CN104568800B - A kind of lead ion detection and minimizing technology based on nanocrystalline cellulose - Google Patents
A kind of lead ion detection and minimizing technology based on nanocrystalline cellulose Download PDFInfo
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Abstract
The present invention relates to a kind of lead ion detection based on nanocrystalline cellulose and minimizing technology.The described method comprises the following steps：The nanocrystalline cellulose solution that will be prepared mixes with acetum；Lead ion solution to be measured is added, is well mixed；Sodium sulfide solution, reaction a period of time, observation solution colour change are added, then is detected at 400nm with ultraviolet-uisible spectrophotometer.Detection method of the invention has selectivity well, and the detection method can specifically detect lead ion；The detection method detection is quick, and stabilization is kept within a certain period of time, and nanocrystalline cellulose is recyclable materials, without modification；Detection method sensitivity of the invention is high, and the least concentration of the lead ion that can be detected is 7.5 μM；Reagent needed for described detection method is few, simple to operate, easy to utilize.
Description
Technical field
The present invention relates to metal ion field of fast detection, more particularly to a kind of lead ion inspection based on nanocrystalline cellulose
Survey and minimizing technology.
Background technology
Lead is a kind of nondegradable pollutant of stabilization, it can with the protein in human body, enzyme and amino acid in
Functional group's (sulfydryl) combines, and is a kind of heavy metal element of serious harm health.Lead can be deposited in vivo, so as to influence machine
The various physiological activities of body, the lead of deposition can hinder the formation of haemocyte, cause the intelligence of people to decline；Deposition is to a certain extent then
People can be caused the slow poisoning symptoms such as phrenoblabia, bad dream, insomnia and headache occur；More seriously heavy metal lead can cause
Gestational period problem, influences the brain functions such as growth and intelligence development, neurobehavioral and the learning and memory of infant, and some are even caused
It is dull-witted.Heavy metal lead is typically widely present in nature with natural concentration, but due to the industrial production activities of the mankind, is caused
Heavy metal lead enters in big gas and water, soil, causes serious environmental pollution.
Technology currently used for lead ion detection mainly has：(1) fluorescence and colorimetric analysis are (including based on small molecule, ring
Aromatic hydrocarbons, the sensor of polymer and the sensor-based system based on DNA enzymatic and nano particle etc.)；(2) Electrochemical Detection；(3) it is enzyme-linked to exempt from
Epidemic disease adsorbs (ELISA)；(4) atomic absorption spectrum (AAS)；(5) inductivity coupled plasma mass spectrometry (ICP-MS).Wherein, utilize
Fluorescence molecule detection lead ion needs to use expensive luminaire.ELISA is relatively costly, and complex operation.Electrochemistry
Detection, ICP-MS and AAS are also required to expensive instrument, and cumbersome.And the above method is difficult while reaching lead
The purpose of ion remaval.There is application and limit in above method technology.
The A of CN 103728264 disclose a kind of detection method of lead, and the method is comprised the following steps：To in sample successively
Reducing agent, screening agent, developer are added, then carries out photometering.Wherein, by detecting absorbance and then obtaining lead in sample
Concentration.The method energy quick detection lead ion has high etc. without poisonous reagent, good security, strong antijamming capability, accuracy
Advantage, but operating procedure is more complicated, and required reagent is more, and needs developer, and the lead ion of detection cannot also be removed.Therefore have
Necessity set up it is a kind of can in the method for Accurate Determining lead ion, can simply, quick detection and remove lead ion.
The content of the invention
It is an object of the invention to provide a kind of lead ion detection based on nanocrystalline cellulose and minimizing technology, can make
Must detect simpler, cheap, efficient.
It is that, up to this purpose, the present invention uses following technical scheme：
On the one hand it is the invention provides the method that one kind detects lead ion based on nanocrystalline cellulose (NCC) including as follows
Step：
(1) preparation of nano crystalline cellulose (NCC) solution and acetic acid (HAC) solution first, then two kinds of solution are mixed；
(2) to lead ion solution to be measured is added in the mixed solution of step (1), it is well mixed；
(3) sodium sulfide solution is added to the solution being well mixed in step (2) again, reaction a period of time, observes solution face
Color change, then detected with ultraviolet-visible spectrophotometer.
Preferably, the final concentration of 0.1-10mg/mL of the nanocrystalline cellulose solution, for example can be 0.5mg/mL,
0.6mg/mL、0.7mg/mL、0.8mg/mL、0.9mg/mL、1.0mg/mL、1.1mg/mL、1.2mg/mL、1.3mg/mL、
1.4mg/mL, 1.5mg/mL, 1.6mg/mL, 1.7mg/mL, 1.8mg/mL, 1.9mg/mL or 2.0mg/mL, preferably 0.5-
2mg/mL, more preferably 1mg/mL.
Preferably, the concentration of the lead ion to be measured is 1-1000 μM, for example can be 7.5 μM, 10 μM, 50 μM, 60 μM,
80μM、100μM、120μM、150μM、180μM、200μM、250μM、300μM、350μM、400μM、500μM、600μM、700μM、
800 μM, 600 μM or 1000 μM, preferably 7.5-500 μM.
Preferably, the Detection wavelength of the ultraviolet-visible spectrophotometer be 300-500nm, for example can be 300nm,
320nm, 350nm, 380nm, 390nm, 400nm, 410nm, 420nm or 450nm, preferably 350-450nm, more preferably
400nm。
Preferably, the reaction time described in step (3) is 3-60 minutes, for example can be 3 minutes, 5 minutes, 8 minutes, 10
Minute, 12 minutes, 15 minutes, 20 minutes, 30 minutes, 40 minutes, 50 minutes or 60 minutes, preferably 3-40 minutes, further
Preferably 10 minutes.
The final concentration of 0.5-10mM of step (3) described sodium sulfide solution, for example can be 0.5mM, 1mM, 2mM, 3mM,
4mM, 5mM, 6mM, 7mM, 8mM, 9mM or 10mM, preferably 1-6mM, more preferably 1mM.
Used as optimal technical scheme, methods described comprises the following steps：
(1) preparation of nano crystalline cellulose solution and acetum, and two kinds of solution are mixed；
(2) to lead ion solution to be measured is added in the mixed solution of step (1), it is well mixed；
(3) to sodium sulfide solution is added in the well mixed solution of step (2), now, the end of nanocrystalline cellulose solution
Concentration is 1mg/mL, and the volume fraction of acetum is 4%, the final concentration of 1mM of vulcanized sodium, is reacted 10 minutes；
(4) the solution colour change of observation of steps (3), then detect extinction under ultraviolet-visible spectrophotometer 400nm
Value.
Preferably, described method also includes：The mixed liquor of above-mentioned steps (3) is centrifuged, supernatant is after layering
To eliminate the liquid of lead ion.
Preferably, the rotating speed of the centrifugation be 10000-18000rpm, for example can be 10000rpm, 11000rpm,
12000rpm, 13000rpm, 14000rpm, 15000rpm, 16000rpm, 17000rpm or 18000rpm, preferably 13000-
16000rpm, more preferably 14000rpm.
Preferably, the time of the centrifugation is 20-60 minutes, for example, can be 20 minutes, 25 minutes, 30 minutes, 35 points
Clock, 40 minutes, 45 minutes, 50 minutes, 55 minutes or 60 minutes, more preferably preferably 25-40 minutes, 30 minutes.
To those skilled in the art, even if not understanding Cleaning Principle of the invention, can equally implement, reproduce this
Whether invention, i.e., Cleaning Principle of the invention is cheer and bright, does not affect implementation of the invention and reproduction.A kind of base of the invention
In the lead ion detection of nanocrystalline cellulose and minimizing technology, Cleaning Principle of the invention is：
After the sample containing lead ion is added, lead ion is dispersed in NCC surfaces by electrostatic interaction, and now solution is nothing
Color.After vulcanized sodium is added, the composite particles of micron-sized vulcanized lead and NCC are formed in solution, solution colour is rendered as yellowish
Color or brown.The effect of NCC dispersed sulfur lead so that solution colour stabilization, you can detected by solution colour change lead from
Son whether there is, and the lead ion in sample can be removed by centrifugation.
Compared with prior art, the present invention has the advantages that：
1) detection method of the invention has selectivity well, because the inventive method is used for Ag+, Ba2+, Cd2+, Co2 +, Cr3+, Cu2+, Fe3+, Hg2+, Mg2+, Mn2+, Ni2+And Zn2+Ion detection, solution colour is unchanged or change is not obvious, only
Pb can solely be detected2+, solution colour just can be changed into brown within 10 minutes by colourless, and keep stabilization within a certain period of time；
2) present invention can be convenient and swift by the way that removal lead ion is centrifuged, and NCC is recyclable materials, without modification；
3) detection method sensitivity of the invention is high, and the least concentration of the lead ion that can be detected is 7.5 μM；
4) reagent needed for detection method of the invention is few, simple to operate, easy to utilize.
Brief description of the drawings
Fig. 1 is the sketch of lead ion Cleaning Principle of the present invention.
Fig. 2 is various concentrations NCC UV spectrophotometer measuring results of the present invention.
Fig. 3 is meter testing result of the present invention to different metal ions.
Fig. 4 is the testing result of true water sample lead ion of the invention.
Fig. 5 is lead at different concentrations ion detection result of the present invention.
Specific embodiment
Further to illustrate technological means and its effect that the present invention is taken, below in conjunction with accompanying drawing and by specific real
Mode is applied to further illustrate technical scheme, but the present invention is not limited in scope of embodiments.
Embodiment 1：Influence of the NCC concentration to testing result
(1) the nanocrystalline cellulose solution and 16% acetum of 2.5mg/mL, 5mg/mL, 10mg/mL are prepared, is taken respectively
The deionized water mixing of the nanocrystalline cellulose solution 0.12mL, acetum 0.15mL and 0.21mL of various concentrations；
(2) to 0.06mL lead ion solution to be measured is added in step (1) solution, it is well mixed；
(3) sodium sulfide solution of 0.06mL 10mM is added to the solution being well mixed in step (2) again, is reacted 10 minutes,
Observation solution colour change, then detect the light absorption value at 400nm with ultraviolet-visible spectrophotometer.
Figure it is seen that when NCC concentration is relatively low, vulcanized lead dispersion is not easy to, its dissolving when NCC concentration is higher
Poor-performing, and it is also easy to produce flocculent deposit when adding the solution containing lead ion.And observe and add solution and sky containing lead ion
The absorption curve change of white control, when NCC concentration is 1mg/mL, changes more obvious.Therefore, the end of this detecting system NCC
Concentration selects 1mg/mL.
Embodiment 2：Influence of the vulcanization na concn to testing result
(1) the nanocrystalline cellulose solution and 16% acetum of 5mg/mL are prepared, by the nanocrystalline cellulose of 0.12mL
The deionized water mixing of solution, the acetum of 0.15mL and 0.21mL；
(2) to 0.06mL lead ion solution to be measured is added in step (1) solution, it is well mixed；
(3) formulating vulcanization sodium solution, concentration is respectively 5mM, 10mM, 20mM, 40mM, 60mM, 80mM and 100mM, now matches somebody with somebody
First use.
(4) sodium sulfide solution of 0.06mL various concentrations is added to the solution being well mixed in step (2) again, vulcanized sodium
Final concentration of 0.5mM, 1mM, 2mM, 4mM, 6mM, 8mM and 10mM.Reaction 10 minutes, observation solution colour change, then with it is ultraviolet-
Visible spectrophotometer detects the light absorption value at 400nm.
Vulcanization na concn and time have no significant effect to testing result, final choice Na2The final concentration of 1mM of S.
Embodiment 3：Influence of the reaction time to testing result
(1) the nanocrystalline cellulose solution and 16% acetum of 5mg/mL are prepared, by the nanocrystalline cellulose of 0.12mL
The deionized water mixing of solution, the acetum of 0.15mL and 0.21mL；
(2) to 0.06mL lead ion solution to be measured is added in step (1) solution, it is well mixed；
(3) sodium sulfide solution of 0.06mL 10mM is added to the solution being well mixed in step (2) again, 3 points is reacted respectively
Clock, 5 minutes, 10 minutes, 20 minutes, 30 minutes, 40 minutes, 50 minutes and 60 minutes, observation solution colour change, then with purple
Outward-light absorption value of the visible spectrophotometer detection at 400nm.
Test result indicate that, to be reacted during 10 minutes reaction time completely, the reaction time is 10 minutes.
Embodiment 4：Influence of the different plumbum ion concentrations to testing result
(1) the nanocrystalline cellulose solution and 16% acetum of 5mg/mL are prepared, by the nanocrystalline cellulose of 0.12mL
The deionized water mixing of solution, the acetum of 0.15mL and 0.21mL；
(2) to the lead ion solution of 0.06mL various concentrations is added in step (1) solution, wherein preparing the μ of plumbum ion concentration 0
M, 50 μM, 75 μM, 100 μM, 250 μM, 500 μM, 750 μM, 1000 μM, 2500 μM, 5000 μM, 7500 μM and 10000 μM, mixing
Uniformly so that final concentration of 0 μM of lead ion, 5 μM, 7.5 μM, 10 μM, 25 μM, 50 μM, 75 μM, 100 μM, 250 μM, 500 μM,
750 μM and 1000 μM；
(3) sodium sulfide solution of 0.06mL 10mM is added to the solution being well mixed in step (2) again, is reacted 10 minutes,
Observation solution colour change, then detect the light absorption value at 400nm with ultraviolet-visible spectrophotometer.
Solution colour can be made to be changed into brown from colourless from figure 3, it can be seen that the lead ion of high concentration is added, with lead ion
Concentration reduction, more substantially, the minimal detectable concentration of the color change that can visually distinguish is 25mM for solution colour change.And with purple
Outward-visible spectrophotometer tests the change of the solution absorbance under different plumbum ion concentrations, the absorbance at 400nm with
Plumbum ion concentration increases and increases, and the least concentration of the lead ion that instrument can be detected is 7.5mM.
Embodiment 5：Influence of other metal ions to testing result
(1) acetum of the NCC solution with volume fraction 16% of 5mg/mL is prepared, and by them according to NCC：HAc：
H2O=4:5:7 ratio mixing；
(2) by Ag+, Ba2+, Cd2+, Co2+, Cr3+, Cu2+, Fe3+, Hg2+, Mg2+, Mn2+, Ni2+And Zn2+These metal ions
Distilled water is dissolved in respectively, and compound concentration is 1mM；
(3) it is separately added into the solution of step (1) to the solution of step (2) so that final concentration of 100 μ of metal ion
M, adds sodium sulfide solution so that the final concentration of 1mM of vulcanized sodium；
(3) observation solution colour change, and using detection solution extinction under ultraviolet-visible spectrophotometer wavelength 400nm
The change of degree.
From fig. 4, it can be seen that lead ion causes that solution colour occurs significant change, other ions then change unobvious or do not have
Change, while detect that its absorbs value changes by ultraviolet-visible spectrophotometer, can be with by the absorption value at 400nm
Judge that the present invention has preferable selectivity to lead ion.
Embodiment 6：The removal of metal ion
(1) the nanocrystalline cellulose solution and 16% acetum of 5mg/mL are prepared, by the nanocrystalline cellulose of 0.12mL
The deionized water mixing of solution, the acetum of 0.15mL and 0.21mL；
(2) corresponding solution is made into being added according to the addition of each metal ion species in following table in step (1) solution,
It is well mixed；
(3) sodium sulfide solution of 0.06mL 10mM is added to the solution being well mixed in step (2) again, 10 is reacted respectively
Minute, observation solution colour change；
(4) above-mentioned mixed liquor centrifuge 14000rpm, is centrifuged 30 minutes, while using inductive coupling plasma emission spectrum
Ion concentration after instrument detection centrifugation in supernatant, as a result as shown in table 1.
Table 1
As it can be seen from table 1 the system can remove 99.2% lead ion, the removal efficiency than other ions will
It is high.
Embodiment 7：The result of actually detected river and rainwater
(1) the nanocrystalline cellulose solution and 16% acetum of 5mg/mL are prepared, by the nanocrystalline cellulose of 0.12mL
The deionized water mixing of solution, the acetum of 0.15mL and 0.21mL；
(2) river and rainwater of the lead ion of the various concentrations added to addition according to the form below 2 in step (1) solution, mixing
Uniformly；
(3) sodium sulfide solution of 0.06mL 10mM is added to the solution being well mixed in step (2) again, 10 is reacted respectively
Minute, observation solution colour change.
(4) above-mentioned mixed liquor centrifuge 14000rpm, is centrifuged 30 minutes, while using inductive coupling plasma emission spectrum
Ion concentration after instrument detection centrifugation in supernatant, as a result as shown in table 2.
Table 2
Be can be seen that after the lead ion of various concentrations is added in water sample from table 2 and Fig. 5, the system is observed that
Color change, and good remove function can be realized, it is consistent with Inductively coupled plasma optical emission spectrometer testing result.
In sum, detection method of the invention has selectivity well, and solution colour just can be by nothing within 10 minutes
Color is changed into brown, and keeps stabilization within a certain period of time；The present invention can be convenient and swift by the way that removal lead ion is centrifuged, and
NCC is recyclable materials, without modification；Detection method sensitivity of the invention is high, the least concentration of the lead ion that can be detected
It is 7.5 μM；And the present invention can direct detection entity water sample, accurate quick, therefore it is considered that the system can apply to it is leaded
Lead ion detection and the removal of ion concentration water sample higher.
Applicant states that the present invention illustrates method detailed of the invention by above-described embodiment, but the present invention not office
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (18)
1. it is a kind of based on nanocrystalline cellulose detect lead ion method, it is characterised in that methods described comprises the following steps：
(1) preparation of nano crystalline cellulose solution and acetum first, then two kinds of solution are mixed；
(2) to lead ion solution to be measured is added in the mixed solution of step (1), it is well mixed；
(3) reaction a period of time, solution colour is observed to sodium sulfide solution is added in the solution being well mixed in step (2) again
Change, then detected with ultraviolet-visible spectrophotometer；
The final concentration of 0.1-10mg/mL of the nanocrystalline cellulose solution, the concentration of the lead ion to be measured is 1-1000 μM,
The Detection wavelength of the ultraviolet-visible spectrophotometer is 300-500nm, and the reaction time described in step (3) is 3-60 minutes,
The final concentration of 0.5-10mM of step (3) described sodium sulfide solution.
2. method according to claim 1, it is characterised in that the final concentration of 0.5- of the nanocrystalline cellulose solution
2mg/mL。
3. method according to claim 2, it is characterised in that the final concentration of 1mg/ of the nanocrystalline cellulose solution
mL。
4. method according to claim 1, it is characterised in that the concentration of the lead ion to be measured is 7.5-500 μM.
5. method according to claim 1, it is characterised in that the Detection wavelength of the ultraviolet-visible spectrophotometer is
350-450nm。
6. method according to claim 5, it is characterised in that the Detection wavelength of the ultraviolet-visible spectrophotometer is
400nm。
7. method according to claim 1, it is characterised in that the reaction time described in step (3) is 3-40 minutes.
8. method according to claim 7, it is characterised in that the reaction time described in step (3) is 10 minutes.
9. method according to claim 1, it is characterised in that the final concentration of 1- of step (3) described sodium sulfide solution
6mM。
10. method according to claim 9, it is characterised in that the final concentration of 1mM of step (3) described sodium sulfide solution.
11. method according to any one of claim 1-10, it is characterised in that methods described comprises the following steps：
(1) preparation of nano crystalline cellulose solution and acetum, and two kinds of solution are mixed；
(2) to lead ion solution to be measured is added in the mixed solution of step (1), it is well mixed；
(3) to sodium sulfide solution is added in the well mixed solution of step (2), now, the final concentration of nanocrystalline cellulose is
1mg/mL, the volume fraction of acetum is 4%, the final concentration of 1mM of vulcanized sodium, is reacted 10 minutes；
(4) the solution colour change of observation of steps (3), then detect light absorption value under ultraviolet-visible spectrophotometer 400nm.
12. methods according to claim 1, it is characterised in that described method also includes：By the mixed liquor of step (3)
It is centrifuged, supernatant is the liquid for eliminating lead ion after layering.
13. methods according to claim 12, it is characterised in that the rotating speed of the centrifugation is 10000-18000rpm.
14. methods according to claim 13, it is characterised in that the rotating speed of the centrifugation is 13000-16000rpm.
15. methods according to claim 14, it is characterised in that the rotating speed of the centrifugation is 14000rpm.
16. methods according to claim 12, it is characterised in that the time of the centrifugation is 20-60 minutes.
17. methods according to claim 16, it is characterised in that the time of the centrifugation is 25-40 minutes.
18. methods according to claim 17, it is characterised in that the time of the centrifugation is 30 minutes.
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| US4269811A (en) * | 1978-10-10 | 1981-05-26 | Nl Industries, Inc. | Production of lead monoxide from lead sulfate with acetic acid |
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2015
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4269811A (en) * | 1978-10-10 | 1981-05-26 | Nl Industries, Inc. | Production of lead monoxide from lead sulfate with acetic acid |
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