CN109211813A - The measurement method of lithium content in PWR of Nuclear Power Station unit coolant - Google Patents
The measurement method of lithium content in PWR of Nuclear Power Station unit coolant Download PDFInfo
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Abstract
The present invention relates to nuclear power plant's core supplement heat rejecter agent systems technology field, provide a kind of measurement method of lithium content in PWR of Nuclear Power Station unit coolant, include the following steps: to prepare multiple elemental lithium concentration are different and the identical calibration solution of boron element concentration；The absorbance for testing multiple calibration solution establishes the relation function of absorbance Yu elemental lithium concentration according to the absorbance of multiple calibration solution and elemental lithium concentration；Measure the initial boron concentration of element in coolant sample；The boron element concentration in coolant sample is adjusted, so that its boron element concentration is identical as the boron element concentration in calibration solution, obtains pretreatment coolant sample；The absorbance of test pretreatment coolant sample, and the elemental lithium concentration in pretreatment coolant sample is obtained according to its absorbance and above-mentioned relation function；Calculate dilution ratio；The elemental lithium concentration in coolant sample is obtained according to the elemental lithium concentration in dilution ratio and pretreatment coolant sample.
Description
Technical field
The present invention relates to nuclear power plant's core supplement heat rejecter agent systems technology fields, more particularly to a kind of PWR of Nuclear Power Station machine
The measurement method of lithium content in group coolant.
Background technique
The pH value that the presurized water reactor unit in nuclear power base carries out primary Ioops coolant usually using lithium hydroxide is adjusted, in
With the acidity introduced due to addition boric acid, make coolant in alkalescent, to reduce the equipment surface and combustion of primary Ioops system
Expect the corrosion rate of involucrum.In a fuel recycle of presurized water reactor unit, with the variation of fuel burn-up, primary Ioops coolant
In boric acid content may also change accordingly, therefore the lithium hydroxide content that must be also adjusted in synchronism in coolant is so that the two phase
Match.Therefore, the lithium content accurately in measurement primary Ioops coolant is an important ring for accuracy controlling primary Ioops coolant pH value.
In the measurement method of traditional technology, the coolant sample of compacted clay liners primary Ioops is carrying out lithium content measurement
Preceding progress acidification, then directly measures, but the accuracy that this measurement method is measured there are lithium content is not high
Defect is not easy to accurately adjust the lithium content in presurized water reactor primary Ioops coolant.
Summary of the invention
Based on this, it is necessary to provide a kind of survey of lithium content in the PWR of Nuclear Power Station unit coolant that measurement accuracy is high
Amount method.
The measurement method of lithium content, includes the following steps: in a kind of PWR of Nuclear Power Station unit coolant
Multiple calibration solution containing elemental lithium and boron element are prepared, the elemental lithium concentration in multiple calibration solution is not
Together, the boron element concentration and in multiple calibration solution is identical；
The absorbance for testing multiple calibration solution, according to the absorbance of multiple calibration solution and multiple schools
The elemental lithium concentration in quasi- solution establishes the relation function of absorbance Yu elemental lithium concentration；
Measure the initial boron concentration of element in coolant sample；
The boron element concentration in the coolant sample is adjusted, so that boron element concentration and institute in the coolant sample
The boron element concentration stated in calibration solution is identical, obtains pretreatment coolant sample；
Test it is described pretreatment coolant sample absorbance, and according to it is described pretreatment coolant sample absorbance and
The relation function of the absorbance and elemental lithium concentration obtains the elemental lithium concentration in the pretreatment coolant sample；
According to the Mass Calculation dilution ratio of the quality of the pretreatment coolant sample and the coolant sample, or
Dilution ratio is calculated according to the volume of the volume of the pretreatment coolant sample and the coolant sample；According to the dilution
Elemental lithium concentration calculation in multiplying power and the pretreatment coolant sample obtains the elemental lithium concentration in the coolant sample.
The measurement method of lithium content, dense according to the boron element in standard solution in above-mentioned PWR of Nuclear Power Station unit coolant
Degree makes the boron member in the boron element concentration and calibration solution in coolant sample to adjust the boron element concentration in coolant sample
Plain concentration is identical to obtain pretreatment coolant sample, so that in the matrix composition and calibration solution in pretreatment coolant sample
Matrix composition reach unanimity, eliminate caused by matrix difference interference and influence, so that in measurement pretreatment coolant sample
Absorbance when accuracy improve, and then improve the accuracy that lithium content in coolant measures, be more convenient for accurately adjusting core
Lithium content in power station PWR unit coolant.
The step of preparation multiple calibration solution containing elemental lithium and boron element wrap in one of the embodiments,
It includes: being separately added into the aqueous solution of boric acid into multiple solution containing elemental lithium, make in multiple solution containing elemental lithium
Boron element concentration is identical and elemental lithium concentration is different, obtain multiple calibration solution.
The step of preparation multiple calibration solution containing elemental lithium and boron element wrap in one of the embodiments,
It includes: boric acid being placed in pure water and is dissolved, be configured to the aqueous solution of the boric acid；Add respectively into multiple solution containing elemental lithium
The aqueous solution for entering the boric acid keeps the boron element concentration in multiple solution containing elemental lithium identical, obtains multiple described
Calibrate solution, wherein the elemental lithium concentration in multiple solution containing elemental lithium is different.
The step of preparation multiple calibration solution containing elemental lithium and boron element wrap in one of the embodiments,
It includes: being separately added into boric acid into multiple solution containing elemental lithium and dissolve, make in multiple solution containing elemental lithium
Boron element concentration is identical, obtains multiple calibration solution, wherein the elemental lithium in multiple solution containing elemental lithium is dense
Degree is different.
The step of absorbance of the multiple calibration solution of the test includes: using former in one of the embodiments,
Sub- absorption spectrometry measures the absorbance of multiple calibration solution.
In one of the embodiments, the step of boron element concentration adjusted in the coolant sample include: to
Diluent is added in the coolant sample to adjust the boron element concentration in the coolant sample, wherein the diluent
At least one of aqueous solution selected from pure water and boric acid, and the boron element concentration in the aqueous solution of the boric acid is greater than the school
Boron element concentration in quasi- solution.
The boron element concentration adjusted in the coolant sample in one of the embodiments, so that the cooling
The step of boron element concentration in agent sample is identical as the boron element concentration in calibration solution, obtains pretreatment coolant sample packet
It includes:
Compare the boron element concentration in the initial boron concentration of element and the calibration solution in the coolant sample；
If the initial boron concentration of element in the coolant sample is greater than the boron element concentration in the calibration solution, to
The pure water is added in the coolant sample to adjust the boron element concentration in the coolant sample, makes the coolant sample
Boron element concentration in product is identical as the boron element concentration in the calibration solution；
If the initial boron concentration of element in the coolant sample is less than the boron element concentration in the calibration solution, to
The aqueous solution of the boric acid is added in the coolant sample to adjust the boron element concentration in the coolant sample, makes described
Boron element concentration in coolant sample is identical as the boron element concentration in the calibration solution.
The boron element concentration adjusted in the coolant sample in one of the embodiments, so that the cooling
The step of boron element concentration in agent sample is identical as the boron element concentration in calibration solution, obtains pretreatment coolant sample packet
It includes:
Compare the initial boron concentration of element in the coolant sample and preset boron element concentration, wherein described default
Boron element concentration be greater than it is described calibration solution in boron element concentration；
If the initial boron concentration of element in the coolant sample is greater than or equal to the preset boron element concentration, root
The coolant sample that part is taken out according to the first formula, is added the pure water so as to take into the coolant sample of taking-up
The boron element concentration in the coolant sample out is identical as the boron element concentration in calibration solution, and it is cold to obtain the pretreatment
But agent sample；
If the initial boron concentration of element in the coolant sample is less than the preset boron element concentration, according to second
Formula takes out the coolant sample of part, and the pure water and the boric acid are added into the coolant sample of taking-up
Aqueous solution so that take out the coolant sample in boron element concentration with calibrate solution in boron element concentration it is identical, obtain
The pretreatment coolant sample；Wherein, the additional amount of the aqueous solution of the boric acid is calculated according to third formula；
First formula are as follows: X=PB*Z/CB, second formula are as follows: X=Z/2, the third formula are as follows: Y=X-
(X*CB)/YB；Wherein, X is the quality of the coolant sample taken out, PBFor the boron element concentration in the calibration solution, Z
For the quality of the pretreatment coolant sample, CBFor the boron element concentration in the coolant sample, Y is the boron being added
The quality of the aqueous solution of acid；YBFor the boron element concentration in the aqueous solution of the boric acid；Alternatively, X is the coolant taken out
The volume of sample, PBFor the boron element concentration in the calibration solution, Z is the volume of the pretreatment coolant sample, CBFor institute
The boron element concentration in coolant sample is stated, Y is the volume of the aqueous solution for the boric acid being added, YBFor the water-soluble of the boric acid
Boron element concentration in liquid.
In one of the embodiments, the step of boron element concentration adjusted in the coolant sample include: to
The dust technology of diluent and predetermined amount is added in the coolant sample to adjust the boron element concentration in the coolant sample,
Wherein, the diluent is selected from least one of pure water and the aqueous solution of boric acid, and the boron member in the aqueous solution of the boric acid
Plain concentration is greater than the boron element concentration in the calibration solution.
Detailed description of the invention
Fig. 1 is the measuring method flow chart of lithium content in the PWR of Nuclear Power Station unit coolant of an embodiment；
Fig. 2 is the calibration curve in the PWR of Nuclear Power Station unit coolant of an embodiment in the measurement method of lithium content
Figure；
Fig. 3 is the calibration graph in the PWR of Nuclear Power Station unit coolant of comparative example 1 in the measurement method of lithium content.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing
Give preferred embodiment of the invention.But the invention can be realized in many different forms, however it is not limited to herein
Described embodiment.On the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more saturating
It is thorough comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
Inventor has found in practical work process, due to the boric acid containing higher concentration in primary Ioops coolant sample,
And boric acid can have an impact lithium content measurement, it is therefore desirable in a series of schools that the measuring instruments such as Atomic Absorption Spectrometer use
A certain amount of boric acid is added in quasi- solution respectively, so that the matrix of calibration solution and coolant sample composition reaches unanimity.But by
In in a fuel recycle, the boron element concentration in primary Ioops coolant sample is consecutive variations, the cooling measured every time
Boron element concentration in agent sample is all different, and is reconfigured calibration solution before measurement every time and is implemented extremely difficult, general
Lead to the consumption of a large amount of manpowers and calibrate the waste of solution, can only several different boron element concentration of subsection setup calibration solution system
Column, this causes when most of actual measurements, coolant sample and calibration solution in matrix composition be still it is discrepant,
To affect the accuracy of lithium content measurement.Simultaneously as it is dense to be provided with several different boron elements in a fuel recycle
The calibration solution series of degree will lead to the measurement result of coolant sample when switching in two calibration solution series
There is a more apparent step, the continuity of lithium content data is bad, this makes nuclear power plant chemist accurately adjust one
Lithium content in the coolant of circuit is more difficult.
Therefore, inventor improves the measurement method of lithium content in PWR of Nuclear Power Station unit coolant, so as to
The lithium content in PWR of Nuclear Power Station unit coolant is accurately adjusted in nuclear power plant chemist.
Refering to fig. 1, the measurement method of lithium content includes as follows in the PWR of Nuclear Power Station unit coolant of an embodiment
Step:
S110, multiple calibration solution containing elemental lithium and boron element, the elemental lithium concentration in multiple calibration solution are prepared
Difference, and the boron element concentration in multiple calibration solution is identical.
In one of the embodiments, in step S110, multiple calibration solution containing elemental lithium and boron element are prepared
Step includes: the aqueous solution that boric acid is separately added into multiple solution containing elemental lithium, makes multiple solution containing elemental lithium
In boron element concentration is identical and elemental lithium concentration is different, obtain multiple calibration solution.Wherein, the boron element calibrated in solution is dense
Degree can be configured according to specific needs.Specifically, first boric acid can be placed in pure water and is dissolved, be configured to the water-soluble of boric acid
Liquid；Then it is separately added into the aqueous solution of boric acid into multiple solution containing elemental lithium, makes in multiple solution containing elemental lithium
Boron element concentration it is identical, obtain multiple calibration solution, wherein the elemental lithium concentration in multiple solution containing elemental lithium is not
Together.Further, prepare calibrate solution when, aqueous solution in addition to boric acid is added into the solution containing elemental lithium can be with
A small amount of 68% nitric acid and pure water are added into the solution containing elemental lithium.
Alternatively, the step of preparing multiple calibration solution containing elemental lithium and boron element may also is that multiple containing lithium
It is separately added into boric acid in the solution of element and dissolves, keeps the boron element concentration in multiple solution containing elemental lithium identical, obtains
Multiple calibration solution, wherein the elemental lithium concentration in multiple solution containing elemental lithium is different.
The absorbance of S120, the multiple calibration solution of test, according to the absorbance of multiple calibration solution and multiple calibration solution
In elemental lithium concentration establish the relation function of absorbance Yu elemental lithium concentration.In one of the embodiments, in step S120,
The step of testing the absorbance of multiple calibration solution includes: the extinction using the multiple calibration solution of aas determination
Degree.
Initial boron concentration of element in S130, measurement coolant sample.Specifically, titration or other surveys can be passed through
Amount method measures the initial concentration of the boron in coolant sample, the present embodiment to this with no restriction.
Boron element concentration in S140, adjusting coolant sample, so that boron element concentration and calibration in coolant sample
Boron element concentration in solution is identical, obtains pretreatment coolant sample.
Specifically, the step of adjusting the boron element concentration in coolant sample includes: that dilution is added into coolant sample
Agent is to adjust the boron element concentration in coolant sample, wherein at least one in aqueous solution of the diluent selected from pure water and boric acid
Kind, and the boron element concentration in the aqueous solution of boric acid is greater than the boron element concentration in calibration solution.
In some embodiments, the boron element concentration in coolant sample is adjusted, so that the boron element in coolant sample
Concentration with calibration solution in boron element concentration it is identical, obtain pretreatment coolant sample the step of include:
Compare the boron element concentration in the initial boron concentration of element and calibration solution in coolant sample；
If the initial boron concentration of element in coolant sample is greater than the boron element concentration in calibration solution, to coolant sample
Addition pure water makes the boron element concentration in coolant sample and calibrates molten in product to adjust the boron element concentration in coolant sample
Boron element concentration in liquid is identical；
If the initial boron concentration of element in coolant sample is less than the boron element concentration in calibration solution, to coolant sample
The aqueous solution of boric acid is added in product to adjust the boron element concentration in coolant sample, makes the boron element concentration in coolant sample
It is identical as the boron element concentration in calibration solution.
In further embodiments, the boron element concentration in coolant sample is adjusted, so that the boron member in coolant sample
Plain concentration with calibration solution in boron element concentration it is identical, obtain pretreatment coolant sample the step of include:
Compare the initial boron concentration of element in coolant sample and preset boron element concentration, wherein preset boron element
Concentration is greater than the boron element concentration in calibration solution.Specifically, presetting boron element concentration can be configured according to specific needs,
As long as guaranteeing the boron element concentration that default boron element concentration is greater than in calibration solution.
If the initial boron concentration of element in coolant sample is greater than or equal to preset boron element concentration, according to the first public affairs
Formula take out part coolant sample, into the coolant sample of taking-up be added pure water so that take out coolant sample in boron
Concentration of element is identical as the boron element concentration in calibration solution, obtains pretreatment coolant sample；
If the initial boron concentration of element in coolant sample is less than preset boron element concentration, taken out according to the second formula
The aqueous solution of pure water and boric acid is added into the coolant sample of taking-up so that the coolant sample taken out for partial coolant sample
Boron element concentration in product is identical as the boron element concentration in calibration solution, obtains pretreatment coolant sample；Wherein, boric acid
The additional amount of aqueous solution is calculated according to third formula；
First formula are as follows: X=PB*Z/CB, the second formula are as follows: X=Z/2, third formula are as follows: Y=X- (X*CB)/YB；Its
In, X is the quality of the coolant sample taken out, PBFor the boron element concentration in calibration solution, Z is pretreatment coolant sample
Quality, CBFor the boron element concentration in coolant sample, Y is the quality of the aqueous solution for the boric acid being added, YBFor the aqueous solution of boric acid
In boron element concentration；Alternatively, X is the volume of the coolant sample taken out, PBFor the boron element concentration in calibration solution, Z is
Pre-process the volume of coolant sample, CBFor the boron element concentration in coolant sample, Y is the body of the aqueous solution for the boric acid being added
Product, YBFor the boron element concentration in the aqueous solution of boric acid.
It should be noted that due to the magnitude of the various solution of addition can not accomplish completely it is consistent with the value of theoretical calculation,
So in certain allowed band, as long as the actual additional amount of accurate recording, so that it may accurately calculate dilution ratio, and then basis
Elemental lithium concentration in dilution ratio and pretreatment coolant sample obtains the elemental lithium concentration in coolant sample.
In traditional PWR of Nuclear Power Station unit coolant in the measurement method of lithium content, in measurement PWR of Nuclear Power Station machine
Only to simple acidification has been carried out in coolant sample before lithium content in group coolant sample, in order to directly use
Measuring instrument measures, and needs to be arranged higher by the concentration for calibrating solution, so that the elemental lithium of the calibration curve obtained is dense
Degree highest point can cover the elemental lithium concentration in coolant sample.But in the measuring instrument of some models, the response of instrument
It is worth excessively high, causes the calibration curve obtained apparent bending occur, level of linearity is bad, so as to cause the accurate of lithium content measurement
Property decline.And in the present embodiment, in the pretreatment coolant sample that can guarantee by the above scheme of the present embodiment
Elemental lithium concentration be less than the highest elemental lithium concentration in calibration solution series, therefore the highest lithium member of calibration solution can be reduced
Plain concentration makes calibration solution that can obtain linear good calibration curve in various types of measuring instruments, thus calibrated
Measuring instrument after solution calibration can carry out the lithium content measurement in coolant sample in linear good region, improve cooling
The accuracy that lithium content measures in agent.
For example the measurement method of lithium content in the PWR of Nuclear Power Station unit coolant of the present embodiment is carried out below
Be described in detail: pure water uses pure water of the conductivity greater than 18M Ω cm at 25 DEG C, and the boron element concentration in the aqueous solution of boric acid is
1000mg/kg, the boron element concentration for calibrating solution is 500mg/kg, and preset boron element concentration is 800mg/kg, multiple calibrations
When elemental lithium concentration maxima in solution is 1.5mg/kg.In fact, as long as the boron element concentration in coolant sample is greater than
500mg/kg only can make the boron element concentration in coolant sample drop to 500mg/kg by the way that pure water is added, but due to
In chemical technology specification, there is the platform area of a lithium content when boron element concentration is near 800mg/kg, in this platform area
Lithium content can be stablized in the range of 2.0mg/kg~2.2mg/kg, if the boron element concentration in coolant sample is in 500mg/
The diluted mode of pure water is still used between kg~800mg/kg, dilution ratio can be made too small, to pre-process in coolant sample
Elemental lithium concentration measurement will be more than highest elemental lithium concentration in calibration solution, i.e., in the elemental lithium concentration in calibration curve
Limit 1.5mg/kg.It is advantageous to take boron element concentration 800mg/kg as line of demarcation, can guarantee in this way in full fuel recycle
In range, no matter the boron element concentration of coolant sample is how many, can guarantee that the elemental lithium in pretreatment coolant sample is dense
It spends measured value and is less than 1.5mg/kg.
The step of adjusting the boron element concentration in coolant sample in one of the embodiments, includes: to coolant sample
The dust technology of diluent and predetermined amount is added in product to adjust the boron element concentration in coolant sample, wherein diluent is selected from
At least one of pure water and the aqueous solution of boric acid, and the boron element concentration in the aqueous solution of boric acid is greater than the boron in calibration solution
Concentration of element.Specifically, the predetermined amount of dust technology can be 2mL.
The measurement method dosing accuracy of lithium content is bad in traditional PWR of Nuclear Power Station unit coolant, affects cold
But the accuracy of agent sample lithium content measurement.And before the lithium content of measurement primary Ioops coolant sample, it needs to coolant
Dust technology is added in sample and carries out acidification, so that coolant sample keeps the acidic environment as calibration solution.In order to
The acidic environment in sample is kept, while can guarantee that the accuracy of lithium content measurement can be with to meet pretreatment coolant sample again
Demand measured directly, the present embodiment are pre- by being added during by coolant sample preparation at pretreatment coolant sample
If the dust technology of amount is acidified coolant sample, allow the acidification of coolant sample boron in adjusting coolant sample
It is synchronously completed during concentration of element, to keep dosing process more accurate, improves the standard that lithium content measures in coolant
True property.
The absorbance of S150, test pretreatment coolant sample, and according to the absorbance and suction of pretreatment coolant sample
Luminosity and the relation function of elemental lithium concentration obtain the elemental lithium concentration in pretreatment coolant sample.Specifically, it can use
The absorbance of the multiple calibration solution of aas determination, i.e., measure multiple calibration solution using Atomic Absorption Spectrometer
Absorbance.
S160, it is diluted again according to the quality of the pretreatment coolant sample and the Mass Calculation of the coolant sample
Rate, or dilution ratio is calculated according to the volume of the pretreatment coolant sample and the volume of the coolant sample.Specifically
Ground, dilution ratio is the ratio of the quality for pre-processing coolant sample and the quality of coolant sample or dilution ratio is pre-
Handle the ratio of the volume of coolant sample and the volume of coolant sample.
S170, it is obtained in coolant sample according to the elemental lithium concentration calculation in dilution ratio and pretreatment coolant sample
Elemental lithium concentration.Specifically, the product for pre-processing elemental lithium concentration and dilution ratio in coolant sample is coolant sample
Elemental lithium concentration in product, according to the elemental lithium concentration in coolant sample it can be learnt that in PWR of Nuclear Power Station unit coolant
Lithium content.
In above-mentioned PWR of Nuclear Power Station unit coolant in the measurement method of lithium content, according to the boron member in standard lithium solution
Plain concentration adjusts the boron element concentration in coolant sample, so that in boron element concentration in coolant sample and calibration solution
Boron element concentration it is identical so that pretreatment coolant sample in matrix composition with calibration solution in matrix composition tend to one
It causes, eliminate interference caused by matrix difference and influences, improve the accuracy that lithium content measures in coolant, it is accurate to be more convenient for
Adjust the lithium content in PWR of Nuclear Power Station unit coolant；And operation is simpler, solves needs according to coolant sample
In boron element concentration difference come adjust calibration solution in boron element concentration cumbersome problem；Meanwhile by setting containing more
A boron element concentration is identical and calibration solution that elemental lithium concentration is different avoids different calibration solution as calibration solution series
The case where series switching, therefore be not in the step of lithium content, so that the lithium content measurement result of coolant sample is continuous
Property it is good, be more convenient for accurately adjust PWR of Nuclear Power Station unit coolant in lithium content.
To sum up, the measurement method of lithium content has been broken original in the PWR of Nuclear Power Station unit coolant proposed in the present invention
By adjusting calibration solution in boron element concentration so that itself and the boron element in PWR of Nuclear Power Station unit coolant sample
The consistent thinking of concentration becomes adjusting the boron element concentration in PWR of Nuclear Power Station unit coolant sample using reverse thinking
So that it is consistent with the boron element concentration in calibration solution, so can disposably solve to exist in the measurement method of traditional technology
Influence lithium content measurement accuracy multiple problems, improve measurement result accuracy and analysis result reliability, reach
More accurate purpose is adjusted to the lithium content made in PWR of Nuclear Power Station unit coolant.For deeper angle, one
The accurate adjusting of circuit coolant pH value can protect the integrality of fuel can, extend the primary Ioops of compacted clay liners
The service life of relevant device is reduced the activation products that material corrosion generates, is radiated as caused by corrosion product to reduce
Property dose advancement, provides basic guarantee for the long-term safety stable operation of compacted clay liners.
The following are specific embodiment parts:
Embodiment 1
1) the lithium standard solution for, using Merck company to produce is as the solution containing elemental lithium, wherein in lithium standard solution
Elemental lithium concentration be 1000mg/kg；
2), pure water is added to be configured to the boric acid solution that boron element concentration is 5000mg/kg using analytically pure boric acid solid；
3) the above-mentioned lithium standard solution of calculation amount, is weighed, the above-mentioned boric acid solution, a small amount of of calculation amount is added thereto
68% nitric acid solution and pure water, is configured to the school that elemental lithium concentration is 0.5mg/kg, boron element concentration is 500mg/kg respectively
Quasi- solution 1, the calibration solution 2 and elemental lithium concentration that elemental lithium concentration is 1.0mg/kg, boron element concentration is 500mg/kg are
1.5mg/kg, the calibration solution 3 that boron element concentration is 500mg/kg.
To above-mentioned calibration solution 1, calibration solution 2 and solution 3 is calibrated respectively using the PE of Perkinelmer Inc.'s production
These three absorbances of calibration solution at 670nm wavelength of AA400 atomic absorption spectrometry, according to absorbance and elemental lithium
Concentration makes calibration curve, and establishes the relation function y=0.2961x+0.0037 of absorbance Yu elemental lithium concentration, wherein
The calibration curve made is as shown in Figure 2.
Comparative example 1
Using the measurement method of lithium content in the PWR of Nuclear Power Station unit coolant before improvement, it is molten to prepare multiple calibrations
Liquid, and using the multiple calibration solution of PE AA400 atomic absorption spectrometry used in embodiment 1 at 670nm wavelength
Absorbance makes calibration curve according to absorbance and elemental lithium concentration, and establishes the relationship letter of absorbance Yu elemental lithium concentration
Number y=0.2529x+0.0162, wherein the calibration curve made is as shown in Figure 3.
By comparing calibration curve shown in Fig. 2 and calibration curve shown in Fig. 3 it can be seen that in Fig. 3, in calibration curve
Highest point is obvious slight bending downwards, it can also be seen that not being overlapped significantly between point and the line and fit line of point；
And in Fig. 2, the point of calibration curve is overlapped very well between the line of point and fit line.Further, from the point of view of fitting data,
The linearly related system of calibration curve obtained in the measurement method of lithium content in the PWR of Nuclear Power Station unit coolant of comparative example 1
Number R2It is 0.9970, and is calibrated obtained in the measurement method of lithium content in the PWR of Nuclear Power Station unit coolant of the present embodiment
The linearly dependent coefficient R of curve2It is 0.9995, level of linearity has obtained certain promotion, thus illustrates the measurement side of the present embodiment
Method is helpful the accuracy for improving lithium content measurement.
Embodiment 2
It takes the PWR of Nuclear Power Station unit coolant at one as coolant sample, two PerkinElmer public affairs is respectively adopted
The PE AA400 Atomic Absorption Spectrometer and a Tai Saimo of taking charge of production fly the ICE3500 Atomic Absorption Spectrometer of your company's production of generation
Measurement method with lithium content in the PWR of Nuclear Power Station unit coolant that uses in embodiment 1 is to the lithium in the coolant sample
Constituent content measures, and the measurement result for using three Atomic Absorption Spectrometers to obtain is compared, and comparison result is such as
Shown in the following table 1.
Comparative example 2
It takes the PWR of Nuclear Power Station unit coolant at one as coolant sample, above-mentioned two Perkin Ai Er is respectively adopted
The PE AA400 Atomic Absorption Spectrometer and a Tai Saimo of silent company's production fly the ICE3500 atomic absorption light of your company's production of generation
Spectrometer, using the measurement method of lithium content in the PWR of Nuclear Power Station unit coolant before improvement to the lithium in the coolant sample
Constituent content measures, and the measurement result for using three Atomic Absorption Spectrometers to obtain is compared, and comparison result is such as
Shown in the following table 1.
Table 1.
As can be seen that the very poor of the measurement result for the elemental lithium content that comparative example 2 obtains is 0.20mg/kg from upper table 1,
And the very poor of the measurement result for the elemental lithium content that embodiment 2 obtains is 0.06mg/kg, and passes through the uncertain of evaluation measurement
It spends and is evaluated using En value method, it is qualified that the measurement result obtained using above-mentioned three Atomic Absorption Spectrometers is also compared,
It can be seen that the measurement method of lithium content makes relative to comparative example 2 in the PWR of Nuclear Power Station unit coolant that embodiment 2 uses
The measurement method of lithium content is significantly improved in accuracy of measurement in PWR of Nuclear Power Station unit coolant.
Each technical characteristic of above embodiments can be combined arbitrarily, for simplicity of description, not to above-described embodiment
In each technical characteristic it is all possible combination be all described, as long as however, the combination of these technical characteristics be not present lance
Shield all should be considered as described in this specification.
Only several embodiments of the present invention are expressed for above embodiments, and the description thereof is more specific and detailed, but can not
Therefore it is construed as limiting the scope of the patent.It should be pointed out that for those of ordinary skill in the art,
Under the premise of not departing from present inventive concept, various modifications and improvements can be made, and these are all within the scope of protection of the present invention.
Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. the measurement method of lithium content in a kind of PWR of Nuclear Power Station unit coolant, which comprises the steps of:
Multiple calibration solution containing elemental lithium and boron element are prepared, the elemental lithium concentration in multiple calibration solution is different,
And the boron element concentration in multiple calibration solution is identical；
The absorbance for testing multiple calibration solution, it is molten according to the absorbance of multiple calibration solution and multiple calibrations
The elemental lithium concentration in liquid establishes the relation function of absorbance Yu elemental lithium concentration；
Measure the initial boron concentration of element in coolant sample；
The boron element concentration in the coolant sample is adjusted, so that the boron element concentration in the coolant sample and the school
Boron element concentration in quasi- solution is identical, obtains pretreatment coolant sample；
Test the absorbance of the pretreatment coolant sample, and according to the pretreatment absorbance of coolant sample and described
The relation function of absorbance and elemental lithium concentration obtains the elemental lithium concentration in the pretreatment coolant sample；
According to the Mass Calculation dilution ratio of the quality of the pretreatment coolant sample and the coolant sample, or according to
The volume of the pretreatment coolant sample and the volume of the coolant sample calculate dilution ratio；
The coolant sample is obtained according to the elemental lithium concentration calculation in the dilution ratio and the pretreatment coolant sample
Elemental lithium concentration in product.
2. the measurement method of lithium content in PWR of Nuclear Power Station unit coolant according to claim 1, which is characterized in that
The step of preparation multiple calibration solution containing elemental lithium and boron element includes: to divide into multiple solution containing elemental lithium
Not Jia Ru boric acid aqueous solution, keep the boron element concentration in multiple solution containing elemental lithium identical and elemental lithium concentration not
Together, multiple calibration solution are obtained.
3. the measurement method of lithium content in PWR of Nuclear Power Station unit coolant according to claim 2, which is characterized in that
The step of preparation multiple calibration solution containing elemental lithium and boron element includes: that boric acid is placed in pure water to dissolve, and is prepared
At the aqueous solution of the boric acid；It is separately added into the aqueous solution of the boric acid into multiple solution containing elemental lithium, makes multiple institutes
The boron element concentration stated in the solution containing elemental lithium is identical, obtains multiple calibration solution, wherein contains lithium described in multiple
Elemental lithium concentration in the solution of element is different.
4. the measurement method of lithium content in PWR of Nuclear Power Station unit coolant according to claim 1, which is characterized in that
The step of preparation multiple calibration solution containing elemental lithium and boron element includes: to divide into multiple solution containing elemental lithium
It boric acid and Jia Ru not dissolve, keep the boron element concentration in multiple solution containing elemental lithium identical, obtain multiple schools
Quasi- solution, wherein the elemental lithium concentration in multiple solution containing elemental lithium is different.
5. the measurement method of lithium content in PWR of Nuclear Power Station unit coolant according to claim 1, which is characterized in that
The step of absorbance of the multiple calibration solution of test includes: using the multiple calibrations of aas determination
The absorbance of solution.
6. the measurement method of lithium content in PWR of Nuclear Power Station unit coolant according to claim 1, which is characterized in that
In the step of initial boron concentration of element measured in coolant sample, measured in the coolant sample using titration
Initial boron concentration of element.
7. the measurement method of lithium content in PWR of Nuclear Power Station unit coolant according to claim 1, which is characterized in that
The step of boron element concentration adjusted in the coolant sample include: be added into the coolant sample diluent with
Adjust the boron element concentration in the coolant sample, wherein in aqueous solution of the diluent selected from pure water and boric acid extremely
Few one kind, and the boron element concentration in the aqueous solution of the boric acid is greater than the boron element concentration in the calibration solution.
8. the measurement method of lithium content in PWR of Nuclear Power Station unit coolant according to claim 7, which is characterized in that
The boron element concentration adjusted in the coolant sample, so that the boron element concentration and calibration in the coolant sample are molten
Boron element concentration in liquid is identical, obtain pretreatment coolant sample the step of include:
Compare the boron element concentration in the initial boron concentration of element and the calibration solution in the coolant sample；
If initial boron concentration of element in the coolant sample is greater than the boron element concentration in the calibration solution, to described
The pure water is added in coolant sample to adjust the boron element concentration in the coolant sample, makes in the coolant sample
Boron element concentration with it is described calibration solution in boron element concentration it is identical；
If initial boron concentration of element in the coolant sample is less than the boron element concentration in the calibration solution, to described
The aqueous solution of the boric acid is added in coolant sample to adjust the boron element concentration in the coolant sample, makes the cooling
Boron element concentration in agent sample is identical as the boron element concentration in the calibration solution.
9. the measurement method of lithium content in PWR of Nuclear Power Station unit coolant according to claim 7, which is characterized in that
The boron element concentration adjusted in the coolant sample, so that the boron element concentration and calibration in the coolant sample are molten
Boron element concentration in liquid is identical, obtain pretreatment coolant sample the step of include:
Compare the initial boron concentration of element in the coolant sample and preset boron element concentration, wherein the preset boron
Concentration of element is greater than the boron element concentration in the calibration solution；
If initial boron concentration of element in the coolant sample is greater than or equal to the preset boron element concentration, according to the
One formula takes out the coolant sample of part, into the coolant sample of taking-up the pure water is added so as to take out
Boron element concentration in the coolant sample is identical as the boron element concentration in calibration solution, obtains the pretreatment coolant
Sample；
If the initial boron concentration of element in the coolant sample is less than the preset boron element concentration, according to the second formula
The water-soluble of the pure water and the boric acid is added into the coolant sample of taking-up for the coolant sample for taking out part
Liquid so that take out the coolant sample in boron element concentration with calibration solution in boron element concentration it is identical, obtain described in
Pre-process coolant sample；Wherein, the additional amount of the aqueous solution of the boric acid is calculated according to third formula；
First formula are as follows: X=PB*Z/CB, second formula are as follows: X=Z/2, the third formula are as follows: Y=X- (X*
CB)/YB；Wherein, X is the quality of the coolant sample taken out, PBFor the boron element concentration in the calibration solution, Z is described pre-
Handle the quality of coolant sample, CBFor the boron element concentration in the coolant sample, Y is the water-soluble of the boric acid being added
The quality of liquid, YBFor the boron element concentration in the aqueous solution of the boric acid；Alternatively, X is the body of the coolant sample taken out
Product, PBFor the boron element concentration in the calibration solution, Z is the volume of the pretreatment coolant sample, CBFor the coolant
Boron element concentration in sample, Y are the volume of the aqueous solution for the boric acid being added, YBFor the boron in the aqueous solution of the boric acid
Concentration of element.
10. the measurement method of lithium content, feature exist in PWR of Nuclear Power Station unit coolant according to claim 1
It include: that dilution is added into the coolant sample in the step of, boron element concentration adjusted in the coolant sample
The dust technology of agent and predetermined amount is to adjust the boron element concentration in the coolant sample, wherein the diluent is selected from pure water
At least one of with the aqueous solution of boric acid, and the boron element concentration in the aqueous solution of the boric acid is greater than in the calibration solution
Boron element concentration.
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