CN102721723A - Hogwash oil identifying method based on volatile matter - Google Patents
Hogwash oil identifying method based on volatile matter Download PDFInfo
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- CN102721723A CN102721723A CN2012102304479A CN201210230447A CN102721723A CN 102721723 A CN102721723 A CN 102721723A CN 2012102304479 A CN2012102304479 A CN 2012102304479A CN 201210230447 A CN201210230447 A CN 201210230447A CN 102721723 A CN102721723 A CN 102721723A
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- molecular wire
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Abstract
The invention discloses a hogwash oil identifying method based on volatile matter. The method comprises the following steps of (1) designing a molecular wire array probe; (2) constructing a molecular wire piezoelectric sensor device; (3) analyzing a known sample; (4) extracting feature identifying information; and (5) identifying a sample to be tested: achieving fast identification of hogwash oil by comparing an output feature value with a feature value of the known sample. The hogwash oil identifying method based on the volatile matter has the advantages of being high in sensitivity, fast in detection, convenient to operate, low in cost and the like, and can provide a reliable basis for the law-enforcing department and inspection bodies to perform sampling inspection on quality of oil products.
Description
Technical field
The present invention relates to the discrimination method of hogwash fat, particularly a kind of hogwash fat discrimination method based on volatility thing group.
Background technology
Hogwash fat (waste oil of narrow sense) is that catering industry washes dishes, washes the dishes, residue leftovers etc. flows into trench, in oil interceptor, fish for, and the grease of handling through pulp water separation, thermal dehydration, decolorization refining.Because hogwash fat is similar with oil with common edible in appearance is difficult to distinguish that some lawless persons are ordered about by juice in recent years, extracts hogwash fat in a large number and sell at a low price to market.Owing to be mixed with sewage, rubbish, washing agent and the sour food that loses in the swill; Contain carcinogens such as a large amount of bacteriotoxins, lipid peroxide, benzopyrene, alkanes and aflatoxins in the hogwash fat after processing is refined; And heavy metal ion, the hydroxyl valency of grease is considerably beyond the edible oil hygienic standard of national regulation.Through hogwash fat is carried out toxicological study, the result shows, takes in hogwash fat for a long time and will cause human development's obstacle; Be prone to suffer from enteritis, and liver, the heart and pathologies such as kidney enlargement and fatty liver are arranged, in addition; Aflatoxin in the hogwash fat; Its toxicity is 68 times of arsenic, is prone to cause the canceration of many internal organs of human body, like position cancerations such as liver cancer, sdenocarcinoma of stomach, kidney, the carcinoma of the rectum, breast cancer and ovary, small intestines.
Existing method of discrimination about hogwash fat can be divided into three major types at present: organoleptic detection, conventional sense and instrument detecting.Organoleptic detection differentiates that through seeing, hear, taste, listen, ask five aspects there is very big subjectivity in this detection method, and strong evidence data can't be provided; Conventional detection discrimination method mainly is that Various Edible total physics and chemical feature are compared; Like acid value, iodine number, peroxide value, degree of unsaturation, density, specific heat, moisture, solidifying point, index of refraction and unsaponifiable matter content etc., thereby the character of grease is estimated; Because conventional method need be done a large amount of early-stage preparations; Process is loaded down with trivial details; Therefore on the conventional method basis, developed some fast detection methods,, whether mingled thereby differentiate edible oil as adopting the acid value and the peroxide value of quick measuring card method fast detecting oil; This method is made card form with the scraps of paper as carrier; React through developer and free fatty acid or superoxide, its degree that on the scraps of paper, develops the color is directly proportional with the content of free fatty acid or superoxide, reaches the sxemiquantitative of acid value or peroxide value with this.Because the similarity of physicochemical characteristic between the grease, these methods are always ineffective.Along with development of science and technology, the appearance of exact instrument, and computing machine is in the infiltration in analytical chemistry field, the advanced analysis instrument occurred utilizing and utilized the method for stoichiometric chemistry to solve the difficult problem that edible oil is mingled, and obtained comparatively satisfied result.Roughly following: the gas chromatography determination cholesterol level detects the method for hogwash fat; Micro-wave digestion-inductivity coupled plasma mass spectrometry (ICP-MS) is measured trace element in the oil simultaneously; The result shows that element of Fe, Cr, Zn, Mn content in hogwash fat obviously exceeds edible oil, and Hg, Sn, Co, Sb, Tl, Mo no matter edible oil still in hogwash fat content all be lower than detectability; Thin-layer chromatographic analysis finds that the thin-layer chromatography of hogwash fat has tangible hangover spot; Qualified edible oil does not then have; Hangover spot composition is through the column chromatography separation and carry out infrared analysis, and the result shows that the hangover composition of hogwash fat is aldehyde, the ketone compounds that qualified edible oil does not contain; Whether adopt the content of fatty acid in the gas chromatography determination edible oil and fat, differentiate in the edible oil and mingle, research shows that the massfraction of the relative degree of unsaturation of fatty acid (U/R) value and fatty acid distributes can differentiate waste oil.But the instrument detecting equipment needed thereby is huge, costs an arm and a leg, complex operation, unsuitable promoting the use of.
Therefore, research easy and simple to handle, hogwash fat discrimination method fast and accurately is imperative.
Summary of the invention
The objective of the invention is to overcome existing method weak point and a kind of hogwash fat discrimination method of easy, quick, accurate, inexpensive is provided.
In order to realize above-mentioned technical purpose, technical scheme of the present invention is that a kind of hogwash fat discrimination method based on volatility thing group may further comprise the steps:
Step 1: with the comb electrode is conductance electrode; With conducting high polymers thing or electrical-conductive nanometer high molecular polymer molecular wire is the sensitive membrane of the special volatility thing of hogwash fat group; Modify to comb electrode final vacuum drying through method of being coated with or infusion process, prepare the molecular wire array probe;
Step 2: with the prepared molecular wire array probe of the step 1 part that is sensor; Setting comprises the hardware system of sensor, frame of reference, display system; Wherein sensor comprises the molecular wire array probe, is used to adorn test bottle, temperature regulating device, oscillatory circuit and the piezoelectric quartz crystal sensor that detects oil sample; Described molecular wire array probe is inserted in the test bottle, and described test bottle is arranged at temperature regulating device, and the output terminal of molecular wire array probe is connected to oscillatory circuit and piezoelectric quartz crystal sensor respectively; The output terminal of piezoelectric quartz crystal sensor is connected to oscillatory circuit; Described frame of reference comprises branch frequency meter, driving circuit and single-chip microcomputer, and the input end of described minute frequency meter is connected to the output terminal of oscillatory circuit, divides the output terminal of frequency meter to be connected to driving circuit and single-chip microcomputer respectively; The output terminal of driving circuit connects single-chip microcomputer; The input end of single-chip microcomputer also is connected to oscillatory circuit, and described display system comprises display, and described display is connected to single-chip microcomputer through the MAX232 interface;
Step 3: oil sample is added in the test bottle, insert the molecular wire array probe, oil sample liquid level and probe keep 4cm; Test bottle is inserted in the temperature regulating device of molecular wire piezoelectric sensing device; Regulate temperature regulating device, it is 70 ° of C that temperature is set, and treats to begin to detect after the temperature balance;
Step 4: will handle through the frequency data of each measured array of molecular wire array probe, and obtain frequency-shift data, frequency-shift data is analyzed, characteristic information extraction obtains the eigenwert that can differentiate hogwash fat.
Described a kind of hogwash fat discrimination method based on volatility thing group, the sensitive membrane material described in the step 1 are wherein at least a of polyaniline, polypyrrole or polythiophene.
Described a kind of hogwash fat discrimination method based on volatility thing group, conducting high polymers thing described in the step 1 or electrical-conductive nanometer high molecular polymer are to adopt chemical oxidative polymerization or interface synthetic method or galvanochemistry synthetic method to be prepared from.
Described a kind of hogwash fat discrimination method based on volatility thing group, the molecular wire array probe described in the step 1 are that 6 comb electrodes adopt 2 * 3 array combination to form.
Described a kind of hogwash fat discrimination method based on volatility thing group, each comb electrode connects independently oscillatory circuit with lead respectively in the described molecular wire array probe.
Described a kind of hogwash fat discrimination method based on volatility thing group is characterized in that, the output data of each molecular wire array adopts frequency shift value Δ F in the step 4
i, frequency shift value Δ F
iObtain through method of difference, formula is:
ΔF
i=F
i-F
0，
F wherein
iBe real-time frequency, F
0Be the piezoelectric quartz crystal original frequency.Adopt frequency shift value Δ F
iPurpose be to avoid the influence that causes because of piezoelectric quartz crystal original frequency value difference in the different oscillatory circuits.
Described a kind of hogwash fat discrimination method based on volatility thing group is characterized in that, extracts eigenwert X in the step 4
iComputing formula be:
X
i=|f
1'(t)|
max+|f
2'(t)|
max+|f
3'(t)|
max+……|f
a'(t)|
max
Wherein, | f
a' (t) |
MaxBe the maximal value of the absolute value of the first derivation value of the frequency displacement of a molecular wire array probe in the i sample-time response curve, wherein a is more than or equal to 1 and smaller or equal to 6 integer.
The innovation that the present invention contrasts prior art is, thereby has proposed to carry out the new method that hogwash fat is differentiated with special volatility thing group in the molecular wire piezoelectric sensing device analysis hogwash fat; Made up the molecular wire piezo-electric device that molecular wire array probe and piezoelectric quartz crystal sensor merge.
Technique effect of the present invention is,
1, is easy to regulate and control output signal strength through the preparation condition of regulating the molecular wire film and the electrode parameter that changes comb electrode;
2, the influence of electric double layer capacitance has been avoided in the use of piezoelectric quartz crystal sensor, has improved the stability of electric signal, has strengthened signal to noise ratio (S/N ratio);
3, molecular wire array probe and piezoelectric quartz crystal sensor have significantly improved the degree of accuracy that detects after merging.
4, but the robotization of the combination implement device of frame of reference, display system is handled in the device.
Description of drawings
Fig. 1 is the structural representation of apparatus of the present invention;
Wherein: A-sensor, B-frame of reference, C-display system;
1-molecular wire array probe; The 2-test bottle; The 3-temperature regulating device; The 4-oscillatory circuit; The 5-piezoelectric quartz crystal sensor; 6-divides frequency meter; The 7-driving circuit; The 8-single-chip microcomputer; The 9-display;
Fig. 2 overlooks the synoptic diagram of (a) and side-looking (b) for the molecular wire array probe;
The 10-comb electrode; The 11-molecular wire; The 12-connector; The 13-lead
Fig. 3 is the frequency displacement response curve of different molecular wire array probe.
Fig. 4 is the first derivation curve of frequency displacement response curve.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further.
The principle of foundation of the present invention is: research shows; Contain abundant volatile ingredient in the oil product; Significant variation can take place in its volatile ingredient if oil quality changes, as produce in acetate, propionic acid, butyric acid, valeric acid, the caproic acid etc. a kind of, two or more; Molecular wire film electrical quantity when adsorb volatile thing group can change, and piezoelectric quartz crystal sensor changes the electrical quantity of the object of serial connection with it sensitive change of frequency is arranged, referring to formula (1):
Δ F=F in the formula
i-F
0, F
iThe expression resonance frequency,
The fundamental frequency of expression quartz crystal;
C
qAnd C
0Dynamic capacity and the direct capacitance of representing quartz crystal sensor respectively;
G and C
sThe electricity that is respectively the object of surveying is led and electric capacity: G=κ χ, κ are the electrode constant of the electrode that is connected in series with piezoelectric quartz crystal sensor, and χ is the conductivity of the object of surveying; C
s=κ ε+C
p, ε is the specific inductive capacity of the object of surveying, C
pBe the stray capacitance between two leads that link to each other with electrode;
Basic thought of the present invention: make up molecular wire piezoelectric sensing device through fusion molecule wire array probe and piezoelectric quartz crystal sensor, realize analysis, thereby propose the new method that hogwash fat is differentiated to the special volatility thing group of hogwash fat.
According to above principle and thought, the technical scheme of being set up is following,
Adopt molecular wire piezoelectric sensing device shown in Figure 1 to realize the discriminating of hogwash fat.Setting comprises the hardware system of sensor, frame of reference, display system; Wherein sensor comprises the molecular wire array probe, is used to adorn test bottle, temperature regulating device, oscillatory circuit and the piezoelectric quartz crystal sensor that detects oil sample; The molecular wire array probe is inserted in the test bottle, and test bottle is arranged at temperature regulating device, and the output terminal of molecular wire array probe is connected to oscillatory circuit and piezoelectric quartz crystal sensor through connector respectively with lead; The output terminal of piezoelectric quartz crystal sensor is connected to oscillatory circuit; Frame of reference comprises branch frequency meter, driving circuit and single-chip microcomputer, and the input end of branch frequency meter is connected to the output terminal of oscillatory circuit, divides the output terminal of frequency meter to be connected to driving circuit and single-chip microcomputer respectively; The output terminal of driving circuit connects single-chip microcomputer; The input end of single-chip microcomputer also is connected to oscillatory circuit, and display system comprises display, and display is connected to single-chip microcomputer.
Wherein the substrate comb electrode that adopted of molecular wire array probe be adopt terahertz wave quasi-optics through open material, sink copper, figure transfer, graphic plating, move back film, etching, moulding, testing process and will organize the unit comb electrode that is arranged in parallel more and be deposited into the substrate of pi film; Conducting high polymers thing or electrical-conductive nanometer high molecular polymer are to adopt chemical oxidative polymerization or interface synthetic method or galvanochemistry synthetic method to be prepared from.Chemical oxidative polymerization, interface synthetic method and galvanochemistry synthetic method can be specifically with reference to H.R. A Er Cook, and the F.W. orchid is general, J.E. mark, contemporary polymer chemistry [M], Beijing: Chemical Industry Press, 2006; D.D.Sawall, R.M.Villahermosa, R.A.Lipeles; And Alan R.Hopkins, Interfacial Polymerization of Polyaniline Nanofibers Grafted to Au Surfaces, Chem.Mater2004; 16,1606-1608; The preparation of molecular wire probe comprises three kinds of methods: 1) through conducting high polymers thing or electrical-conductive nanometer high molecular polymer molecular wire are dissolved in organic solvent such as the dimethyl sulfoxide (DMSO); Process conducting high polymers thing solution; Get 1 this solution of μ L with micropipettor and drip to the comb electrode surface, then vacuum drying and getting through the evenly coating or comb electrode immersed 10 ~ 30min in this solution of spin coating appearance; 2) directly the conducting high polymers thing is deposited on the comb electrode as working electrode through galvanochemistry synthetic method or interfacial polymerization.
Piezoelectric quartz crystal sensor is a 9MHz AT-cut type, and the two sides is silver-plated, purchases 707 factories to Beijing, and the molecular wire array probe is connected through lead with piezoelectric quartz crystal sensor.
In test process, the molecular wire array probe combines with the special volatility thing group of survey oil samples, causes the change of frequency of piezoelectric quartz crystal sensor, obtains response signal.And the collection of signal is by computer control; At first send instructions to single-chip microcomputer through the MAX232 interface, need to gather the signal of which array, computer control hyperchannel SS by computing machine; Open corresponding acquired signal passage; The signal input of gathering divides frequency meter, divides frequency meter that it is passed to single-chip microcomputer, and single-chip microcomputer is passed to display system through data-interface.Eigenwert is handled, analyzes, extracted to all frequency data by single-chip microcomputer, and with the data with existing storehouse in the eigenwert of normal oil sample compare and output identification result.
The flow process of differentiating hogwash fat through molecular wire piezoelectric sensing device is (is example with swill oil sample 5): oil sample to be measured is added in the test bottle, insert the molecular wire array probe, oil sample liquid level and probe keep certain distance; Test bottle is inserted molecular wire piezoelectric sensing Device Testing position; Regulate temperature regulating device, it is 70 ° of C that temperature is set, balance 20min; Starting molecular wire piezoelectric sensing device operation interface detects; Obtain each array of molecular wire (totally 6) frequency data, frequency data are exported (seeing table 1) with frequency displacement, obtain real-time frequency displacement response curve (see figure 3) simultaneously through software.
Frequency shift value (the Δ F of table 1 different molecular wire probe different time in swill oil sample 5
i=F
i-F
0)
With the time in the table 1 be horizontal ordinate, frequency shift value is an ordinate, can get the frequency displacement of 6 molecular wire probes-time response curve, sees Fig. 3, behind each curve first derivation, the maximal value of getting its absolute value is extraction value (referring to Fig. 4), the result sees table 2:
The extraction value of table 2 different molecular wire array
Extraction value to each molecular wire probe is carried out data fusion, and the extraction value sum of 6 sensor output signals in the array is represented the eigenwert of swill oil sample 5, the then eigenwert (X of swill oil sample 5
5) be the extraction value sum of 6 molecular wire arrays in the table 2:
X
5=0.058+0.667+1.808+3.792+3.642+2.508=12.475 (2)
Can know that by formula (2) eigenwert of swill oil sample 5 is 12.475
Use the same method and analyzed 30 of oil samples (each 15 of qualified oil sample and swill oil samples), its eigenwert is seen table 3, can be known by table; The mean eigenvalue of normal oil sample is 5.366 ± 1.582; And the mean eigenvalue of swill oil sample is 12.231 ± 1.351, and two stack features values are carried out the T check, obtains | T
0|=12.7808>2.7633 (T
0.005(28)) result shows two class values there were significant differences in 99% fiducial interval.According to sample results, in this method eigenwert X
i>=9 sample is judged to hogwash fat.
The eigenwert of table 3 oil sample
Claims (7)
1. the hogwash fat discrimination method based on volatility thing group is characterized in that, may further comprise the steps:
Step 1: with the comb electrode is conductance electrode; To be the sensitive membrane of the special volatility thing of hogwash fat group with conducting high polymers thing or electrical-conductive nanometer high molecular polymer molecular wire; Modify to comb electrode final vacuum drying through method of being coated with or infusion process, prepare the molecular wire array probe;
Step 2: with the prepared molecular wire array probe of the step 1 part that is sensor; Setting comprises the hardware system of sensor, frame of reference, display system; Wherein sensor comprises the molecular wire array probe, is used to adorn test bottle, temperature regulating device, oscillatory circuit and the piezoelectric quartz crystal sensor that detects oil sample; Described molecular wire array probe is inserted in the test bottle, and described test bottle is arranged at temperature regulating device, and the output terminal of molecular wire array probe is connected to oscillatory circuit and piezoelectric quartz crystal sensor respectively; The output terminal of piezoelectric quartz crystal sensor is connected to oscillatory circuit; Described frame of reference comprises branch frequency meter, driving circuit and single-chip microcomputer, and the input end of described minute frequency meter is connected to the output terminal of oscillatory circuit, divides the output terminal of frequency meter to be connected to driving circuit and single-chip microcomputer respectively; The output terminal of driving circuit connects single-chip microcomputer; The input end of single-chip microcomputer also is connected to oscillatory circuit, and described display system comprises display, and described display is connected to single-chip microcomputer through the MAX232 interface;
Step 3: oil sample is added in the test bottle, insert the molecular wire array probe, oil sample liquid level and probe keep 4cm; Test bottle is inserted in the temperature regulating device of molecular wire piezoelectric sensing device; Regulate temperature regulating device, it is 70 ° of C that temperature is set, and treats to begin to detect after the temperature balance;
Step 4: will handle through the frequency data of each measured array of molecular wire array probe, and obtain frequency-shift data, frequency-shift data is analyzed, characteristic information extraction obtains the eigenwert that can differentiate hogwash fat.
2. a kind of hogwash fat discrimination method based on volatility thing group according to claim 1 is characterized in that, the sensitive membrane material described in the step 1 is wherein at least a of polyaniline, polypyrrole or polythiophene.
3. a kind of hogwash fat discrimination method according to claim 1 based on volatility thing group; It is characterized in that conducting high polymers thing described in the step 1 or electrical-conductive nanometer high molecular polymer are to adopt chemical oxidative polymerization or interface synthetic method or galvanochemistry synthetic method to be prepared from.
4. a kind of hogwash fat discrimination method based on volatility thing group according to claim 1 is characterized in that, the molecular wire array probe described in the step 1 is that 6 comb electrodes adopt 2 * 3 array combination to form.
5. a kind of hogwash fat discrimination method based on volatility thing group according to claim 4 is characterized in that each comb electrode connects independently oscillatory circuit with lead respectively in the described molecular wire array probe.
6. according to right 1 described a kind of hogwash fat discrimination method, it is characterized in that the output data of each molecular wire array adopts frequency shift value Δ F in the step 4 based on volatility thing group
i, frequency shift value Δ F
iObtain through method of difference, formula is:
ΔF
i=F
i-F
0，
F wherein
iBe real-time frequency, F
0Be the piezoelectric quartz crystal original frequency.
7. according to right 1 described a kind of hogwash fat discrimination method, it is characterized in that, extract eigenwert X in the step 4 based on volatility thing group
iComputing formula be:
X
i=|f
1'(t)|
max+|f
2'(t)|
max+|f
3'(t)|
max+……|f
a'(t)|
max
Wherein, | f
a' (t) |
MaxBe the maximal value of the absolute value of the first derivation value of the frequency displacement of a molecular wire array probe in the i sample-time response curve, wherein a is more than or equal to 1 and smaller or equal to 6 integer.
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| CN103424413A (en) * | 2013-09-03 | 2013-12-04 | 衡阳师范学院 | Method for detecting illegal cooking oil in radioactive measurement mode |
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| CN111579594A (en) * | 2020-05-27 | 2020-08-25 | 上海交通大学 | Application of room temperature gas sensor in nerve agent detection |
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