CN111426716A - Cut tobacco perfuming uniformity detection method based on XPS - Google Patents
Cut tobacco perfuming uniformity detection method based on XPS Download PDFInfo
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- CN111426716A CN111426716A CN202010415282.7A CN202010415282A CN111426716A CN 111426716 A CN111426716 A CN 111426716A CN 202010415282 A CN202010415282 A CN 202010415282A CN 111426716 A CN111426716 A CN 111426716A
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- G01N23/2273—Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]
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Abstract
The invention relates to a cut tobacco perfuming uniformity detection method based on XPS, and belongs to the technical field of cut tobacco detection. The detection method comprises five steps of XPS analysis of unflavored tobacco shreds, XPS analysis of flavored samples, data processing, data calculation and flavoring uniformity judgment. The method does not need to adopt an additional characteristic marker or select a specific component as the characteristic marker for analysis, and is simple and feasible. Compared with other gas chromatography-mass spectrometry uniformity methods, the detection time is only about 3-5min, which is superior to 40-50min of general gas chromatography-mass spectrometry, the detection efficiency is improved by about 10 times, and the method is easy to popularize and apply.
Description
Technical Field
The invention belongs to the technical field of cut tobacco detection, and particularly relates to a cut tobacco flavoring uniformity detection method based on XPS.
Background
Cigarette formula is always regarded as the core technology of cigarette enterprises, however, the addition of flavors and fragrances in cigarettes is more regarded as a key technology. The cut tobacco making and flavoring process is an indispensable key process in the cut tobacco making production of cigarettes, and the task is to accurately and uniformly apply a certain amount of essence to the blended cut tobacco according to the requirements of production and formula. At present, some enterprises make some attempts on controlling the perfuming uniformity, but mainly deduces and calculates from the theoretical point of view, and no relevant system literature report exists in the industry on the aspect of quantitative characterization of the perfuming uniformity.
However, the chemical composition of the tobacco essence perfume is complex, the varieties are various, and the essence added on the tobacco shreds of the cigarettes is the same in composition, only has different contents, and the content of the added essence is less. When one or more characteristic compounds are used as markers for detecting the perfuming uniformity, the markers are difficult to find, and the markers are difficult to add in large-scale production, so that a reasonable comprehensive detection result cannot be obtained.
X-ray photoelectron spectroscopy (XPS) is an electronic energy spectrum obtained by exciting a sample with soft X-rays and taking photoelectron kinetic energy as a horizontal coordinate and relative intensity as a vertical coordinate. XPS is a quantitative spectroscopy technique that can measure the elemental composition, empirical formula, and the chemical and electronic states of the elements contained therein. The X-ray photoelectron spectrum has the advantages of high sensitivity, simple sample preparation, small destructiveness to samples and the like, and is one of the most effective and widely applied analysis techniques in surface analysis.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a cut tobacco flavoring uniformity detection method based on XPS.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an XPS-based cut tobacco flavoring uniformity detection method comprises the following steps:
step (1), XPS analysis of unperfumed cut tobacco:
taking unperfumed cut tobacco before perfuming, and performing XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (2), XPS analysis of the perfumed sample:
taking flavored cut tobacco to perform XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (3), data processing:
respectively calculating [ C ]/[ O ] according to the content [ C ] and [ O ] data of the carbon element and the oxygen element obtained in the step (1) and the step (2), carrying out peak-splitting fitting on C (1s) according to different chemical state corresponding binding energies, and calculating the relative content of each chemical state of [ C-H ], [ C-O ] and [ C ═ O ];
step (4), data calculation:
CU uniformity coefficient calculation formula:
wherein x isiThe relative content of a certain component in the ith analysis; n is the total number of analyses for each sample;
respectively adding C of unperfumed tobacco shreds before flavoring]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
Respectively adding the flavoring tobacco shreds]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
Then calculating the tobacco shred flavoring uniformity coefficient CUGeneral assembly；
CUGeneral assemblyNamely the perfuming uniformity coefficient of the cut tobacco;
and (5) judging perfuming uniformity: when CUGeneral assemblyIf the fragrance is more than 85 percent, the perfuming is judged to be uniform, otherwise, the perfuming is judged to be non-uniform.
Further, it is preferable that in the step (1), the XPS analysis conditions are such that the apparatus is a monochromatized Al target with an energy of α Al K X-ray (1486.6eV) using a radiation excitation source during the experiment, and the background vacuum is maintained at 10 degrees-6Pa order of magnitude, recording full spectrum, C (1s) and O (1s) energy level spectra respectively; the scanning step length of the XPS full spectrum is 0.8eV, and the scanning step length of the core energy level spectrum and the valence band spectrum is 0.125 eV.
Further, it is preferable that the number of analyses n per sample is not less than 10.
The analysis conditions used in the present invention must be consistent for the same sample analysis.
CUGeneral assemblyThe larger the value, the better the perfuming uniformity. By the process of the invention, it is also possible to screen the perfuming process, by CUGeneral assemblyThe magnitude of the value is used for screening a better perfuming method.
Compared with the prior art, the invention has the beneficial effects that:
the method does not need to adopt an additional characteristic marker or select a specific component as the characteristic marker for analysis, and is simple and feasible. Compared with other gas chromatography-mass spectrometry uniformity methods, the detection time is only about 3-5min, which is superior to 40-50min of general gas chromatography-mass spectrometry, the detection efficiency is improved by about 10 times, and the method is easy to popularize and apply.
Drawings
FIG. 1 shows XPS survey spectra and C spectral peak fits of samples from cut tobacco of application example 1 before perfuming;
FIG. 2 shows XPS survey and C spectral peak fit plots of samples of the tobacco shreds of example 1 after they have been flavored.
Detailed Description
The present invention will be described in further detail with reference to examples.
It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The materials or equipment used are not indicated by manufacturers, and all are conventional products available by purchase.
Example 1
An XPS-based cut tobacco flavoring uniformity detection method comprises the following steps:
step (1), XPS analysis of unperfumed cut tobacco:
taking unperfumed cut tobacco before perfuming, and performing XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (2), XPS analysis of the perfumed sample:
taking flavored cut tobacco to perform XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (3), data processing:
respectively calculating [ C ]/[ O ] according to the content [ C ] and [ O ] data of the carbon element and the oxygen element obtained in the step (1) and the step (2), carrying out peak-splitting fitting on C (1s) according to different chemical state corresponding binding energies, and calculating the relative content of each chemical state of [ C-H ], [ C-O ] and [ C ═ O ];
step (4), data calculation:
CU uniformity coefficient calculation formula:
wherein x isiThe relative content of a certain component in the ith analysis; n is the total number of analyses for each sample;
respectively adding C of unperfumed tobacco shreds before flavoring]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
Respectively adding the flavoring tobacco shreds]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
Then calculating the tobacco shred flavoring uniformity coefficient CUGeneral assembly；
CUGeneral assemblyNamely the perfuming uniformity coefficient of the cut tobacco;
and (5) judging perfuming uniformity: when CUGeneral assemblyIf the fragrance is more than 85 percent, the perfuming is judged to be uniform, otherwise, the perfuming is judged to be non-uniform.
Example 2
An XPS-based cut tobacco flavoring uniformity detection method comprises the following steps:
step (1), XPS analysis of unperfumed cut tobacco:
taking unperfumed cut tobacco before perfuming, and performing XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (2), XPS analysis of the perfumed sample:
taking flavored cut tobacco to perform XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (3), data processing:
respectively calculating [ C ]/[ O ] according to the content [ C ] and [ O ] data of the carbon element and the oxygen element obtained in the step (1) and the step (2), carrying out peak-splitting fitting on C (1s) according to different chemical state corresponding binding energies, and calculating the relative content of each chemical state of [ C-H ], [ C-O ] and [ C ═ O ];
step (4), data calculation:
CU uniformity coefficient calculation formula;
wherein x isiThe relative content of a certain component in the ith analysis; n is the total number of analyses for each sample;
respectively adding C of unperfumed tobacco shreds before flavoring]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
Respectively adding the flavoring tobacco shreds]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
Then calculating the tobacco shred flavoring uniformity coefficient CUGeneral assembly；
CUGeneral assemblyNamely the perfuming uniformity coefficient of the cut tobacco;
and (5) judging perfuming uniformity: when CUGeneral assemblyIf the fragrance is more than 85 percent, the perfuming is judged to be uniform, otherwise, the perfuming is judged to be non-uniform.
In the step (1), the XPS analysis conditions are that the instrument adopts a ray excitation source as a monochromatized Al target during the experiment, the energy of the ray excitation source is α Al K X-ray (1486.6eV), and the background vacuum is kept at 10 DEG-6Pa order of magnitude, recording full spectrum, C (1s) and O (1s) energy level spectra respectively; the scanning step length of the XPS full spectrum is 0.8eV, and the scanning step length of the core energy level spectrum and the valence band spectrum is 0.125 eV.
The number of analyses n per sample was not less than 10.
Application example 1
An XPS-based cut tobacco flavoring uniformity detection method comprises the following steps:
step (1), XPS analysis of unperfumed cut tobacco:
taking 10 parts of unperfumed A brand cut tobacco before perfuming, and carrying out XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (2), XPS analysis of the perfumed sample:
taking 10 parts of roll-type flavored A brand cut tobacco samples, and carrying out XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (3), data processing:
respectively calculating [ C ]/[ O ] according to the [ C ] and [ O ] data of the contents of the carbon element and the oxygen element obtained in the step (1) and the step (2), performing peak-splitting fitting on C1s according to different chemical state corresponding binding energies, and calculating the relative content of each chemical state of [ C-H ], [ C-O ] and [ C ═ O ];
step (4), data calculation:
CU is the uniformity coefficient (100%) formula:
wherein x isiThe relative content of a certain component in the ith analysis; n is the total number of analyses per sample, where n is 10;
respectively adding C of unperfumed tobacco shreds before flavoring]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
Respectively adding the flavoring tobacco shreds]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
The results are shown in table 1:
TABLE 1
Substituting:
the flavoring uniformity coefficient of the obtained cut tobacco is more than 90.3 percent and 85 percent, and the flavoring uniformity is judged.
Application example 2
The cut tobacco of brand A without being flavored and the same essence and spice adopted for flavoring in the application example 1 are adopted to be flavored evenly by hands. The analysis method is the same as the above (the obtained data are shown in table 1), the perfuming uniformity coefficient of the manually uniformly perfumed cut tobacco is calculated to be 98.4% or more than 85%, and the perfuming uniformity is judged.
Application example 2 was judged to be more evenly perfumed since 98.4% > 90.3%.
The method can effectively distinguish two groups of samples with different perfuming uniformity, quantifies the perfuming uniformity through the perfuming uniformity coefficient, and has popularization and application values.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (3)
1. An XPS-based cut tobacco flavoring uniformity detection method is characterized by comprising the following steps:
step (1), XPS analysis of unperfumed cut tobacco:
taking unperfumed cut tobacco before perfuming, and performing XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (2), XPS analysis of the perfumed sample:
taking flavored cut tobacco to perform XPS full spectrum scanning, C (1s) spectrum scanning and O (1s) spectrum scanning;
step (3), data processing:
respectively calculating [ C ]/[ O ] according to the content [ C ] and [ O ] data of the carbon element and the oxygen element obtained in the step (1) and the step (2), carrying out peak-splitting fitting on C (1s) according to different chemical state corresponding binding energies, and calculating the relative content of each chemical state of [ C-H ], [ C-O ] and [ C ═ O ];
step (4), data calculation:
CU uniformity coefficient calculation formula:
wherein x isiThe relative content of a certain component in the ith analysis; n is the total number of analyses for each sample;
respectively adding C of unperfumed tobacco shreds before flavoring]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
And
respectively adding the flavoring tobacco shreds]/[O]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain
And
then calculating the tobacco shred flavoring uniformity coefficient CUGeneral assembly；
CUGeneral assemblyNamely the perfuming uniformity coefficient of the cut tobacco;
and (5) judging perfuming uniformity: when CUGeneral assemblyIf the fragrance is more than 85 percent, the perfuming is judged to be uniform, otherwise, the perfuming is judged to be non-uniform.
2. The method for detecting the flavoring uniformity of XPS-based cut tobacco according to claim 1, wherein in step (1), the XPS analysis conditions are that the instrument adopts a ray excitation source as a monochromated Al target with energy of α Al K X-ray (1486.6eV) during experiment, the background vacuum is kept at 10 degrees-6Pa order of magnitude, recording full spectrum, C (1s) and O (1s) energy level spectra respectively; the scanning step length of the XPS full spectrum is 0.8eV, and the scanning step length of the core energy level spectrum and the valence band spectrum is 0.125 eV.
3. The XPS-based cut tobacco flavoring uniformity detection method according to claim 1, wherein each sample is analyzed no less than 10 times n.
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