CN106198173A - A kind of resin anion (R.A.) microfluidic chromatography post separation and concentration, the analysis method of trace rhenium in thiourea spectrphotometric method for measuring Acidic Uranium solution - Google Patents
A kind of resin anion (R.A.) microfluidic chromatography post separation and concentration, the analysis method of trace rhenium in thiourea spectrphotometric method for measuring Acidic Uranium solution Download PDFInfo
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- CN106198173A CN106198173A CN201610527909.1A CN201610527909A CN106198173A CN 106198173 A CN106198173 A CN 106198173A CN 201610527909 A CN201610527909 A CN 201610527909A CN 106198173 A CN106198173 A CN 106198173A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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Abstract
One resin anion (R.A.) microfluidic chromatography post separation and concentration of the present invention, in thiourea spectrphotometric method for measuring Acidic Uranium solution, the analysis method of trace rhenium, relates to analysis technical field.Idiographic flow is as follows: pipette the exchanger resin in certain particle size range being soaked in water, and adds dense HCl, thiourea solution, stannous chloride solution, maps with concentration (rhenium quality) concentration, and draw acquisition working curve with this.For testing sample, according to working curve experimental technique, after first separation and concentration, use the content of the concrete rhenium of thiourea spectrphotometric method for measuring.Separation and concentration used microfluidic chromatography post, first with after the deionized water drip washing of certain volume to neutrality, then reuses after making the transition with certain density dilute sulfuric acid drip washing and maintain upper prop equilibrium acidity.Method of testing of the present invention is simple to operate, and precision is high, favorable reproducibility, and testing cost is low, it is easy under conditions of existing without large-scale instrument, it is achieved the Accurate Determining of the trace rhenium in solution, have certain application value.
Description
Technical field
The present invention relates to analysis technical field, specifically a kind of resin anion (R.A.) microfluidic chromatography post separation and concentration, thiourea luminosity
Method measures the analysis method of trace rhenium in Acidic Uranium solution
Technical background
Currently, the mensuration of trace rhenium depends on big-and-middle-sized precision instrument, as polarography, inductively coupled plasma-
Mass spectrography (ICP-MS), Pulse sample introduction device, neutron activation analysis (NAA) etc.].Voltammetry, electromigration, XRF
Spectrographic method, high performance liquid chromatography etc. measure the rhenium in sample also a relevant report, but restrictive condition in production application
More.
The on-site measurement method of rhenium is most commonly used that spectrophotography, photometry mainly include functional group colour developing photometry,
Fluorescence method, basic stain method, flow injection spec-trophotometry, Catalytic Kinetics and Differential Spectrophotometry.Wherein, in functional group development process
The colour reagent of rhenium is broadly divided into sulfur-bearing regent and containing the organic reagent of oximido, wherein sulfur-bearing regent with thiourea, rhodanate and
Its derivant is main, and thiourea photometry and ore by thiocyanate spectrophotometry are the most universal, although this type of method is modified later, improve
Survey the sensitivity of rhenium, but its degree of accuracy need to promote.Catalytic Spectrophotometric Analysis and extraction spectrophotometric method can solve trace rhenium in sample
Measuring, utilize high rhenium acid group to form ionic associate with basic stain cation, extract colorimetric, conventional basic stain has Luo Dan
Bright class, crystal violet, methylene blue etc., but repeatability is poor, and operate wayward.
As can be seen here, at present for the most quickly mensuration of trace rhenium in complicated substrate, ICP-MS, ICP-are depended on
The large-scale instruments such as AES, NAA, but because of these method instrument apparatus expensive, difficulty applies to the process control in production technology.
Summary of the invention
In order to overcome the deficiency of the method for testing of existing rhenium, the present invention provides this one resin anion (R.A.) microfluidic chromatography post to separate
Enrichment, the analysis method of trace rhenium in thiourea spectrphotometric method for measuring Acidic Uranium solution.The method of testing that the present invention provides has operation
Simply, precision is high, favorable reproducibility, and testing cost is low, it is easy under conditions of existing without large-scale instrument, it is achieved the trace in solution
The Accurate Determining of amount rhenium, has certain application value.
For achieving the above object, the present invention takes techniques below scheme:
(1) making of microfluidic chromatography post:
Pipetting the exchanger resin resin in certain particle size range being soaked in water, decompression wet method loads micro-color of certain specifications and models
Spectrum exchange column, keeps certain resin bed height, balances upper prop acidity with sulfuric acid solution.
(2) separation and concentration of trace rhenium:
Use supercharging microfluidic chromatography post separation and concentration technology, under conditions of controlling necessarily, respectively by the most commensurability rhenium standard solution
After upper prop, with strippant under certain condition, respectively by complete for the rhenium in resin eluting, the used microfluidic chromatography of separation and concentration
Post, first with after the deionized water drip washing of certain volume to neutrality, then makes the transition with certain density dilute sulfuric acid drip washing and maintains upper prop
Reuse after equilibrium acidity.
(3) Determination of Trace Rhenium spectrophotometry:
Add a certain amount of dense HCl, thiourea solution, stannous chloride solution, dilute with water constant volume, shake up, keep certain colour developing
After time stands, with the cuvette of certain specification, with reagent blank as reference, at certain wavelength, measure absorbance.
(4) working curve makes:
Respectively by after the most commensurability rhenium standard solution upper prop, with strippant under certain condition, respectively by complete for the rhenium in resin
Full eluting, operates according to experimental technique in step (3), maps with concentration (rhenium quality)-concentration, and it is bent to draw acquisition work with this
Line.
(5) sample determination:
Respectively by after solution upper prop to be measured, with strippant under certain condition, respectively by complete for the rhenium in resin eluting, press
Operate according to experimental technique in step (3), calculate corresponding solution concentration value to be measured according to measuring the absorbance obtained.
In above-mentioned method of testing, it is characterised in that in the manufacturing process of microfluidic chromatography post: institute's potting resin type is: macropore
Anion exchange resin D302-II, resin size are 120-140 mesh, ion exchange column a size of Ф 3 × 75mm microfluidic chromatography post,
Resin bed height 60-70mm, upper prop equilibrium acidity is the sulfuric acid medium of pH=2.
In above-mentioned method of testing, it is characterised in that during the separation and concentration of trace rhenium, upper column flow rate is 2-4ml/
Min, microfluidic chromatography post acidity is PH=2, and stripping liquid is (1+1) NH4OH, desorbing flow velocity is 2-4ml/min.Upper prop and desorption temperature
Being room temperature, ion exchange resin conversion liquid is 0.5mol/L H2SO4。
In above-mentioned method of testing, it is characterised in that during the spectrophotometry of Determination of Trace Rhenium, sample to be tested adds
The dense HCl of 3-5mL, 3-5mL 5% thiourea solution, 2-3mL 20% stannous chloride solution, it is settled to 25mL with water, shakes up, place
30-60min, uses 5cm cuvette, and reference solution is reagent blank, measures absorbance at 400nm wavelength.
In above-mentioned method of testing, it is characterised in that in working curve drawing process, the solution of taken rhenium standard solution is dense
Degree is 10mg/L, and working curve pipettes the amount of standard solution respectively and is respectively 0,1,2,4,6,8mL.The working curve obtained
Rhenium mass concentration is in the range of 0.02-3.2mg/L, and the mensuration of rhenium follows Beer law, and the regression equation of standard curve is: A
=0.22377 ρ-0.00473.Coefficient R=0.9994.
In above-mentioned method of testing, it is characterised in that in this integrated testability procedure, this method of testing is in retest 5
In the case of secondary, standard deviation is 2.2-4.6%, favorable reproducibility, and precision is high, recovery of standard addition between 95-110%,
In this measures concentration range, the accurate of the minimum rhenium achieving 0.02mg/L concentration is measured, and measures model at 0.02-3.2mg/L simultaneously
In enclosing, removing the K having been reported, the element such as Na, Ca, Mg, Al, Cu, Pa, Zn, Ni, Cd does not affect outside interference, in solution matrix
Ferrum, the content of nitrate anion have substantially no effect on measurement result, but the existence of molybdenum can have severe jamming to assay method, needs separately to adopt
Measure after separating by way.
Method of testing of the present invention is simple to operate, and precision is high, and favorable reproducibility, testing cost is low, it is easy to without large-scale instrument
Under conditions of existence, it is achieved the Accurate Determining of the trace rhenium in solution, there is certain application value.
Accompanying drawing explanation
Fig. 1 is the supercharging microfluidic chromatography post use figure of invention,
Fig. 2 is the microfluidic chromatography rod structure figure of invention.In figure, F is the microtrabeculae head connecting pump line, and G is O, and L is heavy wall glass
Glass pipe, I is modified resins, and H is glass fibre.
Fig. 3 is the working curve of rhenium of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
(1) drafting of working curve
Pipetting 0,1,2,4,6,8mL 10mg/L rhenium standard solution is in handing over the D302-II ion of pH 2.0 solution equilibria
Change in U-shaped post, coutroi velocity 4mL/min, after solution flows to end, divide 2 drip washing with pH 2.0 solution 4mL, then with 1mL (1+1)
NH4Once, leacheate discards in OH drip washing, continues with 9mL (1+1) NH4OH divides 4 eluting, and eluent is undertaken in 25mL volumetric flask,
Adding 8mL concentrated hydrochloric acid, with flowing water cooling capacity bottle to room temperature, then add 3mL 5% thiourea, 2mL stannous chloride (often adds a kind of reagent all
Shake up), it is diluted with water to scale, shakes up.Place 30min, at 400nm wavelength, use 5cm cuvette, blank for ginseng with post
Than measuring absorbance, drawing curve, see Fig. 3.From painted working curve, rhenium mass concentration is at 0.02-3.2mg/L model
In enclosing, the mensuration of rhenium follows Beer law, and surveyed absorbance absorbance surveyed with standard curve is close, and the separation that can be used for rhenium is surveyed
Fixed.The regression equation of standard curve is: A=0.22377 ρ-0.00473.Coefficient R=0.9994, the best, formula
Middle A is the absorbance recorded, and ρ is the mass concentration of rhenium in 25mL solution.
(2) main coexisting ion impact:
Except containing K in uranium ore ground leachate or adsorption tail liquid, outside the common elements such as Na, Ca, Mg, Al, still contain on a small quantity
Transition element Cu, Pa, Zn, Ni, Cd etc., existing document reports that above-mentioned element does not disturb thiourea spectrphotometric method for measuring rhenium, therefore, this reality
Test the interference experiment not carrying out above-mentioned element.Target owing to measuring is uranium ore ground immersion/adsorption tail liquid, it is therefore necessary to for
Ferrum present in uranium ore ground leachate, uranium, molybdenum, nitrate anion carries out coexisting ion interference experiment.
Pipette 5mL 10mg/L rhenium standard solution and be separately added into different amounts of interfering ion, then use the method set up
Measure rhenium amount, when ensureing error less than ± 5%, investigate interfering ion allowance (in terms of mg), uranium (3mg), molybdenum
(0.3mg), ferrum (10mg), nitrate anion (12mg).From the results, it was seen that the method for ferrum and nitrate anion allowance relatively
Greatly, in solution matrix, ferrum, the content of nitrate anion impact substantially without to mensuration；Method is less for the allowance of molybdenum, by
Close in molybdenum, rhenium character, separation and concentration is especially difficult, therefore, in solution even the most a small amount of molybdenum exist also can be to the survey of rhenium
Surely bring the biggest interference, following work must be noted that rhenium, molybdenum mask work.
Embodiment 2
Select mining area, Xinjiang technique waste water (without Re, ρ (U) < 1.6 μ g/mL) and formation water, be separately added into a certain amount of
Pure rhenium solution, is configured to rhenium mass concentration and is respectively 0.5, the test solution of 6 kinds of heterogeneities of 1,2mg/L, specimen coding 1-6.Again
Select the formation water filtering and removing after rhenium and part ferrum, add pure rhenium solution and be configured to rhenium mass concentration and be respectively 0.1,0.05,
0.03mg/L 3 kinds simulates sample, specimen coding 7-9.Joined rhenium-containing solution is shown in Table 1, and totally 9 kinds of simulation samples are as this
The sample of experiment.
The composition of sample simulated by table 1
The mensuration of analog sample
(1) measure rhenium mass concentration 0.5-2.0mg/L simulation sample (sample volume is less than 100mL)
Pipette No. 1-6 simulation sample of different volumes, by D302-II ion exchange column, by the drafting side of working curve
Method operates, and draws the mass concentration of rhenium in solution, per sample (p.s.) parallel assay 5 times, calculates the meansigma methods of rhenium mass concentration, recovery
The multiplying power that rate, standard deviation, RSD and rhenium are enriched with in D302-II ion exchange resin, the results are shown in Table 2.
Specimen Determination result simulated by table 2
From the point of view of the measurement result to No. 1-6 simulation sample, the response rate of rhenium is 96%-104%, and same sample repeats 5
Secondary mensuration, relative standard deviation is 2.2-4.6%, and precision is good.And sample sampling volume is little, upper prop disengaging time is short, point
From effective.
(2) measure rhenium mass concentration 0.1-0.03mg/L simulation sample (sample volume 250-500mL)
Pipette No. 7-9 simulation sample of different volumes, by D302-II ion exchange column, by the drafting side of working curve
Method operates, and draws the mass concentration of rhenium in solution, per sample (p.s.) parallel assay 3 times, calculates the meansigma methods of rhenium mass concentration, recovery
The multiplying power that rate and rhenium are enriched with in D302-II ion exchange resin, the results are shown in Table 3.
Specimen Determination result simulated by table 3
From the point of view of the measurement result to No. 7-9 simulation sample, the measured value of 0.1-0.03mg/L simulation sample and addition rhenium
Measuring close, the response rate is 98.8-102%.Show that rhenium mass concentration 0.1-0.03mg/L sample can use this method accurately to survey
Fixed, but analysis time is longer, needs 2h's to spend the post time.
Embodiment 3
The mensuration of recovery of standard addition
Take the ground immersion of a certain amount of uranium ore, filter off impurity and be adjusted to pH value of solution 2.0, coutroi velocity about 4mL/min, passes through U
Type exchange column, the upper prop cumulative volume every time measured controls as 500mL, needs that 2h is whole crosses post, after solution flows to end, uses 30-40mL
PH2.0 solution by several times drip washing exchange column, removes the impurity such as part ferrum, then with (1+1) NH3·H2O eluting rhenium.Measure uranium parallel 3 times
In the ground immersion of ore deposit, the mass concentration of rhenium, carries out 6 mark-on recovery tests simultaneously, calculates the recovery of standard addition of rhenium, the results are shown in Table 4.
The measurement result of rhenium and recovery of standard addition in table 4 ground immersion
Test result indicate that, take 500mL ground immersion, by D302-II After Anion Exchange Separation rhenium, and use 9mL
(1+1)NH4OH eluting, is enriched with 56 times, and can measure the mass concentration of rhenium in ground immersion is 0.026mg/L, and recovery of standard addition is at 95-
Between 110%.Visible employing large volume test solution upper prop, feasible by Determination of Trace Rhenium result in the ground immersion of thiourea spectrphotometric method for measuring uranium ore,
Though the longest, but can avoid using the expensive instrument and equipments such as ICP-MS, and easy and simple to handle, can meet actual production need
Ask.
Claims (6)
1. a resin anion (R.A.) microfluidic chromatography post separation and concentration, the analysis side of trace rhenium in thiourea spectrphotometric method for measuring Acidic Uranium solution
Method, it is characterised in that this method of testing comprises the steps:
(1) making of microfluidic chromatography post:
Pipetting the exchanger resin resin being soaked in water, decompression wet method loads microfluidic chromatography exchange column, keeps certain resin bed floor height
Degree, balances upper prop acidity with sulfuric acid solution；
(2) separation and concentration of trace rhenium:
Use supercharging microfluidic chromatography post separation and concentration technology, respectively by after the most commensurability rhenium standard solution upper prop, with strippant necessarily
Under the conditions of, respectively by complete for the rhenium in resin eluting, separation and concentration used microfluidic chromatography post, first with deionized water drip washing to neutral
After, then reuse after making the transition with dilute sulfuric acid drip washing and maintain upper prop equilibrium acidity；
(3) Determination of Trace Rhenium spectrophotometry:
Add dense HCl, thiourea solution, stannous chloride solution, dilute with water constant volume, shake up, after keeping certain developing time to stand,
With the cuvette of certain specification, with reagent blank as reference, at certain wavelength, measure absorbance；
(4) working curve makes:
Respectively by after the most commensurability rhenium standard solution upper prop, with strippant under certain condition, respectively the rhenium in resin is washed completely
De-, operate according to experimental technique in step (3), map with concentration (rhenium quality)-concentration, and draw acquisition working curve with this；
(5) sample determination:
Respectively by after solution upper prop to be measured, with strippant under certain condition, respectively by complete for the rhenium in resin eluting, according to step
Suddenly experimental technique operation in (3), calculates corresponding solution concentration value to be measured according to measuring the absorbance obtained.
2. a kind of resin anion (R.A.) microfluidic chromatography post separation and concentration as claimed in claim 1, thiourea spectrphotometric method for measuring Acidic Uranium is molten
The analysis method of trace rhenium in liquid, it is characterised in that in the manufacturing process of microfluidic chromatography post: institute's potting resin type is: macropore cloudy from
Sub-exchange resin D302-II, resin size are 120-140 mesh, ion exchange column a size of Ф 3 × 75 mm microfluidic chromatography post, tree
Lipid layer height 60-70mm, upper prop equilibrium acidity is the sulfuric acid medium of pH=2.
3. a kind of resin anion (R.A.) microfluidic chromatography post separation and concentration, thiourea spectrphotometric method for measuring Acidic Uranium solution
The analysis method of middle trace rhenium, it is characterised in that during the separation and concentration of trace rhenium, upper column flow rate is 2-4ml/min, micro-color
Spectrum post acidity is PH=2, and stripping liquid is (1+1) NH4OH, desorbing flow velocity is that 2-4ml/min, upper prop and desorption temperature are room temperature,
Ion exchange resin conversion liquid is 0.5 mol/L H2SO4 。
4. a kind of resin anion (R.A.) microfluidic chromatography post separation and concentration as claimed in claim 1, thiourea spectrphotometric method for measuring Acidic Uranium is molten
The analysis method of trace rhenium in liquid, it is characterised in that during the spectrophotometry of Determination of Trace Rhenium, sample to be tested adds 3-5
The dense HCl of mL, 3-5 mL 5% thiourea solution, 2-3 mL 20 % stannous chloride solution, it is settled to 25mL with water, shakes up, place 30-
60 min, with 5 cm cuvettes, reference solution is reagent blank, measures absorbance at 400 nm wavelength.
5. a kind of resin anion (R.A.) microfluidic chromatography post separation and concentration as claimed in claim 1, thiourea spectrphotometric method for measuring Acidic Uranium is molten
The analysis method of trace rhenium in liquid, it is characterised in that in working curve drawing process, the solution concentration of taken rhenium standard solution is
10 mg/L, working curve pipettes the amount of standard solution respectively and is respectively 0,1,2,4,6,8 mL, the working curve obtained
Rhenium mass concentration is in the range of 0.02-3.2 mg/L, and the mensuration of rhenium follows Beer law, and the regression equation of standard curve is: A
=0.22377 ρ-0.00473,
Coefficient R=0.9994.
6. a kind of resin anion (R.A.) microfluidic chromatography post separation and concentration as claimed in claim 1, thiourea spectrphotometric method for measuring Acidic Uranium is molten
The analysis method of trace rhenium in liquid, it is characterised in that in this integrated testability procedure, this method of testing is retest 5 times
In the case of, standard deviation is 2.2-4.6%, favorable reproducibility, and precision is high, and recovery of standard addition, between 95-110%, is measured at this
The accurate measurement of the minimum rhenium achieving 0.02mg/L concentration in concentration range, simultaneously in the range of 0.02-3.2 mg/L measures,
Removing the K that has been reported, the element such as Na, Ca, Mg, Al, Cu, Pa, Zn, Ni, Cd does not affect outside interference, ferrum, nitre in solution matrix
The content of acid group has substantially no effect on measurement result, but the existence of molybdenum can have severe jamming to assay method, needs another employing to do
Method measures after separating.
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| CN201610527909.1A CN106198173A (en) | 2016-07-06 | 2016-07-06 | A kind of resin anion (R.A.) microfluidic chromatography post separation and concentration, the analysis method of trace rhenium in thiourea spectrphotometric method for measuring Acidic Uranium solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109975386A (en) * | 2018-12-19 | 2019-07-05 | 核工业北京地质研究院 | A kind of efficient separation method for cadmium isotope measurement |
-
2016
- 2016-07-06 CN CN201610527909.1A patent/CN106198173A/en active Pending
Non-Patent Citations (3)
| Title |
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| 平爱东: "D302-Ⅱ树脂吸附铼性能研究及应用", 《中国优秀硕士学位论文全文数据库•工程科技Ⅰ辑（月刊）》 * |
| 滕洪辉等: "铼的分离富集研究进展", 《辽宁大学学报 自然科学版》 * |
| 蒋小辉等: "D302-II树脂吸附铼的性能研究及应用", 《稀有金属》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109975386A (en) * | 2018-12-19 | 2019-07-05 | 核工业北京地质研究院 | A kind of efficient separation method for cadmium isotope measurement |
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Application publication date: 20161207 |