CN111610214A - Standard substance and standard sample for testing solid fat content and preparation method thereof - Google Patents
Standard substance and standard sample for testing solid fat content and preparation method thereof Download PDFInfo
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- CN111610214A CN111610214A CN201910139230.9A CN201910139230A CN111610214A CN 111610214 A CN111610214 A CN 111610214A CN 201910139230 A CN201910139230 A CN 201910139230A CN 111610214 A CN111610214 A CN 111610214A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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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
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Abstract
A standard substance for testing solid fat content, a standard sample and a preparation method thereof belong to the technical field of testing. A standard sample for testing solid fat content, which is used for testing solid fat content by nuclear magnetic resonance, and comprises: the first standard comprises a first container, a first seal and mineral oil, wherein the mineral oil fills the first container and is sealed by the first seal; the second standard sample comprises a second container, a second sealing object, a first object and mineral oil, wherein the first object is arranged in the second container, and the mineral oil is filled in the second container and sealed by the second sealing object; the third standard sample comprises a third container, a third sealer, a second object and mineral oil, wherein the second object is arranged in the third container, and the mineral oil is filled in the third container and sealed by the third sealer; the first and second bodies are both made of the same or different solid hydrogen-containing polymeric material. The standard sample of the application improves the problem that the existing standard sample can cause inaccurate leakage test data after being used for a long time.
Description
Technical Field
The application relates to the technical field of testing, in particular to a standard substance and a standard sample for testing solid fat content and a preparation method thereof.
Background
The solid fat content of foods such as cocoa butter, margarine, lard and the like is an important quality index, and has great influence on the mouthfeel, flavor and coating property of the grease foods. The method has the advantages that the method has great advantages in testing speed, testing accuracy and testing repeatability compared with the traditional swelling method, but the quantitative analysis method needs to use a standard sample as reference and correct the result to obtain a correction factor during testing, and the correction factor directly participates in the calculation of the solid fat content of the solid fat sample to be tested.
The current part of standard samples may have liquid leakage or gas entering abnormalities after long-term use, which causes test deviation.
Disclosure of Invention
The embodiment of the application provides a standard substance for testing the content of solid fat, a standard sample and a preparation method thereof, and solves the problem that the existing standard sample may have inaccurate leakage test data after being used for a long time.
The application provides a standard for testing solid fat content, which is used for testing the solid fat content by nuclear magnetic resonance and comprises a first standard, a second standard and a third standard;
the first standard comprises a first seal and mineral oil;
the second standard comprises a second sealant, a first object and mineral oil;
the third standard comprises a third seal, a second object and mineral oil;
none of the first, second and third seals reacts with mineral oil and the first and second objects are made of the same or different solid hydrogen-containing polymeric material.
In the technical scheme, the first object and the second object are both made of solid hydrogen-containing polymer materials, and the content of hydrogen in the first object and the content of hydrogen in the second object are calculated and converted into the corresponding solid fat content, so that the solid hydrogen-containing polymer materials are stable in property, difficult to deteriorate and capable of being used for a long time. Meanwhile, the first sealant, the second sealant and the third sealant can respectively and sequentially seal the first standard product, the second standard product and the third standard product, so that the problem that the standard sample is likely to leak after being used for a long time is solved, and the sealing performance of the standard sample is improved.
The second aspect of the application provides a standard for testing solid fat content, which is used for testing solid fat content by nuclear magnetic resonance, and comprises a first standard, a second standard and a third standard;
the first standard comprises a first seal and mineral oil;
the second standard comprises a second sealant, a first object and mineral oil;
the third standard comprises a third seal, a second object and mineral oil;
the first seal, the second seal, the third seal, the first object and the second object each comprise a manufactured article of polymethylmethacrylate and optionally polytetrafluoroethylene.
In the technical scheme, the first object and the second object comprise finished products of polymethyl methacrylate and optional polytetrafluoroethylene, the hydrogen content in the polymethyl methacrylate is stable, the finished products are optionally prepared by matching with the polytetrafluoroethylene, the hydrogen content in the finished products can be effectively controlled, and the corresponding solid fat content is converted by calculating the hydrogen content in the first object and the second object. In addition, polymethyl methacrylate and polytetrafluoroethylene are not easy to deteriorate, can be used for a long time, cannot be influenced by temperature and the like, and have stable properties. Meanwhile, the first sealant, the second sealant and the third sealant can respectively and sequentially seal the first standard product, the second standard product and the third standard product, so that the problem that the standard sample is likely to leak after being used for a long time is solved, and the sealing performance of the standard sample is improved.
In some embodiments of the foregoing second aspect, the article of manufacture comprises, by weight, 90 to 100 parts polymethyl methacrylate and 0 to 10 parts polytetrafluoroethylene.
In the embodiment, the finished product can be completely made of polymethyl methacrylate, polytetrafluoroethylene can also be added to control the hydrogen content in the finished product, the polymethyl methacrylate contains hydrogen elements and can be detected by a nuclear magnetic resonance spectrometer, and the hydrogen content of the finished product is controlled by controlling the content of the polytetrafluoroethylene.
In some embodiments of the foregoing second aspect, the mineral oil comprises a high viscosity silicone oil.
In the embodiment, the high-viscosity silicone oil is not easy to deteriorate, can be used for a long time, is not influenced by temperature and the like, and has stable property. Meanwhile, the viscosity is high, the flow rate is low, and the device can be used for fixing the first object and the second object and preventing the first object and the second object from moving greatly.
In a third aspect of the present application, there is provided a standard sample for testing solid fat content, which is used for testing solid fat content by nuclear magnetic resonance, and comprises:
a first standard comprising a first container, a first seal, and mineral oil filling the first container and sealed by the first seal;
a second standard sample comprising a second container, a second seal, a first object and mineral oil, the first object being disposed within the second container, the mineral oil filling the second container and being sealed by the second seal;
a third standard sample comprising a third container, a third seal, a second object and mineral oil, the second object being disposed in the third container, the mineral oil filling the third container and being sealed by the third seal;
none of the first, second and third seals reacts with mineral oil and the first and second objects are made of the same or different solid hydrogen-containing polymeric material.
In the above technical solution, the first object and the second object are both made of solid hydrogen-containing polymer material, the solid fat content in the second standard sample and the third standard sample can be determined by calculating the hydrogen content in the first object and the second object and converting into the corresponding solid fat content, and the solid fat content can be determined by changing the shape and the volume of the first object and the second object so as to change the solid fat content, and then selecting the appropriate shape and volume.
The solid fat content of the first standard is 0, the solid fat content of the second standard and the third standard are fixed values, and the first standard, the second standard and the third standard can be used as calibration standards.
The first standard sample, the second standard sample and the third standard sample are respectively sealed by a first sealing object, a second sealing object and a third sealing object in sequence, so that the sealing effect is good; the solid hydrogen-containing polymeric material in the interior is not easy to deteriorate, can be used for a long time, is not influenced by temperature and the like, and has stable property; the mineral oil can isolate gas on one hand, and can fix the positions of the first object and the second object on the other hand, so that the solid fat content is more accurate, and the calibration coefficient is more accurate. Meanwhile, the first sealing object, the second sealing object and the third sealing object can respectively and sequentially seal the first standard sample, the second standard sample and the third standard sample, the problem that the standard sample is likely to leak after being used for a long time is solved, and the sealing performance of the standard sample is improved.
In some embodiments of the foregoing third aspect, the standard comprises a seal ring, and the first, second, and third seals are each fitted with a seal ring.
In this embodiment, first sealant, second sealant and third sealant all overlap and are equipped with the sealing washer, can increase first sealant, second sealant and third sealant in proper order respectively with the frictional force of first container, second container and third container, the leakproofness of reinforcing standard sample.
In some embodiments of the foregoing third aspect, the standard includes an adhesive for bonding the first sealant to the inner wall of the first container, the second sealant to the inner wall of the second container, and the third sealant to the inner wall of the third container.
In this embodiment, the first sealant and the inner wall of the first container are bonded by an adhesive, the second sealant and the inner wall of the second container are bonded by an adhesive, and the third sealant and the inner wall of the third container are bonded by an adhesive, so that the sealing performance of the standard sample is further enhanced.
In some embodiments of the foregoing first aspect, the adhesive comprises a photosensitive glue.
In the embodiment, the photosensitive adhesive is fast in bonding, does not introduce gas and has strong controllability.
In a fourth aspect of the present application, there is provided a method for preparing a standard sample for measuring solid fat content:
transferring the mineral oil into a first vessel, a second vessel and a third vessel, respectively;
transferring the first object into a second container and transferring the second object into a third container respectively;
the first container is sealed with a first sealant, the second container is sealed with a second sealant, and the third container is sealed with a third sealant, respectively.
According to the technical scheme, the mineral oil is filled into the container, the solid hydrogen-containing polymer objects are transferred respectively, and finally the first sealing object is used for sealing.
In some embodiments of the foregoing first aspect, after the first container is sealed with the first sealant, the second container is sealed with the second sealant, and the third container is sealed with the third sealant, the first sealant is bonded to the inner wall of the first container, the second sealant is bonded to the inner wall of the second container, and the third sealant is bonded to the inner wall of the third container, respectively, by using an adhesive.
In this embodiment, the first sealant and the inner wall of the first container are bonded by an adhesive, the second sealant and the inner wall of the second container are bonded by an adhesive, and the third sealant and the inner wall of the third container are bonded by an adhesive, so that the sealing performance of the standard sample is further enhanced.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following are specific descriptions of the standard for testing solid fat content, the standard sample and the preparation method thereof in the examples of the present application.
The embodiment of the application provides a standard substance for testing solid fat content, which is used for testing the solid fat content by nuclear magnetic resonance and comprises a first standard substance, a second standard substance and a third standard substance;
the first standard comprises a first seal and mineral oil;
the second standard comprises a second sealant, a first object and mineral oil;
the third standard comprises a third seal, a second object and mineral oil;
none of the first, second and third seals reacts with mineral oil and the first and second objects are made of the same or different solid hydrogen-containing polymeric material.
The first object and the second object are both made of solid hydrogen-containing polymer materials, and the solid hydrogen-containing polymer materials are stable in property, difficult to deteriorate and capable of being used for a long time by calculating the content of hydrogen in the first object and the second object and converting the content into the corresponding solid fat content.
Alternatively, the solid hydrogen-containing polymeric material may be a mixture of polymethylmethacrylate and optionally polytetrafluoroethylene.
Polymethyl methacrylate (PMMA) has the advantages of high transparency, easy machining and the like, and the PMMA has high light transmittance.
Polytetrafluoroethylene (PTFE), which is insoluble in common solvents such as mineral oil.
Optionally, the solid hydrogen-containing polymeric material comprises, by weight, 90 to 100 parts PMMA and 0 to 10 parts PTFE. The content ratio of the solid hydrogen-containing polymeric material PMMA and PTFE is determined according to the size and shape of the actual container and the required solid fat content ratio.
The PMMA contains hydrogen, the PTFE does not contain hydrogen, and the content of the hydrogen is controlled by adjusting the content of the PTFE in the solid hydrogen-containing polymer material.
In addition, the solid hydrogen-containing polymer material may also be Polystyrene (PS), which is a colorless and transparent thermoplastic.
Optionally, the mineral oil comprises a high viscosity silicone oil. The high-viscosity silicone oil is not easy to deteriorate, can be used for a long time, is not influenced by temperature and the like, and has stable property. Meanwhile, the viscosity is high, the flow rate is low, and the device can be used for fixing the first object and the second object and preventing the first object and the second object from moving greatly.
Alternatively, the high viscosity silicone oil comprises polydimethylsiloxane, with a kinematic viscosity up to 350 CS.
The application provides a standard sample of test solid fat content for nuclear magnetic resonance tests solid fat content, it includes:
a first standard comprising a first container, a first seal, and mineral oil filling the first container and sealed by the first seal;
a second standard sample comprising a second container, a second seal, a first object and mineral oil, the first object being disposed within the second container, the mineral oil filling the second container and being sealed by the second seal;
a third standard sample comprising a third container, a third seal, a second object and mineral oil, the second object being disposed in the third container, the mineral oil filling the third container and being sealed by the third seal;
none of the first, second and third seals reacts with mineral oil and the first and second objects are made of the same or different solid hydrogen-containing polymeric material.
In general, the solid fat content in the standard sample for nuclear magnetic resonance measurement of the solid fat content is about 0, 30% and about 70%, so that the solid fat content in the first standard sample is about 0, the hydrogen-to-solid fat content in the second standard sample is about 30%, and the hydrogen-to-solid fat content in the third standard sample is about 70%.
The content of the mineral oil in the first container, the second container and the third container is respectively 70-90%, 25-40% and 10-25% in sequence.
The top end of the first object in the second container and the bottom end of the second closure do not touch.
Optionally, the standard sample comprises an adhesive, and the adhesive can further bond the first sealing material to the inner wall of the first container, bond the second sealing material to the inner wall of the second container, and bond the third sealing material to the inner wall of the third container, so that the sealing performance of the standard sample is improved, and the standard sample is prevented from being leaked or denatured after being stored for a long time.
And after the sealant is bonded with the inner wall of the container by using the adhesive, dripping the adhesive again to the opening of the container.
The adhesive is photosensitive adhesive, the bonding speed of the photosensitive adhesive is high, and the bonding process is easy to control.
The nuclear magnetic tube is used for containing standard products in a container and is sealed.
The inner diameter of a common nuclear magnetic tube is 15mm, the first sealing object, the second sealing object and the third sealing object are all designed in a three-section mode and comprise a cylindrical first section, a cylindrical second section and a cylindrical third section, and the length ratio of the first section to the second section to the third section is (1.9-2.1): 1: (3.7-4.2), the diameter ratio of the first section, the second section and the third section is 1: (0.5-0.75): 1, the diameter of the first section is 15 mm.
The first object is designed in a three-section mode and comprises a first section, a third section and a circular table for connecting the first section and the second section, the length ratio of the first section to the second section to the third section is 1 (0.5-1) to (1.5-2), and the diameter ratio of the first section to the third section is 1: (1.7-1.9), the diameter of the third section is 15mm, and the diameter of the third section is the same as the internal diameter of the nuclear magnetic tube, so that the nuclear magnetic tube can fix the first object, and the first object is prevented from moving and influencing test data.
The second object is designed in a three-section mode and comprises a first section and a third section which are cylindrical and a circular truncated cone connecting the first section and the second section, the length ratio of the first section to the second section to the third section is 1 (0.5-1) to (1.5-2), and the diameter ratio of the first section to the third section is 1: (1.1-1.3), the diameter of the third section is 15mm, and the diameter of the third section is the same as the inner diameter of the nuclear magnetic tube, so that the nuclear magnetic tube can fix the second object, and the second object is prevented from moving to influence test data.
The end of the nuclear magnetic tube, with the larger diameter, of the first object and the end of the second object are arranged at the bottom of the nuclear magnetic tube.
In addition, the first and second bodies have cut surfaces in both the second and third sections thereof to provide a passage for the flow of mineral oil.
Optionally, the first sealant, the second sealant and the third sealant are all sleeved with sealing rings. The sealing washer can increase first sealant, second sealant and third sealant in proper order respectively with the frictional force of first container, second container and third container, the leakproofness of reinforcing standard sample.
It should be noted that the sealing ring is sleeved on the second sections of the first sealing object, the second sealing object and the third sealing object, and the diameters of the first section and the third section are larger than those of the second section, so that the position of the sealing ring can be clamped.
The embodiment of the application also provides a preparation method of the standard sample for testing the solid fat content, which comprises the following steps:
transferring the mineral oil into a first vessel, a second vessel and a third vessel, respectively;
transferring the first object into a second container and transferring the second object into a third container respectively;
the first container is sealed with a first sealant, the second container is sealed with a second sealant, and the third container is sealed with a third sealant, respectively.
Alternatively, after the mineral oil is transferred to the first container, the second container, and the third container, respectively, the first container, the second container, and the third container are placed in a vacuum-pumping apparatus, respectively, to evacuate air bubbles and air in the containers. And after the first object is transferred into the second container and the second object is transferred into the third container, respectively putting the first container, the second container and the third container into vacuumizing equipment for vacuumizing treatment, removing residual mineral oil on the inner wall of the container, and sealing.
The vacuumizing time is 60-180 min each time;
optionally, the vacuumizing time is 80-160 min each time;
optionally, the vacuumizing time is 90-150 min each time.
Optionally, after the first container is sealed by the first sealant, the second container is sealed by the second sealant, and the third container is sealed by the third sealant, the first sealant is bonded to the inner wall of the first container, the second sealant is bonded to the inner wall of the second container, and the third sealant is bonded to the inner wall of the third container by the adhesive, after the sealant is bonded to the inner wall of the container by the adhesive, the adhesive is dripped into the opening of the container again, so that the sealing performance of the standard sample is further enhanced.
And uniformly irradiating the photosensitive adhesive by using an ultraviolet lamp for 5-20 min to solidify the photosensitive adhesive.
The features and properties of the present application are described in further detail below with reference to examples.
Example 1
The embodiment of the application provides a preparation method of a standard sample for testing the solid fat content, which comprises the following steps.
1. According to the weight parts, a solid hydrogen-containing polymer material containing 90 parts of PMMA and 10 parts of PTFE is adopted to prepare a first sealing object, a second sealing object, a third sealing object, a first object and a second object;
2. respectively pouring polydimethylsiloxane into the first nuclear magnetic tube, the second nuclear magnetic tube and the third nuclear magnetic tube, and vacuumizing for 120 min;
3. respectively loading a first object into a first nuclear magnetic tube and a second object into a second nuclear magnetic tube, wherein one ends of the first object and the second object with larger diameters are arranged at the bottom ends of the nuclear magnetic tubes, removing the residual polydimethylsiloxane on the tube walls, and vacuumizing for 120 min;
4. respectively sleeving the rubber rings on second sections of the first sealant, the second sealant and the third sealant, and then sequentially plugging the first sealant, the second sealant and the third sealant into the open ends of the first nuclear magnetic pipe, the second nuclear magnetic pipe and the third nuclear magnetic pipe;
5. respectively dripping photosensitive adhesives between the first sealing object and the inner wall of the first nuclear magnetic tube, and uniformly irradiating by ultraviolet for 8min to solidify;
6. dripping photosensitive adhesive to the container mouth, and uniformly irradiating with ultraviolet light for 15min to solidify.
Example 2
The embodiment of the application provides a preparation method of a standard sample for testing the solid fat content, which comprises the following steps.
1. According to the weight parts, a solid hydrogen-containing polymer material containing 90 parts of PMMA and 10 parts of PTFE is adopted to prepare a first sealing object, a second sealing object, a third sealing object, a first object and a second object;
2. respectively pouring polydimethylsiloxane into the first nuclear magnetic tube, the second nuclear magnetic tube and the third nuclear magnetic tube, and vacuumizing for 180 min;
3. respectively loading a first object into a first nuclear magnetic tube and a second object into a second nuclear magnetic tube, wherein one ends of the first object and the second object with larger diameters are arranged at the bottom ends of the nuclear magnetic tubes, removing the residual polydimethylsiloxane on the tube walls, and vacuumizing for 180 min;
4. respectively sleeving the rubber rings on second sections of the first sealant, the second sealant and the third sealant, and then sequentially plugging the first sealant, the second sealant and the third sealant into the open ends of the first nuclear magnetic pipe, the second nuclear magnetic pipe and the third nuclear magnetic pipe;
5. respectively dripping photosensitive adhesives between the first sealing object and the inner wall of the first nuclear magnetic tube, and uniformly irradiating by ultraviolet light for 10min to solidify the photosensitive adhesives;
6. dripping photosensitive adhesive to the container mouth, and uniformly irradiating with ultraviolet light for 20min to solidify.
Example 3
The embodiment of the application provides a preparation method of a standard sample for testing the solid fat content, which comprises the following steps.
1. According to the weight parts, a solid hydrogen-containing polymer material containing 90 parts of PMMA and 10 parts of PTFE is adopted to prepare a first sealing object, a second sealing object, a third sealing object, a first object and a second object;
2. respectively pouring polydimethylsiloxane into the first nuclear magnetic tube, the second nuclear magnetic tube and the third nuclear magnetic tube, and vacuumizing for 60 min;
3. respectively loading a first object into a first nuclear magnetic tube and a second object into a second nuclear magnetic tube, wherein one ends of the first object and the second object with larger diameters are arranged at the bottom ends of the nuclear magnetic tubes, removing the residual polydimethylsiloxane on the tube walls, and vacuumizing for 60 min;
4. respectively sleeving the rubber rings on second sections of the first sealant, the second sealant and the third sealant, and then sequentially plugging the first sealant, the second sealant and the third sealant into the open ends of the first nuclear magnetic pipe, the second nuclear magnetic pipe and the third nuclear magnetic pipe;
5. respectively dripping photosensitive adhesives between the first sealing object and the inner wall of the first nuclear magnetic tube, and uniformly irradiating by ultraviolet light for 5min to solidify;
6. dripping photosensitive adhesive to the container mouth, and uniformly irradiating with ultraviolet light for 10min to solidify.
Comparative example 1
The comparative example of the present application provides a method for preparing a standard sample for measuring the solid fat content, comprising the following steps.
1. According to the weight parts, a solid hydrogen-containing polymer material containing 90 parts of PMMA and 10 parts of PTFE is adopted to prepare a first object and a second object;
2. respectively pouring polydimethylsiloxane into the first nuclear magnetic tube, the second nuclear magnetic tube and the third nuclear magnetic tube, and vacuumizing for 120 min;
3. respectively loading a first object into a first nuclear magnetic tube and a second object into a second nuclear magnetic tube, wherein one ends of the first object and the second object with larger diameters are arranged at the bottom ends of the nuclear magnetic tubes, removing the residual polydimethylsiloxane on the tube walls, and vacuumizing for 120 min;
4. dripping photosensitive adhesive to the container mouth, and uniformly irradiating with ultraviolet light for 15min to solidify.
Comparative example 2
The comparative example of the present application provides a method for preparing a standard sample for measuring the solid fat content, comprising the following steps.
1. According to the weight parts, a solid hydrogen-containing polymer material containing 90 parts of PMMA and 10 parts of PTFE is adopted to prepare a first sealing object, a second sealing object, a third sealing object, a first object and a second object;
2. respectively pouring mineral oil into the first nuclear magnetic tube, the second nuclear magnetic tube and the third nuclear magnetic tube, and vacuumizing for 120min, wherein the mineral oil contains olefin and alkane;
3. respectively loading a first object into a first nuclear magnetic pipe and a second object into a second nuclear magnetic pipe, wherein one ends of the first object and the second object with larger diameters are arranged at the bottom ends of the nuclear magnetic pipes, removing residual mineral oil on the pipe walls, and vacuumizing for 120 min;
4. respectively sleeving the rubber rings on second sections of the first sealant, the second sealant and the third sealant, and then sequentially plugging the first sealant, the second sealant and the third sealant into the open ends of the first nuclear magnetic pipe, the second nuclear magnetic pipe and the third nuclear magnetic pipe;
5. respectively dripping photosensitive adhesives between the first sealing object and the inner wall of the first nuclear magnetic tube, and uniformly irradiating by ultraviolet for 8min to solidify;
6. dripping photosensitive adhesive to the container mouth, and uniformly irradiating with ultraviolet light for 15min to solidify.
Comparative example 3
The comparative example of the present application provides a method for preparing a standard sample for measuring the solid fat content, comprising the following steps.
1. Preparing a first sealant, a second sealant, a third sealant, a first object and a second object by using a solid hydrogen-containing polymer material containing phenoxy resin;
2. respectively pouring mineral oil into the first nuclear magnetic tube, the second nuclear magnetic tube and the third nuclear magnetic tube, and vacuumizing for 120min, wherein the mineral oil contains olefin and alkane;
3. respectively loading a first object into a first nuclear magnetic pipe and a second object into a second nuclear magnetic pipe, wherein one ends of the first object and the second object with larger diameters are arranged at the bottom ends of the nuclear magnetic pipes, removing residual mineral oil on the pipe walls, and vacuumizing for 120 min;
4. respectively sleeving the rubber rings on second sections of the first sealant, the second sealant and the third sealant, and then sequentially plugging the first sealant, the second sealant and the third sealant into the open ends of the first nuclear magnetic pipe, the second nuclear magnetic pipe and the third nuclear magnetic pipe;
5. respectively dripping photosensitive adhesives between the first sealing object and the inner wall of the first nuclear magnetic tube, and uniformly irradiating by ultraviolet for 8min to solidify;
6. dripping photosensitive adhesive to the container mouth, and uniformly irradiating with ultraviolet light for 15min to solidify.
Stability verification
Firstly, standard samples are prepared according to examples 1 to 3 and comparative examples 1 to 3, stability tests comprise long-term stability and short-term stability, and the research is carried out by referring to a method specified in GB/T15000.3-2008 standard sample value determination general principle and statistical method.
Long-term stability studies were conducted for 12 months, separately prepared standard samples prepared in examples 1-3 and comparative examples 1-3 stored at room temperature were taken every other month, three standard samples were taken for each set of samples, each sample was tested 2 times, 18 sets were used, the average value was used as the test result, the test results are shown in tables 1-4, the long-term stability test in this study was designed as a classical stability study, i.e., samples prepared at the same time were measured over time under the same conditions.
TABLE 1 examples 1-3 Long term stability Studies
As shown in Table 1, intercept b is taken as an empirical mode of a straight line0Equal (within uncertainty) to the measured value. At 95% confidence level, | b1|＜T0.95,n-2.s(b1) Slope b of1Near zero, slope b1Is not significant, i.e., no instability was observed, indicating that the standard samples produced by the preparation method of the present application are stable over time.
TABLE 2 Long term stability study of comparative example 1
As shown in Table 2, | b at 95% confidence level1|＞T0.95,n-2.s(b1) Slope b of1Is significant, i.e., instability is observed, indicating that the standard sample prepared by the preparation method of comparative example 1 is unstable for a long period of time. Comparative example 1 does not seal the container with a sealant, so that the sealing property of the container is not good, and the internal standard substance leaks, affecting the stability of the standard sample.
TABLE 3 Long term stability study of comparative example 2
As shown in Table 3, | b at 95% confidence level1|＞T0.95,n-2.s(b1) Slope b of1Is significant, i.e., instability is observed, indicating that the standard sample prepared by the preparation method of comparative example 2 is unstable for a long period of time. Comparative example 2 using mineral oil containing olefin and alkane, the first and second objects inside the container were displaced, affecting the stability of the standards.
TABLE 4 Long term stability study of comparative example 3
As shown in Table 4, | b at 95% confidence level1|＞T0.95,n-2.s(b1) Slope b of1Is significant, i.e., instability is observed, indicating that the standard sample prepared by the preparation method of comparative example 3 is unstable for a long period of time. Comparative example 3 a first seal, a second seal, a third seal, a first object and a second object were formed using a solid hydrogen-containing polymeric material containing a phenoxy resin, and the first object and the second object inside the container were displaced, affecting the stability of the standards.
In the short-term stability study, the change of a sample in the transportation process before use is simulated, the independently prepared standard samples prepared in the examples 1 to 3 are respectively placed in the indoor environment conditions of 15 ℃, 20 ℃ and 25 ℃ and kept for 7 days, then the change of the solid fat content of the standard sample along with the time is tested, and the detection results are shown in table 5.
TABLE 5 short term stability study
As shown in Table 5, intercept b is taken as an empirical mode of a straight line0Equal (within uncertainty) to the measured value. At 95% confidence level, | b1|＜T0.95,n-2.s(b1) Slope b of1Near zero, slope b1Is not significant, i.e., no instability was observed, indicating that the standard samples produced by the preparation method of the present application are short-term stable.
In summary, the embodiments of the present application provide a standard substance for measuring solid fat content, a standard sample and a preparation method thereof. The first object and the second object reflecting the solid fat content in the standard product are made of a mixed solid hydrogen-containing polymer material of PMMA and PTFE, the PMMA and the PTFE cannot be dissolved in mineral oil and react with the mineral oil, the standard product can be used for a long time, the standard product cannot be influenced by temperature and the like, the property is stable, the hydrogen content in the PMMA is stable, and the standard product can be converted into the corresponding solid fat content. The mineral oil is polydimethylsiloxane which is not easy to deteriorate, can be used for a long time, is not influenced by temperature and the like, and has stable property. Meanwhile, the viscosity is high, the flow rate is low, and the device can be used for fixing a first object and a second object made of PMMA and PTFE and preventing the first object and the second object from moving greatly, so that the stability of the standard sample is influenced. The application standard sample adopts the sealant to seal, and is sealed respond well to have the transparency, prevent that the sample from leaking, influence the stability of sample. The preparation method is simple and convenient in process, and the prepared standard sample is stable and can be repeatedly used for a long time.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. 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 application.
Claims (10)
1. A standard substance for testing solid fat content, which is used for testing solid fat content by nuclear magnetic resonance, and is characterized by comprising a first standard substance, a second standard substance and a third standard substance;
the first standard comprises a first seal and mineral oil;
the second standard comprises a second seal, a first object and mineral oil;
the third standard comprises a third seal, a second object and mineral oil;
none of the first, second and third seals react with the mineral oil, and the first and second objects are made of the same or different solid hydrogen-containing polymeric material.
2. A standard substance for testing solid fat content, which is used for testing solid fat content by nuclear magnetic resonance, and is characterized by comprising a first standard substance, a second standard substance and a third standard substance;
the first standard comprises a first seal and mineral oil;
the second standard comprises a second seal, a first object and mineral oil;
the third standard comprises a third seal, a second object and mineral oil;
none of the first, second and third seals react with the mineral oil, and the first and second objects each comprise a manufactured product of polymethylmethacrylate and optionally polytetrafluoroethylene.
3. The standard for testing solid fat content according to claim 2, wherein the manufactured product comprises 90-100 parts by weight of polymethyl methacrylate and 0-10 parts by weight of polytetrafluoroethylene.
4. The standard for testing solid fat content according to claim 1 or 2, wherein the mineral oil comprises a high viscosity silicone oil.
5. A standard for testing solid fat content for use in nmr testing of solid fat content, the standard comprising:
a first standard comprising a first container, a first seal, and mineral oil filling the first container and sealed by the first seal;
a second standard comprising a second container, a second seal, a first object disposed within the second container, and mineral oil filling the second container and sealed by the second seal;
a third standard comprising a third container, a third seal, a second object disposed within the third container, and mineral oil filling the third container and sealed by the third seal;
none of the first, second and third seals react with the mineral oil, and the first and second objects are made of the same or different solid hydrogen-containing polymeric material.
6. The standard for testing solid fat content of claim 5, wherein the standard comprises a sealing ring, and the first, second and third seals are all sleeved with the sealing ring.
7. The standard for testing solid fat content according to claim 5, comprising an adhesive for bonding the first seal to the inner wall of the first container, the second seal to the inner wall of the second container, and the third seal to the inner wall of the third container.
8. The standard for testing solid fat content according to claim 7, wherein the adhesive comprises a light-sensitive glue.
9. A method of preparing a standard for testing solid fat content according to any one of claims 5 to 8, wherein;
transferring the mineral oil into the first, second and third vessels, respectively;
transferring the first object into the second container and the second object into the third container, respectively;
sealing the first container with the first sealant, sealing the second container with the second sealant, and sealing the third container with the third sealant, respectively.
10. The method for preparing a standard sample for testing solid fat content according to claim 9, wherein after the first container, the second container and the third container are sealed with the first sealant, the second sealant and the third sealant, respectively, the first sealant, the second sealant and the third sealant are bonded to the inner wall of the first container, the inner wall of the second container and the inner wall of the third container, respectively, by using an adhesive.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636510A (en) * | 2011-04-28 | 2012-08-15 | 河南省科学院高新技术研究中心 | Method for detecting quality of edible oil by using hydrogen-nuclear magnetic resonance spectroscopy |
| CN103454224A (en) * | 2013-05-02 | 2013-12-18 | 广东工业大学 | Edible oil quality determination system and method based on light polarization state |
| CN105301031A (en) * | 2015-12-01 | 2016-02-03 | 中山大学 | Method for determining hydrogen-containing silicone oil residual quantity in trisiloxane surfactant by one-dimensional hydrogen nuclear magnetic resonance method |
| CN108827998A (en) * | 2018-05-30 | 2018-11-16 | 中国计量科学研究院 | A method of volatile substances purity is accurately measured using quantitative nuclear magnetic resonance spectroscopy |
| CN109030538A (en) * | 2018-10-25 | 2018-12-18 | 西安近代化学研究所 | A kind of method of nuclear magnetic resonance hydrogen spectruming determining nitroglycerine moisture content |
-
2019
- 2019-02-25 CN CN201910139230.9A patent/CN111610214B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636510A (en) * | 2011-04-28 | 2012-08-15 | 河南省科学院高新技术研究中心 | Method for detecting quality of edible oil by using hydrogen-nuclear magnetic resonance spectroscopy |
| CN103454224A (en) * | 2013-05-02 | 2013-12-18 | 广东工业大学 | Edible oil quality determination system and method based on light polarization state |
| CN105301031A (en) * | 2015-12-01 | 2016-02-03 | 中山大学 | Method for determining hydrogen-containing silicone oil residual quantity in trisiloxane surfactant by one-dimensional hydrogen nuclear magnetic resonance method |
| CN108827998A (en) * | 2018-05-30 | 2018-11-16 | 中国计量科学研究院 | A method of volatile substances purity is accurately measured using quantitative nuclear magnetic resonance spectroscopy |
| CN109030538A (en) * | 2018-10-25 | 2018-12-18 | 西安近代化学研究所 | A kind of method of nuclear magnetic resonance hydrogen spectruming determining nitroglycerine moisture content |
Non-Patent Citations (2)
| Title |
|---|
| 余元祥等: "五种高不饱和多烯脂肪酸甲酯实物标准样品的研制", 《检验检疫科学》 * |
| 魏利斌等: "芝麻籽粒脂肪含量核磁共振无损快速测定方法的建立", 《江苏农业科学》 * |
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