CN105181719A - Online measurement method of centration of uranium in solution - Google Patents
Online measurement method of centration of uranium in solution Download PDFInfo
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- CN105181719A CN105181719A CN201510672433.6A CN201510672433A CN105181719A CN 105181719 A CN105181719 A CN 105181719A CN 201510672433 A CN201510672433 A CN 201510672433A CN 105181719 A CN105181719 A CN 105181719A
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Abstract
The invention discloses an online measurement method of centration of uranium in solution. The online measurement method of centration of uranium in solution comprises the following steps: (i) configuring standard solution; (ii) adding the standard solution in a pipe; (iii) performing measurement by using a NaI crystal detector; (iv) obtaining energy spectrum peak height data; (v) fitting energy spectrum peak height data; (vi) adding uranium solution to be measured in a pipe; (vi) performing measurement by using a NaI crystal detector; (vii) calculating actually measured uranium concentration. Since the online measurement method disclosed by the invention adopts the NaI crystal detector to perform measurement and adopts a multi-channel energy dispersive spectrometer to perform recording, the measurement system is simple, the demand of online measurement of the changing concentration of uranium in a complex solution system can be satisfied, and the disadvantages of complex measurement system and inaccurate measurement data in the prior art are overcome.
Description
Technical field
The invention belongs to a kind of On-line Measuring Method of solution concentration, be specifically related to uranium concentration On-line Measuring Method in a kind of solution.
Background technology
Traditional uranium concentration measurement uses off-line measurement method, and the method needs by hand sampling, carries out sample preparation, then uses the uranium concentration in analytical equipment measurement sample.The shortcoming of this method needs to carry out sample preparation, measures, sampling interval time is long, can not reflect site technique state in real time.
At present, the uranium concentration On-line Measuring Method of prior art has density-conductance simultaneous determination method, X ray absorption edge method, ultrasonic velocity method and x-ray fluorescence method and method of γ-ray absorption.Wherein, density-conductance simultaneous determination method is in the binary system of uranyl nitrtate and nitric acid, at a certain temperature, is obtained the uranium concentration method of solution by the density and conductivity measuring solution; X ray absorption edge method is the method obtaining uranium concentration by measuring uranium in the X-ray beam intensity of K absorption edge or L absorption edge; Ultrasonic velocity method and x-ray fluorescence method are the methods that the secondary x rays fluorescence intensity sent by measuring uranium obtains uranium concentration; Method of γ-ray absorption is by measuring the method for gamma ray through the attenuation degree acquisition uranium concentration of solution.
When but density-conductance simultaneous determination method, ultrasonic velocity method and method of γ-ray absorption measures uranium concentration in solution system complicated and changeable, the interference of the solution composition that can be changed, causing cannot Measurement accuracy; And the on-line measurement system of X ray absorption edge method and x-ray fluorescence method is complicated.
Summary of the invention
The present invention proposes to overcome the shortcoming existed in prior art, its objective is and provides uranium concentration On-line Measuring Method in a kind of solution.
The present invention realizes by following technical scheme:
Uranium concentration On-line Measuring Method in a kind of solution, comprises the steps:
(I) prepares uranium concentration standard solution
Prepare five parts of uranium concentration standard solution, the nitric acid of solvent to be concentration be 5mol/L, by uranium concentration order arrangement from low to high, is respectively 0g/L, 30g/L, 60g/L, 90g/L, 120g/L, S1;
(II) standard solution adds pipeline
First be that the standard solution of 0g/L joins in the pipeline of uranium concentration on-line measurement device by uranium concentration, make solution be full of whole pipeline, S2;
(III) NaI crystal counter is measured
Utilize the NaI crystal counter of uranium concentration on-line measurement device to carry out gamma spectrometry, obtain the gamma ray spectroscopy figure of solution, energy range is 0 ~ 200keV, and Measuring Time continues 20s, S3;
(IV) draws power spectrum peak height data
The hyperchannel energy spectrometer of uranium concentration on-line measurement device show that the energy of uranium radiation is the peak height data at 185.7keV power spectrum peak, to go forward side by side line item, then the solution in pipeline is discharged, four kinds of other uranium concentration standard solution are added respectively in pipeline according to uranium concentration order from low to high, repeat above-mentioned steps (II) ~ (IV) to measure, measure and completely draw five power spectrum peak height data, i.e. y
1=6, y
2=608, y
3=1190, y
4=1773, y
5=2356, uranium concentration of standard solution is designated as: x simultaneously
1=0g/L, x
2=30g/L, x
3=60g/L, x
4=90g/L, x
5=120g/L, S4;
(V) matching power spectrum peak height data
The peak height data y that hyperchannel energy spectrometer is recorded
1~ y
5with the concentration data x of uranium standard solution
1~ x
5use least square method to carry out data fitting, show that the relation formula of power spectrum peak height position between the power spectrum peak height and uranium solution concentration at 185.7keV place is:
y=ax+b①
Wherein y is the power spectrum peak height data of uranium solution to be measured at 185.7keV place, is dimensionless number, and x is uranium solution concentration to be measured, unit is g/L, a is slope, and b is intercept, in the process of data fitting, a=19.427 and b=25.285 is calculated, S5 by least square method;
(VI) uranium solution to be measured adds pipeline
Uranium solution to be measured is joined in the pipeline of uranium concentration on-line measurement device, make solution be full of whole pipeline, S6;
(VII) NaI crystal counter is measured
The NaI crystal counter of uranium concentration on-line measurement device is utilized to measure, obtain the gamma ray spectroscopy figure of solution, energy range is 0 ~ 200keV, Measuring Time continues 20s, the hyperchannel energy spectrometer of uranium concentration on-line measurement device show that the energy of uranium radiation is the peak height data y=1580 at 185.7keV power spectrum peak, S7;
(VIII) calculates actual measurement uranium concentration
According to formula 1., the uranium concentration formula of uranium solution to be measured is drawn:
x=（y-b）/a②
According to the slope a in step (V), intercept b, the gamma-spectrometric data y in step (VII), calculates the degree x=80g/L of uranium solution to be measured, S8 in real time.
By step (i) ~ (v) obtain fitting data, by step (vi) ~ (viii) a unknown uranium solution concentration is measured, carry out measurement altogether six times, measurement result shows that standard deviation RSD is 4%.
Beneficial effect of the present invention
The present invention adopts the nondestructive detecting method of passive measurement uranium radiation gamma ray, respectively the uranium solution of various criterion concentration is positioned in the pipeline before detector and measures, the gamma ray of detector measurement uranium radiation, obtains the relation between gamma ray peak height and normal uranium concentration by data fitting; Overcome the shortcoming that when using traditional off-line measurement method, Measuring Time is long, measuring system is complicated and accuracy is low.
Accompanying drawing explanation
Fig. 1 is the uranium concentration on-line measurement device front sectional view used in measuring method of the present invention;
Fig. 2 is measuring method process flow diagram of the present invention.
In figure:
1 upper cover 2 pipeline
6 baffle plate 7 intermediate plates
9NaI crystal counter 10 hyperchannel energy spectrometer.
Embodiment
Below, with reference to drawings and Examples, uranium concentration On-line Measuring Method in a kind of solution of the present invention is described in detail:
As shown in Figure 1, the measurement mechanism that this measuring method uses, comprise upper cover 1, the first threaded hole 1a that pipeline 2 passes is formed in the horizontal direction at upper cover 1, with the first threaded hole 1a vertical the second threaded hole 1b forming recirculated water and pass through in the horizontal direction, one O type circle 3 and hollow bolt 4 screw in the first threaded hole 1a through pipeline 2, and upper cover 1 bottom is provided with the 2nd O type circle 5, baffle plate 6, intermediate plate 7 successively.
Bolt is connected with the third through-hole 8a at shielding bucket 8 upper edge place through the second through hole 7a of upper cover 1 end along the first through hole 1c located, intermediate plate 7 edge, NaI crystal 9, hyperchannel energy spectrometer 10 is provided with from top to bottom successively in shielding bucket 8, screw 11 is fixed NaI crystal counter 9 through the threaded hole in shielding bucket 8 upper level direction, the square opening 8b that power supply source line passes is formed at shielding bucket 8 bottom, and the base of shielding bucket 8 is provided with the flange through hole 12 of firm banking.
As shown in Figure 2, in a kind of solution, uranium concentration On-line Measuring Method, comprises the steps:
(I) preparing standard solution
Prepare five parts of uranium concentration standard solution, the salpeter solution of solvent to be concentration be 5mol/L, by uranium concentration order arrangement from low to high, is respectively 0g/L, 30g/L, 60g/L, 90g/L, 120g/L, S1;
(II) standard solution adds pipeline
First be that the standard solution of 0g/L joins in the pipeline 2 of uranium concentration on-line measurement device by uranium concentration, make solution be full of whole pipeline 2, S2;
(III) NaI crystal counter is measured
Utilize the NaI crystal counter 9 of uranium concentration on-line measurement device to carry out gamma spectrometry, obtain the gamma ray spectroscopy figure of solution, energy range is 0 ~ 200keV, and Measuring Time continues 20s, S3;
(IV) draws power spectrum peak height data
The hyperchannel energy spectrometer 10 of uranium concentration on-line measurement device show that the energy of uranium radiation is the peak height data at 185.7keV power spectrum peak, to go forward side by side line item, then the solution in pipeline 2 is discharged, four kinds of other uranium concentration standard solution are added respectively in pipeline 2 according to uranium concentration order from low to high, repeat above-mentioned steps (II) ~ (IV) to measure, measure and completely draw five power spectrum peak height data, i.e. y
1=6, y
2=608, y
3=1190, y
4=1773, y
5=2356, uranium concentration of standard solution is designated as: x simultaneously
1=0g/L, x
2=30g/L, x
3=60g/L, x
4=90g/L, x
5=120g/L, S4;
(V) matching power spectrum peak height data
The peak height data y that hyperchannel energy spectrometer 10 is recorded
1~ y
5with the concentration data x of uranium standard solution
1~ x
5use least square method to carry out data fitting, show that power spectrum peak height position is at 185.7keV:
y=ax+b①
Wherein y is the power spectrum peak height data of uranium solution to be measured at 185.7keV place, is dimensionless number, and x is uranium solution concentration to be measured, unit is g/L, a is slope, and b is intercept, in the process of data fitting, a=19.427 and b=25.285 is calculated, S5 by least square method;
(VI) uranium solution to be measured adds pipeline
Uranium solution to be measured is joined in the pipeline 2 of uranium concentration on-line measurement device, make solution be full of whole pipeline 2, S6;
(VII) NaI crystal counter is measured
The NaI crystal counter 9 of uranium concentration on-line measurement device is utilized to measure, obtain the gamma ray spectroscopy figure of solution, energy range is 0 ~ 200keV, Measuring Time continues 20s, the hyperchannel energy spectrometer 10 of uranium concentration on-line measurement device show that the energy of uranium radiation is the peak height data y=1580 at 185.7keV power spectrum peak, S7;
(VIII) calculates actual measurement uranium concentration
According to formula 1., the uranium concentration formula of uranium solution to be measured is drawn:
x=（y-b）/a②
According to the slope a in step (V), intercept b, the gamma-spectrometric data y in step (VII), calculates the degree x=80g/L of uranium solution to be measured, S8 in real time.
By step (i) ~ (v) obtain fitting data, by step (vi) ~ (viii) a unknown uranium solution concentration is measured, carry out measurement altogether six times, measurement result shows that relative standard deviation RSD is 4%, and measurement result is as shown in table 1:
Table 1
| Pendulous frequency | 1 | 2 | 3 | 4 | 5 | 6 | RSD |
| Measure concentration g/L | 0.49 | 0.52 | 0.50 | 0.54 | 0.54 | 0.51 | 4% |
The measuring system of On-line Measuring Method of the present invention is simple, and described gamma-ray detector adopts hyperchannel NaI crystal counter, and this detector is made up of NaI crystal and hyperchannel energy spectrometer, such that the overall volume of detector is little, structure is simple.
Claims (1)
1. a uranium concentration On-line Measuring Method in solution, comprises the steps:
(I) preparing standard solution
Prepare five parts of uranium concentration standard solution, the salpeter solution of solvent to be concentration be 5mol/L, by uranium concentration order arrangement from low to high, is respectively 0g/L, 30g/L, 60g/L, 90g/L, 120g/L, S1;
(II) standard solution adds pipeline
First be that the standard solution of 0g/L joins in the pipeline (2) of uranium concentration on-line measurement device by uranium concentration, make solution be full of whole pipeline (2), S2;
(III) NaI crystal counter is measured
Utilize the NaI crystal counter (9) of uranium concentration on-line measurement device to carry out gamma spectrometry, obtain the gamma ray spectroscopy figure of solution, energy range is 0 ~ 200keV, and Measuring Time continues 20s, S3;
(IV) draws power spectrum peak height data
The hyperchannel energy spectrometer (10) of uranium concentration on-line measurement device show that the energy of uranium radiation is the peak height data at 185.7keV power spectrum peak, to go forward side by side line item, then the solution in pipeline (2) is discharged, four kinds of other uranium concentration standard solution are added respectively in pipeline (2) according to uranium concentration order from low to high, repeat above-mentioned steps (II) ~ (IV) to measure, measure and completely draw five power spectrum peak height data, i.e. y
1=6, y
2=608, y
3=1190, y
4=1773, y
5=2356, uranium concentration of standard solution is designated as: x simultaneously
1=0g/L, x
2=30g/L, x
3=60g/L, x
4=90g/L, x
5=120g/L, S4;
(V) matching power spectrum peak height data
By the peak height data y that hyperchannel energy spectrometer (10) records
1~ y
5with the concentration data x of uranium standard solution
1~ x
5use least square method to carry out data fitting, show that the relation formula of power spectrum peak height position between the power spectrum peak height and uranium solution concentration at 185.7keV place is:
y=ax+b①
Wherein y is the power spectrum peak height data of uranium solution to be measured at 185.7keV place, is dimensionless number, and x is uranium solution concentration to be measured, unit is g/L, a is slope, and b is intercept, in the process of data fitting, a=19.427 and b=25.285 is calculated, S5 by least square method;
(VI) uranium solution to be measured adds pipeline
Uranium solution to be measured is joined in the pipeline (2) of uranium concentration on-line measurement device, make solution be full of whole pipeline (2), S6;
(VII) NaI crystal counter is measured
The NaI crystal counter (9) of uranium concentration on-line measurement device is utilized to measure, obtain the gamma ray spectroscopy figure of solution, energy range is 0 ~ 200keV, Measuring Time continues 20s, the hyperchannel energy spectrometer (10) of uranium concentration on-line measurement device show that the energy of uranium radiation is the peak height data y=1580 at 185.7keV power spectrum peak, S7;
(VIII) calculates actual measurement uranium concentration
According to formula 1., the uranium concentration formula of uranium solution to be measured is drawn:
x=（y-b）/a②
According to the slope a in step (V), intercept b, the gamma-spectrometric data y in step (VII), calculates the degree x=80g/L of uranium solution to be measured, S8 in real time.
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Cited By (7)
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| CN106569250A (en) * | 2016-10-21 | 2017-04-19 | 核工业北京化工冶金研究院 | Device for online measurement of uranium concentration of leach slurry of uranium ore, and application method |
| CN106990428A (en) * | 2017-05-03 | 2017-07-28 | 中国核动力研究设计院 | The method of uranium content and its device is realized in a kind of neutron measurement uranium-bearing liquid |
| CN106990124A (en) * | 2017-03-31 | 2017-07-28 | 中国核动力研究设计院 | The on-line measurement device and measuring method of uranium content in a kind of uranium-bearing liquid |
| CN109557120A (en) * | 2019-01-14 | 2019-04-02 | 东华理工大学 | Gamma spectra combines the method for surveying uranium thorium radium potassium simultaneously with active X-fluorescence |
| CN109580664A (en) * | 2018-12-25 | 2019-04-05 | 中核四0四有限公司 | A kind of high concentration uranium measuring instrument |
| CN110044938A (en) * | 2019-06-05 | 2019-07-23 | 成都理工大学 | A kind of uranium concentration measuring device of spentnuclear fuel extract liquor |
| EP3805808A1 (en) | 2019-10-11 | 2021-04-14 | Umwelt- und Ingenieurtechnik GmbH Dresden | Method and device for the quantification of radionuclides in liquid media |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106569250A (en) * | 2016-10-21 | 2017-04-19 | 核工业北京化工冶金研究院 | Device for online measurement of uranium concentration of leach slurry of uranium ore, and application method |
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| CN106990428A (en) * | 2017-05-03 | 2017-07-28 | 中国核动力研究设计院 | The method of uranium content and its device is realized in a kind of neutron measurement uranium-bearing liquid |
| CN109580664A (en) * | 2018-12-25 | 2019-04-05 | 中核四0四有限公司 | A kind of high concentration uranium measuring instrument |
| CN109580664B (en) * | 2018-12-25 | 2021-11-16 | 中核四0四有限公司 | High concentration uranium measuring apparatu |
| CN109557120A (en) * | 2019-01-14 | 2019-04-02 | 东华理工大学 | Gamma spectra combines the method for surveying uranium thorium radium potassium simultaneously with active X-fluorescence |
| CN110044938A (en) * | 2019-06-05 | 2019-07-23 | 成都理工大学 | A kind of uranium concentration measuring device of spentnuclear fuel extract liquor |
| EP3805808A1 (en) | 2019-10-11 | 2021-04-14 | Umwelt- und Ingenieurtechnik GmbH Dresden | Method and device for the quantification of radionuclides in liquid media |
| WO2021069548A1 (en) | 2019-10-11 | 2021-04-15 | Umwelt- und Ingenieurtechnik GmbH Dresden | Method and device for the quantification of radionuclides in liquid media |
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Application publication date: 20151223 |