CN113686911A - Method for characterizing chemical state of silver element in silver-containing dressing - Google Patents
Method for characterizing chemical state of silver element in silver-containing dressing Download PDFInfo
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Abstract
The invention discloses a method for characterizing the chemical state of silver element in silver-containing dressing, which comprises the following steps: confirming the state of the instrument, confirming the reference peak position of silver in different chemical states, selecting an internal standard calibration method, adopting metal chloride Cl2p (197.8eV) for calibration, and comparing the standard with Ag3d of Ag element in the dressing5/2、Ag3d3/2The valence state of Ag corresponding to the reference peak with the position of the maximum binding energy closer is determined as the valence state of Ag element in the dressing. The method for characterizing the chemical state of the silver element in the silver-containing dressing can effectively confirm the chemical state of the Ag element in the silver-containing dressing, and has the advantages of accurate operation and high precision.
Description
Technical Field
The invention relates to a method for testing the chemical state of an element, in particular to a method for characterizing the chemical state of a silver element in a silver-containing dressing.
Background
Silver has a good antibacterial effect, so that silver-containing products are widely applied to the fields of medical treatment, tableware, food preservation and the like. Dressings are materials used to cover and protect wounds, and are an antimicrobial product that is very common in the medical field. The dressing often contains nano silver and/or silver compounds, so as to control the microbial environment of the dressing and/or the wound surface and create favorable conditions for the healing of the wound surface. However, potential biosafety risks (such as special biological effects and potential toxicity risks) possibly caused by the antibacterial dressing need scientific recognition and evaluation, and the existence form of silver in the silver-containing dressing (the silver particles in an elemental state or silver in a combined state, namely silver ions) can cause cytotoxicity to different degrees, so that the analysis and the characterization of the silver valence state on the surface of the dressing are necessary.
Ag3d in different chemical states5/2、Ag3d3/2The peak positions of the spectral peaks have small differences; and because the chemical environments are not completely the same, Ag3d in the same chemical state in different samples5/2、Ag3d3/2The peak positions will also differ slightly. In addition, the final results of the instrument state, charge calibration and data peak fitting process can cause the peak position of the Ag element to have a deviation of 0.5eV or more (close to the peak position deviation of silver in different chemical states), and thus can cause the wrong determination of the chemical state of the Ag element.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a method for characterizing the chemical state of the silver element in the silver-containing dressing, which can effectively confirm the chemical state of the silver element in the silver-containing dressing, and has accurate operation and high precision.
The purpose of the invention is realized by the following technical scheme:
a method for characterizing the chemical state of silver element in a silver-containing dressing comprises the following steps:
(1) confirming the XPS instrument state;
(2) confirming the charge neutralization state;
(3) determining the judgment basis of the reference peak: ag3d5/2、Ag3d3/2Maximum binding energies at 368.2eV and 374.2eV indicate elemental silver Ag0；Ag3d5/2、Ag3d3/2Maximum binding energy at 367.8eV and 373.8eV indicates monovalent silver ions Ag+；
(4) Testing XPS data of the AgCl reference sample to obtain a peak position P of a metal chloride Cl2P spectrum peak;
(5) preparing a silver-containing dressing sample, testing XPS data, carrying out background deduction through XPS data processing software, calibrating the XPS data of the silver-containing dressing sample according to the peak position P of a spectrum peak of metal chloride Cl2P, and obtaining Ag3d of Ag element in the dressing through fitting5/2、Ag3d3/2The position of the maximum binding energy is determined according to the judgment in the step (3) and is combined with Ag3d of the Ag element in the dressing5/2、Ag3d3/2The valence state of Ag corresponding to the reference peak with the position of the maximum binding energy closer is determined as the valence state of Ag element in the dressing.
Preferably, the XPS instrument status confirmation in step (1) is specifically: and (3) calibrating the XPS instrument by using an energy scale standard substance of an X-ray photoelectron spectrometer to ensure that the difference between the actual measurement result and the reference peak position is less than 0.1 eV.
Preferably, the calibrating of the XPS instrument by using the energy calibration standard substance of the X-ray photoelectron spectrometer specifically comprises: according to the requirements of the national standard GB/T22571-2017, the instrument is calibrated by using an energy scale standard substance of an X-ray photoelectron spectrometer.
Preferably, the standard substance is Au, Ag or Cu foil.
Preferably, the charge neutralization state confirmation in step (2) is specifically: testing the insulation samples PET and MgO samples by using an XPS instrument to obtain a C1s spectrum of the insulation sample PET and a Mg1s spectrum in the MgO sample;
and judging whether the content of three chemical states of C-C, C-O, C-O in the PET sample is close to 3 or not according to the C1s spectrum of the PET sample and the Mg1s spectrum of the MgO sample: 1: 1; if not, adjusting the state of the XPS instrument according to the operating rules of X-ray photoelectron spectrometer instrument calibration owned by the manufacturer;
judging whether the peak position of the Mg1s spectrum in the MgO sample is close to the theoretical peak position; if not, adjusting the state of the XPS instrument according to the operating rules of X-ray photoelectron spectrometer instrument calibration owned by the manufacturer.
Preferably, the method for judging whether the content of three chemical states of C-C, C ═ O, C-O in the insulation sample PET is close to 3: 1: 1, specifically: judging whether the content of three chemical states of C-C, C-O, C-O in the PET of the insulation sample is 3: (0.95-1.05): (0.95-1.05);
judging whether the peak position of the Mg1s spectrum in the MgO sample is close to the theoretical peak position, specifically:
and judging whether the difference between the peak position of the Mg1s spectrum in the MgO sample and the theoretical peak position is less than 0.1 eV.
Specifically, the peak position P of the metal chloride Cl2P spectrum peak is 197.8 eV.
Preferably, the preparation of the silver-containing dressing sample in the step (5) specifically comprises: randomly selecting 1 position by using a clean scissors and shearing out a sample to be detected with a proper size.
Preferably, the XPS data in step (5) is specifically:
fixing a silver-containing dressing sample on a sample table, vacuumizing, and randomly selecting a position for data acquisition after the vacuum meets the requirement; acquisition parameters were 650 microns spot, standard mode neutralization gun.
Preferably, the XPS data processing software of step (5) is Avantage software.
Due to Ag3d in different chemical states5/2、Ag3d3/2The peak positions of the spectral peaks have small differences; and because the chemical environments are not completely the same, Ag3d in the same chemical state in different samples5/2、Ag3d3/2The peak positions will also differ slightly. Thus Ag3d in a particular chemical state5/2、Ag3d3/2There will be a range of corresponding peak positions rather than specific, specific peak values.
When the chemical state is confirmed through the XPS peak position, the instrument state (combination energy scale and charge calibration) needs to be ensured to be normal. If the error of the instrument combined with the energy scale is large, the error may be caused in the sampleThe corresponding peak value readings of each element are inaccurate, and even wrong chemical states and element qualitative identification can be caused; whether the charge calibration state (namely whether the parameters of the neutralization gun can adapt to the current test sample) is normal or not can influence the distortion of the shape of a spectrum peak, so that the accurate determination of the qualitative and relative quantification of each chemical state is influenced; confirming reference peak positions of Ag3d in different chemical states, and performing data acquisition by using AgCl with purity of 99.5% and Ag foil with purity of 99.9% to obtain Ag+And a peak reference value corresponding to elemental silver. The method that the actually measured value is closer to the reference peak position value is utilized to judge the chemical state of Ag in the actual sample.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the method, firstly, the state of the instrument is confirmed, secondly, the reference peak position of silver in different chemical states is confirmed, an internal standard calibration method is selected, and metal chloride Cl2p (197.8eV) is adopted for calibration, so that the chemical state of Ag element in the silver-containing dressing can be effectively confirmed, and the scientific understanding and evaluation of the biological safety risk of the antibacterial dressing are achieved.
(2) The method utilizes the method that the actual measurement value is closer to the reference peak position value to judge the chemical state of the Ag in the actual sample, but not the specific and specific peak position value described in the literature 'characterization of silver in silver-containing dressing and in vitro release experiment technical points', thereby improving the authenticity and the accuracy of the test result.
(3) The method is simple and easy to operate, and experimental errors caused by the state of the instrument and the data processing process are avoided.
(4) The method can be widely applied to qualitative detection of chemical states of Ag element in the silver dressing.
Drawings
FIG. 1 is an XPS spectrum of a PET sample C1s obtained in this example.
FIG. 2 is an XPS spectrum of the MgO sample Mg1s measured in this example.
Fig. 3 shows the reference peak position of Ag3d for the pure Ag foil measured in this example.
Fig. 4 shows the reference peak position of Ag3d in AgCl chemical state measured in this example.
FIG. 5 is a spectrum of metal chloride Cl2p measured in this example.
FIG. 6 is a spectrum of Cl2p of sample 1 measured in this example.
Fig. 7 is a spectrum of Ag3d of sample 1 measured in this example.
FIG. 8 is an X-ray diffraction spectrum of sample 1 measured in this example.
Fig. 9 is a spectrum of Cl2p of sample 2 measured in this example.
Fig. 10 is a spectrum of Ag3d of sample 2 measured in this example.
Fig. 11 is an X-ray diffraction spectrum of sample 2 measured in this example.
Fig. 12 is a partial enlarged view of the X-ray diffraction spectrum of fig. 11.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Examples
The method for characterizing the chemical state of the silver element in the silver-containing dressing comprises the following steps:
(1) XPS instrument status confirmation: according to the requirements of the national standard GB/T22571-2017, the instrument is calibrated by using energy scale standard substances (Au, Ag and Cu foils) of an X-ray photoelectron spectrometer, and the actual measurement result is ensured to meet the technical requirement of JJG (teaching Commission) 013-1996 electronic energy spectrum metrological verification procedure on the metrological calibration of the XPS combined energy scale. Ensuring that the difference between the actual measurement result and the reference peak position is obviously less than 0.1eV, and meeting the technical requirement of JJJG (textbook) 013 & 1996 electronic energy spectrum metrological verification procedure on the metrological calibration of the XPS binding energy scale.
(2) And (3) confirming the charge neutralization state: testing the insulation samples PET and MgO samples by using an XPS instrument to obtain a C1s spectrum of the insulation sample PET and a Mg1s spectrum in the MgO sample;
according to the C1s spectrum of the insulation sample PET and the Mg1s spectrum of the MgO sample, whether the content ratio of three chemical states of C-C, C-O, C-O in the insulation sample PET is close to 3 is judged: 1: 1; if not, adjusting the state of the XPS instrument according to an operation rule of X-ray photoelectron spectrometer instrument calibration carried by a manufacturer (at the moment, the adjustment of the state of the XPS instrument is mainly carried out by optimizing the parameters of a neutralization gun, taking the method for adjusting the parameters of the neutralization gun of the XPS of a Siemens flight manufacturer as an example, the specific method comprises the steps of firstly changing the shift parameters In an internal neutralization gun (In-lens) to enable the internal neutralization gun to carry out spectrum acquisition In the range of-2.5 to 2.5, and when the content of three chemical states of C-C, C-O, C-O In PET is closest to 3: 1: 1 and the corresponding parameters are the most suitable parameter values when the spectral peak splitting is most obvious);
judging whether the peak position of the Mg1s spectrum in the MgO sample is close to the theoretical peak position; if not, adjusting the state of the XPS instrument according to the operating rules of X-ray photoelectron spectrometer instrument calibration owned by the manufacturer (at the moment, the adjustment of the state of the XPS instrument is mainly carried out by optimizing the parameters of a neutralization gun, taking the method for adjusting the parameters of the neutralization gun of the XPS of the Sammer aviation manufacturer as an example).
The steps are based on the following theoretical basis: because the peak position of the peak of the C1s spectrum in the PET of the insulation sample is positioned at the low binding energy end and the corresponding relative contents of 3 specific chemical states are known, and the peak of the Mg1s spectrum in the MgO sample is positioned at the high binding energy end of the binding energy scale and has symmetrical peak shape, the peak shape distortion of the peaks of the C1s and Mg1s spectrums can occur when the charging effect is poor. The state of charge calibration of the instrument is thus confirmed by observing the actual test data of the sample. When the charge calibration state of the instrument is good, the content ratio of the three chemical states C of the PET sample can be found to be approximate to 3: 1: 1 (as shown in figure 1), the peak position of the Mg1s spectrum peak in the MgO sample is close to the theoretical peak position (as shown in figure 2), and the peak shape is quite symmetrical, which indicates that the instrument state can be used for the characterization of the silver-containing dressing product.
(3) Determining the judgment basis of the reference peak: ag3d5/2、Ag3d3/2Maximum binding energies at 368.2eV and 374.2eV indicate Ag0(elemental silver); ag3d5/2、Ag3d3/2Maximum binding energies at 367.8eV and 373.8eV indicate Ag+；
The specific process of determining the reference peak is as follows: collecting data by AgCl with purity of 99.5% and Ag foil with purity of 99.9% to obtain Ag+Ag3d corresponding to elemental silver5/2、Ag3d3/2Peak position reference value.
The actual test results are shown in FIG. 3, which corresponds to pure Ag foil (i.e. in the elemental state)Ag3d5/2、Ag3d3/2The peak positions are 368.3eV and 374.3eV respectively; as shown in FIG. 4, Ag in the chemical state of AgCl+Corresponding Ag3d5/2、Ag3d3/2The peak positions are 367.7eV and 373.7eV, respectively. The data are very close to the data described in the literature, characterization of silver in silver-containing dressing and technical points of in vitro release experiments (difference of 0.1eV), and the peak position difference of an actual sample in two different chemical states is small (about 0.6 eV); therefore, the data described in the technical points of characterization of silver in silver-containing dressing and in vitro release experiment can be used as the judgment basis of the reference peak position, namely Ag3d5/2、Ag3d3/2Maximum binding energies at 368.2eV and 374.2eV indicate Ag0(i.e., elemental silver); ag3d5/2、Ag3d3/2Maximum binding energies at 367.8eV and 373.8eV indicate Ag+. However, in this embodiment, the chemical state of Ag in the actual sample is determined by using which of the two chemical states with the closer measured value corresponds to the reference peak position value.
(4) Testing XPS data of the AgCl reference sample to obtain a peak position P of a metal chloride Cl2P spectrum peak; the spectrum of the metal chloride Cl2p obtained by the test of the example is shown in FIG. 5, and the peak position of the metal chloride Cl2p spectrum is 197.8 eV.
(5) Preparing a silver-containing dressing sample, testing XPS data, carrying out background deduction through Avantage software or other XPS data processing software, calibrating the XPS data of the silver-containing dressing sample according to the peak position P of a spectrum peak of metal chloride Cl2P, and obtaining Ag3d of silver in the silver dressing sample through fitting5/2、Ag3d3/2And (4) judging the valence state of the Ag element in the dressing by confirming the reference peak position of the Ag element in the dressing according to the judgment basis in the step (3): will be mixed with Ag3d of Ag element in dressing5/2、Ag3d3/2The valence state of Ag corresponding to the reference peak with the position of the maximum binding energy closer is determined as the valence state of Ag element in the dressing.
In this example, a silver-containing dressing sample was prepared, and XPS data was tested, specifically: randomly selecting 1 position with clean scissors, cutting to obtain sample of about 0.5cm × 0.5cm, fixing on sample stage, vacuumizing, and randomly selectingTaking a position for data acquisition; acquisition parameters were 650 microns spot, standard mode neutralization gun. Background subtraction by software to obtain Ag3d5/2、Ag3d3/2Peak value of maximum binding energy.
To examine the accuracy of the method of the present invention, this example uses XRD method to confirm the Ag valence:
first, an XRD sample was prepared: randomly selecting 1 position by using a clean scissors, cutting out a sample to be detected with the size of about 20cm multiplied by 20cm, and fixing the sample on a sample table; performing rapid scanning on 2 theta from 3 degrees to 100 degrees to obtain a diffraction primary diffraction spectrum of the sample; according to the X-ray diffraction spectrum after pre-scanning and according to the position and the intensity of a diffraction peak, carrying out X-ray diffraction analysis: the scanning 2 theta range is 5-90 degrees, the step size is 0.0131 degree, and the step scan time is 100 s. The peak searching of the spectrogram is completed by performing operations such as smoothing, peak searching, background removing, peak searching and the like on data selectivity through HighScore (plus) software.
Through the retrieval of a PDF database, the phase of the silver-containing crystal contained in the sample is matched, and the main components of the silver crystal are as follows: silver chloride (AgCl, card number: 01-071-. The XPS result is consistent with the XRD result, and the accuracy of the chemical state of Ag element of the silver-containing dressing is further confirmed by an internal standard calibration method during XPS analysis.
Silver-containing dressing samples were tested and examined using the method described above in this example, as follows:
sample 1: the XPS data of the test sample 1 is subjected to background deduction through software, and the judgment basis is determined: ag3d5/2、Ag3d3/2Maximum binding energies at 368.2eV and 374.2eV indicate Ag0；Ag3d5/2、Ag3d3/2Maximum binding energies at 367.8eV and 373.8eV indicate Ag+(ii) a The Ag3d was obtained by internal standard method (calibrated against 197.8eV of the peak of Cl2p as a metal chloride in the sample) and by fitting5/2、Ag3d3/2The maximum binding energy is 367.6eV and 373.6eV which are closer to Ag+The reference peak position of (2). The spectrum of Cl2p and the spectrum of Ag3d of sample 1 are shown in fig. 6 and 7, respectively.
The XRD method confirms the Ag valence state: the XRD test result of sample 1 is shown in fig. 8, and by using PDF database search, the phase of silver-containing crystals contained in the sample is matched, which results in that the main components of the silver crystals are: silver chloride (AgCl), card number: 01-071-. The XPS result is consistent with the XRD result, and the accuracy of the chemical state of Ag element of the silver-containing dressing is further confirmed by an internal standard calibration method during XPS analysis.
Sample 2: the XPS data of test sample 2 was subjected to background subtraction by software to determine the judgment basis: ag3d5/2、Ag3d3/2Maximum binding energies at 368.2eV and 374.2eV indicate Ag0；Ag3d5/2、Ag3d3/2Maximum binding energies at 367.8eV and 373.8eV indicate Ag+The method of (1); 368.1eV and 374.1eV, closer to Ag, were obtained by internal standard method (calibrated against 197.8eV of the peak of Cl2p spectrum of the metal chloride in the sample), and by fitting0The reference peak position of (2). The spectrum of Cl2p and the spectrum of Ag3d of sample 2 are shown in fig. 9 and 10, respectively.
The XRD method confirms the Ag valence state: the XRD test result of the sample 1 is shown in figures 11-12, and the phase of silver-containing crystals contained in the sample is matched by using PDF database search, so that the elementary silver crystals are obtained by using the following main components: silver (Ag, card No. 01-073-6977, Cubic). The XPS result is consistent with the XRD result, and the accuracy of the chemical state of Ag element of the silver-containing dressing is further confirmed by an internal standard calibration method during XPS analysis.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for characterizing the chemical state of silver element in a silver-containing dressing is characterized by comprising the following steps:
(1) confirming the XPS instrument state;
(2) confirming the charge neutralization state;
(3) determining the judgment basis of the reference peak: ag3d5/2、Ag3d3/2Maximum binding energies at 368.2eV and 374.2eV indicate elemental silver Ag0；Ag3d5/2、Ag3d3/2Maximum binding energy at 367.8eV and 373.8eV indicates monovalent silver ions Ag+；
(4) Testing XPS data of the AgCl reference sample to obtain a peak position P of a metal chloride Cl2P spectrum peak;
(5) preparing a silver-containing dressing sample, testing XPS data, carrying out background deduction through XPS data processing software, calibrating the XPS data of the silver-containing dressing sample according to the peak position P of a spectrum peak of metal chloride Cl2P, and obtaining Ag3d of Ag element in the dressing through fitting5/2、Ag3d3/2The position of the maximum binding energy is determined according to the judgment in the step (3) and is combined with Ag3d of the Ag element in the dressing5/2、Ag3d3/2The valence state of Ag corresponding to the reference peak with the position of the maximum binding energy closer is determined as the valence state of Ag element in the dressing.
2. The method for characterizing the chemical state of silver element in silver-containing dressing according to claim 1, wherein the XPS instrument status confirmation of step (1) is specifically: and (3) calibrating the XPS instrument by using an energy scale standard substance of an X-ray photoelectron spectrometer to ensure that the difference between the actual measurement result and the reference peak position is less than 0.1 eV.
3. The method according to claim 2, wherein the XPS instrument is calibrated by using an energy scale standard substance of an X-ray photoelectron spectrometer, and the method comprises the following steps: according to the requirements of the national standard GB/T22571-2017, the instrument is calibrated by using an energy scale standard substance of an X-ray photoelectron spectrometer.
4. The method for characterizing the chemical state of silver element in silver-containing dressing according to claim 3, wherein the standard substance is Au, Ag or Cu foil.
5. The method for characterizing the chemical state of silver element in silver-containing dressing according to claim 1, wherein the charge neutralization state confirmation in the step (2) is specifically as follows: testing the insulation samples PET and MgO samples by using an XPS instrument to obtain a C1s spectrum of the insulation sample PET and a Mg1s spectrum in the MgO sample;
according to the C1s spectrum of the insulation sample PET and the Mg1s spectrum of the MgO sample, whether the content ratio of three chemical states of C-C, C-O, C-O in the insulation sample PET is close to 3 is judged: 1: 1; if not, adjusting the state of the XPS instrument according to the operating rules of X-ray photoelectron spectrometer instrument calibration owned by the manufacturer;
judging whether the peak position of the Mg1s spectrum in the MgO sample is close to the theoretical peak position; if not, adjusting the state of the XPS instrument according to the operating rules of X-ray photoelectron spectrometer instrument calibration owned by the manufacturer.
6. The method for characterizing the chemical state of silver element in silver-containing dressing according to claim 5, wherein said determining whether the content of three chemical states, C-C, C ═ O, C-O, in the insulation sample PET is close to 3: 1: 1, specifically: judging whether the content of three chemical states of C-C, C-O, C-O in the PET of the insulation sample is 3: (0.95-1.05): (0.95-1.05);
judging whether the peak position of the Mg1s spectrum in the MgO sample is close to the theoretical peak position, specifically:
and judging whether the difference between the peak position of the Mg1s spectrum in the MgO sample and the theoretical peak position is less than 0.1 eV.
7. The method for characterizing the chemical state of silver element in silver-containing dressing according to claim 1, wherein the peak position P of the spectrum peak of metal chloride Cl2P is 197.8 eV.
8. The method for characterizing the chemical state of silver element in silver-containing dressing according to claim 1, wherein the preparing silver-containing dressing sample in the step (5) is specifically as follows: randomly selecting 1 position by using a clean scissors and shearing out a sample to be detected with a proper size.
9. The method for chemical state characterization of silver element in silver-containing dressing according to claim 1, wherein the testing XPS data of step (5) is specifically:
fixing a silver-containing dressing sample on a sample table, vacuumizing, and randomly selecting a position for data acquisition after the vacuum meets the requirement; acquisition parameters were 650 microns spot, standard mode neutralization gun.
10. The method for characterizing the chemical state of silver element in silver-containing dressing according to claim 1, wherein the XPS data processing software of step (5) is Avantage software.
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