CN106770193B - Device and method for detecting content of phosphorus-sulfur in edible vegetable oil - Google Patents
Device and method for detecting content of phosphorus-sulfur in edible vegetable oil Download PDFInfo
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- CN106770193B CN106770193B CN201710024554.9A CN201710024554A CN106770193B CN 106770193 B CN106770193 B CN 106770193B CN 201710024554 A CN201710024554 A CN 201710024554A CN 106770193 B CN106770193 B CN 106770193B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
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Abstract
The invention discloses a device and a method for detecting the content of phosphorus-sesquialter in edible vegetable oil, wherein phosphorus-sesquialter is gasified by adopting a water bath method according to the boiling point difference of the phosphorus-sesquialter and the edible vegetable oil, and the phosphorus-sesquialter is absorbed and gasified by utilizing activated carbon to realize enrichment of the content of the phosphorus-sesquialter. The double-pulse LIBS technology is utilized to excite a sample plasma signal, an integrating sphere is adopted to collect a spectrum signal, and laser energy fluctuation is corrected. And finally, correlating the 9 characteristic analysis spectral lines corrected by the internal standard method with the actual phosphorus-sulfur content of the sample by using multiple linear regression, and establishing a regression equation. The regression equation can be used for rapidly detecting the content of the phosphorus and the sulfur in the edible vegetable oil sample to be detected. The invention discloses a device and a method for detecting the content of phosphorus and sulfur in edible vegetable oil, which have the advantages of high speed, good stability and high detection precision, and can realize the rapid detection of the content of phosphorus and sulfur in the edible vegetable oil.
Description
Technical Field
The invention belongs to the technical field of food safety detection, and particularly relates to a device and a method for detecting the content of phosphorus and sulfur in edible vegetable oil.
Background
The phoxim, also called as Baizhiyu, is an organophosphorus insecticide with low toxicity to human and animal, and is mainly used for preventing and controlling pests of crops of soybean, rice and vegetable, etc.. Edible vegetable oil is a necessity for life of people, and the quality safety of the edible vegetable oil is of great concern. Because of the reasons of spraying the phosphorus-sesquioxide pesticide and the like on the edible vegetable oil raw materials, the edible vegetable oil contains phosphorus-sesquioxide pesticide residues. The national standard GB2763-2014 prescribes that the maximum residual limit of the edible vegetable oil is 0.01mg/kg.
At present, the detection method of the content of the phosphorus sesquioxide in the edible vegetable oil mainly comprises a high performance liquid chromatography method, a gas chromatography-mass spectrometry method, a gas chromatography method, an enzyme-linked immunosorbent assay method and the like. The method has the defects of complicated operation process, long time consumption, high cost, non-environmental protection and the like, and can not realize on-site rapid detection.
The Laser Induced Breakdown Spectroscopy (LIBS) technology is an emerging nondestructive spectrum analysis technology and has the advantages of rapidness, non-contact, simultaneous measurement of multiple components and the like. The basic principle of LIBS is to focus a beam of high-energy short pulse laser on a sample to be tested to generate plasma, and quantitatively detect the content of substances according to the light-emitting spectrum of the plasma. However, the LIBS technology is directly used for detecting the edible vegetable oil stock solution, and the detection accuracy is greatly reduced due to the influence of factors such as liquid splashing and disturbance.
Disclosure of Invention
The invention aims to solve the technical problems of long time consumption, high cost and low precision in the detection of the content of the phosphorus-sesquialter in the existing edible vegetable oil, and provides a device and a method for rapidly detecting the content of the phosphorus-sesquialter in the edible vegetable oil based on a double-pulse LIBS and a rapid enrichment method, which overcome the defects of the existing detection method, improve the detection precision of the phosphorus-sesquialter and enable the detection precision to meet the detection requirements of national standards.
In order to solve the technical problems of the invention, the invention is realized by the following technical scheme: a device and a method for detecting the content of phosphorus-sulfur in edible vegetable oil comprise a computer 1, a high-precision spectrometer 2, a double pulse width solid laser 3, a digital delay generator 4, an energy meter 5, a fan 6, a water bath 7, a glass bottle 8 and a water bath box
A glass tube 9, said glass bottle 8 is placed in the water bath 7 and is connected with +.>
One end of the glass tube 9 is connected, and a valve 10 is arranged at the connection part of the glass tube; said->
The other end of the glass tube 9 is connected with the fan 6; said->
An activated carbon 11 is placed in the middle part of the horizontal section of the glass tube 9, said +.>
An integrating sphere 12, a convex lens 13 and a beam splitter 14 are sequentially arranged above the horizontal section of the glass tube 9 from bottom to top; the saidThe optical fiber 15 is placed on the left side of the integrating sphere 7, the optical fiber 15 is connected with the high-precision spectrometer 2, the high-precision spectrometer 2 is respectively connected with the computer 1 and the digital delay generator 4, the digital delay generator 4 is connected with the double-pulse-width solid laser 3, and the energy meter 5 is connected with the computer 1.
Preferably, the double pulse width solid state laser 3 is arranged on the left side of the beam splitter 14, and the energy meter 5 is arranged on the right side of the beam splitter 14.
A method for detecting the content of phosphorus and sulfur in edible vegetable oil is characterized by comprising the following steps: the method comprises the following steps:
s1: samples of edible oil N1, N2, N3 … … Nn containing different levels of phosphorus and sulfur were collected.
S2: sample N1 is placed in a glass bottle 8, a valve 10 is closed, then the glass bottle 8 is placed in a water bath box 7 at 95 ℃, and according to the boiling point difference of the phosphorus sesquioxide and the edible vegetable oil, the phosphorus sesquioxide in sample N1 is vaporized, and the edible vegetable oil is not vaporized.
S3: the double pulse width solid laser 3 is turned on to generate two laser beams, the laser beams I16 reflected by the beam splitter 14 sequentially pass through the beam splitter 14, pass through the convex lens 13 and then pass through the integrating sphere 12 to be focused on the surface of the active carbon 11, generate plasma signals, enter the optical fiber 15 through the integrating sphere 12, collect spectrum signals entering from the optical fiber 15, obtain LIBS spectrum of the active carbon, and record as R1; the laser beam II 17 not reflected by the beam splitter 14 enters the energy meter 5, the energy value is detected, and the deviation between the detected laser energy value and the set value is calculated and is marked as P R The method comprises the steps of carrying out a first treatment on the surface of the If the deviation P R If the absolute value of (2) is larger than 5%, the energy meter 5 gives an alarm and re-collects LIBS spectrum; if the deviation P R The absolute value of (2) is less than or equal to 5%, the deviation P is then R To the computer 1 by a factor of (1-P R ) 3/2 The spectrum was multiplied by the spectrum R1 to perform spectral correction, and the LIBS spectrum of the corrected activated carbon was designated as R1'.
S4: closing the double pulse width solid laser 3, opening the valve 10, and using the fan 6 to gasify the phosphorus-sulfur gas in
Circulating for 5 minutes in the glass tube 9, and adsorbing the phosphorus-sulfur gas on the surface of the activated carbon 11 to realize enrichment of the phosphorus-sulfur concentration.
S5: closing the fan 6, closing the valve 10, opening the double pulse width solid laser 3, and collecting LIBS spectrum of the activated carbon 11 adsorbed with the phosphorus-sulfur gas according to the step S3 to obtain LIBS spectrum of a sample N1, which is recorded as S1; the LIBS spectrum of the corrected sample N1 is recorded as S1' according to the laser energy value measured by the energy meter 5 and processed according to the principle in the step S3.
S6: the spectra S1'-R1' were taken as the final LIBS spectra for sample N1, designated V1.
S7: and (3) processing the samples N2-Nn according to the steps S2-S6 in sequence to finally obtain spectra of the samples N2-Nn, and marking the spectra as V2-Vn.
S8: for sample spectra V1-Vn, spectral data for wavelengths 247.86nm, 253.40nm, 255.33nm, 384.89nm, 386.04nm, 388.16nm, 426.72nm, 545.38nm, 656.29nm, 771.19nm, 833.52nm, 921.29nm, and 940.57nm were extracted; the analysis spectral line data of 253.40nm and 255.33nm are corrected by taking 247.86nm spectral line as an internal standard (namely, the spectrum data of 253.40nm and 255.33nm are divided by the spectrum data of 247.86 nm), and the corrected analysis spectral line data of 253.40nm and 255.33nm are respectively marked as lambda 253.40/247.86 And lambda (lambda) 255.33/247.86 The method comprises the steps of carrying out a first treatment on the surface of the The 426.72nm spectral line is taken as an internal standard to correct the 384.89nm, 386.04nm, 388.16nm and 545.38nm analysis spectral line data, and the corrected 384.89nm, 386.04nm, 388.16nm and 545.38nm analysis spectral line data are respectively marked as lambda 384.89/426.72 ，λ 386.04/426.72 ，λ 388.16/426.72 Lambda (lambda) 545.38/426.72 The method comprises the steps of carrying out a first treatment on the surface of the The 833.52nm spectral line is taken as an internal standard to correct 656.29nm and 771.19nm analysis spectral line data, and the corrected 656.29nm and 771.19nm analysis spectral line data are respectively marked as lambda 656.29/833.52 Lambda (lambda) 771.19/833.52 The method comprises the steps of carrying out a first treatment on the surface of the Correcting 921.29nm analysis spectral line data by taking 940.57nm spectral line as an internal standard, and marking the corrected 921.29nm analysis spectral line data as lambda 921.29/940.57 。
S9: the actual phosphorus-sulfur-doubling content in the samples N1-Nn is determined by adopting a national standard method GB/T5009.145-2003.
S10: correlating the analysis spectral line data of the N samples subjected to internal standard correction with the actual phosphorus-sulfur content by utilizing a multiple linear regression method, and establishing a regression equation of the phosphorus-sulfur content in the edible vegetable oil;
wherein a1-a9 are coefficients of a regression equation, b is the intercept of the regression equation, and Y is the predicted value of the phosphorus-sulfur-doubling content.
S11: and (3) processing the edible vegetable oil sample to be detected according to the steps S2-S6 to obtain a corrected spectrum of the unknown edible vegetable oil sample, processing the spectrum according to the step S8 to obtain corrected analysis spectral line data, substituting the corrected analysis spectral line data into a regression equation in the step S10, and rapidly obtaining the content of the phosphorus sesquioxide in the edible vegetable oil sample.
Preferably, the time interval between the two lasers in the step S3 is 90ns, which is controlled by the digital delay generator 4.
Preferably, in the step S3, the digital delay generator 4 controls the high-precision spectrometer 2 to start to collect the spectrum signal entering from the optical fiber after the double pulse width solid laser 3 emits the second laser beam 1.28 μs, so as to avoid collecting continuous background noise signals and improve the detection precision.
Compared with the prior art, the invention has the beneficial effects that:
according to the device and the method for detecting the content of the phosphorus-sesquialter in the edible vegetable oil, the phosphorus-sesquialter is vaporized by adopting a water bath method according to the boiling point difference of the phosphorus-sesquialter and the edible vegetable oil, and the phosphorus-sesquialter is adsorbed and vaporized by utilizing the activated carbon, so that the enrichment of the content of the phosphorus-sesquialter is realized. The DP-LIBS technology is utilized to excite a sample plasma signal, an integrating sphere is adopted to collect spectrum signals as much as possible, and laser energy fluctuation is corrected. And finally, correlating the characteristic analysis spectral line corrected by the internal standard method with the actual phosphorus-sulfur content of the sample by using multiple linear regression, and establishing a regression equation. The regression equation can be used for rapidly detecting the content of the phosphorus and the sulfur in the edible vegetable oil sample to be detected. The device and the method for detecting the content of the phosphorus-sulfur in the edible vegetable oil have the advantages of being rapid, good in stability and high in detection precision, and can be used for rapidly detecting the content of the phosphorus-sulfur in the edible vegetable oil.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention.
Reference numerals: 1. a computer; 2. a high-precision spectrometer laser coding machine; 3. a double pulse width solid state laser; 4. a digital delay generator; 5. an energy meter; 6. a blower; 7. a water bath tank; 8. a glass bottle; 9.
a glass tube; 10. a valve; 11. activated carbon; 12. an integrating sphere; 13. a convex lens; 14. a beam splitter; 15. an optical fiber; 16. a laser beam I; 17. laser beam II.
Detailed description of the preferred embodiments
The invention will be further described with reference to the drawings and examples.
Referring to fig. 1, the device for detecting the content of the phosphorus-sulfur in the edible vegetable oil comprises a computer 1, a high-precision spectrometer 2, a double pulse width solid laser 3, a digital delay generator 4, an energy meter 5, a fan 6, a water bath 7, a glass bottle 8 and
a glass tube 9, said glass bottle 8 is placed in the water bath 7 and is connected with +.>
One end of the glass tube 9 is connected, and a valve 10 is arranged at the connection part of the glass tube; said->
The other end of the glass tube 9 is connected with the fan 6; said->
Active carbon 11 is placed in the middle of the horizontal section of the glass tube 9, said/>
An integrating sphere 12, a convex lens 13 and a beam splitter 14 are sequentially arranged above the horizontal section of the glass tube 9 from bottom to top; the optical fiber 15 is placed on the left side of the integrating sphere 7, the optical fiber 15 is connected with the high-precision spectrometer 2, the high-precision spectrometer 2 is respectively connected with the computer 1 and the digital delay generator 4, the digital delay generator 4 is connected with the double-pulse-width solid laser 3, and the energy meter 5 is connected with the computer 1.
Further, the double pulse width solid state laser 3 is disposed on the left side of the beam splitter 14, and the energy meter 5 is disposed on the right side of the beam splitter 14.
A method for detecting the content of phosphorus and sulfur in edible vegetable oil is characterized by comprising the following steps: the method comprises the following steps:
s1: samples of edible oil N1, N2, N3 … … Nn containing different levels of phosphorus and sulfur were collected.
S2: sample N1 is placed in a glass bottle 8, a valve 10 is closed, then the glass bottle 8 is placed in a water bath box 7 at 95 ℃, and according to the boiling point difference of the phosphorus sesquioxide and the edible vegetable oil, the phosphorus sesquioxide in sample N1 is vaporized, and the edible vegetable oil is not vaporized.
S3: the double pulse width solid laser 3 is turned on to generate two laser beams, the laser beams I16 reflected by the beam splitter 14 sequentially pass through the beam splitter 14, pass through the convex lens 13 and then pass through the integrating sphere 12 to be focused on the surface of the active carbon 11, generate plasma signals, enter the optical fiber 15 through the integrating sphere 12, collect spectrum signals entering from the optical fiber 15, obtain LIBS spectrum of the active carbon, and record as R1; the laser beam II 17 not reflected by the beam splitter 14 enters the energy meter 5, the energy value is detected, and the deviation between the detected laser energy value and the set value is calculated and is marked as P R The method comprises the steps of carrying out a first treatment on the surface of the If the deviation P R If the absolute value of (2) is larger than 5%, the energy meter 5 gives an alarm and re-collects LIBS spectrum; if the deviation P R The absolute value of (2) is less than or equal to 5%, the deviation P is then R To the computer 1 by a factor of (1-P R ) 3/2 The spectrum was multiplied by the spectrum R1 to perform spectral correction, and the LIBS spectrum of the corrected activated carbon was designated as R1'.
S4: closing the double pulse width solid laser 3, opening the valve 10, and using the fan 6 to gasify the phosphorus-sulfur gas in
Circulating for 5 minutes in the glass tube 9, and adsorbing the phosphorus-sulfur gas on the surface of the activated carbon 11 to realize enrichment of the phosphorus-sulfur concentration.
S5: closing the fan 6, closing the valve 10, opening the double pulse width solid laser 3, and collecting LIBS spectrum of the activated carbon 11 adsorbed with the phosphorus-sulfur gas according to the step S3 to obtain LIBS spectrum of a sample N1, which is recorded as S1; the LIBS spectrum of the corrected sample N1 is recorded as S1' according to the laser energy value measured by the energy meter 5 and processed according to the principle in the step S3.
S6: the spectra S1'-R1' were taken as the final LIBS spectra for sample N1, designated V1.
S7: and (3) processing the samples N2-Nn according to the steps S2-S6 in sequence to finally obtain spectra of the samples N2-Nn, and marking the spectra as V2-Vn.
S8: for sample spectra V1-Vn, spectral data for wavelengths 247.86nm, 253.40nm, 255.33nm, 384.89nm, 386.04nm, 388.16nm, 426.72nm, 545.38nm, 656.29nm, 771.19nm, 833.52nm, 921.29nm, and 940.57nm were extracted; the analysis spectral line data of 253.40nm and 255.33nm are corrected by taking 247.86nm spectral line as an internal standard (namely, the spectrum data of 253.40nm and 255.33nm are divided by the spectrum data of 247.86 nm), and the corrected analysis spectral line data of 253.40nm and 255.33nm are respectively marked as lambda 253.40/247.86 And lambda (lambda) 255.33/247.86 The method comprises the steps of carrying out a first treatment on the surface of the The 426.72nm spectral line is taken as an internal standard to correct the 384.89nm, 386.04nm, 388.16nm and 545.38nm analysis spectral line data, and the corrected 384.89nm, 386.04nm, 388.16nm and 545.38nm analysis spectral line data are respectively marked as lambda 384.89/426.72 ，λ 386.04/426.72 ，λ 388.16/426.72 Lambda (lambda) 545.38/426.72 The method comprises the steps of carrying out a first treatment on the surface of the The 833.52nm spectral line is taken as an internal standard to correct 656.29nm and 771.19nm analysis spectral line data, and the corrected 656.29nm and 771.19nm analysis spectral line data are respectively marked as lambda 656.29/833.52 Lambda (lambda) 771.19/833.52 The method comprises the steps of carrying out a first treatment on the surface of the 921.29nm analysis spectral line data by taking 940.57nm spectral line as internal standardLine correction, corrected 921.29nm analysis spectral line data is recorded as lambda 921.29/940.57 。
S9: the actual phosphorus-sulfur-doubling content in the samples N1-Nn is determined by adopting a national standard method GB/T5009.145-2003.
S10: correlating the analysis spectral line data of the N samples subjected to internal standard correction with the actual phosphorus-sulfur content by utilizing a multiple linear regression method, and establishing a regression equation of the phosphorus-sulfur content in the edible vegetable oil;
wherein a1-a9 are coefficients of a regression equation, b is the intercept of the regression equation, and Y is the predicted value of the phosphorus-sulfur-doubling content.
S11: and (3) processing the edible vegetable oil sample to be detected according to the steps S2-S6 to obtain a corrected spectrum of the unknown edible vegetable oil sample, processing the spectrum according to the step S8 to obtain corrected analysis spectral line data, substituting the corrected analysis spectral line data into a regression equation in the step S10, and rapidly obtaining the content of the phosphorus sesquioxide in the edible vegetable oil sample.
Further, the time interval between the two lasers in the step S3 is 90ns, which is controlled by the digital delay generator 4.
Further, in the step S3, the digital delay generator 4 controls the high-precision spectrometer 2 to start to collect the spectrum signal entering from the optical fiber after the double pulse width solid laser 3 emits the second laser beam 1.28 μs, so as to avoid collecting continuous background noise signals and improve the detection precision.
The above list is only one of the embodiments of the present invention. It will be obvious that the invention is not limited to the above embodiments, but that many similar variants are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (5)
1. Edible vegetable oil medium-multipleSulfur phosphorus content detection device, its characterized in that: comprises a computer (1), a high-precision spectrometer (2), a double pulse width solid laser (3), a digital delay generator (4), an energy meter (5), a fan (6), a water bath box (7), a glass bottle (8) and a glass bottle
A glass tube (9), the glass bottle (8) is arranged in the water bath box (7) and is matched with +.>
One end of the glass tube (9) is connected, and a valve (10) is arranged at the joint of the glass tube and the valve; said->
The other end of the glass tube (9) is connected with the fan (6); said->
Activated carbon (11) is placed in the middle part of the horizontal section of the glass tube (9), and the ∈10 is arranged in the middle part of the horizontal section>
An integrating sphere (12), a convex lens (13) and a beam splitter (14) are sequentially arranged above the horizontal section of the glass tube (9) from bottom to top; the optical fiber (15) is placed on the left side of the integrating sphere (12), the optical fiber (15) is connected with the high-precision spectrometer (2), the high-precision spectrometer (2) is respectively connected with the computer (1) and the digital delay generator (4), the digital delay generator (4) is connected with the double-pulse-width solid laser (3), and the energy meter (5) is connected with the computer (1).
2. The device for detecting the content of phosphorus and sulfur in edible vegetable oil according to claim 1, wherein: the double pulse width solid state laser (3) is arranged on the left side of the beam splitter (14), and the energy meter (5) is arranged on the right side of the beam splitter (14).
3. The method for using the device for detecting the content of the phosphorus and the sulfur in the edible vegetable oil according to any one of claims 1 to 2, which is characterized in that: the method comprises the following steps:
s1: collecting edible oil samples N1, N2, N3 … … Nn with different sulfur and phosphorus contents;
s2: placing the sample N1 in a glass bottle (8), closing a valve (10), and then placing the glass bottle (8) in a water bath box (7) at 95 ℃ to enable the phosphorus-sesquioxide in the sample N1 to be gasified according to the boiling point difference of the phosphorus-sesquioxide and the edible vegetable oil, wherein the edible vegetable oil is not gasified;
s3: opening a double pulse width solid laser (3) to generate two laser beams, sequentially passing through a beam splitter (14), passing through a convex lens (13) through a laser beam I (16) reflected by the beam splitter (14), then passing through an integrating sphere (12), focusing on the surface of active carbon (11), generating plasma signals, entering an optical fiber (15) through the integrating sphere (12), collecting spectrum signals entering from the optical fiber (15), and obtaining the LIBS spectrum of the active carbon, which is recorded as R1; the laser beam II (17) which is not reflected by the beam splitter (14) enters the energy meter (5), the energy value is detected, and the deviation between the laser energy detection value and the set value is calculated and is recorded as P R The method comprises the steps of carrying out a first treatment on the surface of the If the deviation P R If the absolute value of (2) is larger than 5%, the energy meter (5) gives an alarm and the LIBS spectrum is collected again; if the deviation P R The absolute value of (2) is less than or equal to 5%, the deviation P is then R Is transmitted to the computer (1) by a factor (1-P R ) 32 Multiplying the spectrum R1 to perform spectrum correction, and marking the LIBS spectrum of the corrected active carbon as R1';
s4: closing the double pulse width solid laser (3), opening the valve (10), and adopting the fan (6) to gasify the phosphorus-sulfur gas in the reactor
Circulating for 5 minutes in a glass tube (9), and adsorbing the phosphorus-sulfur gas on the surface of the activated carbon (11) to realize enrichment of the phosphorus-sulfur concentration;
s5: closing a fan (6), closing a valve (10), opening a double pulse width solid laser (3), and collecting LIBS spectra of activated carbon (11) adsorbed with the phosphorus-sulfur gas according to the step S3 to obtain a LIBS spectrum of a sample N1, which is recorded as S1; processing according to the laser energy value measured by the energy meter (5) and the principle in the step S3, and marking the LIBS spectrum of the corrected sample N1 as S1';
s6: the spectrum S1'-R1' was taken as the final LIBS spectrum for sample N1, denoted as V1;
s7: for the samples N2-Nn, sequentially processing according to the steps S2-S6 to finally obtain spectra of the samples N2-Nn, and marking the spectra as V2-Vn;
s8: for sample spectra V1-Vn, spectral data for wavelengths 247.86nm, 253.40nm, 255.33nm, 384.89nm, 386.04nm, 388.16nm, 426.72nm, 545.38nm, 656.29nm, 771.19nm, 833.52nm, 921.29nm, and 940.57nm were extracted; the 247.86nm spectral line is taken as an internal standard to correct 253.40nm and 255.33nm analysis spectral line data, and the corrected 253.40nm and 255.33nm analysis spectral line data are respectively marked as lambda 253.40/247.86 And lambda (lambda) 255.33/247.86 The method comprises the steps of carrying out a first treatment on the surface of the The 426.72nm spectral line is taken as an internal standard to correct the 384.89nm, 386.04nm, 388.16nm and 545.38nm analysis spectral line data, and the corrected 384.89nm, 386.04nm, 388.16nm and 545.38nm analysis spectral line data are respectively marked as lambda 384.89/426.72 ，λ 386.04/426.72 ，λ 388.16/426.72 Lambda (lambda) 545.38/426.72 The method comprises the steps of carrying out a first treatment on the surface of the The 833.52nm spectral line is taken as an internal standard to correct 656.29nm and 771.19nm analysis spectral line data, and the corrected 656.29nm and 771.19nm analysis spectral line data are respectively marked as lambda 656.29/833.52 Lambda (lambda) 771.19/833.52 The method comprises the steps of carrying out a first treatment on the surface of the Correcting 921.29nm analysis spectral line data by taking 940.57nm spectral line as an internal standard, and marking the corrected 921.29nm analysis spectral line data as lambda 921.29/940.57 ；
S9: determining the actual phosphorus-sulfur-doubling content in the samples N1-Nn by adopting a national standard method GB/T5009.145-2003;
s10: correlating the analysis spectral line data of the N samples subjected to internal standard correction with the actual phosphorus-sulfur content by utilizing a multiple linear regression method, and establishing a regression equation of the phosphorus-sulfur content in the edible vegetable oil;
s11: and (3) processing the edible vegetable oil sample to be detected according to the steps S2-S6 to obtain a corrected spectrum of the unknown edible vegetable oil sample, processing the spectrum according to the step S8 to obtain corrected analysis spectral line data, substituting the corrected analysis spectral line data into a regression equation in the step S10, and rapidly obtaining the content of the phosphorus sesquioxide in the edible vegetable oil sample.
4. A method for detecting the content of phosphorus-sulfur in edible vegetable oil according to claim 3, wherein: the time interval between the two laser beams in the step S3 is 90ns, and the time interval is controlled by a digital delay generator (4).
5. A method for detecting the content of phosphorus-sulfur in edible vegetable oil according to claim 3, wherein: in the step S3, the high-precision spectrometer (2) is controlled by the digital delay generator (4) to start to collect the spectrum signal entering from the optical fiber after the double pulse width solid laser (3) emits the second laser beam for 1.28 mu S.
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| CN206540832U (en) * | 2017-01-11 | 2017-10-03 | 江西农业大学 | Content of fenthion detection means in a kind of edible vegetable oil |
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| CN103926216A (en) * | 2014-04-24 | 2014-07-16 | 江西农业大学 | Method and device for rapidly detecting trans-fatty acids in edible vegetable oil |
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