CN103526193A - Source preparing method by nickel foil auto-deposition - Google Patents

Source preparing method by nickel foil auto-deposition Download PDF

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Publication number
CN103526193A
CN103526193A CN201310496933.XA CN201310496933A CN103526193A CN 103526193 A CN103526193 A CN 103526193A CN 201310496933 A CN201310496933 A CN 201310496933A CN 103526193 A CN103526193 A CN 103526193A
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China
Prior art keywords
processed
source
auto
deposition
nickel foil
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CN201310496933.XA
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Chinese (zh)
Inventor
黄秋红
王玉学
郭冬发
王哲
刘立坤
胡小华
潘景荣
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Nuclear Industry Er Si Institute
Beijing Research Institute of Uranium Geology
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Nuclear Industry Er Si Institute
Beijing Research Institute of Uranium Geology
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Priority to CN201310496933.XA priority Critical patent/CN103526193A/en
Publication of CN103526193A publication Critical patent/CN103526193A/en
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Abstract

The invention belongs to the technical field of source preparing, and in particular relates to a source preparing method by nickel foil auto-deposition. Currently, 210Bi and 210Po are simultaneously auto-deposited in a nickel foil quantitatively. The method comprises the following steps: selecting HCl and NaCl solutions as source preparing solution mediums; selecting ascorbic acid as a reducing agent; controlling the source preparing volume, the source preparing temperature, vibration frequency and amplitude, as well as the source preparing time to deposit 210Bi and 210Po in the nickel foil. According to the method, the simultaneous auto-deposition of iradioisotopes can be realized without tracing or separating coexistence elements, the auto-deposition is reclaimed stably, the deposition efficiency is more than 99 percent, the deposition only needs 60 minutes, the tolerance of interference element arsenic can be 2,000mu g/g, and the tolerance of copper to the arsenic can be 600mu g/g.

Description

A kind of nickel foil auto-deposition source side method processed
Technical field
The invention belongs to auto-deposition source production technique field, be specifically related to a kind of nickel foil auto-deposition source side method processed, especially a kind of general 210bi, 210po simultaneous quantitative auto-deposition is in the method for nickel foil.
Background technology
210bi, 210the research aspect that is determined at nuclear geological system geochemical prospecting, coal system detection colliery, petroleum system oil-gas exploration, environmental radiation environmental quality assessment and other field of Po is extremely important.At present 210bi adopts the total β method of masurement in precipitation source processed conventionally, need to adopt to stablize bismuth spike, and self-absorption is difficult to proofread and correct; 210po generally adopts silver foil auto-deposition source processed α method of masurement, but because the rate of recovery is unstable, relies on tracer agent and carry out rate of recovery correction, and radioisotope tracer is difficult to obtain and need cost higher, and silver foil is only right 210po is effective; At present only there is Copper Foil 210bi, 210po is auto-deposition source production technique simultaneously, can realize two nucleic and measure simultaneously, but Copper Foil is limited to the allowance of some interference element.Therefore in the urgent need to a kind of simple, stable 210bi, 210po is auto-deposition source production technique simultaneously, realizes two nucleic in relative broad range and measures simultaneously.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, provide a kind of nickel foil auto-deposition source side method processed, can realize 210bi, 210po simultaneous quantitative auto-deposition.
The present invention is achieved in that
An auto-deposition source side method processed, comprises the following steps,
Step 1: select source processed solution medium, described source processed solution comprises HCl and NaCl solution;
Step 2: selective reduction agent, described reductive agent comprises xitix;
Step 3: control volume source processed, control source temperature processed, vibrational frequency and amplitude, and control source time processed, make 210bi, 210po is deposited on nickel foil.
A kind of nickel foil auto-deposition as above source side method processed, wherein: described step 1 comprises 0.1mol/L HCl and 2.9～3.4mol/L NaCl solution.
A kind of nickel foil auto-deposition as above source side method processed, wherein: described step 2 comprises 0.4～1.0g xitix.
A kind of nickel foil auto-deposition as above source side method processed, wherein: described step 3 comprises controls volume source processed at 20～30mL; Control source temperature processed at 85～90 ℃; Controlling source frequency processed is 160～200r/min, amplitude 20mm; Controlling source time processed is 60～120min.
An auto-deposition source side method processed, uses 0.1mol/L HCl and 2.9～3.4mol/L NaCl solution as source processed solution, gets 20～30mL source processed solution and extracts the sour molten slag behind molten ore deposit, after extraction, solution is proceeded in container, adds 0.4～1.0g xitix; Container is put into shaking bath, and the temperature of controlling water-bath is 85～95 ℃, and vibration velocity is 160～200r/min, and amplitude 20mm takes out after the 60～120min that vibrates.
The invention has the beneficial effects as follows: the nickel foil auto-deposition source side method processed providing by the present invention, can realize double-core element auto-deposition simultaneously, and without spike, without separated coexistence elements, auto-deposition reclaims stable, and sedimentation effect is greater than 99%, and deposition only needs 60min, the allowance of interference element arsenic is reached to 2000 μ g/g, and copper reaches 600 μ g/g to the allowance of arsenic.
The present invention can realize 210bi, 210po simultaneously, quantitatively and stably auto-deposition, once can source processed 24～100 in nickel foil.
Accompanying drawing explanation
Fig. 1 is concentration of hydrochloric acid total chloridion concentration pair while being 0.1mol/L 210po and 210bi auto-deposition on nickel foil reclaims impact;
Fig. 2 is source temperature pair processed 210the impact of Bi auto-deposition rate of recovery on nickel foil;
Fig. 3 is source temperature pair processed 210the impact of Po auto-deposition rate of recovery on nickel foil;
Fig. 4 is source processed liquor capacity pair 210the impact of Po auto-deposition rate of recovery on nickel foil;
Fig. 5 is source processed liquor capacity pair 210the impact of Bi auto-deposition rate of recovery on nickel foil;
Fig. 6 is source processed vibration velocity pair 210the impact of Po auto-deposition rate of recovery on nickel foil;
Fig. 7 is source processed vibration velocity pair 210the impact of Bi auto-deposition rate of recovery on nickel foil;
Fig. 8 is xitix add-on pair 210the impact of Po auto-deposition rate of recovery on nickel foil;
Fig. 9 is xitix add-on pair 210the impact of Bi auto-deposition rate of recovery on nickel foil.
Embodiment
Below in conjunction with embodiment, a kind of nickel foil auto-deposition provided by the invention source side method processed is described further:
An auto-deposition source side method processed, comprises the following steps:
Step 1: select source processed solution medium, described source processed solution comprises HCl and NaCl solution; Selective reduction agent, described reductive agent comprises xitix;
Step 2: control volume source processed, control source temperature processed, vibrational frequency and amplitude, and control source time processed, make 210bi, 210po is deposited on nickel foil.
For obtaining better effect, can select as follows: select 0.1mol/L HCl, 2.9～3.4mol/LNaCl solution, 0.4～1.0g xitix.Control volume source processed at 20～30mL; Control source temperature processed at 85～90 ℃; Controlling source frequency processed is 160～200r/min, amplitude 20mm; Controlling source time processed is 60～120min.
Embodiment 1:
The present invention comprises the following steps successively:
The first step, with the 0.1mol/L HCl+2.9mol/L NaCl solution of 20mL, extract the sour molten slag behind molten ore deposit, proceed in 100mL container, add 0.4g xitix;
Second step, container is put into shaking bath, the temperature of controlling water-bath is 85 ℃, and vibration velocity is 160r/min, and amplitude 20mm takes out after vibration 60min.
In the present embodiment, 210po and 210bi auto-deposition rate of recovery on nickel foil is respectively 99.2% and 99.5%.
Embodiment 2:
The present invention comprises the following steps successively:
The first step, with the 0.1mol/L HCl+3.2mol/L NaCl solution of 25mL, extract the sour molten slag behind molten ore deposit, proceed in 100mL container, add 0.7g xitix;
Second step, container is put into shaking bath, the temperature of controlling water-bath is 90 ℃, and vibration velocity is 180r/min, and amplitude 20mm takes out after vibration 90min.
In the present embodiment, 210po and 210bi auto-deposition rate of recovery on nickel foil is respectively 99.5% and 99.0%.
Embodiment 3:
The present invention comprises the following steps successively:
The first step, with the 0.1mol/L HCl+3.4mol/L NaCl solution of 30mL, extract the sour molten slag behind molten ore deposit, proceed in 100mL container, add 1.0g xitix;
Second step, container is put into shaking bath, the temperature of controlling water-bath is 95 ℃, and vibration velocity is 200r/min, and amplitude 20mm takes out after vibration 120min.
In the present embodiment, 210po and 210bi auto-deposition rate of recovery on nickel foil is respectively 99.3% and 99.2%.
Fig. 1～Fig. 9 is respectively auto-deposition time under total chloridion concentration, differing temps, source processed liquor capacity, vibration velocity and reductive agent consumption pair 210po and 210the impact of Bi auto-deposition rate of recovery on nickel foil.
As seen from Figure 1, when concentration of hydrochloric acid is 0.1mol/L, total chloridion concentration when 2.9～3.4mol/L, 210po and 210the rate of recovery of Bi is stable, can approach 100%; From Fig. 2 and Fig. 3,85 ℃ of above source 60min processed, 210po and 210the sync peaks auto-deposition rate of recovery of Bi approaches 100%, and at source processed 60～120min, in the time period, two nucleic that deposited do not come off; From Fig. 4 and Fig. 5, when source solution 20～30mL processed, more than source 60min processed, 210po and 210the sync peaks auto-deposition rate of recovery of Bi approaches 100%; From Fig. 6 and Fig. 7, source processed vibration velocity between 140～200r/min, 210po and 210bi bis-nucleic all can synchronously reach the auto-deposition recovery that approaches 100% on nickel foil; From Fig. 8 and Fig. 9, when xitix add-on is less than 1g, xitix itself and oxidation (dehydrogenation), hydrolysate thereof are not right 210po and 210bi quantitative auto-deposition on nickel foil exerts an influence, TFe in sample 2o 3content, generally lower than 15%, is pressed sample weighting amount 1.0g and is calculated, and 0.3g xitix can be by the whole Fe in the solution of source processed 3+ion reduction.Consider the existence of other high valence ions, generally in the solution of source processed, add 0.4～1.0g xitix.
The given embodiment of the present invention be only to a kind of nickel foil auto-deposition provided by the present invention source side method processed for example, can not contain whole summary of the invention; The replacement that the present invention is carried out all should belong to protection domain of the presently claimed invention with modification.

Claims (5)

1. a nickel foil auto-deposition source side method processed, is characterized in that: comprises the following steps,
Step 1: select source processed solution medium, described source processed solution comprises HCl and NaCl solution; Selective reduction agent, described reductive agent comprises xitix;
Step 2: control volume source processed, control source temperature processed, vibrational frequency and amplitude, and control source time processed, make 210bi, 210po is deposited on nickel foil.
2. a kind of nickel foil auto-deposition as claimed in claim 1 source side method processed, is characterized in that: described step 1 comprises 0.1mol/L HCl and 2.9～3.4mol/L NaCl solution.
3. a kind of nickel foil auto-deposition as claimed in claim 2 source side method processed, is characterized in that: described step 1 comprises 0.4～1.0g xitix.
4. a kind of nickel foil auto-deposition as claimed in claim 3 source side method processed, is characterized in that: described step 2 comprises controls volume source processed at 20～30mL; Control source temperature processed at 85～90 ℃; Controlling source frequency processed is 160～200r/min, amplitude 20mm; Controlling source time processed is 60～120min.
5. a nickel foil auto-deposition source side method processed, it is characterized in that: use 0.1mol/L HCl and 2.9mol/L～3.4mol/L NaCl solution as source processed solution, get 20～30mL source processed solution and extract the sour molten slag behind molten ore deposit, after extraction, solution is proceeded in Glass Containers, add 0.4～1.0g xitix; Container is put into shaking bath, and the temperature of controlling water-bath is 85～95 ℃, and vibration velocity is 160～200r/min, and amplitude 20mm takes out after the 60～120min that vibrates.
CN201310496933.XA 2013-10-22 2013-10-22 Source preparing method by nickel foil auto-deposition Pending CN103526193A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108020448A (en) * 2016-11-03 2018-05-11 中国辐射防护研究院 A kind of method that polonium purifies source processed in aerosol
CN110438536A (en) * 2019-07-30 2019-11-12 华东师范大学 A kind of electro-deposition-auto-deposition prepares αsource experimental provision and its experimental method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1481726A1 (en) * 1994-10-18 2004-12-01 The Regents Of The University Of California The combinatorial hydrothermal synthesis of novel materials
CN1576393A (en) * 2003-07-02 2005-02-09 罗姆和哈斯电子材料有限责任公司 Metallization of ceramics

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1481726A1 (en) * 1994-10-18 2004-12-01 The Regents Of The University Of California The combinatorial hydrothermal synthesis of novel materials
CN1576393A (en) * 2003-07-02 2005-02-09 罗姆和哈斯电子材料有限责任公司 Metallization of ceramics

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王玉学 等: "210Pb、210Bi、210Po测试技术研究进展与现状", 《中国无机分析化学》, vol. 3, no. 1, 31 March 2013 (2013-03-31) *
蔡佳佳 等: "镍镀片富集-α、β粒子计数法同时测定岩石及土壤中的210Pb、210Bi、210Po", 《冶金分析》, vol. 32, no. 1, 31 January 2012 (2012-01-31) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108020448A (en) * 2016-11-03 2018-05-11 中国辐射防护研究院 A kind of method that polonium purifies source processed in aerosol
CN110438536A (en) * 2019-07-30 2019-11-12 华东师范大学 A kind of electro-deposition-auto-deposition prepares αsource experimental provision and its experimental method

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Application publication date: 20140122