CN108896629A - A kind of 3 flow-type caliberating devices of sodium ion densimeter and its scaling method - Google Patents
A kind of 3 flow-type caliberating devices of sodium ion densimeter and its scaling method Download PDFInfo
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Abstract
A kind of 3 flow-type caliberating devices of sodium ion densimeter and its scaling method, its main feature is that, according to sodium ion densimeter calibration principle, introduce 3 flow-type calibration standard water samples, Nernst equation combined calculation is detected and applied respectively, and detected water sample flow regime, the consistency of flow velocity, guarantee nominal data accuracy when having accomplished to mark timing standard solution and measurement, it solves the sodium ion that whole process is brought into due to various reasons, solves the problems, such as two o'clock flow-type calibration inaccuracy；It develops simultaneously, design a kind of 3 flow-type caliberating devices of sodium ion densimeter, being suitble to scaling method requirement, most preferably performance scaling method, water sample Na ion concentration is more accurate in online, continuous monitoring production procedure, meets the domain requirements such as electric power, petrochemical industry.
Description
Technical field
The present invention relates to a kind of sodium ion densimeters, more particularly to a kind of 3 flow-type calibration dresses of sodium ion densimeter
It sets and its scaling method.
Background technique
Sodium ion densimeter is a kind of on-line chemical analysis instrument, is applied in fields such as electric power, petrochemical industry, main monitoring power generation
The Na ion concentration of factory's boiler feedwater, condensed water, saturated vapor and superheated steam etc..It can continuously monitor water in production procedure
The sodium ions content of sample is suitble to the use environment of industry spot, meets the actual demand of maintenance personnel.Sodium ion densimeter is being surveyed
It must be demarcated before amount Na ion concentration, sodium ion densimeter calibration is accurate, and the measurement of Na ion concentration is with regard to accurate.
Sodium ion densimeter is made of sensor, intelligent high resistant millivoltmeter, control panel and chemical flow path system etc..Sodium ion
The sensor of densimeter is made of sodium selective electrode, reference electrode, temperature electrode and the water sample in measuring cell, also known as
Battery is measured, the relationship measured between the Na ion concentration in the electromotive force and water sample of battery meets Nernst equation：
E=E0+S(T/298.15)lgC/Ciso
E in formula --- measurement cell emf；
E0--- the current potential of equipotential points, the value do not vary with temperature, E after calibration0It is determining numerical value；
The Na ion concentration of C --- water sample；
Ciso--- the Na ion concentration of equipotential points is determining value for determining electrode；
S --- conversion slope, the value and sodium selective electrode, the performance of reference electrode have corresponding relationship, and S is after calibration
Determining numerical value；
T --- water sample temperature.
1, Na ion concentration measures：According to Nernst equation, in known E0、S、CisoUnder conditions of, Na ion concentration measurement
The potential value E and water sample temperature T for measuring detected water sample, with Nernst equation, E=E0+S(T/298.15)lgC/Ciso, solve C
Process.
2, the calibration of sodium ion densimeter：According to Nernst equation, under conditions of known C, sodium ion densimeter measurement
The potential value E of standard water sample out, uses Nernst equation：E=E0+S(T/298.15)lgC/CisoSolve E0, S process.
To be made when calibration two (or more) known to Na ion concentration standard solution (such as C1、C2, Ci), and respectively
Measure their potential value (such as E1、E2、Ei) and standard solution temperature T, establish equation：
E1=E0+S(T/298.15)log(C1/Ciso)
E2=E0+S(T/298.15)log(C2/Ciso)
It solves above equation group and obtains E0, S, that is, demarcate after E0, S and Ciso, thus construct Nernst equation E=E0+S(T/
298.15)lgC/Ciso, using this Nernst equation, sodium ion densimeter measures Na ion concentration.
Sodium ion densimeter caliberating device and its scaling method mainly have sodium ion densimeter dynamic two o'clock calibration dress at present
It sets and its scaling method and sodium ion densimeter two-point additive calibration caliberating device and its scaling method.
Sodium ion densimeter dynamic two o'clock caliberating device as shown in Figure 1, sodium ion densimeter dynamic two o'clock caliberating device and
Its scaling method is mainly reflected in following problems：
It is required that preparation Na ion concentration is C with the chlorination sodium standard solution of fresh extra pure reagent water dilution higher concentration1
And C2Two kinds of standard solution, Electricity Department specification：Fresh extra pure reagent water conductivity is small less than 0.1 μ s/cm, sodium ions content
In 0.2 μ g/L.In actual operation, fresh extra pure reagent water, which is not easy to reach conductivity after producing and save at the scene, is less than
0.1 μ s/cm, sodium ions content are less than 0.2 μ g/L this standard；On the other hand being widely present due to sodium ion is tried mobile
During agent water and preparing standard solution, air, container, experiment equipment, gimmick etc. all may be to reagent waters and standard solution
It pollutes, two aspects combine so that the sodium ion actual concentration value of standard solution when in use is (C1+Cs) and (C2+Cs),
CsIt is reagent water, preparing standard solution process introducing positive error, is uncertain in each calibration.
Sodium ion densimeter two-point additive calibration caliberating device is as shown in Fig. 2, sodium ion densimeter secondary standard adds
Method caliberating device and its scaling method are mainly reflected in the following aspects：
1, operating provision must carry out within the hour of the 2-3 after sodium selective electrode is activated, and sodium ion
Selecting electrode activation processing is to remove one layer of outmoded sodium selective electrode sensitive membrane using corrosive substance, exposes one layer newly
The operation of sensitive membrane, this brings following problems：
A, sodium selective electrode performance is inconsistent in calibration and measurement process, and one of calibration and measuring condition with instrument
Cause property principle has deviation；
B, electrode activation processing reduces the service life of sodium selective electrode, increases maintenance cost；
C, the extremely strong substance of corrosivity is used in electrode activation processing, when operation must wear safety goggles and gloves, increase
The danger of operator is added；
2, mark timing standard solution (volume 190ml) recycles in measuring cup under air stirring；Detected water sample when measurement
(volume 23ml) flows through in measuring cup, and the state of two process liquids, flow velocity are inconsistent, the calibration and measuring condition with instrument
The consistency principle have deviation；
3, solution stirs in measuring cup when demarcating, and the potassium ion (or lithium ion) of reference electrode exudation is also in measuring cup
Circulation, and sodium selective electrode has response to monovalent ions such as potassium ions (or lithium ion), increased this part response is not
It is the sodium ion from standard solution, interference is formed to calibration；
4, two-point additive calibration calibration is operated in instrument use site, horizontal by site environment, condition and operator
Limitation, measuring cup injects volume of water sample V when calibration0, No. 1 standard solution C1Volume V1, No. 2 standard solution C1Volume V2No
It is easy to do to accurate, according to：
dc1=C1×V1/(V1+Vc)
dc2=C2×V2/(V1+V2+Vc)
Guarantee dc1、dc2Accurately acquire a certain degree of difficulty；
5, the Na ion concentration for marking grab sample is not greater than a certain range (micro- sodium table 1 μ g/L, low 19 μ g/L of sodium table) limit
The application for having made calibration, detected water sample Na ion concentration is greater than above range such as within certain period, cannot within this period
Sodium ion densimeter is demarcated；
6, proving operation restrictive condition is more, and proving operation step is more.Ion selective electrode is activated before such as demarcating
Processing；Check that the Na ion concentration of water sample is not greater than a certain range (micro- sodium table 1 μ g/L, low 19 μ g/L of sodium table)；Handover measurement
Cup operation；Check measuring cup in various parts installation whether in place, measuring cup switching valve whether have micro- leakage, determine liquid in measuring cup
The volume of body will input new volume as volume changes；Precisely addition C1、C2, by the multiple confirmation operation of the prompt of instrument
Deng.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of and solving existing sodium ion densimeter calibration technique, according to Na ion concentration
Count calibration principle, design it is a kind of structurally reasonable, it is easy to use, demarcate 3 flow-types calibration dresses of accurate sodium ion densimeter
It sets, and creatively proposes a kind of scientific and reasonable, strong applicability, the good 3 flow-type calibration sides of sodium ion densimeter of effect
Method.
To realize the present invention purpose use technical solution first is that：A kind of 3 flow-type calibration dresses of sodium ion densimeter
It sets, including detected water sample inlet valve 1, level pressure overflow cup 2, water sample pipeline 3, alkalization device 5, temperature electrode 6, ion-selective electrode
7, reference electrode 8, contact conductor 9, intelligent high resistant millivoltmeter 10, flow type measuring cup 11, waste water collector 12 and overflow pipe 13,
The detected water sample inlet valve 1 is arranged on water sample pipeline 3,2 arrival end of level pressure overflow cup and survey sample water inlet valve 1
Outlet end is connected by water sample pipeline 3, and 2 outlet end of level pressure overflow cup and alkalization 5 arrival end of device pass through water sample pipeline 3
Connection, 5 outlet end of alkalization device are connect with temperature electrode 6 by water sample pipeline 3, the temperature electrode 6 and ion
Electrode 7 is selected to connect by water sample pipeline 3, the ion-selective electrode 7 is connect with reference electrode 8 by water sample pipeline 3, institute
Temperature electrode 6, ion-selective electrode 7 and the reference electrode 8 stated are placed in flow type measuring cup 11, the temperature electrode 6, from
Son selection electrode 7 and reference electrode 8 are electrically connected with intelligent high resistant millivoltmeter 10 by contact conductor 9 respectively, and the level pressure is overflow
The overflow port of flow cup 2 is connect with waste water collector 12 by overflow pipe 13, characterized in that further includes distributor 4, basic pattern solenoid valve
14, one solenoid valve 15 of standard specimen, detected water sample solenoid valve 16, two solenoid valve 17 of standard specimen, basic pattern reagent barrel 18, one reagent barrel of standard specimen
19, two reagent barrel 20 of standard specimen, the water sample pipeline 3 that connection level pressure overflow cup 2 is arranged between the device 5 that alkalizes in the distributor 4
On, the detected water sample solenoid valve 16 is arranged on the water sample pipeline 3 between connection level pressure overflow cup 2 and distributor 4, described
Basic pattern solenoid valve 14 is arranged on the water sample pipeline 3 between basic pattern reagent barrel 18 and distributor 4, and one solenoid valve 15 of standard specimen is set
It sets on the water sample pipeline 3 between one reagent barrel 19 of standard specimen and distributor 4, two solenoid valve 17 of the standard specimen setting is tried in standard specimen two
On water sample pipeline 3 between agent bucket 20 and distributor 4, the reference electrode 8 and waste water collector 12 are connected by water sample pipeline 3
It connects, and water sample pipeline 3 is arranged in 11 bottom of flow type measuring cup.
To realize the present invention purpose use technical solution second is that：A kind of 3 flow-type calibration dresses of sodium ion densimeter
It sets, is characterized in：Its scaling method is following steps：
It 1`) prepares 3 flow-types and demarcates standard water sample：
Laboratory with reagent water prepare Na ion concentration be 10-20 μ g/L benchmark water sample, do not consider reagent water sodium from
Sub- concentration, abbreviation basic pattern, taking Na ion concentration is the stock solution of 1000 μ g/L, dilutes 5 times with basic pattern, does not consider basic pattern sodium ion
Concentration is configured to standard solution one, and abbreviation standard specimen one, taking Na ion concentration is the stock solution of 10mg/L, is diluted with 5 times of basic pattern,
It is configured to standard solution two, does not consider basic pattern Na ion concentration, abbreviation standard specimen two；
2) basic pattern is added to the basic pattern reagent barrel 18 of instrument, and standard specimen one is added to one reagent barrel 19 of standard specimen, and standard specimen two is added
Into two reagent barrel 20 of instrument standard specimen；
3) instrument enters calibration state, automatically shuts down detected water sample solenoid valve 16, and standard specimen one inputs 200 μ g/L；Standard specimen two
Input 2000 μ g/L；
4) basic pattern solenoid valve 14 open, one solenoid valve 15 of standard specimen, detected water sample solenoid valve 16, two solenoid valve 17 of standard specimen and by
Sample water inlet valve 1 to be surveyed to close, basic pattern enters and rinses distributor 4, water sample pipeline 3, alkalization device 5, it alkalizes to basic pattern, into
Enter flow through measuring cell 11, intelligent high resistant millivoltmeter 10 starts to detect and show basic pattern temperature T1With electromotive force Es, time to 25
Minute, Es stablized, the Es of intelligent 10 stable storage of high resistant millivoltmeter；
5) one solenoid valve 15 of standard specimen open, basic pattern solenoid valve 14, detected water sample solenoid valve 16, two solenoid valve 17 of standard specimen and by
Survey sample water inlet valve 1 close, standard specimen one enter simultaneously rinses distributor 4, water sample pipeline 3, alkalization device 5, while to standard specimen one into
Row alkalization, the formula that circulates measuring cell 11, intelligent high resistant millivoltmeter 10 detect and show one electromotive force E of standard specimen1, the time is to 20 points
Clock E1Stablize, the E of intelligent 10 stable storage of high resistant millivoltmeter1；
6) two solenoid valve 17 of standard specimen open, basic pattern solenoid valve 14, one solenoid valve 15 of standard specimen, detected water sample solenoid valve 16 and by
Survey sample water inlet valve 1 close, standard specimen two enter simultaneously rinses distributor 4, water sample pipeline 3, alkalization device 5, while to standard specimen two into
Row alkalization, the formula that circulates measuring cell 11, intelligent high resistant millivoltmeter 10 detect and show two electromotive force E of standard specimen2, the time is to 15 points
Clock E2Stablize, the E of intelligent 10 stable storage of high resistant millivoltmeter2；
7) according to Nernst equation, equation group is established：
Es=E0+S(T/298.15)log[Cs/Ciso]
E1=E0+S(T/298.15)log[(Cs+200)/Ciso]
E2=E0+S(T/298.15)log[(Cs+2000)/Ciso]
Es in formula --- basic pattern measures cell emf
E1--- standard specimen one measures cell emf
E2--- standard specimen two measures cell emf
E0--- the current potential of equipotential points
Cs--- the practical Na ion concentration of basic pattern, it is desirable that Cs≯40μg/L
Ciso--- the Na ion concentration (being determining value for determining electrode) of equipotential points
S --- conversion slope, the value have corresponding pass with sodium selective electrode, the performance of reference electrode and water sample temperature
System, calibration
S is determining numerical value afterwards
T --- water sample temperature
Intelligent high resistant millivoltmeter solves these three equations, obtains Cs, S and E0,
Bring calibration result into this special formula journey
E=E0+S(T/298.15)lgC/Ciso
Storage is used for water sample on-line measurement, calculates corresponding concentration value C in intelligent high resistant millivoltmeter.
A kind of 3 flow-type caliberating devices of sodium ion densimeter and its scaling method of the invention have the beneficial effect that：
If 1, according to 3 flow-type scaling method preparing standard solutions (basic pattern, standard specimen one, standard specimen two), reagent water
Practical Na ion concentration a certain range just, without as two o'clock calibration technique preparing standard solution it is so stringent.Such as basic pattern reality
Border Na ion concentration, it is desirable that Cs≯40μg/L；
2, a kind of 3 flow-type scaling method formulas of sodium ion densimeter are：
Es=E0+S(T/298.15)log[Cs/Ciso]
E1=E0+S(T/298.15)log[(Cs+200)/Ciso]
E2=E0+S(T/298.15)log[(Cs+2000)/Ciso]
Calibrated and calculated contains reagent water production and use, standard solution are prepared, the whole process of storage is due to various originals
Because of the sodium ion brought into, solves the problems, such as two o'clock flow-type calibration inaccuracy；
3, three kinds of standard solution are prepared in laboratory, better than live two-point additive calibration preparing standard solution condition, are made
Preparing standard solution is easily operated, and the concentration of standard solution of preparation is relatively accurate；
4, the apparatus structure is simple, and execute-in-place is simple, as long as each standard solution is attached to sodium ion densimeter
In reagent barrel, after sodium ion densimeter enters calibration interface, one 200 μ g/L of input of mark, two 2000 μ g/L of input of mark, instrument after determining
Table is automatically performed proving operation；
5, without that can be demarcated to sodium ion densimeter to sodium selective electrode activation processing, sodium ion selection electricity
Pole is consistent with mark detector timing properties b in measurement；
6, benchmark water sample technology is introduced, artificial adds a certain amount of Na ion concentration, measuring cell E to reagent watersBuild
It is vertical quickly to stablize；
7, the measuring cell of sodium ion densimeter also uses special flow-through design, solution (standard solution or detected water sample)
Temperature electrode and sodium selective electrode are firstly flowed through, reference electrode is again passed through, the potassium ion of reference electrode exudation is taken out of by solution
Measuring cell cannot be diffused into the sodium selective electrode of upstream, it is therefore prevented that interference of the potassium ion to calibration, measurement；
8, detected water sample flow regime, the consistency of flow velocity, guarantee calibration when having accomplished to mark timing standard solution and measurement
Data accuracy.
Detailed description of the invention
Fig. 1 is sodium ion densimeter dynamic two o'clock caliberating device schematic diagram；
Fig. 2 is sodium ion densimeter two-point additive calibration caliberating device schematic diagram；
Fig. 3 is a kind of 3 flow-type caliberating device schematic diagrames of sodium ion densimeter；
Fig. 4 is a kind of 3 flow-type scaling method demarcation flow figures of sodium ion densimeter.
In figure：1, detected water sample inlet valve, 2, level pressure overflow cup, 3, water sample pipeline, 4 distributors, 5, alkalization device, 6, temperature
Degree electrode, 7, ion-selective electrode, 8, reference electrode, 9, contact conductor, 10, intelligent high resistant millivoltmeter, 11, flow type measurement
Cup, 12, waste water collector, 13, overflow pipe, 14, basic pattern solenoid valve, 15, one solenoid valve of standard specimen, 16, detected water sample solenoid valve,
17, two solenoid valve of standard specimen, 18, basic pattern reagent barrel, 19, one reagent barrel of standard specimen, 20, two reagent barrel of standard specimen, 21, air pump, 22, survey
Measuring cup high position overflow valve, 23 measuring cup low level overflow valves, 24, jigger dirt discharging valve.
Specific embodiment
Below in conjunction with Fig. 3, Fig. 4 and specific embodiment, invention is further described in detail, tool described herein
Body embodiment only to explain the present invention, is not intended to limit the present invention.Such as Fig. 3, water sample pipeline 3 connects level pressure overflow cup 2
Entrance, water sample pipeline 3 are equipped with detected water sample inlet valve 1, and the outlet of level pressure overflow cup 2 passes through water sample pipeline 3 with 4 entrance of distributor
Connection, water sample pipeline 3 are equipped with detected water sample solenoid valve 16, and the outlet of distributor 4 passes through water sample pipeline 3 with alkalization 5 entrance of device
Connection, the outlet of alkalization device 5 connect connection by water sample pipeline 3 with 6 bottom of temperature electrode, and 6 middle part of temperature electrode is selected with ion
It selects 7 bottom of electrode to connect by water sample pipeline 3,7 middle part of ion-selective electrode is connected with 8 bottom of reference electrode by water sample pipeline 3
It connects, temperature electrode 6, ion-selective electrode 7 and reference electrode 8 are set in flow type measuring cup 11, temperature electrode 6, ion choosing
Electrode 7 and reference electrode 8 are selected respectively with intelligent high resistant millivoltmeter 10, is connected by contact conductor, and 8 bottom of reference electrode connects water
Sample pipeline 3 is connected by 11 bottom of flow type measuring cup with waste water collector 12,2 overflow port of level pressure overflow cup and wastewater collection
Device 12 is connected by water sample pipeline 3, and basic pattern reagent barrel 18 is connect with 4 entrance of distributor by water sample pipeline 3, on water sample pipeline 3
Equipped with basic pattern solenoid valve 14, one reagent barrel 19 of standard specimen is connect with 4 entrance of distributor by water sample pipeline 3, and water sample pipeline 3 is equipped with
One solenoid valve 15 of standard specimen, two reagent barrel of standard specimen, 20 distributor, 4 entrance are connected by water sample pipeline 3, and water sample pipeline 3 is equipped with standard specimen
Two solenoid valves 17.
Such as Fig. 4：
1) 3 flow-types are prepared and demarcates standard water sample：
Laboratory with reagent water prepare Na ion concentration be 10-20 μ g/L benchmark water sample, do not consider reagent water sodium from
Sub- concentration, abbreviation basic pattern, taking Na ion concentration is the stock solution of 1000 μ g/L, dilutes 5 times with basic pattern, does not consider basic pattern sodium ion
Concentration is configured to standard solution one, and abbreviation standard specimen one, taking Na ion concentration is the stock solution of 10mg/L, is diluted with 5 times of basic pattern,
It is configured to standard solution two, does not consider basic pattern Na ion concentration, abbreviation standard specimen two；
2) basic pattern, standard specimen one, standard specimen two are added separately to the basic pattern reagent barrel 18 of instrument, one reagent barrel 19 of standard specimen, standard specimen
In two reagent barrels 20；
3) instrument enters calibration state, automatically shuts down detected water sample solenoid valve 16, and standard specimen one inputs 200 μ g/L；Standard specimen two
Input 2000 μ g/L；
4) basic pattern solenoid valve 14, one solenoid valve of standard specimen (15), detected water sample solenoid valve (16), two solenoid valve of standard specimen are opened
(17) it is closed with detected water sample inlet valve (1)；
5) basic pattern enters and rinses distributor 4, water sample pipeline 3, alkalization device 5, alkalizes to basic pattern, circulate formula
Measuring cell 11, intelligent high resistant millivoltmeter 10 start to detect and show basic pattern temperature T1With electromotive force Es, the time is steady to 25 minutes Es
It is fixed, the Es of intelligent 10 stable storage of high resistant millivoltmeter；
6) basic pattern solenoid valve 14 is turned off；
7) one solenoid valve 15 of standard specimen, basic pattern solenoid valve (14), detected water sample solenoid valve (16), two solenoid valve of standard specimen are opened
(17) it is closed with detected water sample inlet valve (1)；
8) standard specimen one enters and rinses distributor 4, water sample pipeline 3, alkalization device 5, while alkalizing to standard specimen one, into
Enter flow through measuring cell 11, intelligent high resistant millivoltmeter 10 detects and shows one electromotive force E of standard specimen1, the time to 20 minutes E1Stablize,
The E of intelligent 10 stable storage of high resistant millivoltmeter1；
9) one solenoid valve 15 of standard specimen is closed；
10) two solenoid valve 17 of standard specimen, basic pattern solenoid valve (14), one solenoid valve of standard specimen (15), detected water sample solenoid valve are opened
(16) it is closed with detected water sample inlet valve (1)；
11) standard specimen two enters and rinses distributor 4, water sample pipeline 3, alkalization device 5, while alkalizing to standard specimen two,
The formula that circulates measuring cell 11, intelligent high resistant millivoltmeter 10 detect and show two electromotive force E of standard specimen2, the time to 15 minutes E2Surely
It is fixed, the E of intelligent 10 stable storage of high resistant millivoltmeter2；
12) two solenoid valve 17 of standard specimen is closed；
13) according to Nernst equation, equation group is established：
Es=E0+S(T/298.15)log[Cs/Ciso]
E1=E0+S(T/298.15)log[(Cs+200)/Ciso]
E2=E0+S(T/298.15)log[(Cs+2000)/Ciso]
Es in formula --- basic pattern measures cell emf
E1--- standard specimen one measures cell emf
E2--- standard specimen two measures cell emf
E0--- the current potential of equipotential points
Cs--- the practical Na ion concentration of basic pattern, it is desirable that Cs≯40μg/L
Ciso--- the Na ion concentration (being determining value for determining electrode) of equipotential points
S --- conversion slope, the value have corresponding pass with sodium selective electrode, the performance of reference electrode and water sample temperature
System, S is determining numerical value after calibration
T --- water sample temperature
Intelligent high resistant millivoltmeter solves these three equations, obtains Cs, S and E0,
Bring calibration result into this special formula journey
E=E0+S(T/298.15)lgC/Ciso
Storage judges whether S meets the requirements in intelligent high resistant millivoltmeter；
If 14) S is undesirable, re-scale；
If 15) S meets the requirements, demarcates successfully, store up in intelligent high resistant millivoltmeter, exit calibrating procedure, calibration result
This special formula journey is brought into for water sample on-line measurement, calculates corresponding concentration value C.
The above is only preferred real mode of the invention, it is noted that for the ordinary skill of the art
For personnel, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications
It should be considered as protection scope of the present invention.
Claims (2)
1. a kind of 3 flow-type caliberating devices of sodium ion densimeter, including detected water sample inlet valve (1), level pressure overflow cup (2),
Water sample pipeline (3), alkalization device (5), temperature electrode (6), ion-selective electrode (7), reference electrode (8), contact conductor (9),
Intelligent high resistant millivoltmeter (10), flow type measuring cup (11), waste water collector (12) and overflow pipe (13), the detected water sample
Inlet valve (1) is arranged on water sample pipeline (3), level pressure overflow cup (2) arrival end and survey sample water inlet valve (1) outlet end
It is connected by water sample pipeline (3), level pressure overflow cup (2) outlet end and alkalization device (5) arrival end pass through water sample pipeline
(3) it connects, alkalization device (5) outlet end is connect with temperature electrode (6) by water sample pipeline (3), the temperature electricity
Pole (6) is connect with ion-selective electrode (7) by water sample pipeline (3), the ion-selective electrode (7) and reference electrode (8)
It is connected by water sample pipeline (3), the temperature electrode (6), ion-selective electrode (7) and reference electrode (8) are placed in flow type
In measuring cup (11), temperature electrode (6), ion-selective electrode (7) and the reference electrode (8) respectively with intelligent high resistant millivolt
Meter (10) is electrically connected by contact conductor (9), and the overflow port of the level pressure overflow cup (2) and waste water collector (12) are by overflowing
Flow tube (13) connection, characterized in that further include distributor (4), basic pattern solenoid valve (14), one solenoid valve of standard specimen (15), tested water
Sample solenoid valve (16), two solenoid valve of standard specimen (17), basic pattern reagent barrel (18), one reagent barrel of standard specimen (19), two reagent barrel of standard specimen
(20), on water sample pipeline (3) of the distributor (4) setting between connection level pressure overflow cup (2) and alkalization device (5), institute
Detected water sample solenoid valve (16) setting stated is on the water sample pipeline (3) between connection level pressure overflow cup (2) and distributor (4), institute
On the water sample pipeline (3) that the basic pattern solenoid valve (14) stated is arranged between basic pattern reagent barrel (18) and distributor (4), the standard specimen
On the water sample pipeline (3) that one solenoid valve (15) is arranged between one reagent barrel of standard specimen (19) and distributor (4), two electricity of standard specimen
On the water sample pipeline (3) that magnet valve (17) is arranged between two reagent barrel of standard specimen (20) and distributor (4), the reference electrode (8)
It is connect with waste water collector (12) by water sample pipeline (3), and water sample pipeline (3) is arranged in flow type measuring cup (11) bottom.
2. 3 flow-type caliberating devices of a kind of sodium ion densimeter according to claim 1, are characterized in：Its calibration side
Method is following steps：
1) 3 flow-types are prepared and demarcates standard water sample：
The benchmark water sample that Na ion concentration is 10-20 μ g/L is prepared with reagent water in laboratory, does not consider that reagent water sodium ion is dense
Degree, abbreviation basic pattern, taking Na ion concentration is the stock solution of 1000 μ g/L, dilutes 5 times with basic pattern, does not consider that basic pattern sodium ion is dense
Degree is configured to standard solution one, and abbreviation standard specimen one, taking Na ion concentration is the stock solution of 10mg/L, is diluted, is matched with 5 times of basic pattern
Standard solution two is made, does not consider basic pattern Na ion concentration, abbreviation standard specimen two；
2) basic pattern is added to the basic pattern reagent barrel (18) of instrument, and standard specimen one is added to one reagent barrel of standard specimen (19), and standard specimen two is added
Into two reagent barrel of instrument standard specimen (20)；
3) instrument enters calibration state, automatically shuts down detected water sample solenoid valve (16), and standard specimen one inputs 200 μ g/L；Standard specimen two is defeated
Enter 2000 μ g/L；
4) basic pattern solenoid valve (14) is opened, one solenoid valve of standard specimen (15), detected water sample solenoid valve (16), two solenoid valve of standard specimen (17)
It is closed with detected water sample inlet valve (1), basic pattern enters and rinse distributor (4), water sample pipeline (3), alkalization device (5), to base
Sample alkalizes, the formula that circulates measuring cell (11), and intelligent high resistant millivoltmeter (10) starts to detect and show basic pattern temperature T1With
Electromotive force Es, time stablized to 25 minutes Es, the Es of intelligent high resistant millivoltmeter (10) stable storage；
5) one solenoid valve of standard specimen (15) is opened, basic pattern solenoid valve (14), detected water sample solenoid valve (16), two solenoid valve of standard specimen (17)
It is closed with detected water sample inlet valve (1), standard specimen one enters and rinse distributor (4), water sample pipeline (3), alkalization device (5), together
When alkalize to standard specimen one, the formula that circulates measuring cell (11), intelligent high resistant millivoltmeter (10), which is detected, simultaneously shows one electricity of standard specimen
Kinetic potential E1, the time to 20 minutes E1Stablize, the E of intelligent high resistant millivoltmeter (10) stable storage1；
6) two solenoid valve of standard specimen (17) is opened, basic pattern solenoid valve (14), one solenoid valve of standard specimen (15), detected water sample solenoid valve (16)
It is closed with detected water sample inlet valve (1), standard specimen two enters and rinse distributor (4), water sample pipeline (3), alkalization device (5), together
When alkalize to standard specimen two, the formula that circulates measuring cell (11), intelligent high resistant millivoltmeter (10), which is detected, simultaneously shows two electricity of standard specimen
Kinetic potential E2, the time to 15 minutes E2Stablize, the E of intelligent high resistant millivoltmeter (10) stable storage2；
7) according to Nernst equation, equation group is established：
Es=E0+S(T/298.15)log[Cs/Ciso]
E1=E0+S(T/298.15)log[(Cs+200)/Ciso]
E2=E0+S(T/298.15)log[(Cs+2000)/Ciso]
Es in formula --- basic pattern measures cell emf
E1--- standard specimen one measures cell emf
E2--- standard specimen two measures cell emf
E0--- the current potential of equipotential points
Cs--- the practical Na ion concentration of basic pattern, it is desirable that Cs≯40μg/L
Ciso--- the Na ion concentration (being determining value for determining electrode) of equipotential points
S --- conversion slope, the value and sodium selective electrode, the performance of reference electrode and water sample temperature have corresponding relationship, mark
S is determining numerical value after fixed
T --- water sample temperature
Intelligent high resistant millivoltmeter solves these three equations, obtains Cs, S and E0,
Bring calibration result into this special formula journey
E=E0+S(T/298.15)lgC/Ciso
Storage is used for water sample on-line measurement, calculates corresponding concentration value C in intelligent high resistant millivoltmeter.
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| CN111352058A (en) * | 2018-12-20 | 2020-06-30 | 恩德莱斯和豪瑟尔分析仪表两合公司 | Method for in-process calibration of a potentiometric sensor of a measuring device |
| CN113740407A (en) * | 2021-11-02 | 2021-12-03 | 南京柠檬科技发展有限公司 | Sodium ion concentration analysis measuring equipment |
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