the measuring parameter of the potassium permanganate volume pump of correct permanganate index Water Test Kits, guarantee that instrument is in normally (non-metering error) measurement state, and need not to carry out existing troublesome operation---need look after and guide instrument (mainly being the measuring parameter of adjustment instrument) again.Also can adapt to simultaneously the reagent concentration configuration and occur under the situation of deviation, guarantee that instrument can be through behind the zero point correction accurately, at normal (non-metering error) measurement state (through experiment, can adapt to the reagent concentration deviation in≤± 30% situation).
The present invention has the following advantages than prior art:
(1) can revise the measuring parameter of pump automatically, need not instrument is debugged again, simple fast;
(2) can adapt to the calibration that reagent configuration concentration deviation causes and measure undesiredly, reduce reagent configuration difficulty;
(3) also can be used in the debugging of instrument in the production run, increase work efficiency.
Embodiment
Now the present invention is further described in conjunction with embodiment.
At first to the explanation that makes an explanation of several nouns and term:
Pure water sample, sulfuric acid solution, liquor potassic permanganate or the sodium oxalate solution of standardization equivalent refers to according to adding the fixed amount of regulation, the solution of fixed concentration in the testing standard of the permanganate index Water Test Kits of different model.
When pure water sample refers to carry out the measuring parameter correction or calibrates zero point, do not contain reducing inorganic thing such as nitrite in the water, ferrous salt, sulfide and organism that with this understanding can be oxidized in the water that adds, can not consume potassium permanganate, namely the permanganate index of pure water sample is 0.
Volume pump refers to carry out solution the pump of volume metering and conveying, can be the metering method of pulse measurement formula, time measurement formula or other modes.
The measuring parameter correction refers to the metering method difference according to volume pump, adjusts its parameter to meet the established standards equivalent of expectation, as the number of pulses of passing through to adjust the pulse measurement pump, the timing length of passing through adjustment time measurement pump etc.
Below, for convenience of description, be that standardization equivalent describes with the pure water sample of adding 100mL, the sulfuric acid solution of 10mL normal concentration, the liquor potassic permanganate of 10mL normal concentration, the sodium oxalate solution of 10mL normal concentration.Adopt the realization principle of standardization equivalent of the solution of other capacity not give unnecessary details one by one with reference to this.
The measuring parameter modification method of the permanganate index Water Test Kits of present embodiment comprises step:
A. the permanganate index Water Test Kits add by volume pump pure water sample, the 10mL of 100mL sulfuric acid solution, 6mL liquor potassic permanganate and by temperature control member heated constant temperature certain hour.The permanganate index Water Test Kits of present embodiment is constant temperature after being heated to 97 ℃ 30 minutes;
This steps A stage has only added the liquor potassic permanganate of theoretical value 60% standardization equivalent, is to guarantee that sodium oxalate is excessive after guaranteeing to add sodium oxalate among the later step B, and then guarantees the correct judgement of last titration end-point.Like this, this stage has only added the potassium permanganate of 6mL, even because the volume pump of potassium permanganate error occurs because of the metering after using for a long time, actual addition has larger difference, as error+20%, namely set to add 6mL and be actually and added 7.2mL, but addition also can not surpass the same amount of 10mL potassium permanganate standard reagent.Same, this has also determined the accommodation to reagent configuration deviation, namely during concentration error 30%, even accurate measurement, the nonstandard solution that adds 6mL potassium permanganate but is equivalent to add the potassium permanganate mark liquid of 7.8mL, and addition also can not surpass the same amount of 10mL potassium permanganate standard reagent.Although probability is very low, even but the concentration error of liquor potassic permanganate 30% is again simultaneously during the error in dipping 20% of potassium permanganate volume pump, the nonstandard solution that adds 6mL potassium permanganate but is equivalent to add the potassium permanganate mark liquid of 9.36mL, and addition also can not surpass the same amount of 10mL potassium permanganate standard reagent;
B. the permanganate index Water Test Kits adds the sodium oxalate solution of 10.5mL by volume pump;
This step B stage, we added the 10.5mL sodium oxalate solution, reason is: when the concentration error of liquor potassic permanganate error in dipping very little and the potassium permanganate volume pump is very little, the sodium oxalate of 10mL and the potassium permanganate of 10mL are equivalents, when not having reducing substances in the pure water sample (test distilled water), be the steps A stage not have potassium permanganate consumption, the sodium oxalate that adds equivalent so in this step B stage, the just neutralization fully of this moment sodium oxalate and potassium permanganate then can't be carried out titration and the titration end-point in step C stage and judge;
In addition, the permanganate index Water Test Kits is in real work, the reagent configuration, the measuring accuracy of instrument etc. can not be not have error fully, even the existence of this error makes that control equivalent adds sodium oxalate and potassium permanganate when measuring distilled water, also can not reach potassium permanganate and sodium oxalate equivalent.Therefore we add excessive a little sodium oxalate in subordinate phase, and sodium oxalate is excessive when finishing with the assurance subordinate phase, to reach the judgement of phase III titration and titration end-point.We adopt pure water sample to calibrate zero point simultaneously, the mark liquid of 10mg/L is proofreaied and correct the method for range, the error that elimination brings measurement result because of systematic errors such as reagent deviation, measurement deviations, the potassium permanganate consumption of actual water sample beasurement base potassium permanganate consumption at zero point and 10mg/L mark liquid, the linear measurement result of calculating.Simultaneously, can not add too much sodium oxalate in subordinate phase and guarantee that sodium oxalate is excessive, because maximum variable is (we am limited to 12mL) that is limited in the last titration process, be much to seek titration end-point explanation water sample concentration and exceeded measurement range if reach maximum titration limit value, continuing to drip does not have practical significance again.Therefore should design titrimeter value at zero point be best at 0.2-2mL, too small then titration end-point be judged inaccurate, the excessive measurement range that then influences instrument;
C. the permanganate index Water Test Kits carries out the liquor potassic permanganate titration extremely to titration end-point by volume pump, and the accumulation titrimeter value of record liquor potassic permanganate;
The titration end-point in this step C stage is judged can adopt optical method or ORP electrode method etc.Because the cause that the liquor potassic permanganate in steps A stage and step B stage and sodium oxalate solution addition change, what the accumulation titrimeter value at the zero point that obtain this moment can be original relatively is bigger, but can guarantee the correct titration end-point that obtains;
D. the variable of the liquor potassic permanganate that adds in the steps A is added that variable that the summation of the accumulation titrimeter value of liquor potassic permanganate among the step C deducts 5% 3rd standardization equivalent value again is the standardization equivalent of the liquor potassic permanganate revised, and with the standardization equivalent of this liquor potassic permanganate of revising the liquor potassic permanganate volume pump of permanganate index Water Test Kits is carried out the measuring parameter correction;
The measuring parameter correction in this step D stage just is equivalent to adopt accurately, and sodium oxalate is the benchmark measuring parameter, finally revise inaccurate potassium permanganate measuring parameter, realize arranging automatically the measuring parameter of the potassium permanganate volume pump of correct permanganate index Water Test Kits, guarantee that instrument is in normally (non-metering error) measurement state.
To sum up, the permanganate index Water Test Kits is by the pump measuring parameter of above method correction, can reach desirable school zero result, with school mark result, if this method of alignment error that causes because of the reagent error also is suitable for simultaneously, for example potassium permanganate concentration is higher, then because the amount of the potassium permanganate of phase one adding is less, at last also can reach correct titration process, potassium permanganate concentration is on the low side, also can find titration end-point at last before reaching the maximum titration value of 12mL.Through experiment, can adapt to the reagent concentration deviation in≤± 30% situation.
Although specifically show and introduced the present invention in conjunction with preferred embodiment; but the those skilled in the art should be understood that; in not breaking away from the spirit and scope of the present invention that appended claims limits; can make a variety of changes the present invention in the form and details, be protection scope of the present invention.
Claims (2)
1. the measuring parameter modification method of permanganate index Water Test Kits is characterized in that, comprises step:
A. the permanganate index Water Test Kits add by volume pump pure water sample, second standardization equivalent of first standardization equivalent sulfuric acid solution, 20%-80% the 3rd standardization equivalent liquor potassic permanganate and by temperature control member heated constant temperature certain hour;
B. the permanganate index Water Test Kits adds the sodium oxalate solution of 105% 3rd standardization equivalent by volume pump;
C. the permanganate index Water Test Kits carries out the liquor potassic permanganate titration extremely to titration end-point by volume pump, and the accumulation titrimeter value of record liquor potassic permanganate;
D. the variable of the liquor potassic permanganate that adds in the steps A is added that variable that the summation of the accumulation titrimeter value of liquor potassic permanganate among the step C deducts 5% 3rd standardization equivalent value again is the standardization equivalent of the liquor potassic permanganate revised, and with the standardization equivalent of this liquor potassic permanganate of revising the liquor potassic permanganate volume pump of permanganate index Water Test Kits is carried out the measuring parameter correction.
2. the measuring parameter modification method of permanganate index Water Test Kits according to claim 1, it is characterized in that: the permanganate index Water Test Kits adds the liquor potassic permanganate of 60% 3rd standardization equivalent in the steps A by volume pump.
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| CN104049058B (en) * | 2014-06-11 | 2015-08-19 | 江阴市纤维检验所 | A kind of eider down oxygen utilization high precision measurement method |
| DE102019135486A1 (en) * | 2019-12-20 | 2021-06-24 | Endress+Hauser Conducta Gmbh+Co. Kg | Method for operating an analyzer for determining the permanganate index and an analyzer |
| CN111024888B (en) * | 2019-12-27 | 2022-07-12 | 杭州绿洁环境科技股份有限公司 | Method for testing permanganate index |
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