CN112525874B - Method for measuring peroxide value of grease - Google Patents
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- CN112525874B CN112525874B CN202011319147.9A CN202011319147A CN112525874B CN 112525874 B CN112525874 B CN 112525874B CN 202011319147 A CN202011319147 A CN 202011319147A CN 112525874 B CN112525874 B CN 112525874B
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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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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Abstract
The invention provides a method for measuring the peroxide value of grease, which comprises the following steps: adding the standard oil sample into an organic solvent, standing to completely dissolve the standard oil sample to form a standard oil sample solution; adding a saturated potassium iodide solution into a standard oil sample solution for reaction to form a mixed solution; adding an MOF-Pb phosphorescent material into the mixed solution for reaction; and detecting the phosphorescence intensity of the reacted solution by using a fluorescence spectrometer to calculate the peroxide value of the standard oil sample. The method for measuring the peroxide value of the grease utilizes a phosphorescence method to detect the peroxide value of the grease, and has the characteristics of high sensitivity, quick and simple detection, low cost, environmental protection, good repeatability and the like.
Description
Technical Field
The invention belongs to the technical field of chemical component detection, and particularly relates to a method for measuring a peroxide value of grease.
Background
The peroxide value can reflect the oxidation degree of the grease, and is an important index for identifying the quality of the grease. In the processing and storage processes of the grease, the grease is easily influenced by a series of factors such as temperature, oxygen, moisture, microorganisms and the like, and rancidity and oxidation occur. Some peroxides are generated in the oxidation process, and after the peroxides are decomposed, aldehydes, ketones, alcohols and other substances harmful to human bodies are generated. After the edible oil with high over-oxidation value is eaten for a long time, the harm to the health of human bodies can be caused, so that the over-oxidation value of the oil is very necessary to be detected. The national standard GB/T5009.227-2016 adopts a titration method to detect the peroxide value of the grease, the method is complex to operate and low in sensitivity, and a large amount of organic reagents are used, so that the detection cost is high, and the environment is easily polluted. Therefore, there is a need to develop a detection method that is simple to operate, high in sensitivity, low in cost, and environmentally friendly.
The Room Temperature Phosphorescence (RTP) sensor has the characteristics of simple operation, high sensitivity, high selectivity and the like, and has wide application prospects in the fields of chemical sensing, optical devices, information encryption, biological imaging and the like. Compared with fluorescence sensing, phosphorescence has longer service life and stronger interference resistance to stray light and background light. At present, no report for detecting the peroxide value of the grease by using a room temperature phosphorescence method is available.
Metal-organic frameworks (MOFs) are a novel multifunctional coordination polymer and have wide applications in the fields of catalysis, chemical sensing, biological imaging and the like. Recent research by a subject group shows that lead ions can remarkably enhance the room-temperature phosphorescence of Zn-TPA MOF, thereby realizing the phosphorescent colorimetric sensing of the lead ions in marine products. Nevertheless, the current MOFs materials related to room temperature phosphorescence have fewer properties, which limits the application of room temperature phosphorescence in the field of food safety detection.
Vahan et al, which measures peroxide value of olive oil by chemiluminescence method based on the reaction of bis (2,4,6- (trichlorophenyl) oxalate (TCPO) with peroxide in olive oil, Mn (II) as catalyst, and 9, 10-dimethylanthracene as catalyst fluorophore, evaluate the relationship between chemiluminescence intensity and peroxide value of olive oil, Elena et al, which measures peroxide value of olive oil by fluorescence method based on oxide in original olive oil having specific fluorescence band within the range of 400-, and carrying out colorimetric detection on the peroxide value of the grease. However, these methods have many disadvantages, such as high cost, long detection time, low sensitivity, and environmental friendliness. In order to overcome the limitation of the method for detecting peroxide value, a detection method which is environment-friendly, simple, convenient and quick, simple to operate, high in sensitivity and low in cost is urgently needed.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a method for measuring the peroxide value of the grease, the peroxide value of the grease is detected by using an MOF phosphorescent material, and the method has the characteristics of high sensitivity, quickness, simplicity and convenience in detection, low cost, good repeatability and the like.
The invention provides a method for measuring the peroxide value of grease, which comprises the following steps:
step S1: adding the standard oil sample into an organic solvent, standing to completely dissolve the standard oil sample to form a standard oil sample solution;
step S2: adding a saturated potassium iodide solution into a standard oil sample solution for reaction to form a mixed solution;
step S3: adding an MOF-Pb phosphorescent material into the mixed solution for reaction; and
step S4: the phosphorescence intensity of the reacted solution obtained in step S3 was measured by a fluorescence spectrometer to calculate the peroxide value of the standard oil sample.
In a preferred embodiment, the standard oil sample comprises n-propanol and an oil sample, and the volume ratio of the n-propanol to the oil sample is 3-10: 0-7.
In a preferred embodiment, the mass ratio of the standard oil sample to the organic solvent is in the range of 0.25-4: 16-59.
In a preferred embodiment, the standard oil sample in step S1 is allowed to stand in an organic solvent for 2 minutes. The standard oil sample must be completely dissolved in the organic solvent, and incomplete dissolution can cause incomplete reaction and cause experimental errors.
In a preferred embodiment, the organic solvent comprises one or more of ethanol, dichloromethane, chloroform, N-propanol, and DMF (N, N-dimethylformamide). Preferably, the MOF-Pb has good dispersibility in organic solvents such as ethanol, dichloromethane, trichloromethane, n-propanol and DMF, so that MOF-Pb detection is facilitated, and the phosphorescence intensity is better.
In a preferred embodiment, the mass ratio of the saturated potassium iodide solution to the standard oil sample is 17-68: 25-40.
In a preferred embodiment, the reaction time of the saturated potassium iodide solution and the standard oil-like solution in step S2 is 1 minute. If the reaction time is not enough, KI does not completely react with peroxide in the oil sample, the concentration of KI is larger, the measured peroxide value is smaller, and the experimental result is influenced.
In a preferred embodiment, the mass ratio of the MOF-Pb phosphorescent material to the standard oil sample is in a range of 2.5-40: 0-0.2.
In a preferred embodiment, the reaction time of the mixed solution and the MOF-Pb phosphorescent material in the step S3 is 1-5 minutes.
According to the method for determining the peroxide value of the grease, the MOF-Pb phosphorescent material is used as a detection material, and the peroxide value of the grease is detected by adopting a room temperature phosphorescence method.
Drawings
The accompanying drawings are included to provide a further understanding of the embodiments and are incorporated in and constitute a part of this specification. The drawings illustrate embodiments and together with the description serve to explain the principles of the invention. Other embodiments and many of the intended advantages of embodiments will be readily appreciated as they become better understood by reference to the following detailed description. The elements of the drawings are not necessarily to scale relative to each other. Like reference numerals designate corresponding similar parts.
FIG. 1 is a schematic flow chart of a method for determining the peroxide value of grease according to an embodiment of the present invention;
FIG. 2 is an excitation spectrum and an emission spectrum of MOF-Pb of an embodiment of the invention;
FIG. 3 is a graph of the phosphorescence lifetime of MOF-Pb according to an embodiment of the present invention;
FIG. 4 is a schematic representation of MOF-Pb under fluorescent light of an embodiment of the invention;
FIG. 5 is a PXRD pattern of MOF-Pb according to embodiments of the present invention;
FIG. 6 is an SEM image of MOF-Pb of an embodiment of the invention;
FIG. 7 is a schematic illustration of the effect of different organic solvents on the MOF-Pb phosphorescence intensity of an embodiment of the present invention;
FIG. 8 is a graphical representation of the effect of different reaction times of MOF-Pb and standard oil samples on the MOF-Pb phosphorescence intensity for an embodiment of the present invention;
FIG. 9 is a schematic illustration of the effect of different amounts of added MOF-Pb on the phosphorescence intensity of MOF-Pb according to embodiments of the present invention;
FIG. 10 is a schematic illustration of the reproducibility of MOF-Pb of an embodiment of the invention;
FIG. 11 is a PL profile of different peroxide number standard oil samples for an example of the present invention;
FIG. 12 is a linear plot of peroxide value versus change in phosphorescence intensity for a standard oil sample in accordance with an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention will be described in further detail with reference to the accompanying drawings, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, 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.
As shown in fig. 1, the embodiment of the present application provides a method for determining a fat peroxide value, which includes the following steps:
step S1: adding the standard oil sample into an organic solvent, standing to completely dissolve the standard oil sample to form a standard oil sample solution;
step S2: adding a saturated potassium iodide solution into a standard oil sample solution for reaction to form a mixed solution;
step S3: adding an MOF-Pb phosphorescent material into the mixed solution for reaction; and
step S4: the phosphorescence intensity of the reacted solution obtained in step S3 was measured by a fluorescence spectrometer to calculate the peroxide value of the standard oil sample.
Preparation of MOF-Pb phosphorescent material:
the first step is as follows: 1.1g of lead nitrate, 0.3g of terephthalic acid and 40mL of DMF (N-dimethylformamide) are mixed in a 250mL beaker and stirred until dissolved to form a mixed solution;
the second step: adding 2.3mL of triethylamine into the mixed solution, and stirring for 3 hours at room temperature to obtain milky turbid liquid;
the third step: and centrifuging the milky turbid liquid to obtain a precipitate, washing the precipitate by using DMF (dimethyl formamide), soaking the washed precipitate in a dichloromethane solution, and finally performing vacuum drying to obtain the MOF-Pb phosphorescent material.
The MOF-Pb phosphorescent material is prepared through the steps, and the performance of the MOF-Pb phosphorescent material is characterized. FIG. 2 shows the excitation spectrum and emission spectrum of MOF-Pb, and it can be seen from FIG. 2 that MOF-Pb is excited at 305nm and emitted at 490 nm.
FIG. 3 is a graph showing the phosphorescence lifetime of MOF-Pb, which is 3.70ms as shown in FIG. 3, and the luminescence lifetime indicates that the material is phosphorescent.
FIG. 4 is a schematic diagram of MOF-Pb under fluorescent light, as shown in FIG. 4, the MOF-Pb under fluorescent light shows white turbidity and no luminescence, but the MOF-Pb under ultraviolet lamp can emit strong green phosphorescence.
Fig. 5 is a PXRD pattern of MOF-Pb, as shown in fig. 5, which illustrates from the PXRD pattern of MOF-Pb that MOF-Pb is a crystalline material, which cannot be specifically resolved for crystal structure because the synthesized MOF-Pb cannot generate single crystals required by X-ray single crystal diffraction tests, and cannot be modeled for its standard PXRD pattern.
FIG. 6 is an SEM image of MOF-Pb, and as shown in FIG. 6, it can be seen that the MOF-Pb nanoparticles are in a rod-like structure with uniformly and closely spaced particles.
Preparation of saturated potassium iodide solution:
weighing 2g of potassium iodide, adding 1mL of newly boiled and cooled distilled water, shaking uniformly, storing in a brown bottle, and storing in a dark place for later use to ensure that saturated potassium iodide crystals exist in the solution.
Preparation of standard oil samples:
mixing n-propanol and the fried oil sample with high oxidation number at a ratio of 10:0, 9:1, 8:2, 7:3, 6:4, 5:5, 4:6 and 3:7 to form a standard oil sample.
The first embodiment is as follows:
in one embodiment, a method for determining a peroxide value of grease is provided, which includes the following steps:
step S1: taking 0.05g of a standard oil sample (the proportion of the n-propanol to the oil sample is 9:1), respectively adding the standard oil sample into 4mL of ethanol, dichloromethane, trichloromethane, n-propanol and DMF, oscillating on an oscillator for 30s, and standing for 2min to completely dissolve the grease to form different standard oil sample solutions;
step S2: respectively adding 10 mu L of saturated potassium iodide solution into each standard oil sample solution, and fully reacting for 1min to form a mixed solution;
step S3: respectively adding 10mg of MOF-Pb phosphorescent materials into the mixed solution to react for 1 min; and
step S4: the phosphorescence intensity of the reacted solution obtained in step S3 was measured by a fluorescence spectrometer to calculate the peroxide value of the standard oil sample.
The effect of the experiment on the MOF-Pb phosphorescence intensity by adding different organic solvents through the above steps resulted in the results shown in FIG. 7, from which it can be seen that the MOF-Pb phosphorescence intensity is the highest in ethanol.
Example two:
in the second embodiment, a method for determining the peroxide value of grease is provided, which comprises the following steps:
step S1: respectively adding 0.025 g, 0.05g, 0.1g, 0.2g and 0.4g of standard oil samples (the proportion of n-propanol to the oil samples is 9:1) into 4mL of ethanol, oscillating on an oscillator for 30s, and standing for 2min to completely dissolve the grease to form different standard oil sample solutions;
step S2: respectively adding 10 mu L of saturated potassium iodide solution into each standard oil sample solution, and fully reacting for 1min to form a mixed solution;
step S3: respectively adding 10mg of MOF-Pb phosphorescent materials into the mixed solution to react for 1 min; and
step S4: the phosphorescence intensity of the reacted solution obtained in step S3 was measured by a fluorescence spectrometer to calculate the peroxide value of the standard oil sample.
In order to explore the influence of different standard oil samples on the detection peroxide value of the MOF-Pb, a single variable principle is adopted, the adding amount of the MOF-Pb, the reaction time, the amount of saturated KI and the like are not changed, after different quality standard oil samples are added, the phosphorescence intensity of the oil samples is measured on a fluorescence spectrometer, and when the phosphorescence intensity is measured to be 0.05g, the phosphorescence intensity is highest, so that the optimal result is 0.05 g.
Example three:
in the third embodiment, a method for measuring the peroxide value of the grease is provided, which comprises the following steps:
step S1: adding 0.05g of standard oil sample (the proportion of n-propanol to the oil sample is 9:1) into 4mL of ethanol, oscillating on an oscillator for 30s, and standing for 2min to completely dissolve the grease to form a standard oil sample solution;
step S2: respectively adding 10 mu L of saturated potassium iodide solution into the standard oil sample solution, and fully reacting for 1min to form a mixed solution;
step S3: respectively adding 10mg of MOF-Pb phosphorescent materials into the mixed solution, and reacting for 0.25 min, 0.5min, 1min and 5 min; and
step S4: the phosphorescence intensity of the reacted solution obtained in step S3 was measured by a fluorescence spectrometer to calculate the peroxide value of the standard oil sample.
As shown in FIG. 8, it is understood from the graph that the phosphorescence intensity is substantially maintained after 1min of the reaction, and thus the optimum reaction time is 1min, because the effect of the different reaction times of the MOF-Pb and the standard oil samples on the MOF-Pb phosphorescence intensity is shown.
Example four:
in the fourth embodiment, a method for measuring the peroxide value of the grease is provided, which comprises the following steps:
step S1: adding 0.05g of standard oil sample (the proportion of n-propanol to the oil sample is 9:1) into 4mL of ethanol, oscillating on an oscillator for 30s, and standing for 2min to completely dissolve the grease to form a standard oil sample solution;
step S2: respectively adding 10 mu L of saturated potassium iodide solution into the standard oil sample solution, and fully reacting for 1min to form a mixed solution;
step S3: respectively adding 0mg, 5mg, 10mg, 15mg and 20mg of MOF-Pb phosphorescent materials into the mixed solution to react for 1 min; and
step S4: the phosphorescence intensity of the reacted solution obtained in step S3 was measured by a fluorescence spectrometer to calculate the peroxide value of the standard oil sample.
As shown in FIG. 9, the results of FIG. 9 were obtained by the influence of different amounts of MOF-Pb added in the above steps on the phosphorescent intensity of MOF-Pb, and it is understood that the amount of 10mg added was optimum from the economical point of view because the phosphorescent intensity of MOF-Pb was not substantially changed after 10mg was added.
FIG. 10 shows the repeatability of MOF-Pb, which is shown in FIG. 10, the change of phosphorescence intensity after five repeated applications of MOF-Pb on standard oil sample is detected, and the phosphorescence intensity is slightly reduced after five repeated applications. Before MOF-Pb detection, strong green phosphorescence is emitted, after detection, the green phosphorescence is quenched, after washing, the green phosphorescence is recycled, the strong green phosphorescence is recovered before detection, and after detection, the green phosphorescence is quenched again.
FIG. 11 is a PL diagram of oil samples with different peroxide values, and as shown in FIG. 11, the phosphorescence intensity of MOF-Pb in oil samples with different peroxide values changes, and the phosphorescence intensity increases with the increase of peroxide values.
FIG. 12 is a linear graph of peroxide value and phosphorescence intensity variation, as shown in FIG. 12, a linear relationship between the peroxide value of oil and fat and the MOF-Pb phosphorescence intensity is detected by MOF-Pb room temperature phosphorescence. As can be seen, the peroxide value is in good linear relation between 0 and 25mmol/kg, the linear equation is that y is 24.794x +10.212, and the lowest detection limit is 30 μm/kg.
TABLE 1 national Standard method for determining peroxide values of standard oil samples with different volume ratios
TABLE 2 results of the phosphorescence method at room temperature and the national standard method for the detection of different oil samples
Table 2 shows the results of the room temperature phosphorescence method and the national standard method for the detection of different oil samples, the samples in table 2 are 6 edible oils purchased from supermarkets around schools, the peroxide values of the 6 edible oils are respectively detected by the method and the national standard method, the detection results of the two methods are basically consistent, and the method can be well applied to the detection of actual samples, and has a great prospect in the rapid and simple detection of peroxide values of actual samples.
According to the method for determining the peroxide value of the grease, the MOF-Pb phosphorescent material is used as a detection material, and the peroxide value of the grease is detected by adopting a room temperature phosphorescence method.
While the principles of the invention have been described in detail in connection with the preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing embodiments are merely illustrative of exemplary implementations of the invention and are not limiting of the scope of the invention. The details of the embodiments are not to be interpreted as limiting the scope of the invention, and any obvious changes, such as equivalent alterations, simple substitutions and the like, based on the technical solution of the invention, can be interpreted without departing from the spirit and scope of the invention.
Claims (9)
1. A method for measuring the peroxide value of grease is characterized by comprising the following steps:
step S1: adding an organic solvent into a standard oil sample, and standing to completely dissolve the standard oil sample to form a standard oil sample solution;
step S2: adding a saturated potassium iodide solution into the standard oil sample solution for reaction to form a mixed solution;
step S3: adding a MOF-Pb phosphorescent material into the mixed solution for reaction; and
step S4: and detecting the phosphorescence intensity of the reacted solution obtained in the step S3 by using a fluorescence spectrometer to calculate the peroxide value of the standard oil sample.
2. The method for measuring the peroxide value of the grease, according to claim 1, wherein the standard oil sample comprises n-propanol and an oil sample, and the volume ratio of the n-propanol to the oil sample is 3-10: 0-7.
3. The method for measuring the peroxide value of the oil or fat according to claim 1, wherein the mass ratio of the standard oil sample to the organic solvent is in the range of 0.25-4: 16-59.
4. The method for measuring the peroxide value of oils and fats according to claim 3, wherein the standard oil sample in step S1 is allowed to stand in the organic solvent for 2 minutes.
5. The method for measuring the peroxide value of the grease according to claim 4, wherein the organic solvent comprises one or more of ethanol, dichloromethane, trichloromethane, n-propanol and DMF.
6. The method for measuring the peroxide value of the oil or fat according to claim 1, wherein the mass ratio of the saturated potassium iodide solution to the standard oil sample is in the range of 17-68: 25-40.
7. The method for measuring a peroxide value of an oil or fat according to claim 6, wherein the reaction time of the saturated potassium iodide solution and the standard oil-like solution in step S2 is 1 minute.
8. The method for determining the peroxide value of the grease, according to claim 1, wherein the mass ratio of the MOF-Pb phosphorescent material to the standard oil sample is 2.5-40: 0-0.2.
9. The method for determining the peroxide value of the grease according to claim 1, wherein the reaction time of the mixed solution and the MOF-Pb phosphorescent material in the step S3 is 1-5 minutes.
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