CN108982382A - A kind of calibration method of online total chromium analysis instrument - Google Patents
A kind of calibration method of online total chromium analysis instrument Download PDFInfo
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- CN108982382A CN108982382A CN201810782215.1A CN201810782215A CN108982382A CN 108982382 A CN108982382 A CN 108982382A CN 201810782215 A CN201810782215 A CN 201810782215A CN 108982382 A CN108982382 A CN 108982382A
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Abstract
The present invention relates to a kind of calibration methods of online total chromium analysis instrument, and the calibration method is the following steps are included: (1) carries out the preparations such as the connection of calibrating installation；(2) host computer calculates the amount of the amount and dilution that obtain standard solution mother liquor；(3) second control modules control the second syringe pump and draw dilution from dilution bottle and inject solution mixing arrangement, and the first control module controls the first syringe pump and standard solution mother liquor is injected solution mixing arrangement；Circuit control unit control magnetic stirrer is stirred；(4) computer sends sampling instruction and the analysis information of water quality is uploaded to host computer to online total chromium analysis instrument, online total chromium analysis instrument is detected；(5) host computer carries out analysis detection to online total chromium analysis instrument and calibrates automatically.The calibration method of online total chromium analysis instrument of the invention can realize that the specific aim of online total chromium analysis instrument is calibrated and the correction of constant error automatically.
Description
Technical field
The present invention relates to calibration method, in particular to a kind of calibration method of online total chromium analysis instrument.
Background technique
Chromium in waste water is mainly with trivalent chromium (Cr3+) and Cr VI (CrO4 2-,Cr2O7 2-) two kinds of forms exist, total chromium
Refer to the summation of the chromium of all existence forms.It is the important indicator for evaluating organic substance relative amount in water body, it is mainly used for
The environmental monitoring in the fields such as petroleum, chemical industry, plating.
Total chromium automatic water quality monitoring instrument can be roughly divided into two classes by technical principle, and one kind has plenty of for spectrophotometric, another
Class is electrochemical principle.The wherein principle of spectrophotometry: in acidic dissolution medium, at certain temperature and pressure, sample
The chromium of middle different valence state and form is oxidized to Cr VI.Hexavalent chromium is reacted with diphenylcarbazide (DPC) generates aubergine
Complex compound carries out spectrophotometry at wavelength 540nm, by the measurement to absorbance, can obtain indirectly total in water sample
The content of chromium.Above-mentioned steps are imported by on-line computing model automatic control completion water sample, water sample is cleared up in advance and concentration calculation overall process,
The robot that total chromium monitors is realized from face.
In recent years, the technology for measuring total chromium achieves good development, and the analysis method for total Chromium in Waste also obtains
Very rapidly development.In water the measuring method of total chromium mainly have potassium permanganate oxidation-diphenyl carbazide spectrophotometry,
Atomic absorption spectrophotometry and ferrous ammonium sulfate titration etc..Total chromium analysis instrument online at present, generally uses permanganic acid
Potassium oxidation-hexichol phosphinylidyne is divided two hydrazine photometries and measures total chromium.It factually tests, total chromium in the measurement water body of online total chromium analysis instrument
The correctness of the concentration value of pollutant is by the accuracy of instrument itself, span drift, null offset, precision, linearity, average
The influence of the performance indicators such as non-failure operation time.Therefore it is most important reliably, uniformly to evaluate the instrument performance.
The accuracy and safety that the performance evaluation conclusion of online always chromium analysis instrument can allow research staff to become more apparent upon its instrument
Property avoids caused by defect and misalignment because of instrument to enterprises' loss and environmental injury.Therefore the research of this project is online total chromium point
The magnitude tracing of analyzer provides reliable technical basis.
Current each metrological service does not carry out the research of analogous instrument, and also there has been no the inspections of online total chromium analysis instrument both at home and abroad
Journey of establishing rules or calibrating standard.Meanwhile self-checking device of existing analyzer itself is there are certain constant error, and mesh
The preceding calibrating installation there is no for online total chromium analysis instrument and the correcting scheme to its constant error.
Summary of the invention
The technical problems to be solved by the present invention are: a kind of calibration method of online total chromium analysis instrument is provided, it can be achieved that
The specific aim of the total chromium analysis instrument of line is calibrated automatically and the correction of constant error.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows:
A kind of calibration method of online total chromium analysis instrument, the calibration method are based on calibrating installation and are calibrated, the school
Standard apparatus includes online total chromium analysis instrument, host computer, the first control module, the second control module, third control module, circuit control
Unit, solution mixing arrangement, the first syringe pump, the second syringe pump, peristaltic pump and magnetic stirrer processed；First syringe pump
Injection inlet and standard mother liquid multi-cavity bottle pipeline connection, the injection inlet and dilution bottle pipeline connection of second syringe pump are described
Respectively with the inlet pipeline connection of solution mixing arrangement, the solution is mixed for the injection outlet of first syringe pump and the second syringe pump
Attach together the sample tap pipeline connection of the liquid outlet set and online total chromium analysis instrument, the solution mixing arrangement it is another go out
Liquid mouth and peristaltic pump pipeline connection, the stirring parts of the magnetic stirrer protrude into solution mixing arrangement；
The first control signal that first control module is used to be issued according to host computer control the first syringe pump draw with
Push operation, first syringe pump is for drawing standard mother liquid multi-cavity bottle according to first control signal, liquid root after absorption
It is pushed in solution mixing arrangement according to first control signal；The second control that second control module is used to be issued according to host computer
Signal processed controls the absorption of the second syringe pump and push operation, and second syringe pump is used for according to second control signal to dilution
Bottle is drawn, and liquid is pushed in solution mixing arrangement according to second control signal after absorption；The third control module is used
Solution mixing arrangement is aspirated in the third control signal control peristaltic pump issued according to host computer；The circuit control list
Fourth control signal control magnetic stirrer of the member for being issued according to host computer is stirred；Online total chromium analysis instrument is used
It is detected in the liquid come in from sample tap, and will test result and be uploaded to host computer；The host computer is used for first
Control module, the second control module, third control module and circuit control unit issue first control signal, the second control letter
Number, third control signal and the 4th control signal；The host computer is used to receive the detection knot of online total chromium analysis instrument simultaneously
Fruit, and the judgement result of online total chromium analysis instrument is obtained with national standard according to testing result；
The calibration method the following steps are included:
(1) testing staff will be detected the communication port of host computer in the online always PORT COM and calibrating installation of chromium analysis instrument
Connection passes through the liquid outlet for being detected the sample tap and the solution mixing arrangement of sampling system in online total chromium analysis instrument
Pipeline is attached；The injection inlet pipeline of standard mother liquid multi-cavity bottle and first syringe pump equipped with standard solution mother liquor is connected
It is logical；By the injection inlet pipeline connection of dilution bottle and second syringe pump equipped with dilution；By standard solution mother liquor
Solution concentration after concentration and dilution is input to host computer；
(2) host computer calculates according to the solution concentration after the concentration and dilution of standard solution mother liquor and obtains standard solution mother liquor
Amount and dilution amount, and then obtain the first syringe pump amount of feed and the second syringe pump amount of feed；Host computer is according to the first note
It penetrates pump amount of feed and issues first control signal to the first control module, host computer is controlled according to the second syringe pump amount of feed to second
Module issues second control signal, and host computer issues the 4th control signal to circuit control unit；
(3) second control modules control the second syringe pump according to second control signal and first draw dilution simultaneously from dilution bottle
Dilution is injected into solution mixing arrangement, dilution injects after solution mixing arrangement, and the first control module is according to the first control
Signal controls the first syringe pump and draws standard solution mother liquor from standard mother liquid multi-cavity bottle and standard solution mother liquor injection solution is mixed dress
It sets, and standard solution mother liquor has at least injected when dilution injection is completed；Circuit control unit is according to the 4th control signal
The stirring parts for controlling the magnetic stirrer are stirred driving, and then are stirred to the liquid in solution mixing arrangement；
(4) computer sends sampling instruction to online total chromium analysis instrument is detected, and is detected online total chromium analysis instrument and receives
Sampling operation is carried out to the solution in solution mixing arrangement by sample tap after instruction, is detected online total chromium analysis instrument for water quality
Analysis information be uploaded to host computer；
(5) host computer is according to the analysis information for being detected online total chromium analysis instrument, to be detected online total chromium analysis instrument into
Row analysis detection is simultaneously calibrated automatically；
The concentration value of solution in the solution mixing arrangement are as follows: the target concentration value * of solution in the solution mixing arrangement
Correction factor；
The correction factor are as follows: (first control signal controls the first syringe pump and draws standard solution mother from standard mother liquid multi-cavity bottle
The bulking value of liquid+second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle)/{ the first control
Signal controls bulking value+control letter of (0.48-0.66) * the second that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Number control the second syringe pump from dilution bottle draw dilution bulking value.
The beneficial effects of the present invention are:
The calibration method of online total chromium analysis instrument of the invention, first design include online total chromium analysis instrument, host computer, the
One control module, the second control module, third control module, circuit control unit, solution mixing arrangement, the first syringe pump,
The calibrating installation of two syringe pumps, peristaltic pump and magnetic stirrer designs above-mentioned five calibration steps, first may be used on this basis
To realize the Full-automatic calibration operation of online total chromium analysis instrument, second, for total chromium analysis, the above-mentioned correction of targeted design because
Son, it is known that the target concentration value of solution in solution mixing arrangement can know that the concentration value of solution in solution mixing arrangement is (i.e. real
Border concentration value), and then correct the constant error of online total chromium analysis instrument.
Detailed description of the invention
Fig. 1 is the entity structure connection schematic diagram of the calibrating installation of the embodiment of the present invention.
Label declaration
1, online total chromium analysis instrument；2, solution mixing arrangement；3, the first syringe pump；31, standard mother liquid multi-cavity bottle；4, the second injection
Pump；41, dilution bottle；5, peristaltic pump；6, magnetic stirrer；61, stirring parts；
62, mixing part.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, below in conjunction with embodiment and cooperate attached
Figure is explained.
The most critical design of the present invention is: step and school in the calibration method of the above-mentioned online total chromium analysis instrument of design
Positive divisor.
Fig. 1, a kind of calibration method of online total chromium analysis instrument are please referred to, the calibration method is based on calibrating installation and carries out school
Standard, the calibrating installation include online total chromium analysis instrument 1, host computer, the first control module, the second control module, third control
Module, circuit control unit, solution mixing arrangement 2, the first syringe pump 3, the second syringe pump 4, peristaltic pump 5 and magnetic stirrer 6；
The injection inlet of first syringe pump 3 and 31 pipeline connection of standard mother liquid multi-cavity bottle, the injection inlet of second syringe pump 4 with it is dilute
Release 41 pipeline connection of liquid bottle, the injection outlet of first syringe pump 3 and the second syringe pump 4 respectively with solution mixing arrangement 2
The sample tap pipeline of inlet pipeline connection, a liquid outlet of the solution mixing arrangement 2 and online total chromium analysis instrument 1 connects
Logical, another liquid outlet and 5 pipeline connection of peristaltic pump of the solution mixing arrangement 2, the stirring parts 61 of the magnetic stirrer 6 are stretched
Enter in solution mixing arrangement 2；
The first control signal that first control module is used to be issued according to host computer control the first syringe pump 3 draw with
Push operation, first syringe pump 3 is for drawing standard mother liquid multi-cavity bottle 31 according to first control signal, liquid after absorption
It is pushed in solution mixing arrangement 2 according to first control signal；Second control module be used to be issued according to host computer the
Two control signals control the absorption of the second syringe pump 4 and push operation, and second syringe pump 4 is used for according to second control signal pair
Dilution bottle 41 is drawn, and liquid is pushed in solution mixing arrangement 2 according to second control signal after absorption；The third control
The third control signal control peristaltic pump 5 that molding block is used to be issued according to host computer aspirates solution mixing arrangement 2；It is described
The 4th control signal control magnetic stirrer 6 that circuit control unit is used to be issued according to host computer is stirred；It is described online
Total chromium analysis instrument 1 is used to detect the liquid come in from sample tap, and will test result and be uploaded to host computer；It is described upper
Machine, which is used to issue the first control module, the second control module, third control module and circuit control unit the first control, to be believed
Number, second control signal, third control signal and the 4th control signal；The host computer is for receiving online total chromium point simultaneously
The testing result of analyzer 1, and the judgement result of online total chromium analysis instrument 1 is obtained with national standard according to testing result；
The calibration method the following steps are included:
(1) testing staff will be detected the communication port of host computer in the online always PORT COM and calibrating installation of chromium analysis instrument
Connection passes through the liquid outlet for being detected the sample tap and the solution mixing arrangement of sampling system in online total chromium analysis instrument
Pipeline is attached；The injection inlet pipeline of standard mother liquid multi-cavity bottle and first syringe pump equipped with standard solution mother liquor is connected
It is logical；By the injection inlet pipeline connection of dilution bottle and second syringe pump equipped with dilution；By standard solution mother liquor
Solution concentration after concentration and dilution is input to host computer；
(2) host computer calculates according to the solution concentration after the concentration and dilution of standard solution mother liquor and obtains standard solution mother liquor
Amount and dilution amount, and then obtain the first syringe pump amount of feed and the second syringe pump amount of feed；Host computer is according to the first note
It penetrates pump amount of feed and issues first control signal to the first control module, host computer is controlled according to the second syringe pump amount of feed to second
Module issues second control signal, and host computer issues the 4th control signal to circuit control unit；
(3) second control modules control the second syringe pump according to second control signal and first draw dilution simultaneously from dilution bottle
Dilution is injected into solution mixing arrangement, dilution injects after solution mixing arrangement, and the first control module is according to the first control
Signal controls the first syringe pump and draws standard solution mother liquor from standard mother liquid multi-cavity bottle and standard solution mother liquor injection solution is mixed dress
It sets, and standard solution mother liquor has at least injected when dilution injection is completed；Circuit control unit is according to the 4th control signal
The stirring parts for controlling the magnetic stirrer are stirred driving, and then are stirred to the liquid in solution mixing arrangement；
(4) computer sends sampling instruction to online total chromium analysis instrument is detected, and is detected online total chromium analysis instrument and receives
Sampling operation is carried out to the solution in solution mixing arrangement by sample tap after instruction, is detected online total chromium analysis instrument for water quality
Analysis information be uploaded to host computer；
(5) host computer is according to the analysis information for being detected online total chromium analysis instrument, to be detected online total chromium analysis instrument into
Row analysis detection is simultaneously calibrated automatically；
The concentration value of solution in the solution mixing arrangement are as follows: the target concentration value * of solution in the solution mixing arrangement
Correction factor；
The correction factor are as follows: (first control signal controls the first syringe pump and draws standard solution mother from standard mother liquid multi-cavity bottle
The bulking value of liquid+second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle)/{ the first control
Signal controls bulking value+control letter of (0.48-0.66) * the second that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Number control the second syringe pump from dilution bottle draw dilution bulking value.
As can be seen from the above description, the beneficial effects of the present invention are:
The calibration method of online total chromium analysis instrument of the invention, first design include online total chromium analysis instrument, host computer, the
One control module, the second control module, third control module, circuit control unit, solution mixing arrangement, the first syringe pump,
The calibrating installation of two syringe pumps, peristaltic pump and magnetic stirrer designs above-mentioned five calibration steps, first may be used on this basis
To realize the Full-automatic calibration operation of online total chromium analysis instrument, second, for total chromium analysis, the above-mentioned correction of targeted design because
Son, it is known that the target concentration value of solution in solution mixing arrangement can know that the concentration value of solution in solution mixing arrangement is (i.e. real
Border concentration value), and then correct the constant error of online total chromium analysis instrument.
Further, the automatic calibration includes the error of indication, null offset and stability of display's analysis work.
Further, the correction factor are as follows: (first control signal controls the first syringe pump and draws mark from standard mother liquid multi-cavity bottle
The bulking value of quasi- solution mother liquor+second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle)/
{ first control signal controls bulking value+(0.53-0.58) * that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle }.
Further, the correction factor are as follows: (first control signal controls the first syringe pump and draws mark from standard mother liquid multi-cavity bottle
The bulking value of quasi- solution mother liquor+second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle)/
{ first control signal controls bulking value+(0.56-0.62) * that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle }.
Further, the correction factor are as follows: (first control signal controls the first syringe pump and draws mark from standard mother liquid multi-cavity bottle
The bulking value of quasi- solution mother liquor+second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle)/
{ first control signal controls the first syringe pump and controls from the bulking value+0.57* second that standard mother liquid multi-cavity bottle draws standard solution mother liquor
Signal controls the bulking value that the second syringe pump draws dilution from dilution bottle }.
Further, the stirring parts protrude into the end in solution mixing arrangement and are equipped at least three mixing parts, described to stir
It mixes portion and stirring parts is integrally formed and is arranged, the mixing part is 8 font structures.
Please refer to Fig. 1, the embodiment of the present invention one are as follows:
The calibration method of online total chromium analysis instrument of the present embodiment, the calibration method are based on calibrating installation and are calibrated,
The calibrating installation includes online total chromium analysis instrument 1, host computer, the first control module, the second control module, third control mould
Block, circuit control unit, solution mixing arrangement 2, the first syringe pump 3, the second syringe pump 4, peristaltic pump 5 and magnetic stirrer 6；Institute
State injection inlet and 31 pipeline connection of standard mother liquid multi-cavity bottle, the injection inlet of second syringe pump 4 and the dilution of the first syringe pump 3
The injection outlet of 41 pipeline connection of liquid bottle, first syringe pump 3 and the second syringe pump 4 respectively with solution mixing arrangement 2 into
The sample tap pipeline of liquid mouth pipeline connection, a liquid outlet of the solution mixing arrangement 2 and online total chromium analysis instrument 1 connects
Logical, another liquid outlet and 5 pipeline connection of peristaltic pump of the solution mixing arrangement 2, the stirring parts 61 of the magnetic stirrer 6 are stretched
Enter in solution mixing arrangement 2；
The first control signal that first control module is used to be issued according to host computer control the first syringe pump 3 draw with
Push operation, first syringe pump 3 is for drawing standard mother liquid multi-cavity bottle 31 according to first control signal, liquid after absorption
It is pushed in solution mixing arrangement 2 according to first control signal；Second control module be used to be issued according to host computer the
Two control signals control the absorption of the second syringe pump 4 and push operation, and second syringe pump 4 is used for according to second control signal pair
Dilution bottle 41 is drawn, and liquid is pushed in solution mixing arrangement 2 according to second control signal after absorption；The third control
The third control signal control peristaltic pump 5 that molding block is used to be issued according to host computer aspirates solution mixing arrangement 2；It is described
The 4th control signal control magnetic stirrer 6 that circuit control unit is used to be issued according to host computer is stirred；It is described online
Total chromium analysis instrument 1 is used to detect the liquid come in from sample tap, and will test result and be uploaded to host computer；It is described upper
Machine, which is used to issue the first control module, the second control module, third control module and circuit control unit the first control, to be believed
Number, second control signal, third control signal and the 4th control signal；The host computer is for receiving online total chromium point simultaneously
The testing result of analyzer 1, and the judgement result of online total chromium analysis instrument 1 is obtained with national standard according to testing result；
The calibration method the following steps are included:
(1) testing staff will be detected the communication port of host computer in the online always PORT COM and calibrating installation of chromium analysis instrument
Connection passes through the liquid outlet for being detected the sample tap and the solution mixing arrangement of sampling system in online total chromium analysis instrument
Pipeline is attached；The injection inlet pipeline of standard mother liquid multi-cavity bottle and first syringe pump equipped with standard solution mother liquor is connected
It is logical；By the injection inlet pipeline connection of dilution bottle and second syringe pump equipped with dilution；By standard solution mother liquor
Solution concentration after concentration and dilution is input to host computer；
(2) host computer calculates according to the solution concentration after the concentration and dilution of standard solution mother liquor and obtains standard solution mother liquor
Amount and dilution amount, and then obtain the first syringe pump amount of feed and the second syringe pump amount of feed；Host computer is according to the first note
It penetrates pump amount of feed and issues first control signal to the first control module, host computer is controlled according to the second syringe pump amount of feed to second
Module issues second control signal, and host computer issues the 4th control signal to circuit control unit；
(3) second control modules control the second syringe pump according to second control signal and first draw dilution simultaneously from dilution bottle
Dilution is injected into solution mixing arrangement, dilution injects after solution mixing arrangement, and the first control module is according to the first control
Signal controls the first syringe pump and draws standard solution mother liquor from standard mother liquid multi-cavity bottle and standard solution mother liquor injection solution is mixed dress
It sets, and standard solution mother liquor has at least injected when dilution injection is completed；Circuit control unit is according to the 4th control signal
The stirring parts for controlling the magnetic stirrer are stirred driving, and then are stirred to the liquid in solution mixing arrangement；
(4) computer sends sampling instruction to online total chromium analysis instrument is detected, and is detected online total chromium analysis instrument and receives
Sampling operation is carried out to the solution in solution mixing arrangement by sample tap after instruction, is detected online total chromium analysis instrument for water quality
Analysis information be uploaded to host computer；
(5) host computer is according to the analysis information for being detected online total chromium analysis instrument, to be detected online total chromium analysis instrument into
Row analysis detection is simultaneously calibrated automatically；
The concentration value of solution in the solution mixing arrangement are as follows: the target concentration value * of solution in the solution mixing arrangement
Correction factor；
The correction factor are as follows: (first control signal controls the first syringe pump and draws standard solution mother from standard mother liquid multi-cavity bottle
The bulking value of liquid+second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle)/{ the first control
Signal controls the bulking value+0.65* second control signal control that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Second syringe pump draws the bulking value of dilution from dilution bottle }.
The automatic calibration include the error of indication, null offset and stability of display analysis work, specifically, to it is above-mentioned
The performance requirement of the calibrating installation of the total chromium analysis instrument of line is as follows:
1 A quasi-instrument
The 1.1 temperature errors of indication
In normal work, the temperature error of indication should be no more than 10 DEG C of scholar to instrument.
1.2 thermal field uniformities
The thermal field uniformity of instrument should be not more than 3 DEG C.
1.3 the error of indication
Under prescribed conditions, instrument indication error should be no more than ± 5%
1.4 repeated
Under prescribed conditions, measurement reproducibility should be not more than 3%
1.5 stability
Instrument TCr value in 20min changes not in 5mg/L.
2 generic specifications
2.1 appearance
Instrument should have following mark: instrument title, model, factory number, the name of manufacturer, the date of production, mark, work electricity
Pressure and frequency etc., instrument appearance is without the damage for influencing to work normally.
2.2 security performance
The insulation resistance of instrument is not less than 20M Ω
The control of 3 measurement instruments
Measurement instrument control includes: to examine in calibrating for the first time, subsequent calibrating and use.
3.1 test condition
3.1.1 equipment is used in calibrating
3.1.1.1 thermometer: 100~200 DEG C of measurement range (0.5 DEG C of grade).
3.1.1.2 100.0mg/L Cr VI Standard Reserving Solution
3.1.1.3 stability correcting fluid is diluted to 1.0mg/L with Cr VI Standard Reserving Solution (5.1.1.2), and 4.0mg/L is dense
Degree.
3.1.1.4 electronic stopclock.
3.1.1.5 insulation resistance meter: 500V, 10 grades.
3.1.2 environmental condition
3.1.2.1 5~35 DEG C of environment temperature
3.1.2.2 relative humidity is not more than 85%.
3.1.2.3 the interference of electromagnetic field and vibration of instrument normal work are not influenced.
3.2 calibrating projects are as shown in table 1.
Table 1
3.3 calibration method
3.3.1 appearance and custom requirements
It is carried out with visual means.
3.3.2 the power inleting terminal and casing of people's instrument are connect with insulation resistance meter, are opened instrument switch and are measured insulation resistance.
3.3.3 A quasi-instrument calibration method
3.3.3.1 the temperature error of indication and thermal field uniformity
It after digestion furnace preheats 1h, is uniformly distributed and chooses 6 resolution holes, thermometer is inserted to people respectively and is cleared up in hole, to temperature
After stabilization, interval 1min reads a number and reads 3 times altogether, seeks its arithmetic mean of instantaneous value Ti.Temperature indicating value is asked to miss by formula (1), formula (1)
Difference (△T) and thermal field uniformity (W).
In formula: T0The set temperature of-digestion furnace, DEG C；
The mean temperature of-resolution firehole, DEG C；
Ti3 reading temperature averages of the-the i-th firehole, DEG C；
N-measurement firehole number.
W=Tmax-Tmin (3)
In formula: TmaxThe temperature indicating value of-temperature highest firehole, DEG C；
TminThe temperature indicating value of the minimum firehole of-temperature, DEG C.
3.3.3.2 the digestion time error of indication
After instrument stabilizer, press instrument resolution key, start simultaneously at timing, wait clear up at the end of stop timing, solve the time,
It is repeated 3 times.Digestion time is found out with respect to the error of indication (Δ by formula (4)t)。
In formula: Δt--- digestion time is with respect to the error of indication；
x0--- digestion time setting value；
--- 3 measurement average values of digestion time.
3.3.3.3 the error of indication
After instrument stabilizer, by specification requires to measure 1.0 respectively in 0~5.0mg/L of instrument to instrument calibration,
4.0mg/L TCr solution reference material 3 times calculates the error of indication by formula (5)
In formula:--- instrument indication error；
--- 3 measurement average values；
CS--- the standard value of COD solution.
Take the error of indicationIn maximum value be instrument indication error's verification result.
3.3.3.4 repeated
After instrument stabilizer, by specification requires to measure instrument calibration respectively in 0~5.0m g/L of instrument
1.0mg/L, 4.0mg/L TCr solution reference material 6 times.Repeatability (S is calculated by formula (6)A)
In formula: SA--- repeatability；
Ci--- i-th measured value；
--- n times measure average value；
N --- pendulous frequency, here n=6.
Take repeated SAIn maximum value be instrument repeatability verification result.
3.3.3.5 stability
After instrument stabilizer, by specification requires to be transferred to measuring state, and sample cell fills distilled water, and adjustment instrument zero makes to inhale
Luminosity or TCr value are 0.000, observe 20min, primary every 2min record, by formula (7) computational stability (DA)。
DA=Amax-Amin (7)
In formula: DA--- stability；
Amax--- maximum indicating value；
Amin--- minimum indicating value.
The processing of 3.4 verification results
By the instrument of this regulatory requirements assay approval, calibration certificate is issued.Underproof instrument issues verification result notice
Book, and indicate defective item.
3.5 the re-testing periods
Re-testing periods are usually no more than 1 year.
In conclusion the calibration method of online total chromium analysis instrument provided by the invention can realize the needle of online total chromium analysis instrument
Property is calibrated automatically and the correction of constant error.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright specification and accompanying drawing content are applied directly or indirectly in relevant technical field, similarly include
In scope of patent protection of the invention.
Claims (6)
1. a kind of calibration method of online total chromium analysis instrument, which is characterized in that the calibration method is based on calibrating installation and carries out school
Standard, the calibrating installation include online total chromium analysis instrument, host computer, the first control module, the second control module, third control mould
Block, circuit control unit, solution mixing arrangement, the first syringe pump, the second syringe pump, peristaltic pump and magnetic stirrer；Described
The injection inlet and standard mother liquid multi-cavity bottle pipeline connection of one syringe pump, the injection inlet and dilution bottle pipeline of second syringe pump
Connection, the injection of first syringe pump and the second syringe pump export respectively with the inlet pipeline connection of solution mixing arrangement,
The sample tap pipeline connection of one liquid outlet of the solution mixing arrangement and online total chromium analysis instrument, the solution mixing dress
Another liquid outlet and peristaltic pump pipeline connection set, the stirring parts of the magnetic stirrer protrude into solution mixing arrangement；
The first control signal that first control module is used to be issued according to host computer controls the first syringe pump and draws and push
Operation, first syringe pump is for drawing standard mother liquid multi-cavity bottle according to first control signal, and liquid is according to the after absorption
One control signal is pushed in solution mixing arrangement；The second control that second control module is used to be issued according to host computer is believed
Number control the second syringe pump draw and push operation, second syringe pump be used for according to second control signal to dilution bottle into
Row is drawn, and liquid is pushed in solution mixing arrangement according to second control signal after absorption；The third control module is used for root
The third control signal control peristaltic pump issued according to host computer aspirates solution mixing arrangement；The circuit control unit is used
It is stirred in the 4th control signal control magnetic stirrer issued according to host computer；The online total chromium analysis instrument for pair
The liquid come in from sample tap is detected, and be will test result and be uploaded to host computer；The host computer is used to control first
Module, the second control module, third control module and circuit control unit issue first control signal, second control signal,
Third controls signal and the 4th control signal；The host computer is used to receive the testing result of online total chromium analysis instrument simultaneously,
And the judgement result of online total chromium analysis instrument is obtained with national standard according to testing result；
The calibration method the following steps are included:
(1) testing staff connects the communication port of host computer in the PORT COM and calibrating installation that are detected online total chromium analysis instrument
It connects, the sample tap of sampling system and a liquid outlet of the solution mixing arrangement in online total chromium analysis instrument will be detected and pass through pipe
Road is attached；By the injection inlet pipeline connection of standard mother liquid multi-cavity bottle and first syringe pump equipped with standard solution mother liquor；
By the injection inlet pipeline connection of dilution bottle and second syringe pump equipped with dilution；By the concentration of standard solution mother liquor
And the solution concentration after dilution is input to host computer；
(2) host computer calculates the amount for obtaining standard solution mother liquor according to the solution concentration after the concentration and dilution of standard solution mother liquor
With the amount of dilution, and then the first syringe pump amount of feed and the second syringe pump amount of feed are obtained；Host computer is according to the first syringe pump
Amount of feed issues first control signal to the first control module, and host computer is according to the second syringe pump amount of feed to the second control module
Second control signal is issued, host computer issues the 4th control signal to circuit control unit；
(3) second control modules first draw dilution from dilution bottle according to the second syringe pump of second control signal control and will be dilute
Liquid injection solution mixing arrangement is released, dilution injects after solution mixing arrangement, and the first control module is according to first control signal
The first syringe pump is controlled to draw standard solution mother liquor from standard mother liquid multi-cavity bottle and standard solution mother liquor is injected solution mixing arrangement, and
Standard solution mother liquor has at least injected when dilution injection is completed；Circuit control unit controls institute according to the 4th control signal
The stirring parts for stating magnetic stirrer are stirred driving, and then are stirred to the liquid in solution mixing arrangement；
(4) computer sends sampling instruction to online total chromium analysis instrument is detected, and is detected online total chromium analysis instrument and receives instruction
Sampling operation is carried out to the solution in solution mixing arrangement by sample tap afterwards, is detected online total chromium analysis instrument for point of water quality
Analysis information is uploaded to host computer；
(5) host computer divides according to the analysis information for being detected online total chromium analysis instrument online total chromium analysis instrument is detected
Analysis is detected and is calibrated automatically；
The concentration value of solution in the solution mixing arrangement are as follows: the target concentration value * correction of solution in the solution mixing arrangement
The factor；
The correction factor are as follows: (first control signal controls the first syringe pump and draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Bulking value+second control signal controls the bulking value that the second syringe pump draws dilution from dilution bottle)/{ first control signal
Control bulking value+(0.48-0.66) * second control signal control that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Make the bulking value that the second syringe pump draws dilution from dilution bottle }.
2. the calibration method of online total chromium analysis instrument according to claim 1, which is characterized in that the automatic calibration includes
The error of indication, null offset and stability of display analyze work.
3. the calibration method of online total chromium analysis instrument according to claim 1, which is characterized in that the correction factor are as follows:
(first control signal controls bulking value+second control signal that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Control the bulking value that the second syringe pump draws dilution from dilution bottle)/{ first control signal controls the first syringe pump from standard
Bulking value+(0.53-0.58) * second control signal that mother liquid multi-cavity bottle draws standard solution mother liquor controls the second syringe pump from dilution
Bottle draws the bulking value of dilution }.
4. the calibration method of online total chromium analysis instrument according to claim 1, which is characterized in that the correction factor are as follows:
(first control signal controls bulking value+second control signal that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Control the bulking value that the second syringe pump draws dilution from dilution bottle)/{ first control signal controls the first syringe pump from standard
Bulking value+(0.56-0.62) * second control signal that mother liquid multi-cavity bottle draws standard solution mother liquor controls the second syringe pump from dilution
Bottle draws the bulking value of dilution }.
5. the calibration method of online total chromium analysis instrument according to claim 1, which is characterized in that the correction factor are as follows:
(first control signal controls bulking value+second control signal that the first syringe pump draws standard solution mother liquor from standard mother liquid multi-cavity bottle
Control the bulking value that the second syringe pump draws dilution from dilution bottle)/{ first control signal controls the first syringe pump from standard
Bulking value+0.57* the second control signal that mother liquid multi-cavity bottle draws standard solution mother liquor controls the second syringe pump and draws from dilution bottle
The bulking value of dilution }.
6. the calibration method of online total chromium analysis instrument according to claim 1, which is characterized in that the stirring parts protrude into molten
End in liquid mixing arrangement is equipped at least three mixing parts, and the mixing part and stirring parts, which are integrally formed, to be arranged, the stirring
Portion is 8 font structures.
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| CN113776618A (en) * | 2021-01-29 | 2021-12-10 | 聚光科技(杭州)股份有限公司 | Device and method for self-calibration of liquid volume |
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