ABSTRACT
ObjectiveTo analyze the polarized light microscopic characteristics， the composition of physical phases and their relative contents of Maifanitum from different origins， and to establish the Fourier characteristic fingerprint of Maifanitum powder crystals by X-ray diffraction（XRD）. MethodA total of 26 batches of Maifanitum samples were selected， and the microscopic characteristics of the sample powders and grinding flakes were observed by polarized light microscopy under single polarized light and orthogonal polarized light， and the main phase compositions and their relative contents were analyzed by powder crystal XRD technique， and the XRD Fourier characteristic fingerprint of Maifanitum was established. The incident light source of XRD was Cu target Kβ radiation， the light tube voltage and light tube current were 40 kV and 40 mA， respectively， the divergence slit was 1°， the scattering slit was 1°， the receiving slit was 0.2 mm， the scanning speed was 5°·min-1 with continuous scanning and scanning range of 5-90°（2θ）， and the step length was 0.02°. ResultThe polarized light micrographs of powders and grinding flakes of Maifanitum were obtained， and the main phases were plagioclase， potassium feldspar and quartz， and a few samples also contained illite， pyrite， iron dolomite， calcite， iron amphibole and chlorite， etc. The relative total content of feldspar phases was 61.9%-82.4%， and the relative content of quartz was 12.6%-33.6%. The XRD Fourier fingerprint analysis method of Maifanitum with 13 common peaks as the characteristic fingerprint information was established， and the similarity calculated by the mean correlation coefficient method was 0.920 9-0.997 7， the similarity calculated by the mean angle cosine method was 0.940 5-0.998 4， the similarity calculated by the median correlation coefficient method was 0.921 1-0.997 5， and the similarity calculated by the median angle cosine method was 0.947 5-0.998 2. ConclusionThe polarized light microscopic identification characteristics of Maifanitum are mainly plagioclase， quartz and potassium feldspar， and the technique of powder crystal XRD Fourier fingerprint analysis can be used for the identification of Maifanitum.
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Objective: Ammonium alum is a common counterfeit of Alumen,and the processed product of ammonium alum is a common counterfeits of calcined Alumen. This paper aims to establish a method for identifying Alumen,calcined Alumen,ammonium alum and their processed products. Method: The samples were analyzed by scanning electron microscope (SEM) and X ray diffraction (XRD) in this paper. Result: Ammonium alum and Alumen showed obvious changes in morphology after processing. Both Alumen and ammonium alum showed obvious differences in morphology at×250 and×1 000 times microscope. Alumen presented irregular fragments,clear edge corners,smooth surface,scattered irregular small particles,occasional holes and longitudinal edges. Ammonium alum presented irregular clumps,blunt edges,not obvious edges and corners,uneven surface,scattered smaller and round-like particles. The difference in morphology was not obvious at×250 times microscope between Alumen and ammonium alum processed products. While at×1 000 times,the surface of calcined Alumen was uneven with coarse particles; the surface of counterfeit calcined Alumen was flat,and the coarse particle characteristics were not obvious. XRD can be used to rapidly and accurately identify the primary phase of Alumen,calcined Alumen,ammonium alum and ammonium alum processed products:KAl(SO4)2·12H2O,NH4Al(SO4)2·12H2O,KAl(SO4)2,and NH4Al(SO4)2 respectively, with 2θ angle characteristic value of 23,12,22 and 5 respectively for XRD peak. Conclusion: SEM and XRD techniques can be used for the identification of Alumen,calcined Alumen,ammonium alum and their counterfeit products.
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Objective: To establish a method by which the multi-analysis and identification on the crude and processed Pyritum (natural coppor) could be carried out. Methods: The qualitative and semi-quantitative analyses of the structure, chemical composition, and thermal stability of crude and processed Pyritum were determined by means of far-infrared (FIR) spectroscopy, X-ray diffraction (XRD) analyses, and thermogravimetric differential thermal analysis (TG-DTA). Results: FIR spectroscopy showed that processed Pyritum had the chemical composition of Fe2O3. XRD analysis indicated that in crude Pyritum, the phase was mainly made up of FeS2; however, in processed one, the more complicated phase was made up of Fe7S 8, FeO(OH), Fe2O3, and Fe3O 4, etc and appeared. Thermal analysis suggested that the phase FeS2 can be gradually decomposed, the composition structure of the processed Pyritum changed less than that of the crude one when heated from 400 to 1 000°C. Conclusion: The method of analyzing and identifying the crude and processed Pyritum is feasible.
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Objective: To optimize the including preparation for peppermint oil-β-cyclodextrin polymer (β-CDP) microsphere inclusion compound. Methods: Peppermint oil-β-CDP microsphere inclusion compound was prepared by using co-precipitation. The preparation process was optimized through the L9(34) orthogonal test design and regression analysis. Peppermint oil-β-CDP microsphere inclusion compound was characterized by infrared (IR) spectroscopy, thermogravimetric analysis (TGA), and X-ray diffraction (XRD). Results: The best technological condition was A 2B2C1D3, and the order of the influence factors was the proportion of β-CDP microsphere and water > the percentage of peppermint oil in β-CDP microsphere > inclusion temperature > inclusion time. The formation of peppermint oil β-CDP microspheres inclusion compound was proved by the results of IR, XRD, TGA analyses. Conclusion The method is reasonable and feasible.
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Objective To prepare and identify the andrographolide-hydroxypropyl-?-cyclodextrin(an- drographolide-HP-?-CD)inclusion compound.The tool ratio between andrographolide and HP-?-CD and the thermodynamic constants in inclusion were studied simultaneously.Methods The andrographolide- HP-?-CD inclusion compound was prepared with lyophilization technique.Meanwhile,the inclusion com- pound was identified by differential scanning calorimetry(DSC)methods,infrared spectrometry(IR),and X-ray diffraction(XRD),respectively.The tool ratio between host and guest moleculars and the thermo- dynamic constants during the inclusion process were also researched by phase solubility method.Results An 1:1 molar ratio inclusion complex of andrographolide with HP-?-CD could be formed at 25,35,and 45 C.The phase diagram was A_L type and the procedure of inclusion was a heat release process.Conclusion The solubility of andrographolide-HP-?-CD inclusion compound can be increased obviously by the above- mentioned preparing techniques.
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Objective To parperare and identify the irisquinone-hydroxypropyl-?-cyclodextrin (irisquinone-HP-?-CD) inclusion compound. The inclusion mechanism and mol ratio of irisquinone and HP-?-CD were studied simultaneously. Methods The irisquinone-HP-?-CD was prepared with lyophilization technique. The mol ratio between host and guest moleculars was also researched by molecular gradient and continuing variational methods in inclusion processing. At the same time, the inclusion compound was identified by X-ray diffraction (XRD) and differential scanning calorimetry (DSC) methods, respectively. Results The above-mentioned systems showed the mol ratio of HP-?-CD-irisquinone (2 : 1) and the inclusion compound enhanced remarkably the most solubilization and more combined constant of irisquinone in 25, 35, and 45℃. The lyophilized powder had been formed inclusion compound by identifying. Conclusion It is advantageous to increase the solubilization and to strengthen the stability of irisquinone by preparing inclusion compound.