CN106932458B - The analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution - Google Patents
The analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution Download PDFInfo
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Abstract
The invention belongs to nuclear leve uranium product manufacture fields, and in particular to the analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution.(1) automatical potentiometric titrimeter Instrument working parameter is set；(2) measuring method of acidity in the nitric acid solution of unknown uranium concentration is determined；Accurately pipette V1The nitric acid solution of the unknown uranium concentration of volume is in beaker, end point of the sudden change is titrated on automatical potentiometric titrimeter with NaOH standard solution, 2 jumping points ep1, ep2 are determined in titration process, using second jumping point ep2 as titration end-point, the acidity of solution: A=C × (V is calculated by following equation of linear regression2- V0)/V1+KCU+b；(3) relevant parameter in regression equation is determined.Above-mentioned analytical result reproducibility, different sampling amount analysis results and comparison result are preferable, and production analysis can be suitble to require, and solve the problems, such as a long-term existing industrial analysis in uranium purifying production.
Description
Technical field
The invention belongs to nuclear leve uranium product manufacture fields, and in particular to acidity in a kind of nitric acid system high concentration uranium solution
Analyzing detecting method.
Background technique
In the processing of current nuclear leve uranium product, using high concentration uranium solution TBP extracting and refining technique, extract nitric acid in stoste
Acidity is an important process control parameter of technical process, is had to extraction stoste allotment nitric acid dosage, technical process uranium extraction rate
Great influence.
Extract stoste in addition to containing nitric acid, go back the facile hydrolysis ion such as uranium-bearing, iron, aluminium, influences the measurement of acidity, current process production
Using spent acid in calgon complexing masking method measurement uranium solution, there are biggish analyses for discovery in practice production for this method
Deviation shows that poor, the different sampling amounts of analysis result reproducibility are analyzed result and had differences.
Spent acid this method is also applied in technical process in potassium oxalate method measurement uranium hydrometallurgy leachate, but its
Measurement result differs greatly when measuring low concentration spent acid.
Therefore, need to develop a kind of analyzing detecting method of acidity in nitric acid system high concentration uranium solution, thus solve with
Upper two methods there are the shortcomings that, and guarantee in high concentration uranium solution, no matter the equal energy under high acid concentration or low acid concentration
Carry out Accurate Determining.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of analysis detections of acidity in nitric acid system high concentration uranium solution
Method, to solve the problems, such as mass balance in technique production, preferably to carry out technique production, control related process parameters are provided
Strong data supporting improves production efficiency, reduces consumption.
In order to realize the purpose, the technical solution adopted by the present invention is that:
The analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution, comprising the following steps:
(1) automatical potentiometric titrimeter Instrument working parameter is set
(2) measuring method of acidity in the nitric acid solution of unknown uranium concentration is determined
Accurately pipette V1The nitric acid solution of the unknown uranium concentration of volume is in beaker, with NaOH standard solution in automatic current potential
End point of the sudden change is titrated on titrator, in titration process determine 2 jumpings point ep1, ep2, using second jumping point ep2 as
Titration end-point calculates the acidity of solution by following equation of linear regression:
A=C × (V2- V0)/V1+KCU+b；
In formula: C is the molar concentration of NaOH standard solution, unit mol/L；V1It is single to pipette uranium solution volume of sample
Position is mL；V2For the volume for consuming NaOH standard solution when uranium solution sample titration end-point ep2, unit mL；V0For blank titration
When consume NaOH standard solution volume, unit mL；CUFor uranium content in uranium solution sample, unit g/L；KCU+ b is sample
For middle uranium content to the Volatile material value of acidity measurement, K, b are correction equation coefficient；
(3) in regression equation relevant parameter determination
(3.1) void volume V0Determination
Isometric deionized water is titrated on automatical potentiometric titrimeter to end point of the sudden change with NaOH standard solution, titration go from
Volume=V of NaOH standard solution is consumed when sub- water0；
(3.2) determination of parameter K, b
Accurately pipette the known C of n different sample volumesUWith the solution of A, the nitric acid constructed when according to different sample volumes
C in uranium solutionUWith the equation of linear regression of A, correction equation COEFFICIENT K in the equation of linear regression constructed every time is calculatedi、bi
Value, 1~n of i ∈；K is taken respectivelyi、biAverage value as correction equation COEFFICIENT K, b；
(3.3) uranium concentration CUDetermination
On automatical potentiometric titrimeter, V is titrated with NaOH standard solution1The nitric acid solution of the unknown uranium concentration of volume is to maximum
End point of the sudden change obtains 2 jumping point ep1 and ep2 in titration process, establishes the following equation, and calculates C by measurement △ VU；
CU=[102.4 × △ V × C-1.687]/V1
△ V=Vep2-Vep1, for the NaOH standard consumed between second jumping point and first jumping point in titration process
The volume of solution, unit mL.
Further, in a kind of nitric acid system high concentration uranium solution as described above acidity analyzing detecting method, step
(1) it sets in automatical potentiometric titrimeter Instrument working parameter, specific setting content are as follows:
Uranium solution sample: operating mode is dynamic ph titration；Mixing speed is 8 revolutions per seconds；Measuring signal drift value is
30mv/min；Measurement maximum latency is 5s；Titrating dot density is 9mv/ times；Liquid feeding minimum incrementss are 10 μ L；Liquid feeding is most
Big incrementss are 100 μ L；Stopping equivalent point is 1；Equivalent point criterion of identification is 30mv；Equivalent point recognition mode is maximum；
Blank sample: operating mode is isometric pH titration；Mixing speed is 8 revolutions per seconds；Measuring signal drift value is
50mv/min；Measure maximum latency 5s；Liquid feeding minimum incrementss are 1 μ L；Stopping equivalent point is 1；Equivalent point identification mark
Quasi- 0.3mv；Equivalent point recognition mode is maximum.
The beneficial effect of technical solution of the present invention is: technical solution of the present invention is carried out using accurate automatical potentiometric titrimeter
Analysis experiment, the method for obtaining spent acid in Accurate Determining nitric acid system high concentration uranium solution.Analytical result reproducibility,
Different sampling amount analysis results and comparison result are preferable, and production analysis can be suitble to require, and solve long-term in uranium purifying production
An existing industrial analysis problem.Automatic titering process is corrected in linear regression has determination data precision higher, uses reagent
Few advantage.It is 0.5mol/L~5mol/L that this method, which measures spent acid range, and sample analysis result precision is analyzed than original production
Method improves a lot, and linear regression method recovery of standard addition is 99.6~100.1%.
Specific embodiment
Technical solution of the present invention is further elaborated below by specific embodiment.
The analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution of the present invention, comprising the following steps:
(1) automatical potentiometric titrimeter Instrument working parameter is set
Uranium solution sample: operating mode is dynamic ph titration；Mixing speed is 8 revolutions per seconds；Measuring signal drift value is
30mv/min；Measurement maximum latency is 5s；Titrating dot density is 9mv/ times；Liquid feeding minimum incrementss are 10 μ L；Liquid feeding is most
Big incrementss are 100 μ L；Stopping equivalent point is 1；Equivalent point criterion of identification is 30mv；Equivalent point recognition mode is maximum；
Blank sample: operating mode is isometric pH titration；Mixing speed is 8 revolutions per seconds；Measuring signal drift value is
50mv/min；Measure maximum latency 5s；Liquid feeding minimum incrementss are 1 μ L；Stopping equivalent point is 1；Equivalent point identification mark
Quasi- 0.3mv；Equivalent point recognition mode is maximum.
(2) measuring method of acidity in the nitric acid solution of unknown uranium concentration is determined
Accurately pipette V1The nitric acid solution of the unknown uranium concentration of volume is in beaker, with NaOH standard solution in automatic current potential
End point of the sudden change is titrated on titrator, in titration process determine 2 jumpings point ep1, ep2, using second jumping point ep2 as
Titration end-point calculates the acidity of solution by following equation of linear regression:
A=C × (V2- V0)/V1+KCU+b；
In formula: C is the molar concentration of NaOH standard solution, unit mol/L；V1It is single to pipette uranium solution volume of sample
Position is mL；V2For the volume for consuming NaOH standard solution when uranium solution sample titration end-point ep2, unit mL；V0For blank titration
When consume NaOH standard solution volume, unit mL；CUFor uranium content in uranium solution sample, unit g/L；KCU+ b is sample
For middle uranium content to the Volatile material value of acidity measurement, K, b are correction equation coefficient；
(3) in regression equation relevant parameter determination
(3.1) void volume V0Determination
Isometric deionized water is titrated on automatical potentiometric titrimeter to end point of the sudden change with NaOH standard solution, titration go from
Volume=V of NaOH standard solution is consumed when sub- water0；
(3.2) determination of parameter K, b
Accurately pipette the known C of n different sample volumesUWith the solution of A, the nitric acid constructed when according to different sample volumes
C in uranium solutionUWith the equation of linear regression of A, correction equation COEFFICIENT K in the equation of linear regression constructed every time is calculatedi、bi
Value, 1~n of i ∈；K is taken respectivelyi、biAverage value as correction equation COEFFICIENT K, b；
(3.3) uranium concentration CUDetermination
On automatical potentiometric titrimeter, V is titrated with NaOH standard solution1The nitric acid solution of the unknown uranium concentration of volume is to maximum
End point of the sudden change obtains 2 jumping point ep1 and ep2 in titration process, establishes the following equation, and calculates C by measurement △ VU；
CU=[102.4 × △ V × C-1.687]/V1
△ V=Vep2-Vep1, for the NaOH standard consumed between second jumping point and first jumping point in titration process
The volume of solution, unit mL.
Claims (2)
1. the analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution, which comprises the following steps:
(1) automatical potentiometric titrimeter Instrument working parameter is set
(2) measuring method of acidity in the nitric acid solution of unknown uranium concentration is determined
Accurately pipette V1The nitric acid solution of the unknown uranium concentration of volume is in beaker, with NaOH standard solution in automatic potentiometric titration
It is titrated to end point of the sudden change on instrument, 2 jumpings point ep1, ep2 are determined in titration process, using second jumping point ep2 as titration
Terminal calculates the acidity of solution by following equation of linear regression:
A=C × (V2- V0)/V1+KCU+b；
In formula: C is the molar concentration of NaOH standard solution, unit mol/L；V1To pipette uranium solution volume of sample, unit is
mL；V2For the volume for consuming NaOH standard solution when uranium solution sample titration end-point ep2, unit mL；V0To disappear when blank titration
Consume the volume of NaOH standard solution, unit mL；CUFor uranium content in uranium solution sample, unit g/L；KCU+ b is uranium in sample
For content to the Volatile material value of acidity measurement, K, b are correction equation coefficient；
(3) in regression equation relevant parameter determination
(3.1) void volume V0Determination
Isometric deionized water is titrated on automatical potentiometric titrimeter to end point of the sudden change with NaOH standard solution, titrates deionized water
When consume NaOH standard solution volume=V0；
(3.2) determination of parameter K, b
Accurately pipette the known C of n different sample volumesUWith the solution of A, the uranium nitrates constructed when according to different sample volumes are molten
C in liquidUWith the equation of linear regression of A, correction equation COEFFICIENT K in the equation of linear regression constructed every time is calculatedi、biValue, i
1~n of ∈；K is taken respectivelyi、biAverage value as correction equation COEFFICIENT K, b；
(3.3) uranium concentration CUDetermination
On automatical potentiometric titrimeter, V is titrated with NaOH standard solution1The nitric acid solution of the unknown uranium concentration of volume is to maximum jumping
Terminal obtains 2 jumping point ep1 and ep2 in titration process, establishes the following equation, and calculates C by measurement △ VU；
CU=[102.4 × △ V × C-1.687]/V1
△ V=Vep2-Vep1, for the NaOH standard solution consumed between second jumping point and first jumping point in titration process
Volume, unit mL.
2. the analyzing detecting method of acidity, feature exist in a kind of nitric acid system high concentration uranium solution as described in claim 1
In: step (1) is set in automatical potentiometric titrimeter Instrument working parameter, specific setting content are as follows:
Uranium solution sample: operating mode is dynamic ph titration；Mixing speed is 8 revolutions per seconds；Measuring signal drift value is 30mv/
min；Measurement maximum latency is 5s；Titrating dot density is 9mv/ times；Liquid feeding minimum incrementss are 10 μ L；Liquid feeding maximum increases
Amount is 100 μ L；Stopping equivalent point is 1；Equivalent point criterion of identification is 30mv；Equivalent point recognition mode is maximum；
Blank sample: operating mode is isometric pH titration；Mixing speed is 8 revolutions per seconds；Measuring signal drift value is 50mv/
min；Measure maximum latency 5s；Liquid feeding minimum incrementss are 1 μ L；Stopping equivalent point is 1；Equivalent point criterion of identification
0.3mv；Equivalent point recognition mode is maximum.
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| CN114280221B (en) * | 2021-11-18 | 2024-06-18 | 曲靖市德方纳米科技有限公司 | Method for detecting phosphorus content |
| CN114544858A (en) * | 2021-12-28 | 2022-05-27 | 中核二七二铀业有限责任公司 | Method for analyzing and detecting content of uranium in uranium hexafluoride |
| CN114894925B (en) * | 2022-04-26 | 2024-07-16 | 中国神华煤制油化工有限公司 | Method for measuring oxalic acid content in dimethyl oxalate |
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