CN101349670B - Apparatus and method for rapidly measuring trace amount aluminum content - Google Patents
Apparatus and method for rapidly measuring trace amount aluminum content Download PDFInfo
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- CN101349670B CN101349670B CN2007100700691A CN200710070069A CN101349670B CN 101349670 B CN101349670 B CN 101349670B CN 2007100700691 A CN2007100700691 A CN 2007100700691A CN 200710070069 A CN200710070069 A CN 200710070069A CN 101349670 B CN101349670 B CN 101349670B
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- epiphysin
- electrochemical reaction
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Abstract
The invention provides a device for rapidly measuring the content of trace aluminium and a method thereof, wherein the device comprises an electrochemical reaction tank whose working electrode is coated with a melatonin thin layer, a signal collecting device and a signal processing device, wherein the signal output of the electrochemical reaction tank is connected with the signal input of a volometer and the signal input of the signal collecting device, and the output of the signal collecting device is connected with the signal input of the signal processing device. Signals of melatonin oxidation peak current variation are received through the relationship among the calibration of melatonin oxidation peak current, the decreasing amplitude of melatonin oxidation peak current and the concentration of aluminium which is added, and the content of trace aluminium is calculated according to the relationship between the current variation and the concentration of aluminium through the signal processing device. The invention has the advantages of high measurement precision, no pollution to food and simple operation, which is not easily disturbed, and easily achieves industrialization.
Description
Technical field
The present invention relates to measure the device and method of trace amount aluminum content, especially measure the device and method of trace amount aluminum content in beverage and the biological sample.
Background technology
The research of the physiological action of relevant aluminium in human body has caused medical science, biology, food worker's great attention, especially blunt the and even dull-witted focus that becomes concern of the accumulation initiation of aluminium in human body.Yet, in food and drink and biological sample, caused now the existence of trace Al owing to reasons such as packings, through accumulating over a long period, these trace Al become the element that has about the physiology to human body about inestimable.
At present, the method for trace Al has obtained abundant and development in mensuration food and drink and the biological sample.Yet traditional mensuration aluminum concentration method comprises in the food industry so far: colourimetry, and atomic absorption method etc., speed is slow, sample pre-treatments complex steps, sensitivity are lower.Electroanalysis be expected to realize fast, sensitive, directly detect one of the selection of target.But because the reduction potential of aluminium is about-1.75V, is subject to H+ and disturbs, directly measure aluminium and have any problem.Adsorptive voltammetry utilizes the complex of aluminium and dyestuff or the electrochemical response of dyestuff can measure the aluminium in environment and the food, detects the low 10-9mol/L that reaches of lower limit, still still need add reagent.If part directly is present in human body, then need not to add.With regard to aluminium in surveying food and drink, part must not have serious murder by poisoning.
Therefore, can know the shortcoming that existing tradition measures that the aluminum concentration method exists still that analysis speed is slow, sample pre-treatments complex steps, sensitivity are lower, be subject to disturb, human body is existed potential murder by poisoning from above-mentioned analysis.
Epiphysin is the human brain depths as a kind of amine bormones of size " pineal body " secretion as the pine nut, and it has catechol ammonia structure, is prone to cooperate with Al.Epiphysin is a kind of medicine, and is present in human body again, is mainly used in the Cure for insomnia disease.
Summary of the invention
Primary technical matters to be solved by this invention is to existing background technology the device that measuring accuracy is high, pollution-free, simple to operate to food, be difficult for being disturbed, being easy to the fast measuring trace amount aluminum content of realizing industrialization to be provided.
Another technical matters to be solved by this invention is to existing background technology the method that measuring accuracy is high, pollution-free, simple to operate to food, be difficult for being disturbed, being easy to the fast measuring trace amount aluminum content of realizing industrialization to be provided.
The present invention solves the technical scheme that above-mentioned primary technical matters adopts: a kind of device of fast measuring trace amount aluminum content; It is characterized in that on working electrode, scribbling electrochemical reaction cell, signal pickup assembly, the signal processing apparatus of epiphysin thin layer; The signal output of electrochemical reaction cell goes to connect the signal input of signal pickup assembly, and the output of signal pickup assembly goes to connect the signal input of signal processing apparatus.
Preferably, described its working electrode of electrochemical reaction cell that scribbles the epiphysin thin layer is a glass-carbon electrode, is platinized platinum to electrode, and contrast electrode is a saturated calomel electrode.
As improvement, the described electrochemical reaction cell that scribbles the epiphysin thin layer comprises one or more electrochemical reaction cells that scribble the epiphysin thin layer, is convenient to large-scale promotion application.
As improvement, the described electrochemical reaction cell that scribbles the epiphysin thin layer comprises one or more signal pickup assemblies, is convenient to large-scale promotion application.
Preferably, the output of the signal of described electrochemical reaction cell also is connected with volt ampere meter, preferred differential pulse volt ampere meter.
The present invention solves the technical scheme that above-mentioned another technical matters adopts: a kind of method of fast measuring trace amount aluminum content is characterized in that:
Device is for scribbling electrochemical reaction cell, signal pickup assembly, the signal processing apparatus of epiphysin thin layer on working electrode; The signal output of electrochemical reaction cell goes to connect the signal input of signal pickup assembly, and the output of signal pickup assembly goes to connect the signal input of signal processing apparatus; Steps in sequence is:
(1) demarcates the epiphysin oxidation peak current;
(2) relation of the concentration of demarcation epiphysin oxidation peak current fall and adding aluminium;
(3) signal of the epiphysin oxidation peak current variation of reception measured object;
(4), calculate trace amount aluminum content with the electric current variation and the relation of the concentration of aluminium through signal processing apparatus.
Certainly the output of the signal of electrochemical reaction cell can also be connected with volt ampere meter.
Compared with prior art, the invention has the advantages that:
1) utilizes directly in the human body that own compound---epiphysin detects, reduce and detect food pollution;
2) need not steps such as heating, letting nitrogen in and deoxidizing and preenrichment, stir convection current and accelerated the formation of Al and melatonin epiphysin complex compound again and, accelerated analysis speed greatly to the transmission of electrode surface.This analyzes advantageous particularly for actual batch samples; Finding in the real work provides analysis speed 40%～100% than existing detection technique;
3) instrument is simple, and selectivity, accuracy are all fine, only adopts conventional device such as voltammetric measuring device commonly used and electrochemical reaction cell, is convenient to reduce cost and popularize;
4) the beverage color is noiseless to measuring.Can realize the mensuration of nearly all beverage;
5) measuring accuracy is high, can realize the measurement of μ mol/L trace Al concentration, has improved 10～100 times than existing method precision.
Description of drawings
Fig. 1 is the installation drawing of the fast measuring trace amount aluminum content that uses of the present invention;
Fig. 2 epiphysin is to the DPV response of Al;
Fig. 3 a is the graph of a relation of device sensitivity to end liquid pH value;
Fig. 3 b is the graph of a relation of device sensitivity to melatonin epiphysin concentration;
Fig. 3 c is that the device sensitivity is to NH
4The graph of a relation of Ac buffer concentration.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Examples of implementation
Meaning as shown in Figure 1; A kind of device of fast measuring trace amount aluminum content; It is characterized in that on working electrode, scribbling electrochemical reaction cell 1, volt ampere meter 2, signal pickup assembly 3, the signal processing apparatus 4 of epiphysin thin layer; The signal output of electrochemical reaction cell 1 goes to connect the signal input of volt ampere meter 2, and the signal output of electrochemical reaction cell 1 also goes to connect the signal input of signal pickup assembly 3, and the output of signal pickup assembly 3 goes to connect the signal input of signal processing apparatus 4.
Its working electrode of electrochemical reaction cell that scribbles the epiphysin thin layer is glass-carbon electrode a, is platinized platinum b to electrode, and contrast electrode c is a saturated calomel electrode.
Further improve, the electrochemical reaction cell that scribbles the epiphysin thin layer can comprise one or more electrochemical reaction cells that scribble the epiphysin thin layer.Electrochemical reaction cell also can comprise one or more signal pickup assemblies.
The preferred differential pulse of volt ampere meter volt ampere meter.
A kind of method of fast measuring trace amount aluminum content, its steps in sequence is:
(1) demarcates the epiphysin oxidation peak current;
(2) relation of the concentration of demarcation epiphysin oxidation peak current fall and adding aluminium;
(3) signal of the epiphysin oxidation peak current variation of reception measured object;
(4), calculate trace amount aluminum content with the electric current variation and the relation of the concentration of aluminium through signal processing apparatus.
The application implementation example
1 experimental section
Epiphysin storing solution (1 * 10
-3Mol/L), concentration is proofreaied and correct with ultraviolet spectroscopy.High-purity aluminium powder is dissolved in an amount of concentrated hydrochloric acid, gets aluminium storing solution (0.01mol/L) after the dilution, dilute again during use.Buffer solution is by 0.2mol/L NH
4Ac and 0.1mol/L HAc are by the proper proportion preparation.It is pure that used medicine is analysis, redistilled water, polytetrafluoroethylcontainer container.Glass-carbon electrode (diameter 3.5mm) is a working electrode, and platinized platinum is to electrode, and saturated calomel electrode is a contrast electrode.CHI-660B electroanalysis system (U.S. CHI company).Differential pulse volt-ampere parameter is: sweep fast 20mV/s, pulse height 50mV, pulse width 60 seconds.With 400 purpose fine sandpaper wet-millings polishing glass-carbon electrode; Dab with wet water absorbent paper, record epiphysin differential pulse oxidizes peak current is washed electrode with counter the clearing away of 100mV/s linearity again; Aluminum solutions electromagnetic agitation of every injection 10 minutes leaves standstill record differential pulse oxidizes peak current after 1 minute.
2 results and discussion
2.1 the differential pulse voltammogram of epiphysin and aluminium-epiphysin
Fig. 2 epiphysin is to the DPV of Al response, a:pH4.6 wherein, 0.25mol/L NH
4Ac+1.5 * 10
-4Mol/Lmelatonin; B:a+4 *; C:a+8 *; D:a+12 *; E:a+16 *, f:a+20 *, g:a+24 * 10
-6Mol/L Al
3+
Fig. 2 shows that epiphysin oxidation peak current potential is+0.45V.After adding aluminium, cyclic voltammogram is illustrated in-and 0.5-1.2V do not have new peak and occurs.But the epiphysin oxidation peak current descends, and fall has linear relationship with the concentration that adds aluminium.This is the basis of quantitative measurement aluminium.
2.2 selection of experiment conditions
To end liquid pH value, melatonin concentration and NH
4Experiment conditions such as Ac buffer concentration and stirring rate are selected, and Fig. 3 a, 3b, 3c result show, with the NH of 0.25mol/L
4Ac-HAc damping fluid (pH4.6) is an end liquid, 1.5 * 10
-4The melatonin of mol/L can obtain the sensitiveest Al reaction signal.
2.3 response time, current peak stability, the range of linearity, detection lower limit and relative standard deviation
Under above-mentioned optimum experimental condition, it is very quick that this method is surveyed the Al peak current reduction response time, and 40s just can reach the stable peaks height.Stability and reappearance are also fine, for 5 * 10
-6Mol/L Al, the response peak height remains on 2.5 μ A within 50min.The range of linearity is 1 * 10
-6～2 * 10
-5Mol/L, regression equation is: △ I
p(μ A)=0.0063+0.043 [Al] (* 10
-6Mol/L, r=0.9983), relative standard deviation is 2.2% (n=10,1 * 10
-5Mol/L Al), be limited to 5 * 10 under the detection
-7Mol/L.
2.4 interfering ion influence
Tested the interference that common ion detects Al in the beverage.Experiment shows (5 * 10
-6During mol/L Al): the main interference is Cr
3+(2 times).But Cr in actual water sample
3+Concentration is very low, and is disturbing below the critical value, therefore noiseless to this analysis.The disturbed condition of other ion is: 40 times of In (III), Ga (III), Co (II) Zr (IV), Fe (III), Fe (II), Sn (II), Zn (II), 80 times of Pb (II), Cd (II), MnO
4 -, Ba (II) and cetyl amine bromide, 100 times of Tl (I), V (V), Cr (VI), Mn (II), I
-, Bi (III) and bromination tetrapropyl ammonium, 200 times of Hg (II), SCN
-, citric acid, 200 times of tartrate, C
2O
4 2-, 350 times of Ag (I), Ge (IV), PO
4 3-, F
-, NO
2 -, 600 times of EDTA, ClO
3 -, CO
3 2-, benzoic acid hydrogen potassium.A large amount of sucrose, lactic acid, ethanol, Ca (II), Na (I), K (I) Mg (II), Sr (II), Si (IV), SO
4 2-, NO
3 -Do not disturb.
2.5 actual sample is measured
Adopt standard addition method that more than 10 samples are measured, sample is to buy from the supermarket.Main chemical compositions is in the carbonated beverages such as cola, Finda: carbonic acid, sucrose, phosphoric acid, caramel, sodium pyrosulfite, Sodium Benzoate etc.; Composition is in the beer: maltose, starch, ethanol, carbonic acid; Principal ingredient is in the coconut milk: lactic acid, sucrose.Its medium coke black in color, the Finda is grass green; Beer etc. are khaki, and coconut milk is creamy white.Actual analysis water sample result sees table 1.
With ICP-AES method basically identical, show that this method is reliable.
The mensuration of aluminium in table 1 drink sample (n=3, the μ mol/L of unit)
Tablel.Detection?of?Aluminum?in?beverage?samples
3 conclusions
Set up the new method of aluminium in a kind of quick, simple, sensitive direct beverage.Studied the interference of the yin, yang ion that possibly exist in a series of human bodies.Measure aluminium in the appearance such as mineral water, beverage with standard addition method.The good recovery shows that this method has actual application prospect.Its outstanding advantage has: (1) directly utilizes in the human body own compound to detect; Reduce and detect food pollution; Need not steps such as heating, letting nitrogen in and deoxidizing and preenrichment; Stirring convection current has accelerated the formation of Al and melatonin complex compound again and to the transmission of electrode surface, has accelerated analysis speed greatly.This analyzes advantageous particularly for actual batch samples; (2) instrument is simple, and selectivity, accuracy are all fine.The beverage color is noiseless to measuring.
Claims (10)
1. the device of a fast measuring trace amount aluminum content; It is characterized in that on working electrode, scribbling electrochemical reaction cell (1), signal pickup assembly (3), the signal processing apparatus (4) of epiphysin thin layer; The signal output of electrochemical reaction cell (1) goes to connect the signal input of signal pickup assembly (3), and the output of signal pickup assembly (3) goes to connect the signal input of signal processing apparatus (4).
2. device according to claim 1 is characterized in that the signal output of described electrochemical reaction cell (1) also is connected with volt ampere meter (2).
3. the device of fast measuring trace amount aluminum content according to claim 1 and 2; It is characterized in that described its working electrode of electrochemical reaction cell that on working electrode, scribbles the epiphysin thin layer is a glass-carbon electrode; To electrode is platinized platinum, and contrast electrode is a saturated calomel electrode.
4. the device of fast measuring trace amount aluminum content according to claim 3 is characterized in that the described electrochemical reaction cell that on working electrode, scribbles the epiphysin thin layer comprises one or more electrochemical reaction cells that scribble the epiphysin thin layer.
5. the device of fast measuring trace amount aluminum content according to claim 4 is characterized in that the described electrochemical reaction cell that on working electrode, scribbles the epiphysin thin layer comprises one or more signal pickup assemblies.
6. the device of fast measuring trace amount aluminum content according to claim 5 is characterized in that the preferred differential pulse of described volt ampere meter volt ampere meter.
7. the method for a fast measuring trace amount aluminum content is characterized in that:
Device is for scribbling electrochemical reaction cell (1), signal pickup assembly (3), the signal processing apparatus (4) of epiphysin thin layer on working electrode; The signal output of electrochemical reaction cell (1) goes to connect the signal input of signal pickup assembly (3), and the output of signal pickup assembly (3) goes to connect the signal input of signal processing apparatus (4);
Steps in sequence is:
(1) demarcates the epiphysin oxidation peak current;
(2) relation of the concentration of demarcation epiphysin oxidation peak current fall and adding aluminium;
(3) signal of the epiphysin oxidation peak current variation of reception measured object;
(4), calculate trace amount aluminum content with the electric current variation and the relation of the concentration of aluminium through signal processing apparatus.
8. method according to claim 7 is characterized in that the signal output of described electrochemical reaction cell (1) also is connected with volt ampere meter (2).
9. method according to claim 7 is characterized in that described epiphysin is with 1.25-1.6 * 10
-4Mol/L, the NH of 0.1-0.3mol/L
4Ac-HAc damping fluid, pH4-4.8 are end liquid.
10. method according to claim 8 is characterized in that described epiphysin is with 1.5 * 10
-4Mol/L, the NH of 0.25mol/L
4Ac-HAc damping fluid, pH4.6 can obtain the sensitiveest Al reaction signal for end liquid.
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| CN101349670B true CN101349670B (en) | 2012-01-04 |
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| CN107389568B (en) * | 2017-05-23 | 2020-11-10 | 宁波大学 | Colorimetric detection probe for detecting kanamycin and detection method thereof |
| CN108982638A (en) * | 2018-05-25 | 2018-12-11 | 宁德师范学院 | A kind of method of Trace Aluminum in quick measurement water |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1205435A (en) * | 1997-07-11 | 1999-01-20 | 北京科技大学 | Steel liquid directly fixing aluminium sensor |
| CN1837806A (en) * | 2005-12-15 | 2006-09-27 | 南京大学 | Electrochemical method for measuring aluminium |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1205435A (en) * | 1997-07-11 | 1999-01-20 | 北京科技大学 | Steel liquid directly fixing aluminium sensor |
| CN1837806A (en) * | 2005-12-15 | 2006-09-27 | 南京大学 | Electrochemical method for measuring aluminium |
Non-Patent Citations (2)
| Title |
|---|
| 刘玉新等.脑海马结构研究进展.《宁波大学学报》.2000,第13卷(第3期),105. * |
| 李晔等.络合滴定分析铝的铬酸电化学氧化溶液中铝离子含量.《电镀与精饰》.1984,(第5期),47-48. * |
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