2022 Vol. 28, No. 2

Zhejiang Major Scientific Research Instruments Open and Shared Platform-Column on Electron Microscopy
Characterization of B-Site 1∶2 Ordering Structure for Ba(B′1/3B″2/3)O3 Perovskites Along <113>c Zone Axis by Transmission Electron Microscopy
MA Pian-pian, LIU Guan-fu, QIAO Yin, XU Ren-hao
2022, 28(2): 113-117. doi: 10.16495/j.1006-3757.2022.02.001
Abstract(143) HTML (57) PDF(99)
A new zone axis (< 113>c) has been provided to characterize the 1∶2 ordering structure of Ba(B′1/3B″2/3)O3 (B′ = Zn2+, Mg2+, Co2+ or Ni2+, B″ = Ta5+ or Nb5+) perovskite by transmission electron microscopic (TEM) observation, and the corresponding atomic architecture of ordered perovskites has also been studied firstly. The 1∶2 ordering structure was revealed by the ±1/3{112}-type superlattice spots in the selected area electron diffraction (SAED) pattern. The corresponding high resolution transmission electron microscopic (HRTEM) image clearly displayed the ordering domain size and atomic structure. The composition contrast in HRTEM image matched well with the atomic architecture, further confirmed the 1∶2 ordering structure along < 113>c zone axis.
Characterization on Cellular Structure of SmCo Magnets During Isothermal Aging Using Transmission Electron Microscopy
WU Hai-chen, LIU Zhuang, WANG Xin-ming, CHEN Guo-xin, LU Huan-ming
2022, 28(2): 118-124. doi: 10.16495/j.1006-3757.2022.02.002
Abstract(108) HTML (31) PDF(44)
The magnetic properties of SmCo magnets are closely related to its unique cellular structure, and the isothermal aging process is the main stage of the formation of the cellular structure. The microstructure evolution of 2:17-type SmCo magnets during isothermal aging were characterized using transmission electron microscopy (TEM), and the TEM analysis method of cellular structure was described. The results showed that via selected area electron diffraction (SAED) and dark field analyses under certain zone axis, nanoscale short-range ordered micro-domains in the solution precursor and the embryos of cellular structure at the early stage of aging can be characterized. Combining high resolution transmission electron microscopy (HRTEM), the ordering transformation of 2:17R phase and the growth of cellular structure can be further analyzed, and a composite structure containing 1:5H, 2:17R and 1:3R phases are formed when the isothermal aging process is completed.
Principle and Practice of Conductive Epoxy Resin to Eliminate Charging Problem in Scanning Electron Microscope Images
PENG Yu, ZHANG Zhi-heng, AN Ting, QIAN Kuang-liang
2022, 28(2): 125-131. doi: 10.16495/j.1006-3757.2022.02.003
Abstract(105) HTML (38) PDF(17)
Charging problem often causes the artifacts such as uneven brightness, stripes, etc. on scanning electron microscopic (SEM) images. A method was proposed to eliminate the charging problems of samples with lower strength and porous loose structures by impregnating the samples in the conductive epoxy resin. The adaptability of this solution and the conventional method for the three lower strength and porous loose structural samples, namely the fiber reinforced concrete exposing to high temperature of 1 000 ℃, ceramic soil and archology soil of Henan Shuanghuaishu archeological site, were comparatively studied. The results showed that samples impregnated in the copper powder mixed conductive epoxy resin can effectively eliminate the charging problem induced artifacts of the SEM images. While, samples prepared by the traditional method showed severely charging artifacts. By improving the thickness of conductive layer not only can not reduce the charging problem, but also cover the nano- and micro-structure. The causes of the charging problem caused by the traditional sample preparation method and the improvement principle of the conductive epoxy resin on the charging problem were analyzed.
Progress in Characterization of Controlled Release Microspheres Using Scanning Electron Microscope
CHEN Chao, FAN Hai-li, CAI Zhi-wei, ZHANG Chuan-jie
2022, 28(2): 132-138. doi: 10.16495/j.1006-3757.2022.02.004
Abstract(74) HTML (31) PDF(19)
The important applications of scanning electron microscopy (SEM) in the characterization of controlled release microspheres are reviewed. The SEM method was used to characterize the microspheres, and the SEM-based automatic particle shape and size analysis software was used to perform statistical analysis of the microspheres, and the key application scenarios of SEM in the scientific research or development of microspheres were summarized. Microspheres are a type of formulation that is highly dependent on structure, and its performance and therapeutic effects are largely determined by their microscopic features such as structure and porosity. The size, particle size distribution and shape of microspheres play a decisive role in the drug release. Due to the characteristics of high drug loading, the interbatch consistency of microspheres is particularly important. Image analysis tools are of great significance for the characterization of interbatch consistency. SEM has the advantage of what you see is what you get, and can quickly evaluate the particle size, shape and surface roughness of microspheres intuitively. The results showed that the SEM has a wide application value in the production control and development of microspheres, and provides an advanced characterization tool for research and development of this type of preparation.
Synthesis of BiVO4 by pH-Controlled Hydrothermal Method and Visible-Light Catalytic Degradation of Methyl Orange
QIN Yu-jiao, JIANG Qi-rui, ZHANG Zhi-zhi, WANG Lin-xia
2022, 28(2): 139-143. doi: 10.16495/j.1006-3757.2022.02.005
Abstract(74) HTML (37) PDF(15)
Bismuth vanadate (BiVO4) was synthesized by a hydrothermal method with bismuth nitrate as the Bi source and ammonium metavanadate as the V source, and sodium acetate (NaAc) was used to adjust the pH. The structure and morphology of the product were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The photocatalytic performance of BiVO4 on methyl orange (MO) was investigated under visible-light. The results showed that BiVO4, synthesized at a pH value of 6.0, had a better photocatalytic performance. The degradation rate of MO reached 98.4% after 5 h, and the degradation rate of MO still maintained at over 95% after five cycles. Due to the excellent photocatalytic activity and stability of BiVO4, BiVO4 has a potential application in wastewater treatment.
New Achievement
Degradation of Remazol Brilliant Blue KN-R by Microwave-Assisted Fenton Method Based on Response Surface Optimization
LIN Xiao-sen, XUE Xiang-hang, DONG Hui-min, FANG Shu-bing, DING Mei-qi, LAI Zi-xuan, CHEN Yi-ting
2022, 28(2): 144-152. doi: 10.16495/j.1006-3757.2022.02.006
Abstract(83) HTML (46) PDF(13)
Taking Remazol Brilliant Blue KN-R as the degradation target, the microwave-assisted Fenton degradation method was optimized by a single factor and response surface methodology. The concentration of FeSO4·7H2O, the dosage of 30% H2O2, pH value, microwave temperature and microwave time were investigated, and the process conditions were optimized by the response surface analysis. When the concentration of Fe2+ was 0.10 mmol/L, the dosage of 30% H2O2 was 1.74 mL/L, the microwave power was 222 W, the microwave time was 6 min, and the standing time was 40 min, the results showed that the decolorization rate of Remazol Brilliant Blue KN-R could reach 95.26%.
Common Problems and Error Analysis of High-Temperature Specific Heat Capacity Tests
JIAO Yang, LIU Chun-feng, WANG Xiao-peng, SUN Zhao-yuan, YU Jian-xin
2022, 28(2): 153-158. doi: 10.16495/j.1006-3757.2022.02.007
Abstract(45) HTML (63) PDF(10)
The common problems and causations for errors during high-temperature specific heat capacity tests by the simultaneous thermal analyzer (STA449F3) were analyzed. The specific heat capacity was tested using a three-step method with differential scanning calorimetry. The results showed that the errors between confirmed and tested values can be decreased by improving the instrument stability and heating rate. Furthermore, if the conventional one-stage temperature rising test was divided into several narrow temperature ranges, then the accuracy of high-temperature specific heat capacity tests was improved.
Instrument Management
Operation Management and Open Sharing of Mass Spectrometer Platform
LU Qiao-mei
2022, 28(2): 159-162. doi: 10.16495/j.1006-3757.2022.02.008
Abstract(90) HTML (38) PDF(12)
Mass spectrometry (MS) is an important technology in modern instrumental analysis. Taking the MS platform of Fujian College Association Instrumental Analysis Center of Fuzhou University as an example, the basic configuration, test services and management status of MS are introduced. The open sharing of MS and exiting problems have been discussed in detail. It is hoped to provide some references to other similar large instruments on their open sharing and scientific management.
Thoughts on Promotion of Use Efficiency by Professional Technical Training of Large-Scale Scientific Instruments
ZHANG Li-na, YANG Juan, WU Ai-hua, BAO Yu-ming, WU Xiang-yun, SUN Ying-lu, HAN Yu-gang
2022, 28(2): 163-166. doi: 10.16495/j.1006-3757.2022.02.009
Abstract(82) HTML (28) PDF(9)
Large-scale scientific instruments are an important basis for scientific research and training of technical personnel, professional technical training is an important way to promote the use efficiency of large-scale scientific instruments. In order to further improve the training effect, basic skill training, peer technical exchange training and advanced training of technological innovation should be strengthened.
Zhejiang Major Scientific Research Instruments Open and Shared Platform-Column on Major Scientific Research Instruments Open and Shared Management Research
Study on Open Sharing Operation Mechanism of Large-Scale Scientific Instruments in Colleges and Universities
QI Wen-tao, CHEN Pan, GAO ran
2022, 28(2): 167-172. doi: 10.16495/j.1006-3757.2022.02.010
Abstract(93) HTML (32) PDF(14)
With the rapid development of domestic higher education, the national investment in higher education is increasing year by year, the scope of colleges and universities is becoming larger and larger, and the large-scale scientific instruments purchased by colleges and universities are also increasing. How to purchase large-scale scientific instruments scientifically, and reduce repeated investment and improve the opening rate and utilization rate of large-scale scientific instruments are a thorny problem faced by many colleges and universities in China. In view of the current situation and existing problems of large-scale scientific instruments management in colleges and universities, an open and shared operation mechanism suitable for these instruments in colleges and universities from the aspects of perfecting the system, changing ideas, investing fund, management means and talent team was established, so as to improve the efficiency of large-scale scientific instruments and give full play to the performance of asset use.
Exploration of Importance and Construction Initiatives of Quality Management System in Instrumental Analysis Center of Universities and Research Institutes
ZHANG Li, LI Zi-hou, CHEN Bo, JIA Ya-ru, QI Shu-yan
2022, 28(2): 173-178. doi: 10.16495/j.1006-3757.2022.02.011
Abstract(74) HTML (28) PDF(12)
There are a large number of high-precision instruments and equipments, and interdisciplinary talents in the instrumental analysis center of universities and research institutes. Therefore, vigorously promoting the construction of quality management system not only can strengthen the support for basic research, but also play an important role in improving product quality, optimizing and upgrading industries, and promoting high-quality economic and social development. The importance of quality management system construction is analyzed from several aspects of open sharing of instruments, basic support, and guiding industrial transformation and upgrading. From the aspects of attaching importance to leadership, attaching equal importance to quality and technical supervisors, strengthening external training, cultivating employees' sense of ownership and enthusiasm, and attaching importance to internal audit and management review, the important measures for the construction of the quality management system are expounded.
Application Progress of Ion Chromatography in Analysis of Chemical Components of Traditional Chinese Medicine
XIE Dong-mei, WEI Han-ting, WANG Ning-li, LIU Jian-fei, GUO Mei, DI Duo-long
2022, 28(2): 179-187. doi: 10.16495/j.1006-3757.2022.02.012
Abstract(74) HTML (29) PDF(13)
As a new type of high performance liquid chromatographic technology, ion chromatography (IC) was initially mainly used to determine the content of anions and cations in samples. Ion chromatography has the advantages of simple operation, high sensitivity and good selectivity. In recent years, ion chromatography has been widely used in energy, environment, geology, food, medicine and other fields. The recent research progress of ion chromatography in traditional Chinese medicines such as metal ions, inorganic anions, organic acids, sugars were summarized in order to provide a reference for the study of ion chromatography in the analysis of chemical components of traditional Chinese medicine.
Research Progress of Illegally Added Chemical Medicines and Detection in Chinese Patent Medicines and Health Foods for Regulating Three-Hypers
LI Wen-bin, ZHANG Ping, XU Ying
2022, 28(2): 188-197. doi: 10.16495/j.1006-3757.2022.02.013
Abstract(62) HTML (32) PDF(7)
Hyperglycemia, hypertension and hyperlipemia, collectively known as the "three-hypers", have already become the common diseases that threaten people's health. Chinese patent medicines and health food are more and more frequently used in the daily prevention and treatment of these diseases. However, some chemical substances have been illegally added for profit, causing safety hazards to patients. The types of illegally added chemical medicines in Chinese patent medicines and health foods that regulate "three-hypers" in recent years were summarized, and the research situation of the national standard supplementary testing methods and other analysis methods for these of illegally added medicines were introduced. Finally, according to the current situation of illegal addition, further research directions are analyzed in order to provide reference for the detection on illegal addition.
Exchange Maintenance
Determination of 30 Trace Elements in Blood by Microwave Digestion-Inductively Coupled Plasma-Mass Spectrometry
HUO Ting, MAO Bao-hong, LI Ya-li, REN Wei
2022, 28(2): 198-204. doi: 10.16495/j.1006-3757.2022.02.014
Abstract(82) HTML (31) PDF(11)
The method of determining 30 trace elements in blood has been developed using the microwave digestion-inductively coupled plasma-mass spectrometry. The samples were pretreated with a nitric acid-hydrogen peroxide mixed system with microwave digestion, and then diluted to be determined by inductively coupled plasma-mass spectrometry (ICP-MS). The contents of copper (Cu), lead (Pb), zinc (Zn), silver (Ag), barium (Ba), tin (Sn), nickel (Ni), cobalt (Co), vanadium (V), antimony (Sb), thallium (Tl), mercury (Hg), manganese (Mn), molybdenum (Mo), selenium (Se), chromium (Cr), cadmium (Cd), thorium (Th), titanium (Ti), aluminum (Al), arsenic (As), iron (Fe), calcium (Ca), gallium (Ga), strontium (Sr), lithium (Li), magnesium (Mg), beryllium (Be), sodium (Na) and potassium (K) in the whole blood were determined. The sample pretreatment process and all the instrument parameters were optimized. The matrix interference effect was reduced by the internal standard correction method. The results indicated that all the determined elements were in a good linear relationship with the response abundance of mass spectrometry in the corresponding concentration range. The detection precision was 0.142%~12.856%. The method has the advantages of simple, accurate and rapid, and is suitable for the accurate determination of the contents of various trace elements in the whole blood.
Determination of Nicotine in Tobacco Concrete by Gas Chromatography
KEN Sheng-ye, DUAN Qin, SU Dan-dan, YANG Yi, TIAN Fei-yu, YANG Xue-yan
2022, 28(2): 205-209. doi: 10.16495/j.1006-3757.2022.02.015
Abstract(60) HTML (33) PDF(11)
A gas chromatography-flame ionization (GC-FID) method has been developed for the determination of nicotine in the tobacco concrete using 2-methylquinoline as the internal standards, five tobacco concrete samples were determined. The results showed that the limit of detection and limit of quantitation were 0.27 mg/g and 0.89 mg/g, respectively. The recoveries were 95.00%~98.58%. The contents of nicotine in the samples ranged from 19.66~54.97 mg/g. The method is easy, sensitive and accurate, and is suitable for the determination of nicotine in the tobacco concrete.
Test and Study on Inner Surface Tolerance of Drug Packaging Materials for Glass Injection
2022, 28(2): 210-221. doi: 10.16495/j.1006-3757.2022.02.016
Abstract(60) HTML (44) PDF(7)
In order to screen out a fast and effective method for the detection of glass flake, a test method for the tolerance of the inner surface of glass has been initially established for the reference of drug research and development personnel. Visual inspection, methylene blue staining test, insoluble particles, scanning electron microscope and ion detection were used to investigate the inner surface tolerance of drug packaging materials for glass injection from different angles. The inner surface tolerance of glass ampoules was stronger than that of glass injection bottles, the inner surface tolerance of medium borosilicate glass ampoules was better than that of low borosilicate glass ampoules, and the inner surface tolerance of sodium calcium glass infusion bottles was the worst. The corrosion ability of NaOH solution to glass containers was much stronger than the other four corrosion solutions, and the higher the concentration of NaOH, the stronger the corrosion ability. Five different detection methods were used for the investigation. From the different angles, it was found that the shape and material of glass, the property, concentration and time of the corrosion solution affected the tolerance of the inner surface of glass. The five methods have their own advantages and disadvantages, which can be used for reference and selection by drug developers when screening glass packaging materials in the early stage of drug development.
Determination and Relationship of Ammonia Nitrogen, Nitrite Nitrogen, Nitrate Nitrogen and Total Nitrogen in Upstream Reservoir Water
ZHAO Wen-bin
2022, 28(2): 222-227. doi: 10.16495/j.1006-3757.2022.02.017
Abstract(70) HTML (27) PDF(7)
The total nitrogen, nitrate nitrogen, ammonia nitrogen, and nitrite nitrogen in the upstream reservoir water were determined by the spectrophotometry. The contents of total nitrogen, nitrate nitrogen, ammonia nitrogen, and nitrite nitrogen in the samples collected from the fixed monitoring point of the upstream reservoir in recent two years were determined using the ultraviolet spectrophotometry. The test results were analyzed and compared, and the relationships among the total nitrogen, nitrate nitrogen, ammonia nitrogen, and nitrite nitrogen in the upstream reservoir water were discussed, thus a certain reference for the data analysis and comprehensive evaluation of water quality data in upstream reservoirs is provided.
Troubleshoot Maintenance
Fault Analysis and Troubleshooting of Two Cases of HydraII C Automatic Mercury Analyzer
WANG Dong, SUN Chun-xiao, WANG Wei, MA Ling, LV Xing-ming, XU Xin-zhong
2022, 28(2): 228-231. doi: 10.16495/j.1006-3757.2022.02.018
Abstract(57) HTML (30) PDF(11)
The HydraII C automatic mercury analyzer is widely used in the detection of mercury content in food, mineral products, water and coal. Through the analysis and troubleshooting of the causes of two cases of faults, a solution for the troubleshooting of automatic mercury analyzer in use is provided.