CN216117406U - Solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride test - Google Patents
Solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride test Download PDFInfo
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- CN216117406U CN216117406U CN202122480509.9U CN202122480509U CN216117406U CN 216117406 U CN216117406 U CN 216117406U CN 202122480509 U CN202122480509 U CN 202122480509U CN 216117406 U CN216117406 U CN 216117406U
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Abstract
The solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride testing comprises a sleeve body made of fluoride and used as an external standard, and a sleeve cover detachably connected with the sleeve body, wherein an accommodating cavity used for accommodating a sample is formed in the sleeve body, and the accommodating cavity is in a closed state when the sleeve cover is connected with the sleeve body. According to the solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride testing, when solid NMR testing is carried out, a sample is filled in the accommodating cavity of the sleeve body, then the sleeve cover and the sleeve body are connected and covered, and the accommodating cavity is in a closed state, so that the sample can be concentrated in the accommodating cavity, the uniformity is improved, and meanwhile semi-solid and solid samples can be prevented from overflowing. Meanwhile, when a solid NMR test is performed, the casing body made of fluoride can be used as an external standard for an external standard absolute quantification method.
Description
[ technical field ] A method for producing a semiconductor device
The utility model relates to the technical field of chemical element detection, in particular to a solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride test.
[ background of the utility model ]
The fluorine of the current test method of the fluorine-containing compound is ionic fluorine determined by a fluorine ion selective electrode method, and the fluorine and organic fluorine in a combined state cannot be directly determined; the colorimetric method has complex operation and high requirement on reagents; the gas chromatography has the advantages of high sensitivity, no interference of other ions, good repeatability and the like, but the biological materials still need to be pretreated and mineralized. These methods all have certain limitations, and the common defects are that the type and structure of the fluorine-containing compound cannot be determined, and the test method is relatively complex. With the rapid development of the chemical industry, more and more new fluorine-containing compounds appear, and the qualitative and quantitative analysis of the existing detection method is difficult to realize simultaneously. Compared with the traditional method, the method has the advantages that,19f NMR has the characteristics of less sample consumption, high specificity, synchronous completion of qualitative identification and quantitative analysis, less interference of other substances and impurities, and great advantages in the aspects of sensitivity, accuracy, analysis speed and the like. Liquid NMR and solid NMR are again separated by NMR techniques according to the material morphology. The liquid NMR experiment of solid and paste samples requires pretreatment such as dissolution, but the fluorine-containing compound has more types of acid resistance, alkali resistance and high temperature resistance, so the dissolution is difficult, and the liquid NMR is difficult to perform. For such solid and semi-solid samples, such as fluoroplastics, fluorine-containing coatings and solid wastes, the solid NMR analysis is suitable for qualitative and quantitative analysis. In addition, solid-state NMR is also more advantageous for the study of the surface properties, heterogeneous adsorption and heterogeneous catalysis mechanisms of some functional materials. The solid NM test needs to be performed in a high-speed rotating environment, the uniformity of a solid sample in a sample tube must be guaranteed at the moment, otherwise, the rotation is difficult, and for a semi-solid sample, the semi-solid sample must be guaranteed not to overflow, so that the damage to an instrument is avoided.
[ Utility model ] content
The utility model solves the technical problems of insufficient sample uniformity and easy overflow in the solid NMR test at present, and provides a solid nuclear magnetic rotor inner sleeve for assisting the quantitative test of fluoride.
The utility model is realized by the following technical scheme:
the utility model provides an interior sleeve pipe of solid nuclear magnetism rotor of supplementary fluoride quantitative test, include by the fluoride make and be used for as the sleeve pipe body of outer standard, and with the sleeve pipe lid of connection can be dismantled to the sleeve pipe body, this internal cavity that holds that is used for holding the sample that is equipped with of sleeve pipe, the sleeve pipe lid with make during this body coupling of sleeve pipe it is in airtight state to hold the cavity.
The solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride testing comprises a sleeve body, wherein the sleeve body comprises a solid part, and the solid part, the accommodating cavity and the sleeve cover are sequentially distributed from the bottom to the top of the sleeve body.
The solid nuclear magnetic rotor inner sleeve for assisting the quantitative fluoride test has the length of one third of the total length of the sleeve body.
According to the solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride testing, the sleeve body is in threaded fit with the sleeve cover, the sleeve body is provided with the internal thread, and the sleeve cover is provided with the external thread.
The solid nuclear magnetic rotor inner sleeve for assisting the fluoride quantitative test is characterized in that the sleeve body and the sleeve cover are both made of polytetrafluoroethylene.
According to the solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride testing, the outer diameter of the sleeve body is matched with the inner diameter of the solid nuclear magnetic rotor, so that the sleeve body can enter the solid nuclear magnetic rotor.
Compared with the prior art, the utility model has the following advantages:
according to the solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride testing, when solid NMR testing is carried out, a sample is filled in the accommodating cavity of the sleeve body, then the sleeve cover and the sleeve body are connected and covered, and the accommodating cavity is in a closed state, so that the sample can be concentrated in the accommodating cavity, the uniformity is improved, and meanwhile semi-solid and colloid samples can be prevented from overflowing. Meanwhile, when a solid NMR test is performed, the casing body made of fluoride can be used as an external standard for an external standard absolute quantification method.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic view of the present invention placed in a solid nuclear magnetic rotor.
[ detailed description ] embodiments
In order to make the technical solutions and the advantages of the technical problems solved by the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the utility model and are not intended to limit the utility model.
When embodiments of the present invention refer to the ordinal numbers "first", "second", etc., it should be understood that the terms are used for distinguishing only when they do express the ordinal order in context.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The utility model provides an interior sleeve pipe of solid nuclear magnetism rotor of supplementary fluoride quantitative test, include by the fluoride make and be used for as the sleeve pipe body 1 of outer subject, and with sleeve cover 2 of connection can be dismantled to sleeve pipe body 1, be equipped with the holding cavity 11 that is used for holding the sample in the sleeve pipe body 1, sleeve cover 2 with make when sleeve pipe body 1 connects holding cavity 11 is in airtight state.
According to the solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride testing, when solid NMR testing is conducted, a sample is filled in the accommodating cavity of the sleeve body, then the sleeve cover and the sleeve body are connected and covered, the accommodating cavity is in a closed state, the sample can be concentrated in the accommodating cavity, uniformity is improved, and meanwhile semi-solid and colloid samples can be prevented from overflowing. Meanwhile, when a solid NMR test is performed, the casing body made of fluoride can be used as an external standard for an external standard absolute quantification method.
Further, as a preferred embodiment of the present invention, but not limited thereto, the casing body 1 includes a solid portion 12, and the solid portion 12, the accommodating cavity 11, and the casing cover 2 are sequentially distributed from the bottom of the casing body 1 to the top.
Further, as a preferred embodiment of the present solution, but not limited thereto, the length of the solid portion 12 is one third of the total length of the casing body 1. Since the lower third of the sample in the solid nuclear magnetic rotor is relatively inefficient to excite in solid NMR, the lower third of the inner casing is made solid in quantitative analysis and is not the site where the sample is placed.
Further, as a preferred embodiment of the present invention, but not limited thereto, the sleeve body 1 is in threaded fit with the sleeve cover 2, the sleeve body 1 is provided with an internal thread, and the sleeve cover 2 is provided with an external thread.
Further, as a preferred embodiment of the present solution, but not limiting, said sleeve body 1 is made of polytetrafluoroethylene. The polytetrafluoroethylene is used as a material for manufacturing the inner sleeve, and the inner sleeve is directly used as an external standard to realize quantitative analysis of fluoride. The sleeve body may also be made of other fluorine-containing compounds. If the material of the inner sleeve is specified, such as polytetrafluoroethylene, the inner sleeve can be converted by the standard substance of known fluoride, so that the inner sleeve can be used as an external standard substance for other fluoride quantitative tests.
Further, as a preferred embodiment of the present solution, but not limited thereto, the cannula cover 2 is made of fluoride. In particular, the cannula cover 2 is made of polytetrafluoroethylene. The inner sleeve of the embodiment enables the sample to be concentrated in the inner sleeve, is beneficial to the solid nuclear magnetic rotor to rotate, and prevents the sample from overflowing from the solid nuclear magnetic rotor.
Further, as a preferred embodiment of the present solution, but not limited thereto, the outer diameter of the casing body 1 is matched with the inner diameter of the solid nuclear magnetic rotor 3, so that the casing body 1 enters the solid nuclear magnetic rotor. The dimensions of the inner casing are based on the dimensions of the solid nuclear magnetic rotor, as shown in fig. 1. The outer diameter of the inner sleeve body is matched with the inner diameter of the solid nuclear magnetic rotor so as to be suitable for being just arranged in the solid nuclear magnetic rotor.
Further, the sleeve body may have a scale thereon.
The embodiment also provides an external standard absolute quantitative method using the inner sleeve as an external standard, which realizes simultaneous qualitative and quantitative analysis of fluoride in the collected sample and assists the rotation of the semi-solid sample. The external standard absolute quantitative method comprises the following steps: the method comprises the steps of firstly converting an inner sleeve into a considerable amount of NaF standard substance, calculating the fluorine content in the inner sleeve, and then testing a sample, namely calculating the fluoride content of the sample by taking the fluoride content in the inner sleeve as an external standard substance.
The method comprises the following specific steps:
before the sample test, the fluoride in the inner sleeve is quantitatively converted because the inner sleeve is made of fluoride. Firstly, a certain NaF standard sample with known mass is filled in an inner sleeve, and the inner sleeve is placed in a solid NMR instrument for testing according to optimized instrument parameter conditions.
According to the quantitative principle of NMR, under certain experimental conditions, the signal intensity is proportional to the number of resonant nuclei at the frequency of the signal, i.e.
Wherein A is the integrated area and n is the amount of substance;
according to
M is mass, M is molar mass;
the amount of species of fluorine in the NaF,
wherein m issIs the mass of sodium fluoride; msIs the molar mass of sodium fluoride;
the amount of fluorine-containing species in the polytetrafluoroethylene,
in, Mb4 represents the number of fluorine atoms per structural polyethylene monomer in terms of the molar mass of the polytetrafluoroethylene monomer.
The reason for the conversion by NaF is that in the solid NMR laboratory, one third of the middle part of the solid nuclear magnetic rotor is the most efficient excitation, the upper and lower third parts have lower nuclear excitation efficiency, and the amount of fluorine nuclei in the actual excited polytetrafluoroethylene can be calculated by the conversion by NaF.
Thus, the effective excited polytetrafluoroethylene content in the inner casing is:
the effective excited fluorine content mbf＝0.76×mbWherein 0.76 is a polytetrafluoroethylene monomer knotThe mass ratio of fluorine in the structure;
in the subsequent test of unknown sample fluoride, under the same experimental conditions, the fluorine content in the sample can be calculated by using the inner sleeve as an external standard substance.
And the advantages of NMR (nuclear magnetic resonance) qualitative determination are combined, the fluoride in the sample is determined, and the qualitative and quantitative analysis of the fluoride is realized.
The working principle of the embodiment is as follows:
the inner sleeve can solve the problems that semi-solid samples, such as toothpaste samples, are not easy to rotate or overflow in a solid nuclear magnetic rotor;
when the solid NMR test is carried out, the sleeve body made of fluoride can be used as an external standard of an external standard absolute quantitative method, so that qualitative and quantitative analysis of a fluorine-containing sample is realized.
The foregoing is illustrative of embodiments provided in connection with the detailed description and is not intended to limit the disclosure to the particular forms set forth herein. Similar to the structure of the method, or several technical deductions or substitutions made on the premise of the conception of the present application, should be regarded as the protection scope of the present application.
Claims (6)
1. The utility model provides a solid nuclear magnetism rotor inner sleeve pipe of supplementary fluoride quantitative test which characterized in that: the sample collecting device comprises a sleeve body (1) which is made of fluoride and used as an external standard, and a sleeve cover (2) detachably connected with the sleeve body (1), wherein a containing cavity (11) used for containing a sample is arranged in the sleeve body (1), and the containing cavity (11) is in a closed state when the sleeve cover (2) is connected with the sleeve body (1).
2. The solid nuclear magnetic rotor inner sleeve for assisting the quantitative fluoride test according to claim 1, wherein: the sleeve body (1) comprises a solid part (12), the containing cavity (11) and the sleeve cover (2) are distributed from the bottom to the top of the sleeve body (1) in sequence.
3. The solid nuclear magnetic rotor inner sleeve for assisting the quantitative fluoride test according to claim 2, wherein: the length of the solid part (12) accounts for one third of the total length of the sleeve body (1).
4. The solid nuclear magnetic rotor inner sleeve for assisting the quantitative fluoride test according to claim 1, wherein: the sleeve is characterized in that the sleeve body (1) is in threaded fit with the sleeve cover (2), an internal thread is arranged on the sleeve body (1), and an external thread is arranged on the sleeve cover (2).
5. The solid nuclear magnetic rotor inner sleeve for assisting the quantitative fluoride test according to claim 4, wherein: the sleeve body (1) and the sleeve cover (2) are both made of polytetrafluoroethylene.
6. The solid nuclear magnetic rotor inner sleeve for assisting the quantitative fluoride test according to claim 1, wherein: the outer diameter of the sleeve body (1) is matched with the inner diameter of the solid nuclear magnetic rotor, so that the sleeve body (1) can enter the solid nuclear magnetic rotor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122480509.9U CN216117406U (en) | 2021-10-14 | 2021-10-14 | Solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride test |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122480509.9U CN216117406U (en) | 2021-10-14 | 2021-10-14 | Solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride test |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216117406U true CN216117406U (en) | 2022-03-22 |
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| CN202122480509.9U Active CN216117406U (en) | 2021-10-14 | 2021-10-14 | Solid nuclear magnetic rotor inner sleeve for assisting quantitative fluoride test |
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