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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.
Usage and Maintenance of InVia-Reflex Micro-Confocal Raman Spectrometer
LI Xue, ZHENG Zhen, HONG Guang-hui, XU Chao, CUI Xi-ping, ZENG Gang, YANG Lei
2021, 27(4): 233-239.   doi: 10.16495/j.1006-3757.2021.04.001
Abstract(42) HTML(21) PDF(9)
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Micro-confocal Raman spectrometer can be effectively used to analyze the chemical composition, microstructure, stress-strain and other characteristics of substances. As a high-frequency analysis device, it is widely used in life, medicine, food, chemistry, materials and other fields, and plays an important role in the Raman research. The working principle and usage of InVia-Reflex micro-confocal Raman spectrometer were introduced, and the typical problems of laser damage to samples, change of Raman spectral characteristics caused by the change of laser intensity, the hiding of Raman signal in the strong background signal were analyzed. The corresponding solutions were given. Finally, how to effectively manage and maintain the equipment were described in detail, so as to improve the use efficiency of the instrument and provide management experience for the operation of the same type of instrument.

Study on Electron Beam Induced Degradation of CL-20 Based on In Situ X-ray Photoelectron Spectroscopy-Mass Spectrometry Analysis Technique
HAO Xiao-fei, ZHU Chun-hua
2021, 27(4): 240-244.   doi: 10.16495/j.1006-3757.2021.04.002
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X-ray photoelectron spectroscopy (XPS) is one of the important methods for qualitative and semi-quantitative analysis of surface elements of materials, especially the chemical states of the elements. By connecting mass spectrometry (MS) within its analysis cavity, surface element changes and gas products can be obtained simultaneously, thus realized the in situ analysis. Based on the obvious decomposition phenomenon of explosive CL-20 under light irradiation, the changes of surface elements and gas products of CL-20 under electron beam irradiation were obtained based on XPS-MS. The experimental results showed that with the increase of irradiation time, the peak intensity of N and O decreased rapidly, while the peak of gaseous products can be obtained effectively by mass spectrometry. The result proved that XPS-MS analysis technology can effectively realize the in situ tracking of solid state electron beam induced degradation reaction.
Principle and Application of TAG High-Temperature Oxidation and Corrosion Analyzer
JIAO Yang, LIU Chun-feng, SUN Zhao-yuan, WANG Xiao-peng, YU Jian-xin, CHEN Xin
2021, 27(4): 245-251.   doi: 10.16495/j.1006-3757.2021.04.003
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The characteristics, principle and application of TAG high-temperature oxidation and corrosion analyzer were introduced. The TAG high-temperature oxidation and corrosion analyzer can realize the in situ testing under controllable atmosphere (dry, wet and corrosive) and controllable temperature conditions. The design of double furnace body minimized the interference of the buoyancy effect. Moreover, the suspension sample was designed to contact the whole atmosphere, which can accurately measure the small mass change. The TAG high-temperature oxidation and corrosion analyzer can be used to study the decomposition of inorganic and organic materials at high temperature. It can also apply to investigate the oxidation and corrosion mechanisms of metals and ceramics under single or multiple atmospheres.
Comparation of Three Measuring Methods for Thermodynamic Stability of Protein
ZHOU Cui-yan, YU Min-da, LI Wen-qi
2021, 27(4): 252-259.   doi: 10.16495/j.1006-3757.2021.04.004
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Thermodynamic stability describes the tendency of protein unfolding, generally showed by the melting temperature (Tm) at which 50% of the protein is unfolded. In order to compare the detection characteristics and effects of different methods, differential scanning calorimetry (DSC), circular dichroism (CD) and differential scanning fluorimetry (DSF) were used to measure the Tm values of five proteins with different structural feature. The Tm values of different proteins gained using DSC, CD and DSF methods were compared. In summary, the Tm values of the same protein measured by the three methods were rather consistent, but differences were also observed. Additionally, proteins with complex structures did not show multiple Tm values.
Preparation of Molecular Imprinting on Surface of Magnetic Metal-Organic Framework and Application of Enrichment of 2, 4-Dichlorophenoxyacetic Acid in Vegetables Samples
MA Min-rui, ZHU Xin-yue, LIU Xiao-yan, ZHANG Hai-xia
2021, 27(4): 260-272.   doi: 10.16495/j.1006-3757.2021.04.005
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The magnetic molecular-imprinted material Fe3O4@ZIF-MIP was prepared by a sol-gel method at room temperature with magnetic metal-organic frameworks as the matrixes, 2, 4-dichlophenol as the pseudotemplate molecule and 3-aminopropyltriethoxysilane as the functional monomer. The molecular-imprinted materials were characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption. The adsorption capacity of Fe3O4@ZIF-MIP was 120.31 mg/g at a concentration of 500 μg/mL of 2, 4-phenoxyacetic acid, and the blotting factor was 3.64, the properties of the material remained above 95% after repeated use for 6 times, and the established method is suitable for the enrichment of low content 2, 4-dichlorophenoxyacetic acid in vegetables.
Progress in Mass Spectrometer, Current Present Situation of Independent Innovation, and Open Sharing of Resources
ZHANG Li-na, WANG Jin, WU Ai-hua, GUO Zhen-xi, BAO Yu-ming, HUANG Chun-juan, ZHANG Wen-juan, HAN Yu-gang
2021, 27(4): 273-277.   doi: 10.16495/j.1006-3757.2021.04.006
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The history of development of mass spectrometer was summarized, and the independent innovation of mass spectrometer in China was summarized. Since 2011, researchers have successfully developed several fairly mature high resolution mass spectrometer, which has effectively promoted the development of independent innovational instruments in China. Based on the analysis of the evaluation data of the open sharing of large-scale instruments, the open and sharing use of mass spectrometer in universities and research institutes were analyzed.
Effect of Sample Preparation Methods on X-ray Photoelectron Spectroscopic Testing Results of Solid Powder
XU Jun, XU Jian-fang, ZHOU Wei-dong
2021, 27(4): 278-285.   doi: 10.16495/j.1006-3757.2021.04.007
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In order to obtain accurate and high-resolution X-ray photoelectron spectroscopic (XPS) data, different sample preparation methods were used to study the XPS testing results of different types of conductive powders, non-conductive powders and mixed powders. The effect of different sample preparation methods on testing results were discussed from the aspects of half-peak width, charge, authenticity, sample preparation efficiency and data processing. The results showed that the adhesive sample preparation was better than the indium chip sample preparation for conductive powders and non-conductive powders, and the carbon conductive tape was better. For mixed samples, the results of Scotch double-sided tape were better than those of the other three sample preparation methods. In addition, the indium chip sample preparation can be used as a reference method for the charge correction in data processing.
Migration and Safety Evaluation of Bromide in Bromobutyl Rubber Stopper for Freeze-Dried Powder Injection
MA Yan, HE Xiao-ling, HUANG Wu-ping, YU Qiu-ling, MOU Qiong
2021, 27(4): 286-291.   doi: 10.16495/j.1006-3757.2021.04.008
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The extraction method of bromide in bromobutyl rubber stopper has been established, and the leaching level of bromide in freeze-dried powder was investigated. A chromatographic column IonPac AS 11-H (4.0 mm×250 mm) and a guard column IonPac AS 11-HC (4.0 mm×50 mm), and a 24 mmol/L potassium hydroxide solution were used for the isocratic elution. Bromide was detected by suppressed conductivity with an AERS 500(4 mm) suppressor at a current of 60 mA. The column temperature was 30 ℃ and the flow rate was 1.0 mL/min. The calibration curve showed a good linearity (r=0.999 9) in the range of 0.2~10.0 mg/L and the limit detection (LOD) was 0.007 mg/L. The brominated butyl rubber stopper was extracted by 30% isopropanol aqueous solution at 80 ℃ for 7 hours. The freeze-dried powder was redissolved in ultrapure water to detect the amount of bromide migration directivity. The average recoveries of the migration test were between 98.1% and 104.3%, and the relative standard deviations (RSD, n=6) were from 2.9% to 4.3%. The method can be used for the detection of real samples in the compatibility test of packaging materials.
Determination of Main Products of Direct Hydroalkylation of Benzene by Gas Chromatography
CHEN Shi-ping, JING Xiao-lian, LIN Li-qin, CHEN Le-jun, ZHU Lin-xi, WANG Xing-zhu
2021, 27(4): 292-296.   doi: 10.16495/j.1006-3757.2021.04.009
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A gas chromatographic analysis method for the products from direct hydroalkylation of benzene has been established. The chromatographic conditions were as follows: AT.FFAP column (50 m×0.32 mm×0.50 μm), hydrogen flame detector, split ratio: 50∶1, injector temperature: 180 ℃, detector temperature: 200 ℃, column temperature programmed: initial temperature was kept at 80 ℃ for 4 min, then heated to 180 ℃ at 15 ℃/min and kept for 8 min. The injection volume was 0.2 μL. Under these conditions, methyl cyclopentane, cyclohexane, cyclohexene, benzene, cyclohexylbenzene and dicyclohexylbenzene were effectively separated, and the detection limits were 1.4×10-7, 1.4×10-7, 1.4×10-7, 1.6×10-7, 2.7×10-7 and 5.3×10-6 mg/L, respectively, the limits of detection and quantification were low. The linear relationship of all substances was good. The correlation coefficient r was above 0.996. The method is simple and accurate, and can be used for the determination direct hydroalkylation of benzene of the reaction products.
Detection of 4 Fungicides in Water by Solid Phase Extraction- Ultra-High Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry
YE Lin, GE Yan, SHAO Juan, ZHANG Yang-yang
2021, 27(4): 297-302.   doi: 10.16495/j.1006-3757.2021.04.010
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A solid phase extraction-ultra-high performance liquid chromatography-triple quadrupole mass spectrometry method has been established to detect four fungicides (azoxystrobin, tebuconazole, pyrazole ether ester and oxime ester) in water. The fungicides in water samples were enriched on a HLB solid phase extraction column, separated on a C18 chromatographic column, and analyzed by ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS) with an external standard. The detection method was a multiple reaction monitoring (MRM). And the effects of pH, elution solvent, and the amount of elution solvent on the extraction effect were investigated. The experimental quantitative analysis adopted the external standard method. The four fungicides displayed a good linear relationship in the concentration range of 0.10~50.0 μg/L, the detection limit was 0.004~0.095 μg/L, the recoveries were 68.7%~95.4%, and the relative standard deviations (n=5) were less than 10%. Using the method to detect fungicides is simple, fast, accurate, and sensitive.
Determination of Vitamin C in Nanking Cherry by High Performance Liquid Chromatography
XU Ya-qian, ZHENG Long-hua, YANG Fan, JIANG Yu-ting, CAO Yu-zhen, TIAN Chao, ZHANG Xiao-yan
2021, 27(4): 303-308.   doi: 10.16495/j.1006-3757.2021.04.011
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A high performance liquid chromatography (HPLC) method was established for the simultaneous determination of L-ascorbic acid and D-isoascorbic acid. Under the chromatographic conditions, 0.05 mol/L phosphoric acid solution∶methanol (98∶2) was used as the mobile phase, the ultraviolet detection wavelength was 245 nm, the column temperature was 25 ℃, and the flow rate was 0.70 mL/min. The standard curves of L-ascorbic acid and D-isoascorbic acid displayed a good linear relationship (r=1.0). Precision (RSD) was 0.6%. The recoveries of L-ascorbic acid and D-isoascorbic acid were 90.83%~92.52% and 91.93%~92.99%, respectively. The method has the advantages of simple operation, fast extraction, high sensitivity and good recovery. The content of L-ascorbic acid was 8.24 mg/100 g, and no D-isoascorbic acid was detected. The method can be used to determine the contents of L-ascorbic acid and D-isoascorbic acid in other fruits and vegetables similar to Nanking cherry.
Determination of Trifluralin in Water by Gas Chromatography with Electron Capture Detector
ZHANG Jia-chen, WANG Jin-yu, DING You
2021, 27(4): 309-313.   doi: 10.16495/j.1006-3757.2021.04.012
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A method of determination of Trifluralin in water by gas chromatography has been established. Trifluralin in water was extracted by the liquid-liquid extraction (LLE) and solid phase extraction (SPE) respectively. The LLE method is easy to operate and saves time. The SPE method can realize automatic processing and save labor. These two pre-treatment methods have their own advantages. Then the enriched organic phase was separated on a HP-5 column, and an electron capture detector (ECD) was used in the measurement. The result showed that when the mass concentration of Trifluralin in water was in the range of 0.05~1.0 μg/L, the correlation coefficient of the regression equation of working curves was higher than 0.999. The detection limit (3 S/N) was 0.02 μg/L. The recovery and precision were tested under two different concentration levels. The recovery and relative standard deviation were obtained in the range of 84.0%~98.0% and 3.0%~5.8%, respectively.
Determination of Gold by Inductively Coupled Plasma Atomic Emission Spectrometry in Cyaniding Deplating Solution Treated by Alkaline Chlorination and Tellurium Co-Precipitation Method
YI Bing-zhi, CHENG Jian-feng, YAO Tian-tian, SUN Yu-jiao, PENG Jin-xin
2021, 27(4): 314-320.   doi: 10.16495/j.1006-3757.2021.04.013
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The alkaline chlorination method was used to oxidize and decompose cyanide, and the tellurium co-precipitation method was used for the separation and enrichment of gold in the cyanide-breaking solution. The method of determination of gold in cyaniding deplating solution by inductively coupled plasma atomic emission spectrometry (ICP-AES) has been established. Under alkaline conditions, sodium hypochlorite was used to oxidize and decompose the cyanide in the deplating solution and convert it into carbon dioxide and nitrogen: sodium sulfite solution was used to neutralize the residual chlorine in the cyanide-breaking solution and eliminate the effect of oxides on the cyanide test package. The cyanide-breaking effect of deplating solution can be easily and quickly judged. In the acid medium of 3.6 mol/L hydrochloric acid, the 12.5 mL tellurium solution of 2.5 g/L and 11 mL stannous chloride solution of 1mol/L could quantitatively precipitate 5~500 μg Au, and 50 times excess [ion/Au(w/w)] interfering ions does not interfere determination. The mass concentration of gold was linear with its emission intensity in the range of 0.05~25.00 mg/L. The calibration equation was y=46.487x+0.343, the correlation coefficient (r) was greater than 0.999 9, and the detection limit was 0.004 4 mg/L. The accuracy of the actual sample was investigated, the relative standard deviation (RSD, n=7) was less than 1.0%, and the recoveries were 96.9%~103.1%. The measurement result of experiment method is in good agreement with the comparison of the fire assay method.
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Copyright Information

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