CN106814151A - The measurement apparatus and measuring method of trace anion in a kind of strong basic reagent - Google Patents
The measurement apparatus and measuring method of trace anion in a kind of strong basic reagent Download PDFInfo
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- CN106814151A CN106814151A CN201510860646.1A CN201510860646A CN106814151A CN 106814151 A CN106814151 A CN 106814151A CN 201510860646 A CN201510860646 A CN 201510860646A CN 106814151 A CN106814151 A CN 106814151A
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Abstract
The present invention relates to a kind of large reagent measuring field of nuclear power plant's core level, and in particular to the measurement apparatus and measuring method of trace anion in a kind of strong basic reagent.A kind of measurement apparatus of trace anion in strong basic reagent, the device includes suppressor control unit, sample injection unit, suppresses unit, sample bottle, and suppressor control unit is connected to the data-interface for suppressing unit；Sample bottle is connected to the plunger displacement pump pump head arrival end of sample injection unit, and the plunger displacement pump pump head port of export of sample injection unit is connected to the sample inlet for suppressing unit；Suppress sample sealing receiving flask after the sample export connection treatment of unit.The problems such as device and method solves the trace anion Monitoring lower-cut of the large reagent of Nuclear Power Station grade higher than control limit, eliminates and is present in primary Ioops and the impure risk for causing water chemistry control out of control of secondary circuit addition reagent in nuclear power station.
Description
Technical field
The present invention relates to a kind of large reagent measuring field of nuclear power plant's core level, and in particular to a kind of strong basic reagent
The measurement apparatus and measuring method of middle trace anion.
Background technology
Large reagent that field gulf nuclear power station is used refers to be directly appended in primary Ioops and secondary circuit, Yi Jiyong
The general designation of the chemical reagent used in the batch of the purposes such as resin treatment.As process system chemistry addition reagent
The chemical reagent for being added to primary Ioops and secondary circuit has 4 kinds.4 kinds of primary Ioops：Boric acid, potassium hydroxide,
Ammoniacal liquor, hydrazine；2 kinds of secondary circuit：Ammoniacal liquor, hydrazine；Reagent for water process has：NaOH, salt
Acid, nitric acid.The hydrochemical purpose of control nuclear power plant, is to exempt from destruction in order to avoid equipment occurs corrosion,
Ensure that power plant safety is stabilized the economy operation.When primary Ioops and secondary coolant circuit system run at high temperature under high pressure, in order to
Maintaining chemical working condition control needs to add a large amount of above-mentioned large reagents, and due to production technology and the limit of cost
System, even the large reagent of core level can also have impurity.Particularly it is directly added into large examination of one, secondary circuit
Agent boric acid, hydrogen-oxygen agent, hydrazine, ammoniacal liquor quality control it is critically important, and wherein in the large reagent of strong basicity
The trace analysis of anionic impurity can not meet domestic new nuclear power station relative to external or slower development
The demand supervised with supercritical unit.
Wherein field gulf nuclear power station one, the system such as secondary circuit medicine system such as QCE, QCF, KBD clearly will
The content of control anion is sought, and the GB analysis method of trace anion is traditional in high purity reagent at present
Wet chemistry method (turbidimetry and colorimetric method) and the chromatography of ions.The analysis of conventional anion includes F-、Cl-、SO4 2-、
NO3 -、PO4 3-Deng multiple projects.In traditional wet chemical method, nephelometer or ultraviolet-visible light splitting are used
Detection of the photometer to chlorion uses silver nitride precipitation than turbid method, and sulfate radical uses chlorination precipitated barium ratio
Turbid method, using than turbid detection limit for height, such as the turbidimetry detection minimum 0.2mg/L of chlorion, sulfate radical 0.4
Mg/L, and the influence of many factors such as temperature, time, acidity is easily subject to, detect cumbersome, it is actual
Operation is often up to offline less than theoretical detection, and the test limit of colorimetric method is also often up to the concentration less than trace,
Can only also detect single ion every time.
Conventional ion chromatographic method measures potassium hydroxide due to the limitation of drip washing system and present analysis technology
The trace anion of large reagents such as solid, lithium hydroxide solid, high concentration ammoniacal liquor, high concentration hydrazine solution
During content, because the concentration of the hydroxide ion in such concentrated base sample is far above in ion chromatogram eluate
Concentration, directly can cause component retention time to shorten using chromatography of ions measurement, and baseline is irregular and can not be complete
Fully separating, background conductance increase cannot accurately measure the content of each component to be measured, even if dilution measurement also can
Cause measurement result poor reproducibility because peak type is poor, shift to an earlier date appearance, Monitoring lower-cut is higher than the problems such as control is limited.
By taking ammoniacal liquor as an example, the high strength ammonia water sample of 25%-28% is diluted to fairly small concentration (0.05%),
Analysis of spectra is shown in Fig. 1.
Even if 25% high concentration ammoniacal liquor is diluted to 0.05% low concentration solution as can be seen from Figure, it is cloudy from
Sub- appearance peak shape or very poor, unstability of base line.Leacheate brings component to be measured into analytical column during this analysis
While also brought the high alkalinity in sample solution into analytical column, and adopted during by analysis anion-content
Leacheate is also simultaneously alkaline solution, and so two kinds of alkalescence are superimposed so that the intensity of leacheate
Increase, the also just corresponding enhancing of drip washing ability, the consequence brought therewith is component to be measured after post by analysis
Can not be completely segregated, that is, enable and separate, that must also result in each component appearance time and much shift to an earlier date in mark
Quasi- appearance, and can greatly increase background conductance so cannot just to accurately measure each component to be measured
Content, and dilution ratio is up to 500 times, detects that offline is 1mg/L (as chloride ion), and field gulf core
Power station chemical supervision requirement Cl-≤ 500ug/L, it is impossible to meet power station requirement.Similarly, analysis potassium hydroxide, connection
This phenomenon also can all occur in the large reagent of strong basicity during ammonia solution etc..The reappearance of the method analysis result is poor,
Precision of analysis is poor, and recovery of standard addition has that analysis is out of control between 60-120%.
Problem above can cause the core large reagent of level into factory's supply cannot accurately to carry out quantitative analysis, so that
In the presence of the risk that anionic impurity is introduced to nuclear power plant's primary Ioops and secondary circuit, primary Ioops material can be caused to occur
Stress-corrosion cracking, secondary circuit the steam generator heat-transfer pipe risk that once lateral secondary circuit side is revealed, directly
Have impact on the safe operation of nuclear power station.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of measurement apparatus of trace anion in strong basic reagent
And measuring method, being neutralized without reagent for high concentration basic solution is solved, do not introducing the situation of contaminated ion
Lower elimination OH-The interference of matrix, while removing the heavy metal cation of influence ion chromatography post post effect.
The detection for reducing chromatography of ions instrument is offline, is analyzed using Large Copacity quantitative loop or evaporating column, while
Ensure reliability and accuracy high.
In order to solve the above technical problems, in a kind of strong basic reagent of the invention trace anion measurement apparatus,
The device includes suppressor control unit, sample injection unit, suppresses unit, sample bottle, suppressor control unit
It is connected to the data-interface for suppressing unit；Sample bottle is connected to the plunger displacement pump pump head arrival end of sample injection unit, enters
The plunger displacement pump pump head port of export of sample unit is connected to the sample inlet for suppressing unit；Suppress the sample export of unit
Sample sealing receiving flask after connection treatment.
Described suppressor electrolysis liquid control system, electrolyte bottle, electrolyte bottle is connected to suppressor electricity
The Peristaltic pump head arrival end of pole control system for electrolyte；The peristaltic pump of suppressor electrolysis liquid control system
The pump head port of export is connected to the electrolyte entrance for suppressing unit；Suppress the electrolyte outlet connection electrolyte of unit
Waste discharge pipeline.
The measuring method of the measurement apparatus of trace anion in a kind of strong basic reagent, specifically include following step
Suddenly：
Step one, using it is preceding rinse suppress unit, sample bottle is loaded into high purity water, sample line is put after treatment
Enter in waste liquid cup, open the peristaltic pump of suppressor electrolysis liquid control system, be then then turned on suppressor control
Unit power supply processed, circulation flushing；Flushing closes suppressor control unit and peristaltic pump after terminating；
Step 2, take appropriate amount of sample dilution after, be put into sample bottle, record extension rate；
Step 3, sample bottle is connected and is put into repacking, sample line is put into waste liquid cup after treatment, opens suppression
The peristaltic pump of device electrolysis liquid control system processed, is then then turned on suppressor control unit power supply, after sample preparation
Nesting tube is inserted after cleaned treatment in sample sealing receiving flask, sample preparation is once to the upper of receiving flask
Graduation mark, and sample pH value is measured with test paper, pH≤8 item are directly entered chromatography of ions measurement, if be unsatisfactory for
It is required that then entering step 4；
Step 4, sample bottle is laid down, sample sealing receiving flask after the treatment in step 3 is replaced into sample bottle
Position, by sample sealing receiving flask after the cleaned new treatment of sample line insertion after treatment, opens suppression
The peristaltic pump of device electrolysis liquid control system processed, is then then turned on suppressor control unit power supply, then treat from
Sub- chromatogram measurement, if being unsatisfactory for condition, repeat step four；
Step 5, the sample become reconciled by, are measured with the ion chromatograph with evaporating column, and record is surveyed
Amount result, final result will be multiplied by extension rate.
Sample sealing receiving flask and fall sample bottle and all carry out high purity water and repeatedly rinse after the treatment for being used, and point
Analysis background level.
In the step 2, the extension rate of raw sample is controlled below 10 times.
Advantageous Effects of the invention are：Anion trace is fast in working out a kind of strong basicity high purity reagent
Fast detection technique, its Monitoring lower-cut, the degree of accuracy, precision and stability from far away exceed it is domestic at this stage
Detection technique.Detection limit can as little as 0.10ug/L, recovery of standard addition in the range of 100% ± 3%, measurement range
According to the difference of dilution ratio, can be with wide in range to 0-50mg/L, precision is inclined with the relative standard of 10 measurements
Difference assessment RSD≤3%, with excellent reappearance and stability.New method is in trace anion detection field
With epoch-making effect, a fast, two steady, analytical technologies for the triathlon of three standards are reached, solved
The problems such as trace anion Monitoring lower-cut of the large reagent of Nuclear Power Station level is higher than control limit, eliminates and is present in
Primary Ioops and secondary circuit add the impure risk for causing water chemistry control out of control of reagent in nuclear power station.
Brief description of the drawings
Fig. 1 be diluted to 0.05% ammoniacal liquor anion chromatographic figure；
Fig. 2 is a kind of schematic diagram of the measurement apparatus of trace anion in strong basic reagent.
In figure：1st, suppressor control unit 2, suppressor electrolysis liquid control system 3, peristaltic pump
First 4, wriggling pump controller 5, sample injection unit 6, plunger displacement pump pump head 7, sample introduction pump controller 8, sample introduction
Sample sealing receiving flask 12, electrolyte waste pipe after pipeline 9, sample bottle 10, suppression unit 11, treatment
Electrolyte line 16 after sample line 15, peristaltic pump after line 13, suppressor control data line 14, treatment,
Electrolyte connecting pipeline 17, electrolyte bottle.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
The measurement apparatus of trace anion in a kind of strong basic reagent, including suppressor control unit 1, suppressor
Electrolysis liquid control system 2, sample injection unit 5, suppression unit 10, sample bottle 9, electrolyte bottle 17, suppression
Device control unit 1 processed is connected to the data-interface for suppressing unit 10 by cable, to suppressor control unit 1
There is provided and suppress signal and suppression electric current；Electrolyte bottle 17 is connected to suppressor by electrolyte connecting pipeline 16
The arrival end of Peristaltic pump head 3 of electrolysis liquid control system 2；Suppressor electrolysis liquid control system 2
The port of export of Peristaltic pump head 3 by electrolyte line after peristaltic pump 15 be connected to suppress unit 10 electrolysis
Liquid entrance；Suppress the electrolyte outlet connection electrolyte waste discharge pipeline 12 of unit 10；Sample bottle 9 passes through sample introduction
Pipeline is connected to the arrival end of plunger displacement pump pump head 6 of sample injection unit 5, and the plunger displacement pump pump head 6 of sample injection unit 5 goes out
Mouth end is connected to the sample inlet for suppressing unit 10 by sample introduction pipeline 8；Suppress the sample export of unit 10
Sample seals receiving flask 11 after the connection of sample line after treatment 14 is processed.
Step one, using it is preceding rinse suppress unit 10, by neutralize module sample bottle 9 load high purity water, locate
Sample line 14 is put into waste liquid cup after reason, the peristaltic pump of suppressor electrolysis liquid control system is opened,
Then the power supply of suppressor control unit 1, circulation flushing 20min or so are then turned on；Flushing closes suppression after terminating
Device control unit 1 processed and peristaltic pump；
Step 2, take appropriate amount of sample (KOH, LiOH, NH3H2O or N2H4) be diluted to 2% or so it is dense
After degree, it is put into sample bottle 9, records extension rate；
Step 3, sample bottle 9 is connected and is put into repacking, sample line 14 is put into waste liquid cup after treatment,
The peristaltic pump of suppressor electrolysis liquid control system is opened, the power supply of suppressor control unit 1 is then then turned on,
Nesting tube is inserted after cleaned treatment in sample sealing receiving flask 11 after sample preparation 10min, sample preparation one
The secondary high scale line to receiving flask, and sample pH value is measured with test paper, pH≤8 item are directly entered chromatography of ions survey
Amount, enters step 4 if being unsatisfactory for requiring；
Step 4, sample bottle 9 is laid down, sample sealing receiving flask 11 after the treatment in step 3 is replaced into sample
The position of bottle 9, sample seals receiving flask 11 after sample line after treatment 14 is inserted into cleaned new treatment
In, the peristaltic pump of suppressor electrolysis liquid control system is opened, then it is then turned on suppressor control unit 1
Power supply, then treat that chromatography of ions is measured, if being unsatisfactory for condition, repeat step four；
Step 5, the sample become reconciled by, are measured with the ion chromatograph with evaporating column, and record is surveyed
Amount result, final result will be multiplied by extension rate.
Sample sealing receiving flask 11 and fall sample bottle 9 and all carry out high purity water and repeatedly rinse after the treatment for being used,
And analysis background level.
When pH test paper is checked, it is careful not to allow the outlet mouth of pipe directly to encounter pH test paper, in order to avoid stain.
All set with the parameter of module in suppressor pre-treatment, forbidden changing operation ginseng in measurement process
Number.
The extension rate of raw sample tries one's best control below 10 times, reduces systematic error.
Claims (5)
1. in a kind of strong basic reagent trace anion measurement apparatus, it is characterised in that：The device includes suppression
Device control unit (1) processed, sample injection unit (5), suppression unit (10), sample bottle (9), suppressor control
Unit (1) is connected to the data-interface for suppressing unit (10)；Sample bottle (9) is connected to sample injection unit (5)
Plunger displacement pump pump head (6) arrival end, plunger displacement pump pump head (6) port of export of sample injection unit (5) is connected to suppression
The sample inlet of unit (10) processed；Sample sealing is received after suppressing the sample export connection treatment of unit (10)
Collection bottle (11).
2. in a kind of strong basic reagent according to claim 1 trace anion measurement apparatus, it is special
Levy and be：Described suppressor electrolysis liquid control system (2), electrolyte bottle (17), electrolyte bottle (17)
It is connected to Peristaltic pump head (3) arrival end of suppressor electrolysis liquid control system (2)；Suppressor electricity
Peristaltic pump head (3) port of export of pole control system for electrolyte (2) is connected to the electricity for suppressing unit (10)
Solution liquid entrance；The electrolyte outlet for suppressing unit (10) connects electrolyte waste discharge pipeline (12).
3. in a kind of strong basic reagent of usage right requirement any one of 1-2 trace anion measurement apparatus
Measuring method, it is characterised in that specifically include following steps：
Step one, using it is preceding rinse suppress unit (10), by sample bottle (9) load high purity water, after treatment
Sample line (14) is put into waste liquid cup, opens the peristaltic pump of suppressor electrolysis liquid control system, so
After be then turned on suppressor control unit (1) power supply, circulation flushing；Suppressor control is closed in flushing after terminating single
First (1) and peristaltic pump；
Step 2, take appropriate amount of sample dilution after, be put into sample bottle (9), record extension rate；
Step 3, sample bottle (9) is connected and is put into repacking, sample line (14) is put into waste liquid cup after treatment
In, the peristaltic pump of suppressor electrolysis liquid control system is opened, then it is then turned on suppressor control unit (1)
Power supply, inserts during sample after cleaned treatment seals receiving flask (11) nesting tube after sample preparation, sample system
The standby high scale line for once arriving receiving flask, and sample pH value is measured with test paper, pH≤8 item are directly entered ion color
Spectrometry, enters step 4 if being unsatisfactory for requiring；
Step 4, sample bottle (9) is laid down, sample after the treatment in step 3 is sealed into receiving flask (11) replaces
The position of sample bottle (9) is changed, by sample after the cleaned new treatment of sample line after treatment (14) insertion
In sealing receiving flask (11), the peristaltic pump of suppressor electrolysis liquid control system is opened, be then then turned on
Suppressor control unit (1) power supply, then treat that chromatography of ions is measured, if being unsatisfactory for condition, repeat step four；
Step 5, the sample become reconciled by, are measured with the ion chromatograph with evaporating column, and record is surveyed
Amount result, final result will be multiplied by extension rate.
4. in a kind of strong basic reagent according to claim 3 trace anion measuring method, it is special
Levy and be：Sample seals receiving flask (11) and falls sample bottle (9) after the treatment for being used all carries out high purity water
Repeatedly rinse, and analysis background level.
5. in a kind of strong basic reagent according to claim 4 trace anion measuring method, it is special
Levy and be：In the step 2, the extension rate of raw sample is controlled below 10 times.
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| CN108152438A (en) * | 2017-11-17 | 2018-06-12 | 海南核电有限公司 | The analysis method of anion-content in a kind of high-concentration alkali liquor |
| CN110320312A (en) * | 2019-06-26 | 2019-10-11 | 中核霞浦核电有限公司 | The detection method of trace chlorine content in a kind of nuclear leve metallic sodium |
| CN111735882A (en) * | 2020-07-01 | 2020-10-02 | 沧州信联化工有限公司 | High-purity TMAH reagent ion chromatography detection device and detection method thereof |
| CN112834664A (en) * | 2021-03-02 | 2021-05-25 | 青岛盛瀚色谱技术有限公司 | Anion analysis pretreatment system and method for metal ion enrichment solution |
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| CN112834664A (en) * | 2021-03-02 | 2021-05-25 | 青岛盛瀚色谱技术有限公司 | Anion analysis pretreatment system and method for metal ion enrichment solution |
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