CN111665205A - Optical sensor for detecting formaldehyde content in milk - Google Patents

Optical sensor for detecting formaldehyde content in milk Download PDF

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Publication number
CN111665205A
CN111665205A CN202010489306.3A CN202010489306A CN111665205A CN 111665205 A CN111665205 A CN 111665205A CN 202010489306 A CN202010489306 A CN 202010489306A CN 111665205 A CN111665205 A CN 111665205A
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China
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detecting
sensor
formaldehyde content
formaldehyde
milk
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CN202010489306.3A
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Chinese (zh)
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李锦安
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry

Abstract

The invention discloses an optical sensor for detecting formaldehyde content in milk, which comprises an optical fiber 1, a middle cavity 2 and a convex lens 3. The end of the optical fiber 1 is coated with a polyoxometallate film 4. The top of the middle cavity 2 is provided with an open slot, and the bottom of the middle cavity is provided with an exhaust hole. The liquid to be detected is injected into the middle cavity 2 from the open slot at the top, and flows out from the vent hole at the bottom of the middle cavity after the detection is finished. The formaldehyde in the liquid to be detected reacts with the polyoxometallate film 4, so that the light penetrating through the polyoxometallate film is changed, and the content of the formaldehyde in the milk can be indirectly and quantitatively detected by detecting the ultraviolet-visible absorption spectrum of the light penetrating through the polyoxometallate film through a spectrophotometer. The data obtained by detecting the formaldehyde content by using the optical sensor is accurate and reliable, a heating link in the traditional formaldehyde detection method is omitted, and the method has good practical application value.

Description

Optical sensor for detecting formaldehyde content in milk
Technical Field
The invention relates to the technical field of milk detection, in particular to an optical sensor for detecting formaldehyde content in milk.
Background
Milk known as 'white blood' is rich in mineral substances, calcium, phosphorus, iron, zinc, copper, manganese and molybdenum. The milk is the best source of calcium for human body, and the proportion of calcium and phosphorus is proper, thus being beneficial to the absorption of calcium.
Formaldehyde is very effective in inhibiting microbial growth and extending the shelf life of the product. Formaldehyde is added not only to milk for human consumption but also to skimmed milk for animal husbandry. Although formaldehyde is a natural metabolite in humans, high dose exposure increases the risk of acute poisoning, and chronic respiratory diseases, nasopharyngeal carcinoma, colon cancer, etc. may be caused by chronic exposure to low doses of formaldehyde.
The existing milk adulteration analysis and detection methods are mostly based on the spectroscopy technology, and although the methods have high sensitivity, the detection equipment is expensive. Chinese patent (patent publication No. CN 110849945A) A method for rapid nondestructive testing of milk properties and milk adulterants, which utilizes an open coaxial probe combined with a vector network analyzer to measure S parameters of milk, designs a quasi-static model method to analyze and calculate the S parameters, and finally obtains the dielectric constant of a substance. And (3) detecting the properties of the milk and the milk adulteration substance by using the dielectric constant change curve of the milk. The method is easy to cause the reduction of the test accuracy due to the mutual interference of substances in the milk, and simultaneously has higher cost. Another approach is to detect one or a class of adulterants. Chinese patent (patent publication No. CN 107219284A) discloses a method for detecting milk adulteration by a fluorine ion electrode, which overcomes the defect of complex milk adulteration detection process and provides a method for detecting milk adulteration by a fluorine ion electrode. Chinese patent (patent publication No. CN 105588925A) A method for rapidly identifying and detecting milk adulteration realizes the detection of milk water by collecting the fingerprint of a milk sample to be detected and identifying the milk sample to be detected by adopting a qualitative identification model. The patent statement for detecting one or a plurality of adulterants can not realize the detection of the formaldehyde content in the milk. A commonly used method for measuring formaldehyde content is acetylacetone spectrophotometry. In an ammonium acetate buffer solution with the pH =6, formaldehyde reacts with acetylacetone under the condition of boiling water bath to quickly generate a stable yellow compound; the method is a laboratory method, and simultaneously needs boiling water bath heating, so that potential safety hazards exist, and the method has great limitation.
The method aims to solve the problem that the detection cost of the milk adulteration based on the spectroscopy technology is high; the invention discloses an optical sensor for detecting formaldehyde content, which has higher requirement on the test environment and certain danger. The optical sensor is utilized to test the formaldehyde content, the heating link in the traditional method for detecting the formaldehyde content can be omitted, and the method has the advantages of simple operation, low cost, high detection speed and high efficiency, and reduces the requirement on detection equipment.
Disclosure of Invention
Technical problem to be solved
In order to solve the technical problem, the invention provides a sensor for detecting the content of formaldehyde in milk. The sensor has the advantages of simple operation, low cost, high detection speed and high efficiency, and solves the problems that the methods for detecting the formaldehyde content in the milk in the prior art are laboratory methods, boiling water bath heating is needed, and potential safety hazards exist.
(II) technical scheme
The technical scheme of the invention is that a sensor is designed on the basis of a polyoxometallate film which is insoluble in water and can react with trace formaldehyde in a solution, the content of the formaldehyde in the solution is indirectly detected by utilizing the change of light penetrating through the sensor along with the content of the formaldehyde in the solution, and the sensor comprises optical fibers 1 and 6, a middle cavity 2, a convex lens 3, a polyoxometallate film 4 and an SMA adapter 5.
Preferably, the core at the end of the optical fiber 1 is bare.
Preferably, the bare core end of the optical fiber 1 is washed.
Preferably, the bare core end of the optical fiber 1 is coated with a polyoxometalate film 4.
Preferably, the polyoxometalate film 4 is insoluble in water.
Preferably, the polyoxometalate film 4 is capable of reacting with formaldehyde in solution.
Preferably, the middle cavity 2 is made of a polymer material with stable chemical properties.
Preferably, the top of the middle cavity 2 is provided with an open slot, and the bottom is provided with an exhaust hole.
Preferably, the open slots at the top and the vent holes at the bottom of the middle chamber 2 need to be closed by threaded plugs during the test.
Preferably, the liquid to be detected is injected from an open slot of the middle cavity 2.
Preferably, the liquid to be detected is discharged from the vent hole of the middle cavity 2 after being detected.
Preferably, the middle chamber 2 is washed with a special detergent before and after the detection.
Preferably, the convex lens 3 focuses the light transmitted through the polyoxometalate film 4 on the optical fiber 6.
Preferably, the SMA adapter 5 is connected to a light source.
Preferably, the optical fiber 6 is connected to a spectrophotometer.
Advantageous effects
Compared with the prior art, the invention provides a sensor for detecting formaldehyde in milk, which has the following beneficial effects:
1. the optical sensor has better sensitivity and accuracy;
2. compared with a common acetylacetone spectrophotometry for detecting formaldehyde, the optical sensor has the advantages that the heating step is omitted, the safety is better, the requirement on detection equipment is reduced, and the applicability is wider.
3. The optical sensor has better performance stability.
Drawings
FIG. 1 is a schematic structural diagram of an optical sensor for detecting formaldehyde content in milk
FIG. 2 is a schematic diagram of the operation of an optical sensor for detecting the formaldehyde content in milk
FIG. 3 shows the UV-VIS absorption spectrum measured according to the specific embodiment
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Preparation of polyoxometallate ([ (C)4H9)4N]4H[PMo10V2O40]) 0.40 g of tetra-n-butylammonium bromide (C)16H36BrN) and 0.40 g of polyoxometalate (H)5[PMo10V2O40]·11H2O) was dissolved in 10 mL of aqueous solution and the reaction yielded an orange solid. The suspension was stirred for 1 hour, then the solid was filtered off, washed with four 5 mL portions of water and dried in a vacuum desiccator. Preparing sensitive membrane solution by mixing polyvinyl chloride (PVC) (33%), o-nitro octyl ether (NPOE) (66%) and [ (C)4H9)4N]4H [PMo10V2O40](1%) was mixed in 1 mL of Tetrahydrofuran (THF) and reacted to form a sensitive membrane that reacted with formaldehyde in solution. And (3) treating a base material, namely removing an outer coating from the tail end of the optical fiber 1 with a pure fused silica core of 600 mu m by using a blade, and removing a cladding by using a longitudinal optical fiber stripping clamp to expose the core for 3 mm. And (3) coating the fiber core of the optical fiber, cleaning the bare fiber core by using ethanol, immersing the bare fiber core into a film solution, taking out and drying for 12 hours in a natural state. The middle chamber 2 is prepared, and the middle chamber 2 with the capacity of 1.5 mm is prepared by polyether ether ketone (PEEK). And (3) transmitting light, namely, focusing the light penetrating through the oxometallate film by using a convex lens 7 with the focal length of 30 mm, and transmitting the focused light to a spectrophotometer by using another optical fiber 6.
The device is connected according to the method shown in figure 2, and the optical sensor is used for detecting the content of formaldehyde in the milk. And stabilizing the light source 7, and turning on the deuterium lamp 7 and standing for 30 min. Instrument calibration, spectrophotometer 8 was calibrated using fiber 1 in the middle chamber 2 with zero transmission measured in the dark setting and 100% transmission measured with uncoated fiber. And (3) carrying out coating treatment on the fiber core of the optical fiber, taking out the optical fiber 1, coating the tail end fiber core of the optical fiber, drying the optical fiber in air for 12 h, and then putting the optical fiber into the middle cavity 2. And (3) sample detection, namely pouring the liquid to be detected into an open top slot in the middle cavity 2 by using a Pasteur pipette under the condition that the bottom vent hole is closed, and closing the top of the middle cavity by using a threaded plug. The UV-visible absorption spectrum (in absorbance units) is preserved after stabilization. After the measurement, the middle chamber 2 is opened, the top and bottom screw plugs are unscrewed, and the liquid to be measured is emptied by gravity. The inner wall of the middle chamber was washed with ultrapure water Milli-Q water between the analyses of the two solutions to be tested.
FIG. 3 shows the UV-VIS absorption spectrum measured by the above-described method. The prepared optical sensor has obvious response to the formaldehyde content in the solution, and the absorbance is reduced along with the increase of the formaldehyde content in the solution.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (15)

1. The invention provides a sensor for detecting formaldehyde in milk, which comprises optical fibers 1 and 6, a middle cavity 2, a convex lens 3, a polyoxometallate film 4 and an SMA adapter 5.
2. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the fiber core at the tail end of the optical fiber 1 is exposed.
3. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the bare core end of the optical fiber 1 needs to be washed.
4. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the bare core end of the optical fiber 1 needs to be coated with a polyoxometallate film 4.
5. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the polyoxometalate film 4 is insoluble in water.
6. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the polyoxometalate film 4 is capable of reacting with formaldehyde in solution.
7. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the middle cavity 2 is made of a high polymer material with stable chemical properties.
8. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the top of the middle cavity 2 is provided with an open slot, and the bottom is provided with an exhaust hole.
9. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the open slot at the top of the middle cavity 2 and the vent hole at the bottom need to be closed by screw thread plugs in the detection process.
10. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the liquid to be detected is injected from an open slot of the middle cavity 2.
11. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: and the liquid to be detected is discharged from the exhaust hole of the middle cavity 2 after being detected.
12. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the middle chamber 2 needs to be washed with a special detergent before and after the detection.
13. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the convex lens 3 focuses the light transmitted through the polyoxometalate film 4 on the optical fiber 6.
14. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: and the SMA connecting port 5 is connected with a light source.
15. The sensor for detecting the formaldehyde content in the milk according to claim 1, is characterized in that: the optical fiber 6 is connected with a spectrophotometer.
CN202010489306.3A 2020-06-02 2020-06-02 Optical sensor for detecting formaldehyde content in milk Pending CN111665205A (en)

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CN202010489306.3A CN111665205A (en) 2020-06-02 2020-06-02 Optical sensor for detecting formaldehyde content in milk

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111665278A (en) * 2020-06-02 2020-09-15 李锦安 Hydrogen sulfide gas sensor for medical inspection waste pre-alarming

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105665021A (en) * 2016-01-11 2016-06-15 吉林省东成环保集团有限公司 Formaldehyde degradation catalyst

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105665021A (en) * 2016-01-11 2016-06-15 吉林省东成环保集团有限公司 Formaldehyde degradation catalyst

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
MARTA I.S. VERÍSSIMO ET AL.: "A new formaldehyde optical sensor: Detecting milk adulteration", 《FOOD CHEMISTRY》 *
丁元生 等: "Keggin型配合物H5PMo(10)V2O(40)催化剂催化氧化反应研究", 《吉林化工学院学报》 *
谢乐芳 等: "6种多金属氧酸盐的抑菌作用", 《应用化学》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111665278A (en) * 2020-06-02 2020-09-15 李锦安 Hydrogen sulfide gas sensor for medical inspection waste pre-alarming

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