CN107748150A - Utilize the method for iron concentration in nitrogen-doped carbon quantum dots characterization solution - Google Patents
Utilize the method for iron concentration in nitrogen-doped carbon quantum dots characterization solution Download PDFInfo
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention discloses a kind of method for utilizing the nitrogen-doped carbon quantum dots characterization iron concentration using pancreatin as the former synthesis of carbon, including：Step 1: preparing the standard liquid of the iron ion of the quantum dot containing nitrogen-doped carbon of various concentrations, the fluorescence intensity of examination criteria solution, the fluorescence spectra of standard liquid is obtained, the linear relationship established between fluorescence intensity and iron concentration；Step 2: preparing the sample solution of the iron ion of the quantum dot containing nitrogen-doped carbon, the fluorescence intensity of sample solution is detected, the concentration of iron ion in sample solution is determined by linear relationship.The present invention is using nitrogen-doped carbon quantum dot as probe, using the characteristic of iron ion quenching nitrogen-doped carbon quantum dot, iron concentration is detected, detection process is simple and convenient, high sensitivity, test limit are low, and the online rapid sensitive detection in situ of real iron concentration can be achieved.
Description
Technical field
The present invention relates to iron concentration detection field.It is more particularly related to a kind of utilize N doping carbon amounts
The method of iron concentration in son point detection solution
Background technology
Iron is one of required trace element in human body, is one of main component for forming hemoglobin and ferroheme,
Key player is play in terms of health.Iron content is very few in human body or excessively can all give rise to diseases, such as anemia
Parkinsonism and Alzheimer disease, cancer etc., therefore iron content is detected significant.At present, there are a variety of surveys
Determine the method for ferro element, such as ultraviolet spectroscopy, atomic absorption method, but these methods are mostly cumbersome, and time-consuming, test fee
With height.Compared with these traditional detection methods, fluorescent nano material detection is good, easy to operate with high sensitivity, selectivity
Advantage.
Carbon nanomaterial (such as CNT, fowler refining, graphite it is dilute), due to its many unique new property oneself through turning into
The focus studied at present.The one kind of carbon point as carbon nanomaterial, it is the nano material for being most expected to substitute heavy metal quantum dot.Carbon
The size of point is generally less than 10nm, has size and the adjustable photoluminescent property of excitation wavelength.Since carbon point is found, it
It is always a star slowly in carbon material family.Carbon point not only has good fluorescence and fast light Bleachability outer, also very
Good water-soluble, low cytotoxicity and good biocompatibility, so as to promote carbon point progressively to replace traditional heavy metal amount
Application of the son point in biological field such as biological cell mark, bio-imaging, biological detection, insoluble drug release etc..
The content of the invention
It is an object of the present invention to provide a kind of process is simple and convenient, high sensitivity, test limit is low, and tangible line can be achieved
The method using iron concentration in nitrogen-doped carbon quantum dots characterization solution of in situ detection.
In order to realize according to object of the present invention and further advantage, there is provided one kind is examined using nitrogen-doped carbon quantum dot
The method for surveying iron concentration in solution, comprises the following steps：
Step 1: prepare multiple standards of the quantum dot of nitrogen-doped carbon containing same concentrations and the iron ion containing various concentrations in equal volume
Solution, and its fluorescence intensity value I respectively；
Step 2: the control for preparing nitrogen-doped carbon quantum dot concentration identical with step 1 Plays solution same volume is molten
Liquid, and detect its fluorescence intensity level I0；
Step 3: establishLinear relation between iron concentration；
Step 4: preparing identical with step 1 Plays solution same volume nitrogen-doped carbon quantum dot concentration but iron ion is dense
Unknown solution to be measured is spent, and detects its fluorescence intensity level, then is substituted into the linear relation that step 3 obtains, is calculated to be measured
Iron concentration in solution.
Preferably, the preparation process of the nitrogen-doped carbon quantum dot includes：
Step I, will pancreatin add ultra-pure water in mix 5min obtain mixed liquor；
Step II, by made from step I mixed liquor carry out hydro-thermal reaction 12h obtain the thick liquid of nitrogen-doped carbon quantum dot, hydro-thermal
The temperature control of reaction is at 180 DEG C.
Step III, the thick liquid of nitrogen-doped carbon quantum dot obtained in step II also centrifuged, take supernatant liquor to filter, then
Filtrate is dialysed, dried, isolates nitrogen-doped carbon quantum dot.
Preferably, the process for preparation of step 1 Plays solution specifically includes：
Step a, the original solution containing iron ion is prepared using iron chloride and ultra-pure water；
Step b, the original solution of different volumes is measured respectively in the original solution prepared from step a, and use same concentrations respectively
PBS cushioning liquid be diluted to same volume, be configured to the standard liquid of the iron ion containing various concentrations；
Step c, same concentrations, identical are separately added into the standard liquid of the step b iron ions containing various concentrations prepared
The nitrogen-doped carbon quantum dot solution of volume.
Preferably, iron concentration is not in the standard liquid of the iron ion containing various concentrations and step 3 in detecting step one
The excitation wavelength used in standard liquid known is 320nm.
Preferably, the concentration of the PBS cushioning liquid added in step b is 0.1mol/L.
Preferably, the concentration of the nitrogen-doped carbon quantum dot solution added in step c is 1mg/mL.
Preferably, also make after adding nitrogen-doped carbon quantum dot solution in various concentrations iron ion standard liquid in step c
It is stirred with microsyringe.
Preferably, also carried out between step I and step II：
S1, mixed liquor made from step 1 is subjected to ultrasonic disperse, ultrasonic frequency be 28~33KHz, the time for 20~
35min, then the mixed liquor after supersound process is subjected to infrared heating processing, programming rate is 2 DEG C/min, and final temperature is 54~58
DEG C, vacuum distillation operation is carried out in heating process, air pressure size presses 250Pa/min decrease of speed, at the end of temperature-rise period,
Air pressure also stops reducing, and maintains temperature and air pressure conditions 30min, temperature then is risen into 78 with 3 DEG C/min programming rate
~84 DEG C, air pressure size presses 400Pa/min decrease of speed, after assigned temperature is reached, maintains temperature and air pressure conditions
50min, room temperature is finally cooled the temperature to 4 DEG C/min cooling rate, air is passed through by gas with 100ml/min gas flow rate
Pressure is slowly recovered to an atmospheric pressure.
The present invention comprises at least following beneficial effect：
1st, detection process is simple and convenient, and high sensitivity, test limit are low, and the online in situ quick of real iron concentration can be achieved
Sensitive Detection.
2nd, it is the nitrogen-doped carbon quantum dot of Material synthesis to the high specificity of iron ion using pancreatin, by other metal ions
Disturb it is less, testing result accurately and reliably, while using pancreatin as the nitrogen-doped carbon quantum dot of Material synthesis exciting light spectrum compared with
Width, convenient detection, especially using 320nm exciting light, obtained fluorescence spectrum effect is preferable.
3rd, it is Material synthesis nitrogen-doped carbon quantum dot in solution is detected using pancreatin after using subsequent treatments such as ultrasonic disperses
Detection limit further reduces during iron concentration.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Brief description of the drawings
Fig. 1 is medium volume nitrogen-doped carbon containing the same concentrations quantum dot of the embodiment of the present invention 1 and iron ion containing various concentrations
Multiple standard liquids fluorescence spectra；
Fig. 2 is the linear relationship curve between fluorescence intensity and iron concentration in the embodiment of the present invention 1；
Embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to specification
Word can be implemented according to this.
It should be noted that experimental method described in following embodiments, is conventional method unless otherwise specified, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained.
<Embodiment 1>
The method of iron concentration, comprises the following steps in a kind of quantum dots characterization solution using nitrogen-doped carbon：
Step 1: preparing nitrogen-doped carbon quantum dot, 2.5g pancreatin first is added into mixing 5min in 10ml ultra-pure waters obtains
Mixed liquor, then obtained mixed liquor is transferred in 25ml reactors under the conditions of 180 DEG C and carries out hydro-thermal reaction 12h and obtains nitrogen and mix
The miscellaneous thick liquid of carbon quantum dot, by the obtained thick liquid of nitrogen-doped carbon quantum dot with 6000rad/min rotating speed centrifuging and taking supernatant liquor mistake
Filter, is filtered to get filtrate with 0.22 μm of filter, and then the bag filter that filtrate is 1000Da with molecular weight is dialysed to obtain dialyzate, will
Dialyzate is dried in vacuo 24 hours nitrogen-doped carbon quantum dots for obtaining water-soluble yellow fluorescence at 60 DEG C, finally mixes obtained nitrogen
Miscellaneous carbon quantum dot is configured to the nitrogen-doped carbon quantum dot solution that concentration is 1mg/mL；
Step 2: prepare multiple standards of the quantum dot of nitrogen-doped carbon containing same concentrations and the iron ion containing various concentrations in equal volume
Solution, first weigh 0.1622g iron chloride and be dissolved in 10ml ultra-pure waters, be configured to the iron ion original solution that concentration is 100mM, then
Measure 0 μ L, 0.9 μ L, 1.8 μ L, 2.7 μ L, 3.9 μ L respectively from iron ion original solution to be out placed in different containers, then
The PBS cushioning liquid for adding 0.1mol/L into this six containers equipped with different volumes iron ion original solution respectively is diluted
To 3mL, the solution after dilution is stirred 60 times, juxtaposition 1min at room temperature, so that it may the mark of isometric various concentrations is made
Quasi- solution, its concentration value are followed successively by：A=0mol/L, b=3 × 10-5Mol/L, c=6 × 10-5Mol/L, d=9 × 10-5mol/
L, e=1.3 × 10-4Mol/L, being most separately added into 5 μ L concentration in the standard liquid of these iron ions containing various concentrations backward is
The 1mg/mL nitrogen-doped carbon quantum dot solution as made from step 1；
Step 3: multiple standard liquids made from step 2 are used to sepectrophotofluorometer respectively in 320nm excitation wave
Long lower fluorescence intensity I, testing result is shown in Fig. 1, while takes the fluorescence intensity of the standard liquid of 0mol/L iron ions as I0；
Step 4: it can be obtained according to Stern-Volmer equationsWherein Ksv is Stern-Volmer side
The quenching constant of journey, [Q] represents the concentration of iron ion, with (I0- I)/I be ordinate, with iron ion in various criterion solution
Concentration is that abscissa draws standard curve as shown in Figure 2, so as to draw (I0- I)/linear pass between I and iron concentration
System, wherein linear equation is (I0- I)/I=4.11 × 103[Q], coefficient R2=0.996；
Step 5: the unknown solution 3mL to be measured of iron concentration is measured, and it is 1mg/ to add 5 μ L concentration thereto
The mL nitrogen-doped carbon quantum dot solution as made from step 1, then examined with sepectrophotofluorometer under 320nm excitation wavelength
Fluorescence intensity is surveyed, the linear equation that the fluorescence intensity for detecting obtained solution to be measured is brought into step 4, you can calculate and treat
Iron ion is dense in survey solution.
6.95 × 10 can reach to the test limit of iron ion in the present embodiment-6Mol/L, carrying out fluorescence detection in addition
In, from taking an excessive numerical value to be tested between 300nm~400nm, final determination is existed excitation wavelength used using wavelength
The fluorescence spectrum best results that 320nm exciting light obtains.
Copper ions, lead ion or zinc will be added to respectively with the nitrogen-doped carbon quantum dot solution of the present embodiment step 1
In the solution of ion, then with sepectrophotofluorometer under 320nm excitation wavelength fluorescence intensity, be see it is more apparent
Fluorescent effect, illustrate that using pancreatin be the nitrogen-doped carbon quantum dot of Material synthesis to the high specificity of iron ion, by other metals
The interference of ion is less, and testing result is accurately and reliably.
<Comparative example>
The detection method of iron ion, the method can only the half-quantitative detection aqueous solution in a kind of disclosed water solution system
Iron concentration in system, i.e., it can only judge whether iron concentration is higher than 1 × 10 in water solution system-5Mol/L, no standard measure
Detection.
<Embodiment 2>
A kind of method of iron concentration in quantum dots characterization solution using nitrogen-doped carbon, its process and embodiment 1 are substantially
Identical, difference is：When progress step 1 prepares nitrogen-doped carbon quantum dot, pancreatin is added mixed liquor is made in ultra-pure water
Afterwards, mixed liquor carries out ultrasonic disperse, ultrasonic frequency 28KHz, time 20min, then the mixed liquor after supersound process is entered
The processing of row infrared heating, programming rate are 2 DEG C/min, and final temperature is 54 DEG C, vacuum distillation operation is carried out in heating process, air pressure is big
The small decrease of speed by 250Pa/min, at the end of temperature-rise period, air pressure also stops reducing, and maintains temperature and air pressure conditions
30min, temperature then being risen to 78 DEG C with 3 DEG C/min programming rate, air pressure size presses 400Pa/min decrease of speed,
After assigned temperature is reached, temperature and air pressure conditions 50min are maintained, room is finally cooled the temperature to 4 DEG C/min cooling rate
Temperature, air is passed through with 100ml/min gas flow rate and slowly recovers air pressure to an atmospheric pressure.
4.26 × 10 can reach to the test limit of iron ion in the present embodiment-6mol/L。
<Embodiment 3>
A kind of method of iron concentration in quantum dots characterization solution using nitrogen-doped carbon, its process and embodiment 1 are substantially
Identical, difference is：When progress step 1 prepares nitrogen-doped carbon quantum dot, pancreatin is added mixed liquor is made in ultra-pure water
Afterwards, mixed liquor carries out ultrasonic disperse, ultrasonic frequency 33KHz, time 35min, then the mixed liquor after supersound process is entered
The processing of row infrared heating, programming rate are 2 DEG C/min, and final temperature is 58 DEG C, vacuum distillation operation is carried out in heating process, air pressure is big
The small decrease of speed by 250Pa/min, at the end of temperature-rise period, air pressure also stops reducing, and maintains temperature and air pressure conditions
30min, temperature then being risen to 84 DEG C with 3 DEG C/min programming rate, air pressure size presses 400Pa/min decrease of speed,
After assigned temperature is reached, temperature and air pressure conditions 50min are maintained, room is finally cooled the temperature to 4 DEG C/min cooling rate
Temperature, air is passed through with 100ml/min gas flow rate and slowly recovers air pressure to an atmospheric pressure.
3.57 × 10 can reach to the test limit of iron ion in the present embodiment-6mol/L。
<Embodiment 4>
A kind of method of iron concentration in quantum dots characterization solution using nitrogen-doped carbon, its process and embodiment 1 are substantially
Identical, difference is：When progress step 1 prepares nitrogen-doped carbon quantum dot, pancreatin is added mixed liquor is made in ultra-pure water
Afterwards, mixed liquor carries out ultrasonic disperse, ultrasonic frequency 30KHz, time 28min, then the mixed liquor after supersound process is entered
The processing of row infrared heating, programming rate are 2 DEG C/min, and final temperature is 56 DEG C, vacuum distillation operation is carried out in heating process, air pressure is big
The small decrease of speed by 250Pa/min, at the end of temperature-rise period, air pressure also stops reducing, and maintains temperature and air pressure conditions
30min, temperature then being risen to 81 DEG C with 3 DEG C/min programming rate, air pressure size presses 400Pa/min decrease of speed,
After assigned temperature is reached, temperature and air pressure conditions 50min are maintained, room is finally cooled the temperature to 4 DEG C/min cooling rate
Temperature, air is passed through with 100ml/min gas flow rate and slowly recovers air pressure to an atmospheric pressure.
2.78 × 10 can reach to the test limit of hexavalent chromium in the present embodiment-6mol/L.Although the embodiment party of the present invention
Case is disclosed as above, but it is not restricted to listed utilization in specification and embodiment, and it can be applied to respectively completely
The suitable the field of the invention of kind, for those skilled in the art, is easily achieved other modification, therefore do not carrying on the back
Under the universal limited from claim and equivalency range, the present invention is not limited to specific details and shown here as with retouching
The legend stated.
Claims (8)
1. a kind of method of iron concentration in quantum dots characterization solution using nitrogen-doped carbon, it is characterised in that including following step
Suddenly：
Step 1: it is molten to prepare multiple standards of the quantum dot of nitrogen-doped carbon containing same concentrations and the iron ion containing various concentrations in equal volume
Liquid, and its fluorescence intensity value I respectively；
Step 2: the contrast solution of nitrogen-doped carbon quantum dot concentration identical with step 1 Plays solution same volume is prepared, and
Detect its fluorescence intensity level I0；
Step 3: establishLinear relation between iron concentration；
Step 4: prepare identical with step 1 Plays solution same volume nitrogen-doped carbon quantum dot concentration but iron concentration not
The solution to be measured known, and its fluorescence intensity level is detected, then substitute into the linear relation that step 3 obtains, calculate solution to be measured
Middle iron concentration.
2. utilizing the method for hexavalent chromium concentration in nitrogen-doped carbon quantum dots characterization solution as claimed in claim 1, it is special
Sign is that the preparation process of the nitrogen-doped carbon quantum dot includes：
Step I, will pancreatin add ultra-pure water in mix 5min obtain mixed liquor；
Step II, by made from step I mixed liquor carry out hydro-thermal reaction 12h obtain the thick liquid of nitrogen-doped carbon quantum dot, hydro-thermal reaction
Temperature control at 180 DEG C.
Step III, the thick liquid of nitrogen-doped carbon quantum dot obtained in step II also centrifuged, take supernatant liquor to filter, then will filter
Liquid dialysis, dry, isolate nitrogen-doped carbon quantum dot.
3. utilizing the method for iron concentration in nitrogen-doped carbon quantum dots characterization solution as claimed in claim 1, its feature exists
In the process for preparation of step 1 Plays solution specifically includes：
Step a, the original solution containing iron ion is prepared using iron chloride and ultra-pure water；
Step b, the original solution of different volumes is measured in the original solution prepared from step a respectively, and uses the PBS of same concentrations respectively
Cushioning liquid is diluted to same volume, is configured to the standard liquid of the iron ion containing various concentrations；
Step c, same concentrations, same volume are separately added into the standard liquid of the step b iron ions containing various concentrations prepared
Nitrogen-doped carbon quantum dot solution.
4. utilizing the method for iron concentration in nitrogen-doped carbon quantum dots characterization solution as claimed in claim 1, its feature exists
In the unknown standard liquid institute of iron concentration in the standard liquid of the iron ion containing various concentrations and step 3 in detecting step one
Excitation wavelength is 320nm.
5. utilizing the method for iron concentration in nitrogen-doped carbon quantum dots characterization solution as claimed in claim 3, its feature exists
In the concentration of the PBS cushioning liquid added in step b is 0.1mol/L.
6. utilizing the method for iron concentration in nitrogen-doped carbon quantum dots characterization solution as claimed in claim 3, its feature exists
In the concentration of the nitrogen-doped carbon quantum dot solution added in step c is 1mg/mL.
7. utilizing the method for iron concentration in nitrogen-doped carbon quantum dots characterization solution as claimed in claim 3, its feature exists
In, in step c in various concentrations iron ion standard liquid add nitrogen-doped carbon quantum dot solution after also entered using microsyringe
Row stirring.
8. utilizing the method for iron concentration in nitrogen-doped carbon quantum dots characterization solution as claimed in claim 2, its feature exists
In also being carried out between step I and step II：
S1, mixed liquor made from step 1 is subjected to ultrasonic disperse, ultrasonic frequency be 28~33KHz, the time for 20~
35min, then the mixed liquor after supersound process is subjected to infrared heating processing, programming rate is 2 DEG C/min, and final temperature is 54~58
DEG C, vacuum distillation operation is carried out in heating process, air pressure size presses 250Pa/min decrease of speed, at the end of temperature-rise period,
Air pressure also stops reducing, and maintains temperature and air pressure conditions 30min, temperature then is risen into 78 with 3 DEG C/min programming rate
~84 DEG C, air pressure size presses 400Pa/min decrease of speed, after assigned temperature is reached, maintains temperature and air pressure conditions
50min, room temperature is finally cooled the temperature to 4 DEG C/min cooling rate, air is passed through by gas with 100ml/min gas flow rate
Pressure is slowly recovered to an atmospheric pressure.
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Application publication date: 20180302 |