CN108152343A - The analytical equipment and method of a kind of hydriodic acid concentration containing iodine - Google Patents
The analytical equipment and method of a kind of hydriodic acid concentration containing iodine Download PDFInfo
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- CN108152343A CN108152343A CN201711124392.2A CN201711124392A CN108152343A CN 108152343 A CN108152343 A CN 108152343A CN 201711124392 A CN201711124392 A CN 201711124392A CN 108152343 A CN108152343 A CN 108152343A
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- G—PHYSICS
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Abstract
A kind of concentration analysis device and method of hydroiodic acid containing iodine, belong to electrochemistry and technical field of analytical chemistry.The equipment of the present invention includes computer, hydrogen ion indicator electrode, oxidation-reduction potential electrode, temperature sensor, potentiometer, measuring cell, liquid level gauge, KI dilutions storage tank, KCl electrode soaks storage tank, waste liquid tank and pump and pipeline.When measuring the feed concentration of hydroiodic acid containing iodine, the KI dilutions of feed liquid to be measured and specific factor are input in measuring cell, under the auxiliary of computer, the temperature value measured according to temperature sensor, and the voltage value that hydrogen ion indicator electrode, oxidation-reduction potential electrode measure, it can rapidly calculate the concentration of the feed liquid of hydroiodic acid containing iodine.The present invention has well solved the problems such as sampling faced during conventional determining, continuous mode is cumbersome, operation is time-consuming and can not monitor in time, it can quickly and accurately realize that container, pipeline include the measure of iodine hydroiodic acid feed concentration, are conducive to the control to associated production technique.
Description
Technical field
The present invention relates to a kind of hydroiodic acid containing iodine (i.e. hydrogen iodide-iodo- water ternary solution, HI-I2-H2O) analysis of concentration is set
Standby and method, belongs to electrochemistry and technical field of analytical chemistry.
Background technology
The feed liquid of hydroiodic acid containing iodine (i.e. hydrogen iodide-iodo- water ternary solution, HI-I2-H2O constituent analysis operation), daily
It can all be used in lab analysis, heat chemistry iodine-sulfur process hydrogen production by water decomposition technique and hydroiodic acid production technology.With heat chemistry
For iodine-sulfur process hydrogen production by water decomposition technique (abbreviation iodine-sulfur process), which reacts the hydroiodic acid of generation by Bunsen, by
In adding excessive iodine, HI-I is formd2-H2O object phases, accurately determine HI-I2-H2The concentration of each component in O, to phase
Close the research of technique or even all extremely important to the control of site technique flow.
HI-I2-H2O has stronger volatility and strong corrosivity, particularly under heating, the operating condition pressurizeed.
It well imagines, which is very difficult to manually sample, analyze in the pipeline, container of actual production line
's.Due to more than, need for HI-I2-H2O finds suitable concentration analysis.
Currently, conventional HI-I2-H2O concentration analysis is titration, is had been manually done mostly in the form of constant-current titration
Or completed using autotitrator, the concentration of HI is specifically determined with acid-base titration, and with hypo solution
Titration, i.e. iodimetric titration determine I2Concentration, HI-I can be obtained in this way2-H2Concrete component and content (remaining one in O
Component, i.e. H2The content of O can then be obtained by MaterialBalance Computation), wherein acid-base titration is generally using hydrogen ion instruction electricity
Pole (or hydrogen ion selective electrode, pH electrodes) indicates titration end-point；With iodometric titrationiodimetry titration I2When, then using redox
Potential electrode is as indicator electrode.Although titration has many advantages, such as that amount of samples is few, sampling, sample needed for it claim
Amount, sample dilution and titration operation in itself etc. a series of flows take it is longer.And due to I in material-、I2Presence, drop
The accuracy for determining method is relatively difficult to guarantee, this is because I2/I-The normal potential of oxidation-reduction pair is neither high nor low, I2It can be used as
Oxidant and reducing agent strong by restores, I-Also it can be used as reducing agent and strong by or strong oxidant aoxidizes, because
The factors such as the oxygen in the acid-base value of this material to be measured, air disturb to titration process, less reproducible.Other one
Point, titration are needed to carry out titrating solution used preparation in advance, Accurate Calibration and rationally be preserved, can obtain satisfactory
As a result.In conclusion the defects of titration generally used at present takes there are cumbersome, process, is less reproducible.
By Gibbs phase rules it is found that under the conditions of thermodynamical equilibrium, the pass between the number of components of system, the number of phases and number of degrees of freedom,
It is to be：
F=C-P+2
In formula：The number of degrees of freedom, of F- systems；The number of components of C- systems；The number of P- phases in selected system；And in formula
What " 2 " represented is pressure, temperature the two factors.
Number of degrees of freedom, F be when system be equilibrium state when, do not changing object number of phases purpose, can independently change because
The number of plain (independent variable, such as temperature, pressure, density, year).For HI-I2-H2This three compositions system of O, in normal pressure
Under,
(given pressure, pressure as usual, 1)=3 this entry value is to F=C (3 kinds of components)-P (1 phase)+1.
Number of degrees of freedom, F is 3, is shown：Other than finding out solution temperature, as long as determining HI-I2-H22 of O systems can be only
The vertical factor (i.e. independent variable) changed, all physico-chemical properties of the system are as true (naturally including its composition and concentration)
Definite value.Therefore, it can select to be relatively easy to 2 independent variables of acquisition, HI-I determined by them except collecting temperature2-
H2The concentration data of O samples.
It is pointed out in Chinese patent literature (ZL201210517847.8)：Under normal pressure and fixed temperature, HI-I2-H2O bodies
System only has 2 degree of freedom, may be selected to be relatively easy to 2 independent variables of acquisition, HI-I is determined by them2-H2O samples
Concentration data.According to principles above, Chinese patent literature (ZL201210517847.8) discloses a kind of point of hydroiodic acid containing iodine
Analysis method, tank voltage value when using density value and flowing through constant-current electrolysis-electrodialytic cell is as location parameter, in computer
HI-I to be measured is calculated under auxiliary2-H2The concentration of O.And Chinese patent literature (ZL201210518434.1) then utilizes the above method
Provide a kind of container for the hydroiodic acid containing iodine for being capable of Real time displaying feed concentration.The above method and container are using fixed temperature before
It carries, there is many limitations, HI-I to be measured2-H2O samples need accurate temperature adjustment, and reaching the temperature needed for assay method can obtain
Accurate result.In addition electrolysis-electrodialytic cell that said determination method uses is not standard device, in use due to temperature
The reasons such as variation, fatigue of materials cause electrolysis-electrodialytic cell gasket deformation, can make interpolar away from changing, and tank voltage and pole
Spacing is strongly related, and small interpolar can cause collected tank voltage that very big fluctuation occurs away from variation, final to cause very
Big evaluated error.
As previously mentioned, hydrogen ion indicator electrode, oxidation-reduction potential electrode have been used as titration measuring hydroiodic acid containing iodine
Indicator electrode during solution concentration and used, but related work person, researcher not yet recognize：Hydrogen ion indicator electrode,
Electrode potential measured by oxidation-reduction potential electrode is related to the hydrogen ion concentration of solution, integrated oxidation reduction potential respectively
Connection, be the independent variable closely related with solution concentration, they can together with temperature value, become normal pressure (or other determine pressure
Power) under determine 3 independent variables of hydroiodic acid containing iodine solution concentration.In addition, most hydrogen ions instruction of existing market supply
Electrode, oxidation-reduction potential determination of electrode are limited in scope, to HI, I2For the solution of hydroiodic acid containing iodine of excessive concentration, being can not
Directly carry out the Accurate Determining of current potential.For the system of hydroiodic acid containing iodine in iodine-sulfur process process for making hydrogen, HI, I2It is dense
Degree has exceeded the use scope of electrode commonly greater than 3mol/L, after impregnating for a long time or even can occur the damage of electrode.This
It is that electrode can not directly apply to the reason of solution concentration of hydroiodic acid containing iodine measures.
Invention content
The purpose of the present invention is to provide a kind of concentration analysis device and method of hydroiodic acid containing iodine, can be well
Solve that the sampling that faces, continuous mode during conventional determining are cumbersome, and operation takes, the problems such as can not monitoring in time, can quickly, standard
Really realize that container, pipeline include the measure of iodine hydroiodic acid feed concentration, so as to be conducive to the control to associated production technique.
Technical scheme is as follows：
A kind of concentration analysis equipment of the hydroiodic acid containing iodine, it is characterised in that：The equipment includes computer, hydrogen ion indicates
Electrode, oxidation-reduction potential electrode, temperature sensor, potentiometer, measuring cell, KI dilutions storage tank, the storage of KCl electrodes soak
Slot, waste liquid tank and pump；The pump includes feed pump to be measured, KI diluting pumps, KCl electrodes immersion liquid pump and waste drains pump；It measures
Pond is connect by feed pump to be measured and pipeline with feed liquid storage tank to be measured, conveyance conduit or the tower in process equipment；The KI is dilute
Liquid storage tank is released to connect with measuring cell by KI diluting pumps and pipeline；The KCl electrodes soak storage tank is impregnated by KCl electrodes
Liquid pump and pipeline are connect with measuring cell；The measuring cell is connect by pipeline and waste drains pump with waste liquid tank；It is equipped in measuring cell
Hydrogen ion indicator electrode, oxidation-reduction potential electrode and temperature sensor, the hydrogen ion indicator electrode and redox electricity
Position electrode is connected by conducting wire with the potentiometer；The potentiometer and temperature sensor respectively by signal wire with it is described
Computer connects.
Preferably, the temperature sensor can be free-standing sensor, can also be built in hydrogen ion indicator electrode or oxygen
Among change reduction potential electrode.
In above-mentioned technical proposal, the measuring cell, KI dilutions storage tank, feed pump to be measured, KI diluting pumps, KCl electricity
The pipeline that liquid pump, waste drains pump and connection pump are impregnated in pole carries temperature control and lagging facility.
Another feature of the present invention is：Feed pump to be measured, KI diluting pumps, KCl electrodes immersion liquid pump and the waste liquid
Pump is connect with computer by control circuit.
A further feature of the present disclosure is：Liquid level gauge is equipped in the measuring cell, the liquid level gauge is by control circuit with calculating
Machine connects.
The concentration analysis of a kind of hydroiodic acid containing iodine provided by the invention, it is characterised in that this method includes following step
Suddenly：
1) open waste drains pump, measuring cell is emptied, effluent flow into waste liquid tank, be then shut off waste drains pump, make measuring cell and
Logistics pipeline between waste liquid tank is ended；
2) feed pump to be measured is opened, by 0.1 to the 500mL feed liquid of hydroiodic acid containing iodine to be measured by feed liquid storage tank to be measured, conveying
Pipeline or tower are delivered in measuring cell, are then shut off feed pump to be measured, make feed liquid storage tank to be measured, conveyance conduit or tower and survey
Logistics pipeline between amount pond is ended；
3) KI diluting pumps are opened, KI dilutions are input to measuring cell by KI dilution storage tanks, are then shut off KI dilutions
Liquid pump is ended the logistics pipeline between KI dilutions storage tank and measuring cell；The KI diluent concentrations are 0.1 to 3mol/
L, delivered volume are 0.1 to 1000mL；
4) potentiometer measures two of solution in measuring cell by hydrogen ion indicator electrode and oxidation-reduction potential electrode respectively
Group potential value u1And u2, temperature sensor measures the temperature value t of solution in measuring cell, by two groups of potential value u1And u2And temperature
Value t sends computer to, and computer calculates the concentration of out-feed liquid using the software for calculation in being stored in and shown；
The software for calculation is calculated by following equations group：
u1=f1(t,cHI,cI2)
u2=f2(t,cHI,cI2)
Equation f1(t,cHI,cI2) it is t, cHIAnd cI2Three variables are to u1Mathematic(al) representation, f2(t,cHI,cI2) it is t, cHI
And cI2Three variables are to u2Mathematic(al) representation, c in formulaHIFor the concentration of HI in the feed liquid of hydroiodic acid containing iodine, cI2For I2Concentration, t
Temperature value for solution in measuring cell；
By two above equations simultaneousness, by t, the u measured1And u2Calculate the concentration data c of solution in measuring cellHIWith
cHI；Again by KI dilutions and the volume ratio of the original feed liquid of hydroiodic acid containing iodine to be measured, i.e. inverse goes out original hydroiodic acid containing iodine to be measured
The concentration data of feed liquid；
5) it opens waste drains pump to empty measuring cell feed liquid, the feed liquid of discharge is sent to waste liquid tank, is then shut off waste drains pump, is made survey
Logistics pipeline between amount pond and waste liquid tank is ended；
6) KI diluting pumps are opened, KI dilutions are input to measuring cell by KI dilution storage tanks, close KI diluting pumps,
Ended the logistics pipeline between KI dilutions storage tank and measuring cell；KI dilutions delivered volume is 5 to 1000mL；It opens useless
Liquid pump empties measuring cell, and the feed liquid of discharge is sent to waste liquid tank, is then shut off waste drains pump, the logistics between measuring cell and waste liquid tank
Pipeline is ended；
7) KCl electrodes are opened and impregnate liquid pump, KCl electrodes soak is input to measuring cell by KCl electrode soak storage tanks,
It closes KCl electrodes and impregnates liquid pump, the logistic pipeline between KCl electrode soak storage tanks and measuring cell is ended, the KCl electrodes
Soak a concentration of 0.1 to 4mol/L.
The present invention has the following advantages and the technique effect of high-lighting：The present invention is referred to using feed temperature and hydrogen ion
Show that the concentration information of the hydroiodic acid containing iodine is calculated in potential value that electrode and oxidation-reduction potential electrode are surveyed, data acquisition is convenient
Fast, analysis result is accurate, can overcome the shortcomings of conventional titration analysis method sampling-analysis operation is cumbersome, process takes.Originally it sets
Temperature sensor, hydrogen ion indicator electrode and the oxidation-reduction potential electrode that standby and method uses can easily choose ripe quotient
Industry standardized product, debugging, the maintenance of equipment are more convenient；The application is impregnated by metering pump, KI dilutions, KCl electrodes simultaneously
The use of liquid carries out feed liquid to be measured quantitative dilution, and is washed in time to measuring pond body, ensures that electrode is in good work
Make state, well solve hydrogen ion indicator electrode, oxidation-reduction potential electrode when measuring the solution concentration of hydroiodic acid containing iodine
Applicable sex chromosome mosaicism.
Description of the drawings
Fig. 1 is a kind of principle schematic diagram of the analytical equipment embodiment of hydriodic acid concentration containing iodine provided by the invention.
In figure：1- computers；2- hydrogen ion indicator electrodes；3- oxidation-reduction potential electrodes；4- temperature sensors；5- current potentials
Meter；6- measuring cells；7a-KI dilution storage tanks；7b-KCl electrode soak storage tanks；8- waste liquid tanks；9a-KI diluting pumps；9b-
KCl electrodes impregnate liquid pump；10- waste drains pumps；11- feed pumps to be measured；12- feed liquid storage tanks to be measured, conveyance conduit or tower；13- liquid
Position meter.
Specific embodiment
Device structure, principle and the course of work of the present invention are described in further details below in conjunction with the accompanying drawings.
The application proposes a kind of concentration analysis device and method of the hydroiodic acid containing iodine, is to measure hydriodic acid concentration containing iodine
When, 3 independent variables closely related with solution concentration including measuring containing temperature, and standard is used when measuring variable
Commercial devices, ensure measure accuracy.Specifically, it is with the temperature of temperature sensor measurement hydroiodic acid containing iodine solution
Value, with two voltage (current potential) values of hydrogen ion indicator electrode, oxidation-reduction potential determination of electrode solution, under area of computer aided
Rapidly calculate feed concentration.Under the conditions of current technical status, market supply, temperature sensor, hydrogen ion indicator electrode,
Oxidation-reduction potential electrode is conventional device, can ensure repeatability, the accuracy of measurement result.
As shown in Figure 1, a kind of concentration analysis equipment of hydroiodic acid containing iodine provided by the invention, the equipment include computer 1,
Hydrogen ion indicator electrode 2, oxidation-reduction potential electrode 3, temperature sensor 4, potentiometer 5, measuring cell 6, KI dilutions storage tank 7,
KCl electrode soak storage tanks 7b, waste liquid tank 8 and pump；The pump includes feed pump 11 to be measured, KI diluting pump 9a, KCl electrodes
Impregnate liquid pump 9b and waste drains pump 10；Measuring cell 6 passes through feed pump 11 to be measured and pipeline and feed liquid storage tank to be measured, conveyance conduit or tower
Device 12 connects；The KI dilutions storage tank 7 is connect by KI diluting pumps 7a and pipeline with measuring cell 6；The KCl electrodes impregnate
Liquid storage tank 7b impregnates liquid pump 9b by KCl electrodes and pipeline is connect with measuring cell 6；The measuring cell 6 passes through pipeline and waste drains pump
10 connect with waste liquid tank 8；Hydrogen ion indicator electrode 2, oxidation-reduction potential electrode 3 and temperature sensor are equipped in measuring cell 6
4, the hydrogen ion indicator electrode 2 and oxidation-reduction potential electrode 3 are connected by conducting wire with the potentiometer 5；The electricity
Position meter 5 and temperature sensor 4 are connect respectively by signal wire with the computer 1.
Temperature sensor 4 of the present invention can be free-standing sensor, can also be placed in hydrogen ion indicator electrode 2 or oxygen
Change in reduction potential electrode 3, i.e., described hydrogen ion indicator electrode 2 or oxidation-reduction potential electrode 3 can built-in temperature sensors.
To make measured temperature closer to actual conditions, the measuring cell 6, KI dilutions storage tank 7, feed pump to be measured
11st, KI diluting pumps 9a, KCl electrodes, which impregnate the pipeline that liquid pump 9b, waste drains pump 10 and connection pump, should all carry temperature control and heat preservation
Facility.Feed pump to be measured 11, KI diluting pump 9a, KCl electrode immersion liquid pump 9b and the waste drains pump 10 passes through with computer 1
Control circuit connects, to realize remote control of the computer to the pump；While measuring cell 6 can also be equipped with liquid level and refer to 13, the liquid
Position meter is connect by control circuit with computer, can carry out remotely monitor by computer.
A kind of concentration analysis of hydroiodic acid containing iodine provided by the invention, specifically comprises the following steps：
1) it before testing, first turns on waste drains pump 10 to empty measuring cell 6, the material of discharge flows into waste liquid tank 8, closes useless
Liquid pump 10, the logistic pipeline measured between 6 and waste liquid tank 8 are ended；
2) open feed pump 11 to be measured, by 0.1 to 500mL hydroiodic acid containing iodine to be measured by contain feed liquid to be measured storage tank,
Conveyance conduit or tower 12 are delivered to measuring cell 6) in, close feed pump 11 to be measured, feed liquid storage tank to be measured, conveyance conduit or tower
Logistic pipeline between 12 and measuring cell 6 is ended；
3) KI dilution pumps 9a are opened, KI dilutions are input to measuring cell 6 by KI dilutions storage tank 7, close KI dilution pumps
Logistic pipeline between 9, KI dilution storage tanks 7 and measuring cell 6 is ended；KI diluent concentrations are 0.1 to 3mol/L, convey body
Product is 0.1 to 1000mL；When HI concentration is less than 1mol/L, and I in known hydroiodic acid containing iodine to be measured2Concentration is less than 0.5mol/L
When, KI dilutions can not be inputted, i.e.,：To the dilution of the feed liquid of hydroiodic acid containing iodine that is delivered in measuring cell without KI dilutions,
But directly carry out the measure of following temperature, current potential；
4) hydrogen ion indicator electrode 2, oxidation-reduction potential electrode 3 measure two groups of solution in measuring cell 6 by potentiometer 5
Potential value, temperature sensor 4 measure the temperature value of solution in measuring cell 6, and above-mentioned potential value, temperature value send computer 1 to, meter
Calculation machine 1 calculates concentration and the display of out-feed liquid using the software for calculation in being stored in；The mathematical model that the software relies primarily on is
The concentration c of HI in the feed liquid of hydroiodic acid containing iodineHI、I2Concentration cI2, feed temperature t and hydrogen ion indicator electrode, oxidation-reduction potential
It (is respectively u that electrode, which surveys potential value,1And u2) relational expression：
u1=f1(t,cHI,cI2)
u2=f2(t,cHI,cI2)
Two above equations simultaneousness, you can by t, the u measured1And u2Calculate the concentration data of mixed solution in measuring cell
cHIAnd cHI；And by the volume ratio of KI dilutions and the original feed liquid of hydroiodic acid containing iodine to be measured, then can inverse go out it is original to be measured containing iodine
The concentration data of hydroiodic acid feed liquid；
5) after measuring, measuring cell is emptied, is emptied measuring cell 6 at this point, opening waste drains pump 10, the material stream of discharge
Enter waste liquid tank 8, be then shut off waste drains pump 10, the logistic pipeline between measuring cell 6 and waste liquid tank 8 is ended；
6) after emptying measuring cell, in order to ensure the accuracy subsequently measured, measuring cell is once cleaned, i.e.,：It opens
KI dilutions are input to measuring cell 6 by KI dilutions storage tank 7, close KI dilution pumps 9a, KI dilution storage tank by KI dilution pumps 9a
Logistic pipeline between 7 and measuring cell 6 is ended；KI dilutions delivered volume is 5 to 1000mL；Opening waste drains pump 10 will measure
Pond 6 empties, and the material of discharge flows into waste liquid tank 8, closes waste drains pump 10, and the logistic pipeline between measuring cell 6 and waste liquid tank 8 is cut
Only；
7) after above-mentioned cleaning, electrode soak (equilibrium liquid) is filled in measuring cell, to ensure that electrode is in good
State, and be ready to measure next time.Concrete operations are：Open KCl electrodes impregnate liquid pump 9b by KCl electrodes soak by
KCl electrode soak storage tanks 7b is input to measuring cell 6, close KCl electrodes impregnate liquid pump 9b, KCl electrode soak storage tank 7b with
Logistic pipeline between measuring cell 6 is ended, KCl electrode soaks a concentration of 0.1 to 4mol/L.
The feed liquid that the present invention is measured is come inside self-contained iodine hydroiodic acid storage tank, pipeline or rectifying column.
Embodiment 1
It is that the storage tank of hydroiodic acid containing iodine 12 that volume is 20L is assembled with concentration mensuration equipment according to attached drawing 1 and its principle, temperature
The G703595 type K-type thermocouples that sensor 4 is WATLOW companies are spent, hydrogen ion indicator electrode 2 is Wan Tong companies of Switzerland
6.0262.100 type pH electrodes, the compound platinum electricity of PT TITRODE WOC types of the oxidation-reduction potential electrode 3 for Wan Tong companies of Switzerland
Pole.The effective volume of measuring cell 6 is 100mL.KI diluent concentrations used are 2mol/L, and KCl electrodes soak is 3mol/L.Figure
KI diluting pumps 9a and the corresponding pump of feed pump to be measured 11 are the QG150-Q1CKC of the FMI companies of the U.S. with counterbalance valve in 1
Type metering pump.In Fig. 1 KCI electrodes impregnate liquid pump 9b and waste drains pump 10 it is corresponding be the Pu Luomingte GAL types with counterbalance valve
Diaphragm pump.The start and stop respectively pumped above carry out remote control by computer.
Feed concentration is measured using following steps：
1) it before testing, first turns on waste drains pump 10 to empty measuring cell 6, the material of discharge flows into waste liquid tank 10, closes
Waste liquid tank 10 is pumped, the logistic pipeline between measuring cell 6 and waste liquid tank 8 is ended；
2) feed pump 11 to be measured is opened, the hydroiodic acid containing iodine to be measured of 5mL is delivered to measuring cell 6 by feed liquid storage tank 12 to be measured
In, feed pump 11 to be measured is closed, the logistic pipeline between feed liquid storage tank 12 and measuring cell 6 to be measured is ended；
3) KI diluting pump 9a are opened, the KI dilutions of 45mL are input to measuring cell 6 by KI dilution storage tanks 7a, are closed
Logistic pipeline between KI diluting pumps 9a, KI dilution storage tank 7 and measuring cell 6 is ended；
4) hydrogen ion indicator electrode 2, oxidation-reduction potential electrode 3 measure two groups of solution in measuring cell 6 by potentiometer 5
Potential value, temperature sensor 4 measure the temperature value of solution in measuring cell 6, and above-mentioned potential value, temperature value send computer to, meter
Calculation machine 1 calculates concentration and the display of out-feed liquid using the software for calculation in being stored in.
5) after measuring, measuring cell is emptied, at this time：It opens waste drains pump 10 to empty measuring cell 6, the material stream of discharge
Enter waste liquid tank (8), close waste drains pump 10, the logistic pipeline between measuring cell 6 and waste liquid tank 8 is ended；
6) after emptying measuring cell, in order to ensure the accuracy subsequently measured, measuring cell is once cleaned, i.e.,：It opens
The KI dilutions of 100mL are input to measuring cell 6 by KI dilutions storage tank 7, close KI diluting pump 9a by KI diluting pump 9a,
Logistic pipeline between KI dilutions storage tank 7 and measuring cell 6 is ended.It opens waste drains pump 10 to empty measuring cell 6, the object of discharge
Stream enters waste liquid tank 8, closes waste drains pump 10, and the logistic pipeline between measuring cell 6 and waste liquid tank 8 is ended；
7) after above-mentioned cleaning, electrode soak (equilibrium liquid) is filled in measuring cell, to ensure that electrode is in good
State, and be ready to measure next time.Concrete operations are：It opens KCI electrodes and impregnates liquid pump, the KCl electrodes of 60mL are soaked
Bubble liquid is input to measuring cell 6 by KCl electrode soak storage tanks 7b, closes KCI electrodes and impregnates liquid pump, KCl electrode soak storage tanks
Logistic pipeline between 7b and measuring cell 6 is ended.
1#, 2# and 3# sample of hydroiodic acid containing iodine to be measured are stored in feed liquid storage tank or tower 12 to be measured respectively, is used with above-mentioned
Device and method carry out concentration mensuration, and measurement result as shown in the following chart, is also listed as a comparison, in table using conventional titration method
The obtained concentration of 1#, 2# and 3# sample.
Embodiment 2：
According to attached drawing 1 and its principle, on the conveyance conduit of a hydroiodic acid containing iodine, concentration mensuration equipment is assembled with, i.e.,
Feed pump 11 and its pipeline to be measured will be sampled from the pipeline.
Hydrogen ion indicator electrode 2 is the i-Ecotrode plus type pH electrodes of Wan Tong companies of Switzerland, and oxidation-reduction potential is electric
Pole 3 is the compound platinum electrode of PT TITRODE WOC types of Wan Tong companies of Switzerland.Due to above-mentioned i-Ecotrode plus types pH electrodes
Temperature detection function is incorporated, therefore this equipment does not set individual temperature sensor separately.
The effective volume of measuring cell 6 is 300mL.KI diluent concentrations used are 3mol/L, and KCl electrode soaks are
3mol/L.Pump corresponding with KI dilutions 9a in attached drawing 1 and feed pump to be measured 11 is the FMI companies of the U.S. with counterbalance valve
QG150-Q1CKC type metering pumps.It is the Pu Luomingte with counterbalance valve that feed pump 11 and waste drains pump 10 to be measured are corresponding in Fig. 1
GAL type diaphragm pumps.The start and stop respectively pumped above carry out remote control by computer.
Measuring cell 6, can be by computer monitoring liquid level equipped with liquid level gauge 13, hydrogen ion indicator electrode during ensuring to measure
2 and oxidation-reduction potential electrode 3 effectively submerged by liquid.
Feed concentration is measured using following steps：
1) it before testing, first turns on waste drains pump 10 to empty measuring cell 6, the material of discharge flows into waste liquid tank 8, closes useless
Liquid pump 10, measuring cell 6) logistic pipeline between waste liquid tank 8 ended；
2) feed pump 11 to be measured is opened, by the hydroiodic acid containing iodine to be measured of 10mL as the pipeline where it to measuring cell 6
In, feed pump 11 to be measured is closed, the logistic pipeline between feed liquid pipeline 12 and measuring cell 6 to be measured is ended；
3) KI diluting pump 9a are opened, the KI dilutions of 90mL are input to measuring cell 6 by KI dilutions storage tank 7, are closed
Logistic pipeline between KI diluting pumps 9a, KI dilution storage tank 7 and measuring cell 6 is ended；
4) hydrogen ion indicator electrode 2, oxidation-reduction potential electrode 3) pass through potentiometer 5) measure two of solution in measuring cell 6
Group potential value, the temperature value that the temperature sensor of 2 internal integration of above-mentioned potential value and hydrogen ion indicator electrode measures are sent to
Computer, computer 1 calculate concentration and the display of out-feed liquid using the software for calculation in being stored in.
5) after measuring, measuring cell is emptied, at this time：It opens waste drains pump 10 to empty measuring cell 6, the material stream of discharge
Enter waste liquid tank 8, close waste drains pump 10, the logistic pipeline between measuring cell 6 and waste liquid tank 8 is ended；
6) after emptying measuring cell, in order to ensure the accuracy subsequently measured, measuring cell is once cleaned, i.e.,：It opens
The KI dilutions of 300mL are input to measuring cell 6 by KI dilutions storage tank 7, close KI diluting pump 9a by KI diluting pump 9a,
KI dilutions storage tank 7 and the logistic pipeline measured between 6 are ended.It opens waste drains pump 10 to empty measuring cell 6, the material of discharge
Waste liquid tank 8 is flowed into, closes waste drains pump 10, the logistic pipeline between measuring cell 6 and waste liquid tank 8 is ended；
7) after above-mentioned cleaning, electrode soak (equilibrium liquid) is filled in measuring cell, to ensure that electrode is in good
State, and be ready to measure next time.Concrete operations are：It opens KCI electrodes and impregnates KCl electrode leaching of the liquid pump by 200mL
Bubble liquid is input to measuring cell 6 by KCl electrode soak storage tanks 7b, closes KCI electrodes and impregnates liquid pump, KCl electrode soak storage tanks
Logistic pipeline between 7b and measuring cell 6 is ended.
When conveying 4#, 5# hydroiodic acid containing iodine sample in pipeline respectively, use and carry out concentration survey with the above apparatus and method
Fixed, measurement result as shown in the following chart, also lists 4# the and 5# samples that are obtained using conventional titration method as a comparison, in table
Concentration.
Embodiment 3：
Concentration analysis equipment in embodiment 2 is arranged at the tower reactor of the rectifying column of hydroiodic acid containing iodine, i.e., feed pump to be measured
11 and its pipeline will be sampled from the tower reactor of the rectifying column.Feed concentration is measured using following steps：
1) it before testing, first turns on waste drains pump 10 to empty measuring cell 6, the material of discharge flows into waste liquid tank 8, closes useless
Liquid pump 10, the logistic pipeline between measuring cell 6 and waste liquid tank 8 are ended；
2) feed pump 11 to be measured is opened, the hydroiodic acid containing iodine to be measured of 60mL is conveyed as the HIx tower bottom of rectifying tower where it
Into measuring cell 6, feed pump 11 to be measured is closed, the logistic pipeline between feed liquid conveyance conduit 12 and measuring cell 6 to be measured is ended；
3) KI diluting pump 9a are opened, the KI dilutions of 90mL are input to measuring cell 6 by KI dilutions storage tank 7, are closed
Logistic pipeline between KI diluting pumps 9a, KI dilution storage tank 7 and measuring cell 6 is ended；
4) hydrogen ion indicator electrode 2, oxidation-reduction potential electrode 3 measure two groups of solution in measuring cell 6 by potentiometer 5
Potential value, the temperature value that the temperature sensing device of 2 internal integration of above-mentioned potential value and hydrogen ion indicator electrode measures are sent to
Computer 1, computer calculate concentration and the display of out-feed liquid using the software for calculation in being stored in.
5) after measuring, measuring cell is emptied, at this time：It opens waste drains pump 10 to empty measuring cell 6, the material stream of discharge
Enter waste liquid tank 8, close waste drains pump 10, the logistic pipeline between measuring cell 6 and waste liquid tank 8 is ended；
6) after emptying measuring cell, in order to ensure the accuracy subsequently measured, measuring cell is once cleaned, i.e.,：It opens
The KI dilutions of 80mL are input to measuring cell 6 by KI dilutions storage tank 7, close KI diluting pumps 9a, KI by KI diluting pump 9a
Logistic pipeline between dilution storage tank 7 and measuring cell 6 is ended.It opens waste drains pump 10 to empty measuring cell 6, the material of discharge
Waste liquid tank 8 is flowed into, closes waste drains pump 10, the logistic pipeline between measuring cell 6 and waste liquid tank 8 is ended；
7) after above-mentioned cleaning, electrode soak (equilibrium liquid) is filled in measuring cell, to ensure that electrode is in good
State, and be ready to measure next time.Concrete operations are：It opens KCI electrodes and impregnates KCl electrode immersion of the liquid pump by 60mL
Liquid is input to measuring cell 6 by KCl electrode soak storage tanks 7b, closes KCI electrodes and impregnates liquid pump, KCl electrode soaks storage tank 7b)
Logistic pipeline between measuring cell 6 is ended.
When conveying 6#, 7# hydroiodic acid containing iodine sample in pipeline respectively, use and carry out concentration survey with the above apparatus and method
Fixed, measurement result as shown in the following chart, also lists 6# the and 7# samples that are obtained using conventional titration method as a comparison, in table
Concentration.
Claims (6)
1. a kind of concentration analysis equipment of hydroiodic acid containing iodine, it is characterised in that：The equipment includes computer (1), hydrogen ion refers to
Show electrode (2), oxidation-reduction potential electrode (3), temperature sensor (4), potentiometer (5), measuring cell (6), KI dilution storage tanks
(7), KCl electrodes soak storage tank (7b), waste liquid tank (8) and pump；The pump includes feed pump to be measured (11), KI diluting pumps
(9a), KCl electrodes impregnate liquid pump (9b) and waste drains pump (10)；Measuring cell (6) by feed pump to be measured (11) and pipeline with it is to be measured
Feed liquid storage tank, conveyance conduit or tower connection；The KI dilutions storage tank (7) is by KI diluting pumps (7a) and pipeline with measuring
Pond (6) connects；The KCl electrodes soak storage tank (7b) is impregnated liquid pump (7b) and pipeline by KCl electrodes and is connected with measuring cell (6)
It connects；The measuring cell (6) is connect by pipeline and waste drains pump (10) with waste liquid tank (8)；Refer in measuring cell (6) equipped with hydrogen ion
Show electrode (2), oxidation-reduction potential electrode (3) and temperature sensor (4), the hydrogen ion indicator electrode (2) and oxidation are also
Former current potential electrode (3) is connected by conducting wire with the potentiometer (5)；The potentiometer (5) and temperature sensor (4) lead to respectively
Signal wire is crossed to connect with the computer (1).
2. a kind of analytical equipment of hydriodic acid concentration containing iodine according to claim 1, it is characterised in that：The temperature passes
Sensor (4) is stand alone type setting or is placed within hydrogen ion indicator electrode (2) or is placed in oxidation-reduction potential electrode (3).
3. a kind of analytical equipment of hydriodic acid concentration containing iodine according to claim 1, it is characterised in that：The measuring cell
(6), KI dilutions storage tank (7), feed pump to be measured (11), KI diluting pumps (9a), KCl electrodes impregnate liquid pump (9b), waste drains pump
(10) and the pipeline of connection pump carries temperature control and lagging facility.
4. a kind of analytical equipment of hydriodic acid concentration containing iodine according to claim 1,2 or 3, it is characterised in that：Described
Feed pump (11) to be measured, KI diluting pumps (9a), KCl electrodes impregnate liquid pump (9b) and waste drains pump (10) passes through with computer (1)
Control circuit connects.
5. a kind of analytical equipment of hydriodic acid concentration containing iodine according to claim 4, it is characterised in that：The measuring cell
(6) liquid level gauge (13) is equipped in, which is connect by control circuit with computer (1).
A kind of 6. concentration analysis of hydroiodic acid containing iodine using equipment as described in claim 1, it is characterised in that this method
Include the following steps：
1) waste drains pump (10) to be opened, measuring cell (6) is emptied, effluent flows into waste liquid tank (8), is then shut off waste drains pump (10),
Ended the logistics pipeline between measuring cell (6) and waste liquid tank (8)；
2) feed pump (11) to be measured is opened, by 0.1 to the 500mL feed liquid of hydroiodic acid containing iodine to be measured by feed liquid Pipeline transport to be measured extremely
In measuring cell (6), be then shut off feed pump to be measured (11), make feed liquid storage tank to be measured, conveyance conduit or tower and measuring cell (6) it
Between logistics pipeline ended；
3) KI diluting pumps (9a) are opened, KI dilutions are input to measuring cell (6) by KI dilutions storage tank (7a), are then shut off
KI diluting pumps (9a) are ended the logistics pipeline between KI dilutions storage tank (7a) and measuring cell (6)；The KI dilutions
A concentration of 0.1 to 3mol/L, delivered volume is 0.1 to 1000mL；
4) potentiometer (5) is measured by hydrogen ion indicator electrode (2) and oxidation-reduction potential electrode (3) in measuring cell (6) respectively
Two groups of potential value u of solution1And u2, temperature sensor (4) measures the temperature value t of solution in measuring cell (6), by two groups of potential values
u1And u2And temperature value t sends computer to, computer (1) calculates the concentration of out-feed liquid using the software for calculation in being stored in
And it is shown；
The software for calculation is calculated by following equations group：
u1=f1(t,cHI,cI2)
u2=f2(t,cHI,cI2)
Equation f1(t,cHI,cI2) it is t, cHIAnd cI2Three variables are to u1Mathematic(al) representation, f2(t,cHI,cI2) it is t, cHIAnd cI2
Three variables are to u2Mathematic(al) representation, c in formulaHIFor the concentration of HI in the feed liquid of hydroiodic acid containing iodine, cI2For I2Concentration, t for survey
Measure the temperature value of solution in pond；
By two above equations simultaneousness, by t, the u measured1And u2Calculate the concentration data c of solution in measuring cellHIAnd cHI；
Again by KI dilutions and the volume ratio of the original feed liquid of hydroiodic acid containing iodine to be measured, i.e. inverse goes out the original feed liquid of hydroiodic acid containing iodine to be measured
Concentration data；
5) it opens waste drains pump (10) to empty measuring cell (6) feed liquid, the feed liquid of discharge is sent to waste liquid tank (8), is then shut off waste liquid
It pumps (10), is ended the logistics pipeline between measuring cell (6) and waste liquid tank (8)；
6) KI diluting pumps (9a) are opened, KI dilutions are input to measuring cell (6) by KI dilutions storage tank (7a), it is dilute to close KI
Liquid pump (9a) is released, is ended the logistics pipeline between KI dilutions storage tank (7a) and measuring cell (6)；KI dilution delivered volumes
It is 5 to 1000mL；It opens waste drains pump (10) to empty measuring cell (6), the feed liquid of discharge is sent to waste liquid tank (8), is then shut off giving up
Liquid pump (10), the logistic pipeline between measuring cell (6) and waste liquid tank (8) are ended；
7) KCl electrodes are opened and impregnates liquid pump (9b), KCl electrodes soak is input to survey by KCl electrode soak storage tanks (7b)
It measures pond (6), closes KCl electrodes and impregnate liquid pump (9b), the stream tube between KCl electrode soak storage tanks (7b) and measuring cell (6)
Line is ended, the KCl electrodes soak a concentration of 0.1 to 4mol/L.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711124392.2A CN108152343B (en) | 2017-11-14 | 2017-11-14 | Iodine-containing hydriodic acid concentration analysis equipment and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711124392.2A CN108152343B (en) | 2017-11-14 | 2017-11-14 | Iodine-containing hydriodic acid concentration analysis equipment and method |
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| Publication Number | Publication Date |
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| CN108152343B CN108152343B (en) | 2020-01-17 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005077145A (en) * | 2003-08-28 | 2005-03-24 | Japan Atom Energy Res Inst | Quantitative analytical method for (iodine + hydroiodic acid + sulfuric acid) solution |
| KR20100078182A (en) * | 2008-12-30 | 2010-07-08 | 한국에너지기술연구원 | The method of quantitative analysis for h2so4-hi-h2o-i2 system solution in high concentration condition of i2 without calibration |
| CN103048220A (en) * | 2012-12-05 | 2013-04-17 | 清华大学 | Iodine hydroiodic acid container capable of displaying liquid concentration on line |
| CN103048219A (en) * | 2012-12-05 | 2013-04-17 | 清华大学 | Analytical method of iodine-containing hydriodic acid concentration |
| CN105675809A (en) * | 2016-01-15 | 2016-06-15 | 清华大学 | Analysis method of concentration of HI-I2-H2O ternary solution |
-
2017
- 2017-11-14 CN CN201711124392.2A patent/CN108152343B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005077145A (en) * | 2003-08-28 | 2005-03-24 | Japan Atom Energy Res Inst | Quantitative analytical method for (iodine + hydroiodic acid + sulfuric acid) solution |
| KR20100078182A (en) * | 2008-12-30 | 2010-07-08 | 한국에너지기술연구원 | The method of quantitative analysis for h2so4-hi-h2o-i2 system solution in high concentration condition of i2 without calibration |
| CN103048220A (en) * | 2012-12-05 | 2013-04-17 | 清华大学 | Iodine hydroiodic acid container capable of displaying liquid concentration on line |
| CN103048219A (en) * | 2012-12-05 | 2013-04-17 | 清华大学 | Analytical method of iodine-containing hydriodic acid concentration |
| CN105675809A (en) * | 2016-01-15 | 2016-06-15 | 清华大学 | Analysis method of concentration of HI-I2-H2O ternary solution |
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