CN105067751B - A kind of method of photocatalysis Visual retrieval Silver From Ore content - Google Patents
A kind of method of photocatalysis Visual retrieval Silver From Ore content Download PDFInfo
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- CN105067751B CN105067751B CN201510435915.XA CN201510435915A CN105067751B CN 105067751 B CN105067751 B CN 105067751B CN 201510435915 A CN201510435915 A CN 201510435915A CN 105067751 B CN105067751 B CN 105067751B
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Abstract
A kind of method of photocatalysis Visual retrieval Silver From Ore content, is to clear up sample ore by the heating of simple furnace device to make the silver in Ore clear up to become Ag+, utilize Ag+With cytosine in DNA (C) specific binding formation C Ag+C hairpin structure, the EB DNA complex that ethidium bromide (EB) embedding hairpin structure produces, under the irradiation of LED, aoxidizes colourless TMB and becomes blue, it is achieved visualization semi-quantitative analysis.This method, without steps such as separation, enrichments, with the naked eye can detect concentration as little as 0.1 ng mL in sample ore digestion solution‑1Ag+.It is expected to be used for the on-site measurement of silver content in sample ore, and according to silver deposit production industry standard (DZ/T0214 2002), whether silver content in sample ore is reached exploitation standard and make evaluation.
Description
Technical field
The invention belongs to rock-mineral analysis technical field, be specifically related to the visual analyzing side of silver content in a kind of ore sample
Method.
Background technology
Silver is one of numerous metals being widely used in industry.Along with the development of science and technology, the consumption demand of silver is significantly
Increase, be no longer limited to traditional currency and ornament craft product aspect, center of gravity is transferred to the application of industrial technology and sends out
Exhibition field.And silver is as noble metal, must be with analysis result as important evidence during exploration, exploitation etc..Therefore, development is fast
The method that speed measures Silver From Ore content is particularly important to mining firm.
The analysis method of existing silver ore silver content mainly have radiosiotope X-ray (P.G.Burkhalter,
Analytical chemistry, 1971,43,10-17), atomic absorption spectrography (AAS) (Sun Wenjun, rock and mineral testing, 2012,31,
829-833), inductive coupling plasma emission spectrograph (G.Chakrapani, P.L.Mahanta, D.S.R.Murty,
B.Gomathy, Talanta, 2001,53,1,139 1147), the comparision contents that these methods measure silver is ripe, measurement result
Accurately and there is higher sensitivity, but these methods instrument to be used is complicated, needs the professional through training
Operate, and when silver content is relatively low in sample ore, be also performed to enrichment and pretreatment.These factors limit these and survey
The method of fixed silver cannot be carried out field in-situ analysis, and quickly provides analysis result.
By contrast, visual analysis method can with the naked eye detect, it is to avoid use large complicated instrument, is suitable for
Field assay.In current detection silver ore the visual analysis method of silver content mainly have dithizone-extraction photometry (Wang Ye,
Cao Lifeng, gold, 2011,32,60-62), Ag+-Phen-bromopyrogallol red ternary complexes development process
(R.M.Dagnall,T.S.West,Talanta,1964,11,1533-1541).But this in two colorimetry need extraction, formality
Loaded down with trivial details, and sensitivity is relatively low, the Ag of mg L-1 rank, can only be detected+.Therefore, exploitation it is highly desirable to a kind of without richness
Collection, the method for detection Silver From Ore content highly sensitive, simple and quick.
Summary of the invention
It is an object of the invention to utilize and work as Ag+In the presence of, DNA and the ethidium bromide (EB) of rich C base can
Form this characteristic of EB-DNA complex of high photochemical catalytic oxidation ability, it is provided that a kind of simple, selectivity quick and highly sensitive, high
The method of silver content in ground detection sample ore.Technical scheme is as follows:
(1) accurately weigh 0.5000g sample ore in 25mL politef crucible, use water-wet sample, add the dense nitre of 5mL
Acid, after vigorous reaction, is heated to liquor capacity and is about 3mL.Take off crucible the coldest, add the dense perchloric acid of 1mL, 5mL Fluohydric acid.
It is heated to emitting a large amount of white cigarette on 200 DEG C of electric furnaces, closes electric furnace, utilize waste heat to make sample clear up completely, and steam near dry.Add
10mL 1% salpeter solution dissolves again, and transfer solution in volumetric flask and uses ultra-pure water constant volume, suitably measures after dilution.
(2) being sequentially added into sequence in clean culture plate is the DNA solution of 5 '-CTCTCTCCAACCTCTCTC-3 ', silver
Standard/sample ore digestion solution, EB solution, the PBS buffer solution of pH 4.0, at room temperature hatch 15min；
(3) in above-mentioned mixed solution, add TMB solution, irradiate 15min with portable green LED lamp array, carry out light
Catalysis oxidation TMB, produces blue solution；
(4) taking the solution after illumination to observe, contrast sample ore digestion solution and the color of standard series, sxemiquantitative obtains ore deposit
Ag in sample+Content, according to measurement result and silver deposit production industry standard (DZ/T0214-2002), sample ore is made evaluation.
The present invention can also select ultraviolet-visible spectrophotometer measure the absorbance of solution, measure sample ore exactly
The content of middle silver.
Invention effect
Compared with prior art, present invention have the advantage that
(1) sensitivity is high, can realize as little as 0.02 μ g L in solution-1Ag+Visual retrieval；
(2) sample ore digestion procedure is simple, uses electric furnace can complete to clear up；
(3) without separation and concentration step, can be directly used for judging in sample ore, whether silver content reaches silver deposit production industry
Standard；
(4) silver content during method is expected to be used for Site Detection sample ore.
Detailed description of the invention
Embodiment 1
Accurately weigh 0.5000g sample ore in 25mL politef crucible, use water-wet sample, add 5mL concentrated nitric acid,
After vigorous reaction, it is heated to solution and is about 3mL.Take off crucible the coldest, add the dense perchloric acid of 1mL, 5mL Fluohydric acid. in 200 DEG C
It is heated on electric furnace emitting a large amount of white cigarette, closes electric furnace, make sample clear up the most completely with waste heat, and steam near dry.Add 10mL
1% salpeter solution dissolves again, and transfer solution in 50mL volumetric flask and uses ultra-pure water constant volume.And suitably dilute.Totally
Culture plate in be sequentially added into 10 μMs of DNA solutions (sequence is 5 '-CTCTCTCCAACCTCTCTC-3 ') of 10 μ L, 1mL different
The Ag of concentration+Diluent cleared up by standard solution/standard environment sample ore, lmL concentration is 0.1mol L-1PBS buffer solution (pH=
4.0), 20 μ L concentration be the ethidium bromide solution of 100mM, at room temperature hatch 30min；Adding 40 μ L concentration is 10mg mL-1's
TMB solution, irradiates 15min by green LED lamp；Contrast sample ore digestion solution and the color of standard series, carry out semi-quantitative analysis, root
According to the result obtained, sample ore is evaluated.
Embodiment 2
Accurately weigh 0.5000g sample ore in 25mL politef crucible, use water-wet sample, add 5mL concentrated nitric acid,
After vigorous reaction, it is heated to solution and is about 3mL.Take off crucible the coldest, add the dense perchloric acid of 1mL, 5mL Fluohydric acid. in 200 DEG C
It is heated on electric furnace emitting a large amount of white cigarette, closes electric furnace, make sample clear up the most completely with waste heat, and steam near dry.Add 10mL
1% salpeter solution dissolves again, and transfer solution in volumetric flask and uses ultra-pure water constant volume, suitably measures after dilution.With clean
Culture plate is sequentially added into 10 μ L concentration be 10 μMs of DNA solutions (sequence is 5 '-CTCTCTCCAACCTCTCTC-3 '), 1mL not
Ag with concentration+Standard solution/environment sample ore digestion solution, 1mL concentration are 0.1mol L-1PBS buffer solution (pH=4.0),
20 μ L concentration are the ethidium bromide solution (ultimate density is 100 μMs) of 10mM, and at room temperature lucifuge hatches 15min；Add 40 μ L
Concentration is 10mg mL-1TMB solution, irradiate 30min by green LED lamp；Contrast sample ore digestion solution and the color of standard series,
Carry out semi-quantitative analysis.According to measurement result and silver deposit production industry standard (DZ/T0214-2002), sample ore is made evaluation.
Use embodiment 1,2 to record the content of silver in environment sample ore 1,2,3,4,5 and standard sample ore (GBW07256) to be shown in Table
1, semiquantitative determination result is coincide good with graphite furnace atomic absorption spectrometry value or standard sample ore reference value, shows measurement result
Reliably.According to measurement result and silver deposit production industry standard (DZ/T0214-2002), sample ore is made evaluation.
The test result of silver content in table 1 actual sample
| Sample | Visualization method (gt-1) | Sampling Graphite Furnace Atomic Absorption measured value or reference value (gt-1) | Sample ore is evaluated |
| Environment sample ore 1 | 40–80 | 52.88±0.17 | Can be with calculated reserves |
| Environment sample ore 2 | 80–400 | 117.8±0.16 | There is potential extraction value |
| Environment sample ore 3 | 80–400 | 155.0±0.19 | There is potential extraction value |
| Environment sample ore 4 | 40–80 | 76.10±0.14 | Can be with calculated reserves |
| Environment sample ore 5 | 0-40 | Do not detect | Barren rock |
| Standard environment sample ore | 80-400 | 112 ± 4 (standard values) | — |
Table 2 silver deposit production industry standard (DZ/T0214-2002)
| Project | Index |
| Cutoff grade gt-1 | 40～50 |
| Minimum economic ore grade gt-1 | 80～100 |
| Mineral deposit average grade gt-1 | >150 |
| Minimum mining width m | 0.8～1 |
| Horsestone eliminating thickness m | 2～4 |
Claims (4)
1. the method for a photocatalysis Visual retrieval Silver From Ore content, it is characterised in that include following four step:
(1) appropriate sample ore is accurately weighed in politef crucible, with adding concentrated nitric acid after water-wet sample；Treat vigorous reaction
After, it is heated to solution and is about 3 mL；
Take off crucible the coldest, add perchloric acid, fluoric acid and be heated to emitting a large amount of white cigarette on electric furnace, close electric furnace, make sample with waste heat
Product are completely dissolved in solution, until being evaporated completely；
Adding 1 % salpeter solution heating for dissolving, transfer solution in volumetric flask and uses ultra-pure water constant volume, suitably measures after dilution；
(2) in clean culture plate, aptamers solution, the phosphorus that sequence is 5 '-CTCTCTCCAACCTCTCTC-3 ' it is sequentially added into
Hydrochlorate buffer solution, ethidium bromide solution (EB), Ag+Standard solution or sample ore digestion solution, when at room temperature lucifuge hatches one section
Between；
(3) in (2) mixed solution, 3,3', 5,5'-tetramethyl benzidine (TMB) solution are added, with LED light irradiation one
The section time, it is achieved photochemical catalytic oxidation TMB develops the color；
(4) taking the solution described in (3) to observe, contrast sample ore digestion solution and the color of standard series, sxemiquantitative obtains sample ore
Middle Ag+Content, it is judged that the silver content during sample ore is no reaches silver deposit production industry standard DZ/T0214-2002.
2. the method as described in claim 1, it is characterised in that lucifuge incubation time is 10-40 min.
3. the method as described in claim 1, it is characterised in that during illumination, the pH of solution is 3.5-5.0.
4. the method as described in claim 1, it is characterised in that LED lamp color is green, and light application time is 10-40 min.
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| US7662640B2 (en) * | 2004-09-28 | 2010-02-16 | Kyoto University | Method for silver staining of biological substances |
| CN101477001A (en) * | 2009-01-12 | 2009-07-08 | 河南科技大学 | DNA silver staining method |
| CN101482508A (en) * | 2009-01-21 | 2009-07-15 | 苏州纳米技术与纳米仿生研究所 | High-sensibility detection method for trace metal ion |
| CN102252880B (en) * | 2010-05-19 | 2012-12-12 | 攀钢集团钢铁钒钛股份有限公司 | Digestion method and detection method of iron ore |
| CN102353637B (en) * | 2011-06-16 | 2013-01-16 | 山东正元地质资源勘查有限责任公司烟台分公司 | Method of determining silver content in rock minerals |
| CN104111244B (en) * | 2014-07-23 | 2016-08-24 | 中国科学院化学研究所 | A kind of method of fluoroscopic examination silver ion content |
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