阅读说明：本技术 一种基于xps一步法测量烟丝加香均匀性的方法 (Method for measuring perfuming uniformity of cut tobacco based on XPS one-step method ) 是由 王晋 张承明 雷声 许�永 陈建华 刘欣 孔维松 李晶 黄海涛 李雪梅 陈章玉 于 2020-05-15 设计创作，主要内容包括：本发明涉及一种基于XPS一步法测量烟丝加香均匀性的方法,属于烟丝检测技术领域。该方法包括加香烟丝样品的XPS分析、数据处理、数据计算、加香均匀性判定四大步骤。本发明不用采用外加特征标记物或选择特定成分作为特征标记物进行分析,与其他气相色谱-质谱分析均匀性方法比较,其检测时间只需要3-5min左右,优于一般的气相色谱-质谱分析的40-50min,检测效率提高了近10倍,简单可行,易于推广应用。(The invention relates to a method for measuring perfuming uniformity of cut tobacco based on an XPS one-step method, and belongs to the technical field of cut tobacco detection. The method comprises four steps of XPS analysis of a flavored cut tobacco sample, data processing, data calculation and flavoring uniformity judgment. The invention does not need to adopt an additional characteristic marker or select a specific component as the characteristic marker for analysis, compared with other gas chromatography-mass spectrometry uniformity methods, the detection time is only about 3-5min, which is superior to 40-50min of the common gas chromatography-mass spectrometry, the detection efficiency is improved by nearly 10 times, and the method is simple and feasible, and is easy to popularize and apply.)

1. A method for measuring perfuming uniformity of cut tobacco based on an XPS one-step method is characterized by comprising the following steps:

step (1), XPS analysis of flavored cut tobacco samples:

taking flavored cut tobacco to perform XPS full spectrum scanning, C (1s) and O (1s) spectrum scanning and metal spectrum scanning;

step (2), data processing:

respectively calculating [ C ] according to the energy spectrum data obtained in the step (1)]/[O]And [ M₁]/[M₂]The metal content ratio is calculated, and the peak fitting is carried out on C (1s) according to different corresponding binding energies of the chemical states, and [ C-H ] is calculated]、[C-O]And [ C ═ O]The relative content of each chemical state;

wherein M is₁And M₂Respectively the metal with the largest content and the metal with the second largest content in the flavored cut tobacco;

step (3), data calculation:

CU uniformity coefficient calculation formula:

x_ithe relative content of a certain component in the ith analysis is shown, and n is the total analysis times of each sample;

respectively adding C of unperfumed tobacco shreds before flavoring]/[O]、[M₁]/[M₂]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain CU_[C]/[O]、CU_[C-H]、CU_[C-O]、CU_C＝OAnd CU_[M1]/[M2](ii) a Then adding fragrance to the cut tobacco with uniformity coefficient CU_{General assembly}And (3) calculating:

CU_{general assembly}Namely the perfuming uniformity coefficient of the cut tobacco;

and (4) judging the perfuming uniformity: when CU_{General assembly}If the fragrance is more than 250 percent, the perfuming is judged to be uniform, otherwise, the perfuming is judged to be non-uniform.

2. The method for measuring perfuming uniformity of cut tobacco based on XPS one-step method according to claim 1, wherein in step (1), XPS analysis conditions are that the instrument adopts ray excitation source as monochromated Al target with energy of α Al K X-ray (1486.6eV) as radiation source during experiment, and background vacuum is kept at 10%^-6Pa order of magnitude, recording full spectrum, C (1s), O (1s) and metal energy level spectrum 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 method for measuring perfuming uniformity of cut tobacco based on XPS one-step method according to claim 1, wherein the total number of analysis n of each sample is not less than 10.

4. The method for measuring perfuming uniformity of tobacco shreds based on XPS one-step method of claim 1, wherein the selected metal spectrum is 2 metal energy spectra with maximum content in the tobacco shreds of the sample, namely two metal peaks with maximum peak intensity in the whole spectrum.

Technical Field

The invention belongs to the technical field of cut tobacco detection, and particularly relates to a method for measuring flavoring uniformity of cut tobacco based on an XPS one-step method.

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 method for measuring the flavoring uniformity of cut tobacco based on an XPS one-step method.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows:

a method for measuring perfuming uniformity of cut tobacco based on an XPS one-step method comprises the following steps:

step (1), XPS analysis of flavored cut tobacco samples:

taking flavored cut tobacco to perform XPS full spectrum scanning, C (1s) and O (1s) spectrum scanning and metal spectrum scanning;

step (2), data processing:

respectively calculating [ C ] according to the energy spectrum data obtained in the step (1)]/[O]And [ M₁]/[M₂]The metal content ratio is calculated, and the peak fitting is carried out on C (1s) according to different corresponding binding energies of the chemical states, and [ C-H ] is calculated]、[C-O]And [ C ═ O]The relative content of each chemical state;

wherein M is₁And M₂Respectively the metal with the largest content and the metal with the second largest content in the flavored cut tobacco;

step (3), data calculation:

CU uniformity coefficient calculation formula:

x_ithe relative content of a certain component in the ith analysis is shown, and n is the total analysis times of each sample;

respectively adding C of unperfumed tobacco shreds before flavoring]/[O]、[M₁]/[M₂]、[C-H]、[C-O]And [ C ═ O]Substituting into CU formula, and calculating to obtain CU_[C]/[O]、CU_[C-H]、CU_[C-O]、CU_C＝OAnd CU_[M1]/[M2](ii) a Then adding fragrance to the cut tobacco with uniformity coefficient CU_{General assembly}And (3) calculating:

CU_{general assembly}Namely the perfuming uniformity coefficient of the cut tobacco;

and (4) judging the perfuming uniformity: when CU_{General assembly}If the fragrance is more than 250 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 uses a ray excitation source as a monochromated Al target with energy of α Al K X-ray (1486.6eV) as a radiation source and a background vacuum is maintained at 10 degrees^-6Pa order of magnitude, recording full spectrum, C (1s), O (1s) and metal energy level spectrum 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 total number of analyses n per sample is not less than 10.

Further, it is preferable that the selected metal spectrum is 2 metal energy spectra with the largest content in the sample tobacco shred, that is, two metal peaks with the largest peak intensity in the whole spectrum.

The analysis conditions used in the present invention must be consistent for the same sample analysis.

CU_{General assembly}The larger the value, the better the perfuming uniformity. By the process of the invention, it is also possible to screen the perfuming process, by CU_{General assembly}The magnitude of the value is used for screening a better perfuming method.

Compared with the prior art, the invention has the beneficial effects that:

1) the tobacco shred flavoring uniformity detection is based on X-ray photoelectron spectroscopy, adopts a one-step 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.

2) Compared with other gas chromatography-mass spectrometry analysis uniformity detection methods, the detection time of the method only needs about 3-5min, which is superior to 40-50min of general gas chromatography-mass spectrometry analysis, the detection efficiency is improved by about 10 times, and the method is easy to popularize and apply.

Drawings

Figure 1 XPS survey of flavored samples of example tobacco shreds.

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.