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The aim of the journal «Analysis and Testing Technology and Instruments» is to offer a platform for the publication of new technologies, new theories, new methods and new achievements in the field of analytical chemistry. It follows the guiding principles of combining technical work with academic study and applied science with basic research, and highlights on innovation.
Preparation of Biochars and Its Applications in Adsorption
DING Na-na, LIANG Jin-hua, WU Lan, ZHANG Hai-xia
2022, 28(4): 363-374.   doi: 10.16495/j.1006-3757.2022.04.001
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Pesticides, heavy metals, dyes, pharmaceuticals and personal care products are common pollutants in water. Some compounds among them are characterized by highly toxic, difficult to decomposite and long residue period, which can easily to accumulate in the food chain and endanger the human health. The treatment technologies of pollutants in water include biodegradation, chemical oxidation, membrane filtration, adsorption and photocatalytic degradation, among which adsorption is the most widely used method to remove pollutants due to its simple operation, high efficiency and less toxic by-products. Biochar has a high specific surface area, high porosity and a variety of functional groups, and has a good adsorption effect on a variety of pollutants, which plays an important role in the study of adsorption of pollutants. The preparation methods, properties and applications of biochar in pollutant adsorption were introduced in detail.
Progress on Sample Preparation of Synthetic Polymers Analysis by Matrix-Assisted Laser Desorption Ionization Time-of-Flight Mass Spectrometry
DAI Li-li
2022, 28(4): 375-383.   doi: 10.16495/j.1006-3757.2022.04.002
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Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) has irreplaceable advantages in the characterization of synthetic polymers, and provides information on the mass distribution, block length and end groups of polymers. However, sample preparation is critical for successful analysis because of the poor ionization efficiency of synthetic polymers. The research progress on sample preparation of synthetic polymers analyzed by MALDI-TOF was reviewed from three aspects: matrix, matrix additives and sample mixing methods.
Application and Research Progress on Capillary Electrophoresis for Biological Macromolecular Analysis
PENG Le, CHENG Jia-wei, LI Shu-nan, LI Wen-long
2022, 28(4): 384-391.   doi: 10.16495/j.1006-3757.2022.04.003
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The technology of capillary electrophoresis has been widely used in the field of biological macromolecular analysis in recent years because of its advantages such as high separation efficiency, small injection volume and diverse separation modes. The application of the capillary electrophoresis in the fields of biological macromolecules, such as polysaccharides, proteins, nucleic acids and lipids, were reviewed. And the problems related to this technology, such as sample preparation, capillary wall adsorption, instrument reproducibility and sensitivity, were analyzed and prospected. The purpose is to provide a reference for the application of the technology of capillary electrophoresis in the field of biological macromolecular analysis.
Modification and Test of Physical Adsorption System
CHEN Pei-li, WANG Shu-jia, CHEN Kai-yue, CHEN Xiao-li, FU Juan, SU Qiu-cheng
2022, 28(4): 392-399.   doi: 10.16495/j.1006-3757.2022.04.004
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The existed physical adsorption analysis system was functionally upgraded according to the experimental requirements and the performance of the physical adsorption analysis system. A set of pretreatment equipment for the gas adsorption method was developed to solve the current problems of insufficient degassing equipment, incomplete degassing of materials of ultra-high surface area and ultra-fine pore size, and the collapse of the internal structure of new materials such as metal-organic framework materials (MOF) and organic covalent framework materials (COF) caused by the large temperature fluctuations of the existed pretreatment equipment. A new analysis station was built to upgrade the current inefficient and cost effective testing from the single station testing to the high efficiency dual station testing. The improvement of the addition tool of liquid nitrogen, avoids the frostbite of the tester and the effect of temperature of transferring liquid nitrogen tools on the test data. Based on a large number of inorganic adsorbent tests, the physical adsorption instrument was extended to organic gas adsorbent tests such as methane, propane and methanol, the physical adsorption tests of duality adsorbents was realized and the functional range of the instrument was enhanced. The physical adsorption system and its test method were improved by the improvement of the adsorption environment device, the solution of the phenomenon of condensation in the sample tube during the adsorption process, and the avoidance of the large adsorption amount.
Preparation and Study on Electrochemical Performance of Co3O4/CeO2 Supercapacitor Electrode Materials
TANG Ming-hua, WANG Ying
2022, 28(4): 400-404.   doi: 10.16495/j.1006-3757.2022.04.005
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The wheat-leaf Co3O4/CeO2 composite electrode material has been synthesized through a hydrothermal method using cerium nitrate hexahydrate, cobalt nitrate hexahydrate and urea. And its electrochemical performance were analyzed. The experimental results showed that the Co3O4/CeO2 composite electrode material has good electrochemical reversibility and power characteristics, and its capacitive characteristics and high-current discharge characteristics are also superior, making it an ideal supercapacitor material.
Determination of R-valsartan in Valsartan Active Pharmaceutical Ingredients by Ultra Performance Convergence Chromatography
DING Jian-ying, LIU Fa-gui, WANG Hua, LIU Si-guang, LI Tie-jian, ZHANG Gui-min
2022, 28(4): 405-410.   doi: 10.16495/j.1006-3757.2022.04.006
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An analytical method based on the ultra performance convergence chromatography (UPCC) has been established for the separation and detection of the enantiomer R-valsartan in valsartan raw materials, and the main influencing factors have been discussed. A polysaccharide-derived chiral column (CHIRALPAK IC-3, 100 mm×3.0 mm, 3 μm) was used with methanol (containing 0.5% ethanolamine)∶carbon dioxide as the mobile phase and an isocratic elution at a flow rate of 1 mL/min with a detection wavelength of 230 nm and a dynamic back pressure (ABPR) of 13.79 MPa. The R-valsartan was effectively isolated in the range of 10.072~100.720 μg/mL, the linear regression equation was Y=428.910 5X−1.059 8 (r=0.998 0, n=7), the detection limit was 3.357 μg/mL, and the average recovery rate was 104.35% (n=9). The detection and analysis method of R-valsartan by UPCC was established, which is fast, efficient, economical and environmentally friendly, and provides a new method and idea for the determination of R-valsartan in valsartan raw materials.
Determination of Free Cresol Content in Tricresyl Phosphate by High Performance Liquid Chromatography
WANG Shi-ping, NIU Jing-jing, DU Ya-zhen
2022, 28(4): 411-415.   doi: 10.16495/j.1006-3757.2022.04.007
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The mass fraction of free cresol content in tricresyl phosphate has been determined using the high performance liquid chromatography (HPLC). The samples were separated and detected by HPLC with the external standard method, the optimum chromatographic conditions were obtained. The experimental results showed that the best chromatographic conditions were: a C18 column (250 mm×4.6 mm×5 μm), methanol and water as the mobile phase (volume ratio is 8∶2), the flow rate: 1.0 mL/min, detected by an UV detector, with a detection wavelength of 280 nm, the column temperature of 35 ℃, and an isocratic elution and injection volume of 10 μL. The recovery was 95.9%~98.9%, and the relative standard deviation was 1.02%~2.55%. The method has the characteristics of simple, fast and high accuracy.
Study on Extraction Method of Chlorogenic Acid from Honeysuckle
LI Hui, LU Tao-tao, CHEN Jia, ZHAO Liang, QIU Hong-deng
2022, 28(4): 416-421.   doi: 10.16495/j.1006-3757.2022.04.008
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The content of chlorogenic acid in honeysuckle was determined by high performance liquid chromatography (HPLC), the extraction conditions of chlorogenic acid from honeysuckle were optimized using a thermal reflux method and the orthogonal test was carried out. The results showed that the best extraction conditions of chlorogenic acid from honeysuckle was ethanol with a volume fraction of 80%, a solid-liquid ratio of 1∶20 (g/mL), an extraction temperature of 100 ℃, an extraction time of 2 h, and the extraction rate of chlorogenic acid was 7.1%. The method can be used for quality control, development and utilization of honeysuckle with accurate analysis, simple operation and low equipment requirements.
Determination of Ferromolybdenum Alloy by Microwave Digestion-Inductively Coupled Plasma Atomic Emission Spectrometry
ZHAO Bing-jian, ZHAO Hao-nian, ZHAO Yue, SHI Qi, LI Xiao-lin, YUAN Hui
2022, 28(4): 422-426.   doi: 10.16495/j.1006-3757.2022.04.009
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The ferromolybdenum alloy (molybdenum content 55%~65%) was determined by inductively coupled plasma atomic emission spectrometry (ICP-OES), and good linearity was obtained using the single point calibration. The sample was acidified and microwave digestion was carried out, yttrium was added as the internal standard element to reduce the influence of instrument fluctuation and the optimum emission intensity of molybdenum was measured at the analytical line of 202.030 nm. The results showed that the microwave digestion can reduce the dissolution time of the sample to 14% of the weight method, and the relative standard deviation was 0.17%~0.22%. The accuracy of the validation results for standard samples was equaled to that of the gravimetric method, which provides a reference for the ICP-OES method to detect high content components.
Determination of Pb, As, Hg, Cd, Cu in Pheretima by Inductively Coupled Plasma Mass Spectrometry
MA Yu, LI Zheng-gang, QU Han-ting, ZHAO Yan, WANG Lu-hong
2022, 28(4): 427-432.   doi: 10.16495/j.1006-3757.2022.04.010
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An Inductively coupled plasma mass spectrometry (ICP-MS) method has been set up to determine the contents of five heavy metal elements, namely lead (Pb), arsenic (As), mercury (Hg), cadmium (Cd) and copper (Cu), in different habitats and batches of Pheretima. The sample was pretreated by microwave digestion. The results showed that the linearity of the five heavy metal elements were good (r≥0.999 6), the average recoveries were in the range of 92.8%~95.2%, and the detection limits of the method were in the range of 0.0010~0.092 mg/kg. The detection method is of highly sensitive, repeatable and accurate. Five heavy metal elements were detected in samples from different habitats and batches. These five heavy metal elements of Pb, As, Hg, Cd and Cu in Pheretima need to be monitored with emphasis.
Application of Freeze Fracture Method of Cryo-Scanning Electron Microscopy in Observation of Biological Samples
HUANG Ke-rang, WANG Zhen, CHEN Lei, CUI Feng-zhan, PENG Jie-ying, ZHANG Min
2022, 28(4): 433-438.   doi: 10.16495/j.1006-3757.2022.04.011
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Cryo-scanning electron microscopy (Cryo-SEM) is a powerful tool in the life science research because of its advantages such as observing aqueous samples under high vacuum condition, high resolution, simple and rapid sample preparation, fracture etching of samples, etc. Through the surface morphology observation of biological samples using Cryo-SEM's freeze fracture method, both the surface structural information and the internal structural information of the samples can be observed. The plant samples from the upper and middle assimilated branches of Haloxylon Ammodendron and the liquid samples of whey protein fiber (WPIF) were taken as the experimental materials, and the samples were subjected to a freeze fracture treatment to observe and compared the structures of the samples before and after the freeze fracture treatment. The results showed that the chloroplasts of plant cells and the fine hairs between the cells could be observed under the test conditions of a sublimation temperature of −100 ℃, a sublimation time of 10 min, a cold platform temperature of −175 ℃, and an observation voltage of 5 kV. And the lamellar structure of medium chain triglyceride and protein fiber can be observed under the test conditions of a sublimation temperature of −100 ℃, a sublimation time of 5 min, a cold stand temperature of −175 ℃, and observation voltage of 5 kV after freeze fracture of WPIF. However, the above results could not be observed for the samples without a frozen fracture treatment.
Simultaneous Determination of 50 Prohibited Drugs in Cosmetics by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry
LIAO Wen-rong, HUANG Jian-hao
2022, 28(4): 439-450.   doi: 10.16495/j.1006-3757.2022.04.012
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A method for the quantitative analysis of 50 prohibited drugs in cosmetics by ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) has been developed. The samples were extracted with acetonitrile (containing 0.5% formic acid) by ultrasonic extraction, freezing centrifuged, and the supernatant was fixed in an ethylenediaminetetraacetic acid disodium salt solution (2 mg/L). Then the analytes were separated using a CAPCELL CORE C18 chromatographic column with mobile phase A (methanol) and mobile phase B (0.1% formic acid in water) by gradient elution, finally analyzed by positive and negative mode with electrospray ion source (ESI). The data were acquired by a multiple reactions monitoring (MRM) mode. In the mass concentration range of 10~100 ng/mL, 50 prohibited drugs showed good linear relationship with all their correlation coefficients (r) more than 0.991 0. The detection limits were within 0.05~33 ng/g, and the quantification limits were within 0.15~99 ng/g. The average recovery rates of the samples were within 87.2%~109.7% with the relative standard deviations(RSD) not greater than 10.0%. The method is simple, sensitive and reproducible, and can be used for the rapid and accurate qualitative screening and quantitative determination of 50 prohibited drugs in cosmetics.
Determination of Impurity Elements in Ruthenium Trichloride Solution by Inductively Coupled Plasma Atomic Emission Spectrometry
ZHANG Yu-de, LIU Rong-zheng, LUO Xiong, CHONG Biao, BAI Wen-gang
2022, 28(4): 451-456.   doi: 10.16495/j.1006-3757.2022.04.013
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A method for the determination of impurity elements in ruthenium trichloride solution by the inductively coupled plasma atomic emission spectrometry has been established. The ruthenium matrix was converted into ruthenium tetrachloride by adding an oxidant to volatilize the sample to eliminate the matrix interference. The experimental conditions such as oxidant, acidity and determination spectrum were optimized. The results showed that the relative standard deviations (RSD, n=7) of the determination results of each impurity element were less than 5.00%, and the spiked recovery of the method was 90.0%~106.0%. The method is of high accuracy and good repeatability, which can meet the actual production needs.
Determination of Asbestos in Cosmetics by Polarizing Microscopy and X-ray Diffractometry
ZHANG Lei, SU Fen-liang, WANG Hai-rui, HU Ji-dong
2022, 28(4): 457-462.   doi: 10.16495/j.1006-3757.2022.04.014
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Through the organic combination of a X-ray diffractometer and a polarizing microscope, a variety of asbestos can be characterized quickly, simply and accurately, which avoids the misjudgment of the test results caused by some impurity components. Then, the improved sample and standard material processing method is used to combine the K-value method with the internal standard method to quantify the asbestos accurately. The RSD of the reference strength of different asbestos were 0.17%~0.81%, which not only met the requirements of the test method, saved the testing cost, but also ensured the effectiveness of the testing results. It has a strong promotion role for the testing of asbestos.
Determination of Calcium Carbonate Content in Xiaokening Tablets by Powder X-ray Diffraction Method
ZHANG Jian-ping, SUN Qian-nan, ZHOU Xue-mei, WANG Dong
2022, 28(4): 463-468.   doi: 10.16495/j.1006-3757.2022.04.015
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The content of calcium carbonate in Xiaokening tablets has been determined by the powder X-ray diffraction (PXRD) method. The full spectrum fitting internal standard quantification method was used, with zinc oxide as the internal standard, using Cu Kα rays, the voltage was 40 kV, and the current was 45 mA, the scan type was Coupled Two Theta/Theta, the scan mode was Continuous PSD fast, and the diffraction angle (2θ) scanning range was 8 °~40 °, with a step size of 0.02 °. The PXRD pattern was obtained by scanning, and the percentage content of calcium carbonate was obtained by the internal standard quantitative analysis with a Total Pattern Solution (TOPAS) software. The methodological validation results showed that the mean spiked recovery was 98.9% [relative standard deviation (RSD) was 1.0%, n=6]. The mock samples were validated using three levels of low, middle and high, and the average recovery was 96.9% (RSD was 1.0%, n=6). The RSD of repeatability was 1.2% (n=6). The X-ray diffraction method is fast, sensitive and specific, and the full spectrum fitting internal standard quantitative method is of good accuracy and repeatability, which can solve the problem of determination of calcium carbonate content in Xiaokening tablets.
Application of Resin Embedding in Transmission Electron Microscopy
WANG Xiao-man, LIANG Zheng, LU Si
2022, 28(4): 469-472.   doi: 10.16495/j.1006-3757.2022.04.016
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In the process of embedding samples in epoxy resin, some samples are easy to float in the resin and not easy to be in fixed position, thus affecting the efficiency of ultrathin sections and the observation effect of the samples under transmission electron microscope. It is especially suitable for the rapid and efficient preparation of nanowires, rods and other cross section samples by embedding and positioning the samples easily floating in epoxy resin for many times, and then preparing the cross section samples for transmission electron microscopy through the steps of block modification and section. The method of multiple embedding is simple and practical, and the sample section prepared by ultrathin section is clearer and more complete.
Fault Analysis and Elimination of Isoprime 100 Stable Isotope Ratio Mass Spectrometer
GU Shu-bo, XU Yi, JIN Min
2022, 28(4): 473-479.   doi: 10.16495/j.1006-3757.2022.04.017
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In order to eliminate the common faults of Isoprime 100 stable isotope ratios mass spectrometer in the determination of δ13C and δ15N, the causes of the failure of leak detection, unqualified peak center detection and unsatisfactory stability of the system have been analyzed. Combined with the actual operation, the preventive measures of instrument faults were summarized from the aspects of pre-test state inspection, test process monitoring, maintenance of all components after test, etc. At the same time, troubleshooting methods were proposed for system leakage, ion source damage, mechanical pump damage, etc. By taking the above measures, the accuracy of test data is ensured, the failure rate of the instrument is reduced, the service life of the instrument is prolonged, and the timely and efficient application of the instrument in teaching and scientific research work is guaranteed.
Routine Maintenance of EVO MA 15 Tungsten Filament Scanning Electron Microscope
CHEN Xin-fang, ZHOU Jing-yun
2022, 28(4): 480-484.   doi: 10.16495/j.1006-3757.2022.04.018
Abstract(44) HTML(35) PDF(7)
The tungsten filament scanning electron microscope is of low price and maintenance cost, wide applicability of samples, and high utilization rate in various research institutions. Its routine maintenance is a necessary means to ensure the performance of tungsten filament scanning electron microscope. In addition to the conventional scanning electron microscope maintenance, there are some maintenance points that are different from other types of scanning electron microscope due to the structural characteristics of the tungsten filament scanning electron microscope. Taking EVO MA 15 tungsten filament scanning electron microscope as an example, the specific methods of routine maintenance of tungsten filament scanning electron microscope were introduced from three aspects of electron optical system, vacuum system and imaging system, so as to provide reference for pepole of the same trade.
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Supervisor: Chinese Academy of Sciences

Sponsor: Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences

Honorary Editor-in-Chief: Yu WeiLe

Editor-in-Chief: SHI Yanping

Publisher: “Analysis and Testing Technology and Instruments” Editorial Department

Address: 18 Tianshui Zhong Rd., Lanzhou 730000, China.

Postcode: 730000

Tel: 86-0931-4968280

FAX: 0931-8277088

Email: fxcs@licp.cas.cn

CN 62-1123/O6

ISSN 1006-3757

Postal Code: 54-90

Price: RMB 15/issue,RMB 60/year