CN107907493A - The high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution and water environment - Google Patents

The high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution and water environment Download PDF

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CN107907493A
CN107907493A CN201711143815.5A CN201711143815A CN107907493A CN 107907493 A CN107907493 A CN 107907493A CN 201711143815 A CN201711143815 A CN 201711143815A CN 107907493 A CN107907493 A CN 107907493A
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rhenium
technetium
spectrophotometry
solution
high sensitivity
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胡晖
孙龙利
张鑫
张昌杰
陈晓晖
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Fuzhou University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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

The invention discloses the high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution and water environment.The technical solution of use is：Into rhenium-containing or solution containing technetium, hydrochloric acid, color developing agent and reducing agent are added, shakes up, stand；Add extractant, extract and separate；Solution upper organic phase is transferred in volumetric flask, with extractant constant volume, is shaken up, rhenium or technetium content in solution are measured with ultraviolet-uisible spectrophotometer.Compared with existing detection method, the present invention has the advantages that easy to operate, favorable reproducibility, high sensitivity, the range of linearity are wide and detection sample liquid need not pre-process.

Description

The high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution and water environment
Technical field
The invention belongs to analyze detection field, and in particular to the high sensitivity of rhenium or technetium in a kind of measure solution and water environment Spectrophotometry.
Background technology
Rhenium（Re）It is a kind of dissipated metal, the content in the earth's crust is less than 1.0 ppb, with fusing point is high, density is big, corrosion resistant Erosion, the various advantages energy such as wear-resistant and hardness is big, are mainly used in aerospace field and petroleum chemical industry, are also applied to The field such as electronics industry and radiation medicine.Rhenium is mainly present in molybdenite and porphyry copper in the form of isomorphous, It is present in Pb-Zn deposits, pyrite, columbite, sperrylite, uranium ore, platinum ore and oil shale deposit.Rhenium mainly from molybdenite and Refine in porphyry copper, or recycled from the secondary resource such as rhenium-containing superalloy waste material and useless platinum-rhenium reforming catalyst.Either from Pyrogenic process or hydrometallurgy in metallic ore, or pyrogenic process or hydrometallurgic recovery from secondary resource, rhenium is mainly with high rhenium acid group ion (ReO4 -) form enters aqueous solution, which generally has the characteristics of coexisting ion is complicated, and rhenium content is low.Develop low dense in solution The easy and highly sensitive analyzing detecting method for spending rhenium is most important to the separation and Extraction process of rhenium.
Technetium（Tc）It is a kind of radioactive element, its radio isotope99Tc is a kind of long half-lift（213000 years）Pure β Emitter, has very strong bio-toxicity, is the main composition of nuclear fuel waste, by235U（Fission yield is up to 6.03%）With239Pu fissions produce, while are also the common contaminant of nuclear plant earth's surface and underground water；In addition, medical radioisotope99mTc （Half-life period only 6.02 h）It can also be produced by gamma decay99Tc.It is estimated that from nineteen forty-three to 2010, nuclear reactor and nuclear weapon Device experiment generates up to 305 tons99Tc.Pertechnetate anion（TcO4 -）It is technetium most stable of chemistry in geographical water environment Form, its geochemical activity is big, is not easy, by the earth's crust, soil retardance, can especially to move in land and ocean in the ecosystem Move.Cause99The chemism of Tc is high, and biological transfer activity is big, the long-term risk for making it forever handle and dispose in radwaste Occupy critical role in evaluation, cause the attention of environment, geology and chemist.With the rapid hair of Nuclear Electricity Exhibition, to the monitoring of technetium content has become one and can not be ignored in water environment near the post processing of power reactor spentnuclear fuel and nuclear plant Problem.Due to technetium long half time and food chain circulation is easily entered, develops monitoring nuclear waste storage and treatment process in real time During solution and water environment in the high sensitivity simple analyzing method of technetium seem of crucial importance.
Conventionally, as rhenium or this high atomic number metal element of technetium are difficult to excite, and it is difficult to be reduced into low Valency, therefore should not be carried out with atomic absorption spectrography (AAS) and electrochemical process measure；X-ray fluorescence spectrometry, neutron activation analysis, The methods of ICP-AMS, ICP-OES and ICP-MS, measures rhenium, and instrument and equipment is expensive, complicated and operating cost is high, from And limit its application.Spectrophotometry is using the method for most measure rhenium and technetium, mainly there is thiocarbamide spectrophotometry, fourth Two ketoxime spectrophotometry and rhodanate spectrophotometry.Thiocarbamide spectrophotometry and dimethylglyoxime spectrophotometry are suitable for Measure high concentration rhenium or technetium, method sensitivity is low and anti-SO4 2-Interference performance is weak.Existing rhodanate spectrophotometry rhenium Or technetium, there is preferable selectivity and test limit, but trivial operations, reagent dosage are big and method sensitivity is relatively low.
In conclusion due to rhenium in solution and water environment or technetium content is low, coexisting ion is complicated, existing analysis method measure There are the complicated, shortcoming such as testing cost is high, method sensitivity is low for rhenium or technetium.Therefore, exploitation test it is easy, of low cost, The good analysis method of high sensitivity, selectivity, is to realize the key of rhenium or technetium Site Detection in solution and water environment.
The content of the invention
To solve the above-mentioned problems, the present invention provides the high sensitivity of rhenium or technetium point in a kind of measure solution and water environment Light photometry.
The technical solution adopted by the present invention is：Into rhenium-containing or solution containing technetium, hydrochloric acid, color developing agent and reducing agent are added, is shaken Even, standing；Add extractant, extract and separate；Solution upper organic phase is transferred in volumetric flask, with extractant constant volume, is shaken up, is used Rhenium or technetium content in ultraviolet-visible spectrophotometer measure solution.
The hydrochloric acid, concentration are 1 ~ 10 mol/L, and dosage is 2-10 mL.
The color developing agent is ammonium thiocyanate solution or potassium thiocyanate solution, and concentration is 10 ~ 30 wt%, dosage 0.2-1 mL。
The reducing agent is stannous chloride solution, and concentration is 10 ~ 45 wt%, and dosage is 0.1-1 mL.
The stannous chloride solution, in process for preparation, using 1 ~ 10 mL concentrated hydrochloric acids as solvent dissolved solid protochloride Tin, then it is heated at high temperature 30 ~ 80 s, it is cooled to room temperature, is transferred in volumetric flask, with deionized water constant volume, shakes up.
The standing is that time of repose is 20 ~ 60 min at room temperature.
The extractant is acetone, butyl acetate, chloroform, ethyl acetate, isoamyl alcohol, isoamyl acetate, isopropyl ether, 4- It is one or more of in methyl -2 pentanone organic solvent.
The test wavelength of the ultraviolet-visible spectrophotometer is 300 nm or 427 nm.
Beneficial effects of the present invention and outstanding advantage are：
1. the method for the present invention is simple and efficient, cost-effective without putting into large scale equipment.
2. the present invention, without being pre-processed to sample liquid, the testing time is reduced, and is conducive to waste liquid and is contained with rhenium in environment or technetium The field assay detection of amount.
3. the molar absorption coefficient of spectrophotometry of the present invention is up to 4.65 × 105 M-1 cm-1, existing spectrophotometry Molar absorption coefficient：0.097×105~1.36×105 M-1 cm-1；The Sandell's sensitivity of spectrophotometry of the present invention reaches 0.00040 μg cm-2, existing spectrophotometry Sandell's sensitivity：0.01923~0.00137 μg cm-2；It is as it can be seen that of the invention The more existing spectrophotometry of spectrophotometry have significant raising in sensitivity, be applied in solution and water environment The analysis detection of rhenium or technetium content, has the characteristics that good selectivity, high sensitivity, the range of linearity are wide.
Brief description of the drawings
Fig. 1 is length scanning figure of the present invention.
Embodiment
With reference to case study on implementation, the present invention will be further described, and case study on implementation will facilitate a better understanding of the present invention, But the present invention is not limited only to following embodiments.
Embodiment 1
Rhenium-containing test sample liquid derive from copper smelting plant, wherein mainly contain Re (VII), Cu (II), Fe (III), As (III) and H2SO4；The test sample liquid containing technetium is nuclear waste, wherein mainly containing Tc (VII), Ni (II), Fe (III), HCO3 -And NO3 -。
2 mol/L hydrochloric acid solutions, 10 wt% ammonium thiocyanate solutions and 20 wt% stannous chloride solutions are prepared first.Take respectively 10 mL rhenium-containings/waste liquid containing technetium adds 5 mL hydrochloric acid solutions, 0.5 mL ammonium thiocyanate solutions and 0.5 mL in screw socket bottle with cover Stannous chloride solution, stands 30 min of reaction.After reaction, 10 mL chloroforms are added, upper organic phase is moved into 10 mL holds Measuring bottle, with chloroform constant volume, shakes up, and it is 2.51 mg/L, technetium content to measure rhenium content in waste liquid with ultraviolet-visible spectrophotometer For 5.13 mg/L.Molar absorption coefficient is 2.58 × 105 M-1 cm-1, Sandell's sensitivity is 0.0007 μ g cm-2。
Embodiment 2
Rhenium-containing test sample liquid derives from lead smeltery, wherein mainly containing Re (VII), Pb (II), Zn (II), Fe (III), As (III) And H2SO4；The test sample liquid containing technetium is nuclear waste, wherein mainly containing Tc (VII), Mg (II), Al (III), HCO3 -And NO3 -。
4 mol/L hydrochloric acid solutions, 20 wt% potassium thiocyanate solutions and 35 wt% stannous chloride solutions are prepared first.Take respectively 10 mL rhenium-containings/waste liquid containing technetium adds 8 mL hydrochloric acid solutions, 0.3 mL potassium thiocyanate solutions and 0.5 mL in screw socket bottle with cover Stannous chloride solution, stands 40 min of reaction.After reaction, 10 mL ethyl acetate are added, upper organic phase is moved into 10 ML volumetric flasks, with ethyl acetate constant volume, shake up, and it is 6.53 mg/ to measure rhenium content in waste liquid with ultraviolet-visible spectrophotometer L, technetium content is 2.58 mg/L.Molar absorption coefficient is 9.84 × 104 M-1 cm-1, Sandell's sensitivity is 0.0019 μ g cm-2。
Embodiment 3
Rhenium-containing test sample liquid derives from molybdenum smeltery, wherein mainly containing Re (VII), Mo (VI), Cu (II), Fe (III), Pb (II) And H2SO4；The test sample liquid containing technetium is nuclear waste, wherein mainly containing Tc (VII), Ca (II), Al (III), Cl-、HCO3 -And NO3 -。
6 mol/L hydrochloric acid solutions, 25 wt% potassium thiocyanate solutions and 35 wt% stannous chloride solutions are prepared first.Take respectively 1.5 mL rhenium-containings waste liquids and 0.5 mL waste liquids containing technetium add 2 mL hydrochloric acid solutions, 0.4 mL potassium rhodanides in screw socket bottle with cover Solution and 0.2 mL stannous chloride solutions, stand 60 min of reaction.After reaction, 10 mL acetone are added, by upper organic phase 10 mL volumetric flasks are moved into, with acetone constant volume, are shaken up, it is 25.2 to measure rhenium content in waste liquid with ultraviolet-visible spectrophotometer Mg/L, technetium content are 79.4 mg/L.Molar absorption coefficient is 8.57 × 104 M-1 cm-1, Sandell's sensitivity is 0.0022 μ g cm-2。
Embodiment 4
Rhenium-containing test sample liquid from uranium ore rhenium extraction workshop, wherein mainly contain Re (VII), Mo (VI), Cu (II), U (VI), Pb (II), Ni (II) and HNO3；Containing technetium test sample liquid be nuclear waste, wherein mainly contain Tc (VII), Zn (II), Mn (II), SO4 2-、HCO3 -And NO3 -。
5 mol/L hydrochloric acid solutions, 20 wt% ammonium thiocyanate solutions and 15 wt% stannous chloride solutions are prepared first.Take respectively 10 mL rhenium-containings/solution containing technetium adds 1 mL hydrochloric acid solutions, 0.5 mL ammonium thiocyanate solutions and 0.5 mL in screw socket bottle with cover Stannous chloride solution, stands 30 min of reaction.After reaction, 10 mL butyl acetates are added, after stratification, upper strata is had Machine mutually moves into 10 mL volumetric flasks, with butyl acetate constant volume, shakes up, and rhenium content in solution is measured with ultraviolet-visible spectrophotometer It is 2.64 mg/L for 2.32 mg/L, technetium content.Molar absorption coefficient is 3.06 × 105 M-1 cm-1, Sandell's sensitivity is 0.0006 μg cm-2。
Embodiment 5
Rhenium-containing test sample liquid leaches laydown area underground water water sample for copper mine；The test sample liquid containing technetium is Groundwater near nuclear power station Sample.
5 mol/L hydrochloric acid solutions, 20 wt% ammonium thiocyanate solutions and 15 wt% stannous chloride solutions are prepared first.Take respectively 10 mL rhenium-containings/water sample of underground water containing technetium in screw socket bottle with cover, add 6 mL hydrochloric acid solutions, 0.1 mL ammonium thiocyanate solutions and 0.4 mL stannous chloride solutions, stand 30 min of reaction.After reaction, 10 mL butyl acetates are added, upper organic phase is moved Enter 10 mL volumetric flasks, with butyl acetate constant volume, shake up, rhenium content in underground water water sample is measured with ultraviolet-visible spectrophotometer It is 2.64 mg/L for 2.32 mg/L, technetium content.Molar absorption coefficient is 1.29 × 105 M-1 cm-1, Sandell's sensitivity is 0.0014 μg cm-2。
Embodiment 6
Rhenium-containing test sample liquid is underground water water sample near molybdenum smeltery；The test sample liquid containing technetium is underground water near nuclear waste storage point Water sample.
6 mol/L hydrochloric acid solutions, 25 wt% potassium thiocyanate solutions and 20 wt% stannous chloride solutions are prepared first.Take respectively 10 mL rhenium-containings/water sample of underground water containing technetium in screw socket bottle with cover, add 5 mL hydrochloric acid solutions, 0.5 mL potassium thiocyanate solutions and 0.5 mL stannous chloride solutions, stand 40 min of reaction.After reaction, 10 mL isoamyl alcohol are added, upper organic phase is moved into 10 mL volumetric flasks, with isoamyl alcohol constant volume, shake up, and measuring rhenium content in underground water water sample with ultraviolet-visible spectrophotometer is 4.87 mg/L, technetium content are 5.09 mg/L.Molar absorption coefficient is 4.17 × 105 M-1 cm-1, Sandell's sensitivity is 0.0004μg cm-2。
Embodiment 7
Rhenium-containing test sample liquid is copper smelting plant Adjacent Sea Area seawater sample；The test sample liquid containing technetium is seawater sample near nuclear power station.
4 mol/L hydrochloric acid solutions, 20 wt% ammonium thiocyanate solutions and 30 wt% stannous chloride solutions are prepared first.Take respectively 10 mL rhenium-containings/seawater sample containing technetium adds 2 mL hydrochloric acid solutions, 0.8mL ammonium thiocyanate solutions and 0.4 in screw socket bottle with cover ML stannous chloride solutions, stand 30 min of reaction.After reaction, 10 mL isoamyl acetates are added, upper organic phase is moved into 10 mL volumetric flasks, with isoamyl acetate constant volume, shake up, and measuring rhenium content in seawater sample with ultraviolet-visible spectrophotometer is 2.62 mg/L, technetium content are 2.48 mg/L.Molar absorption coefficient is 7.69 × 104 M-1 cm-1, Sandell's sensitivity is 0.0024 μg cm-2。
Embodiment 8
Rhenium-containing test sample liquid is molybdenum smeltery Adjacent Sea Area seawater sample；The test sample liquid containing technetium is seawater near nuclear waste storage point Water sample,
6 mol/L hydrochloric acid solutions, 20 wt% potassium thiocyanate solutions and 10 wt% stannous chloride solutions are prepared first.10 are taken respectively ML rhenium-containings/seawater sample containing technetium in screw socket bottle with cover, sequentially add 3 mL hydrochloric acid solutions, 0.4 mL potassium thiocyanate solutions and 0.6 mL stannous chloride solutions, stand 30 min of reaction.After reaction, 10 mL isopropyl ethers are added, upper organic phase is moved into 10 mL volumetric flasks, with isopropyl ether constant volume, shake up, and it is 5.04 to measure rhenium content in seawater sample with ultraviolet-visible spectrophotometer Mg/L, technetium content are 4.92 mg/L.Molar absorption coefficient is 8.43 × 104 M-1 cm-1, Sandell's sensitivity is 0.0022 μ g cm-2。
The present invention detection solution in and the rhenium in water environment or technetium content range it is wide, concentration is in 0.01 ~ 100 mg/L scopes It inside can detect and influenced from complicated solution matrix.The molar absorption coefficient (ε) of the present invention is up to 4.65 × 105 M-1 cm-1 (ε > 1×103 M-1 cm-1Belong to sensitive method), illustrate that the present invention has higher sensitivity；Linearly dependent coefficient is more than 0.9995, illustrate that there is good linear relationship between test concentrations of the present invention and its absorbance；The relative standard of the present invention Deviation (RSD) illustrates that the present invention has high precision between 0.6% ~ 1.5%.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, should all belong to the covering scope of the present invention.

Claims (8)

  1. A kind of 1. high sensitivity spectrophotometry of rhenium or technetium in measure solution and water environment, it is characterised in that：To rhenium-containing or contain In technetium solution, hydrochloric acid, color developing agent and reducing agent are added, shakes up, stand；Add extractant, extract and separate；Solution upper strata is organic Mutually it is transferred in volumetric flask, with extractant constant volume, shakes up, rhenium or technetium content in solution is measured with ultraviolet-visible spectrophotometer.
  2. 2. the high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution according to claim 1 and water environment, its It is characterized in that：The hydrochloric acid, concentration are 1 ~ 10 mol/L, and dosage is 2-10 mL.
  3. 3. the high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution according to claim 1 and water environment, its It is characterized in that：The color developing agent is potassium thiocyanate solution or ammonium thiocyanate solution, and concentration is 10 ~ 30 wt%, dosage 0.2-1 mL。
  4. 4. the high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution according to claim 1 and water environment, its It is characterized in that：The reducing agent is stannous chloride solution, and concentration is 10 ~ 45 wt%, and dosage is 0.1-1 mL.
  5. 5. the high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution according to claim 4 and water environment, its It is characterized in that：The stannous chloride solution, in process for preparation, using 1 ~ 10 mL concentrated hydrochloric acids as solvent dissolved solid protochloride Tin, then it is heated at high temperature 30 ~ 80 s, it is cooled to room temperature, is transferred in volumetric flask, with deionized water constant volume, shakes up.
  6. 6. the high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution according to claim 1 and water environment, its It is characterized in that：The standing is that time of repose is 20 ~ 60 min at room temperature.
  7. 7. the high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution according to claim 1 and water environment, its It is characterized in that：The extractant for acetone, butyl acetate, chloroform, ethyl acetate, isoamyl alcohol, isoamyl acetate, isopropyl ether, One or more in 4-methyl-2 pentanone.
  8. 8. the high sensitivity spectrophotometry of rhenium or technetium in a kind of measure solution according to claim 1 and water environment, its It is characterized in that：The test wavelength of the ultraviolet-visible spectrophotometer is 300 nm or 427 nm.
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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN109856069A (en) * 2019-01-23 2019-06-07 福州大学 A kind of spectrophotometry measuring aqueous solution meso-perrhenic acid root concentration
CN113970778A (en) * 2021-09-06 2022-01-25 中国辐射防护研究院 Method for rapidly analyzing technetium-99 content in water sample

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CN101644682A (en) * 2009-08-28 2010-02-10 江西铜业股份有限公司 Fast detecting method of rhenium
CN106770696A (en) * 2016-07-06 2017-05-31 东华理工大学 A kind of resin cation microfluidic chromatography post separation enrichment, ore by thiocyanate spectrophotometry determines the analysis method of Determination of Trace Rhenium in alkaline uranium solution

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109856069A (en) * 2019-01-23 2019-06-07 福州大学 A kind of spectrophotometry measuring aqueous solution meso-perrhenic acid root concentration
CN113970778A (en) * 2021-09-06 2022-01-25 中国辐射防护研究院 Method for rapidly analyzing technetium-99 content in water sample
CN113970778B (en) * 2021-09-06 2023-07-25 中国辐射防护研究院 Rapid analysis method for technetium-99 content in water sample

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