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
- Publication number
- CN106932458B CN106932458B CN201511022828.8A CN201511022828A CN106932458B CN 106932458 B CN106932458 B CN 106932458B CN 201511022828 A CN201511022828 A CN 201511022828A CN 106932458 B CN106932458 B CN 106932458B
- Authority
- CN
- China
- Prior art keywords
- uranium
- solution
- point
- acidity
- nitric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
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.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201511022828.8A CN106932458B (en) | 2015-12-30 | 2015-12-30 | The analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201511022828.8A CN106932458B (en) | 2015-12-30 | 2015-12-30 | The analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106932458A CN106932458A (en) | 2017-07-07 |
CN106932458B true CN106932458B (en) | 2019-01-08 |
Family
ID=59441063
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201511022828.8A Active CN106932458B (en) | 2015-12-30 | 2015-12-30 | The analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106932458B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU1659829A1 (en) * | 1989-02-14 | 1991-06-30 | Государственный научно-исследовательский и проектный институт лакокрасочной промышленности | Method of determining acid value of polyester resins |
CN102023197A (en) * | 2010-11-09 | 2011-04-20 | 广西大学 | Continuous potentiometric titration analysis method for micromolecule carboxylic acid and amino acid |
CN102323377A (en) * | 2011-09-16 | 2012-01-18 | 中核二七二铀业有限责任公司 | Measurement method for uranium content in ammonium diuranate |
CN102590316A (en) * | 2011-11-07 | 2012-07-18 | 郑州飞机装备有限责任公司 | Method for detecting chloride ion impurities in high concentration chromic anhydride solution |
CN105067755A (en) * | 2015-08-03 | 2015-11-18 | 上海电气电站设备有限公司 | Method for determining content of iron in nickel-based high temperature alloy |
-
2015
- 2015-12-30 CN CN201511022828.8A patent/CN106932458B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU1659829A1 (en) * | 1989-02-14 | 1991-06-30 | Государственный научно-исследовательский и проектный институт лакокрасочной промышленности | Method of determining acid value of polyester resins |
CN102023197A (en) * | 2010-11-09 | 2011-04-20 | 广西大学 | Continuous potentiometric titration analysis method for micromolecule carboxylic acid and amino acid |
CN102323377A (en) * | 2011-09-16 | 2012-01-18 | 中核二七二铀业有限责任公司 | Measurement method for uranium content in ammonium diuranate |
CN102590316A (en) * | 2011-11-07 | 2012-07-18 | 郑州飞机装备有限责任公司 | Method for detecting chloride ion impurities in high concentration chromic anhydride solution |
CN105067755A (en) * | 2015-08-03 | 2015-11-18 | 上海电气电站设备有限公司 | Method for determining content of iron in nickel-based high temperature alloy |
Non-Patent Citations (2)
Title |
---|
Potentiometric Titration of Free Acid and Uranium in Uranium(VI) Solutions with Alkali;KENJI MOTOJIMA 等;《ANALYTICAL CHEMISTRY》;19640430;第36卷(第4期);第733-735页 |
电位滴定法测定铀溶液中的游离酸;岳廷盛;《兰州大学学报(自然科学版)》;19931231;第29卷(第3期);第131-134页 |
Also Published As
Publication number | Publication date |
---|---|
CN106932458A (en) | 2017-07-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106932458B (en) | The analyzing detecting method of acidity in a kind of nitric acid system high concentration uranium solution | |
CN102914600B (en) | Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography | |
EP2995940B1 (en) | Karl fischer titrator and karl fischer titration method | |
CN103913506A (en) | Method for simultaneous measurement of 17 trace elements in reconstituted tobacco by using inductively coupled plasma mass spectrometry | |
CN103454351B (en) | Ion chromatographic method for simultaneously measuring trace amount of anions in high-purity phosphoric acid | |
CN108956815B (en) | Method for testing chloride ion content in sea sand | |
CN104730139A (en) | Method for analyzing fluorine ion concentration under radioactive condition | |
CN105372371A (en) | Ion chromatography method for simultaneous determination of oxalic ion, succinate ion, sulfate ion and phosphate ion in reconstituted tobacco and application thereof | |
CN104330521B (en) | The assay method of calcium oxide content in metallurgical raw and auxiliary material | |
CN104502520B (en) | The assay method of p-methyl benzenesulfonic acid content in a kind of butyl acrylate reactor | |
CN104422685A (en) | Method for determining content of metal aluminum in ladle slag modifying agent | |
CN105675709A (en) | Method for rapidly measuring trace osmium with inductively coupled plasma-massspectrometry | |
CN106226454B (en) | The ion chromatographic method of trace chloro ion in a kind of measure trimethyl gallium | |
CN101936962A (en) | Method for determining weight percent of sodium chloride in common salt | |
CN102175746B (en) | Analytical reagent and method for analyzing content of sulfuric acid and ferric irons | |
CN102901765B (en) | Potentiometric titration method for measuring content of Hg<2+> in solution | |
CN104280368A (en) | Method for efficiently and accurately detecting main content of industrial magnesium oxide | |
CN101592644B (en) | Method for detecting barium ions in oil field water | |
CN103323552B (en) | Quick analysis method of N,N-dimethylhydroxylamine and methyl hydrazine | |
CN103792269B (en) | Fluoride ion electrode method directly measures the analytical approach of content of fluoride ion in carbonated rare earth | |
CN102435691B (en) | Cl in phenol-containing samples-Content determination method | |
CN106404870A (en) | Measuring method of trivalent and tetravalent vanadium ions in vanadium battery electrolyte | |
CN105651851B (en) | The assay method of fluorine content in a kind of thorium tetrafluoride | |
CN110736805A (en) | method for measuring content of aluminum ions in lithium solution containing fluorine and aluminum | |
CN110850025A (en) | Method for determining chloride ion content in industrial iron oxide by automatic potentiometric titration |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |