分析测试技术与仪器

Design and Implementation of a Multifunctional Integrated Controller Module in Shared Development Platform of Portable Gas Chromatograph

CHEN Lian, XIAO Ying, LIU Chong-li

2017, 23(2): 63-71. doi: 10.16495/j.1006-3757.2017.02.001

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Abstract:
Based on the design concept of a shared development platform, we developed a multi-functional all-in-one controller module, consisting of a programmable logical controller(PLC), a driver module, and a signal acquisition system. Our module can be integrated directly into portable gas chromatographs (GC). Through evaluation, it was confirmed that the chromatography temperature fluctuation was ≤±0.1℃. The fluctuation RSD of 60℃/min warming-up was < 0.15%. The temperature fluctuation in the sampler inlet and detector was ≤±0.1℃ and the RSD of qualitative and quantitative repeated deviation were 0.1% and 4.6% (peak height) respectively. The temperature and humidity range in which the device works were 0~40℃ and 95% respectively. The module successfully passed the tests of sine wave and XYZ direction vibration of 25.4 mm displacement, 1.5 g acceleration and 5~200~5 Hz frequency. The application of the module to 3 new types of analytical instruments achieved desirable results. The module meets the demand of on-site and field application and features versatility, sturdiness, small volume and low power consumption.

Advances of Application of Laser Diffraction Technique of Particle Size Analysis in Pharmaceutical Quality Analysis

HAO Fu, HU Xiang-qing, BA Xiao-yu, Xu Gui-ling, Zhang Gang, LI Zhi-gang

2017, 23(2): 72-80. doi: 10.16495/j.1006-3757.2017.02.002

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Laser diffraction technique of particle size analysis was widely used in pharmaceutical quality control recently. In this review, the principle of the laser diffraction technique, normal test requirements for the instruments, influence factor for the determination, method validation and current application in pharmaceutical science fields were discussed. It provides references for the further study of pharmaceutical particle size analysis.

Ultrasonic-Assisted Extraction of Anthocyanins from RubusCorchorifolius L. f and Antioxidant Activity

WANG Yu-wei, HU Na, SUO You-rui

2017, 23(2): 81-86. doi: 10.16495/j.1006-3757.2017.02.003

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Based on single factor experiments, extraction times, extraction reagent, solid-liquid ratio, ultrasonic time were selected for the Box-Behnken central composite design. Response surface method was employed to study the effect of these factors on the yield of anthocyanins and the antioxidant activity of anthocyanins. 2, 2-diphenyl-1-picrylhydrazyl(DPPH) and 2, 2'-Azinobis-(3-ethylbenzthiazoline-6-sulphonate)(ABTS)method were used, respectively to study the antioxidant activity of anthocyanins in raspberry. The results indicated that optimal conditions were:ultrasonic extraction for 3 times, 1:46 g/mL as the ratio of liquid to solid with 44 min extraction. Under these optimized conditions, the extraction yield of anthocyanins was up to 6.79%. The clearance of DPPH was 13.68 μmol/g and the clearance of ABTS was 8.37 μmol/g. The study provides scientific and theoretical basis for the research and utilization of RubusCorchorifolius L. f.

Species Identification and Analysis of Causes of Bryophyte Bred on Earthen Archaeological Site of Tang West Market

ZHAO Gang, LI Yu-hu, XIAO Ya-ping, ZHAO Jun-ni

2017, 23(2): 87-92. doi: 10.16495/j.1006-3757.2017.02.004

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Optical microscopy and scanning electron microscopy (SEM) were used to identify bryophyte that breeds on the surface of earthen archaeological site in Tang west market, and it was identified as Hyophila setschwanica (Broth.). On this basis, X-ray diffraction (XRD) and X-ray fluorescence (XRF) were used to analyze five soil samples within the site, the results showed that the soil of the site is calcareous soil, and the soil moisture content was up to 23%, and pH was weakly alkaline. The soil environment provides a favorable condition for the reproduction of Hyophila setschwanica, leading to its widespread occurrence, which fully explained the root causes of the vigorous growth of Hyophila setschwanica, and thus provides some theoretical basis for the late effective treatment of the disease.

Ferroelectric Relaxor Behaviour of Ca、Bi Doped Ba_0.67Sr_0.33TiO₃ Ceramics

XU Jing, HE Bo

2017, 23(2): 93-99. doi: 10.16495/j.1006-3757.2017.02.005

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Ca、Bi doped Ba_0.67Sr_0.33TiO₃ ceramics were prepared using the lowcost solid phase method. The relaxor characteristics have been investigated by TEM and complex impedance spectroscopy analysis. The results showed that Ba_0.67Sr_0.33TiO₃ ceramics exhibit distinct ferroelectric relaxor behaviors by doping Ca、Bi, and with the increase of Ca、Bi content, the diffusion of the dielectric peak and the degree of relaxor characteristics also increased.

Study on Spectral Lines of Determination of Iridium in Gold Alloy Jewelry by ICP-AES

WANG Ping, LIU Xue-song, MA Xiao, SHAN Guang-qi, ZHU Pei-ming

2017, 23(2): 100-105. doi: 10.16495/j.1006-3757.2017.02.006

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ICP-AES was employed to measure Ir in gold matrix standard solutions. The recommended several Ir spectral lines of National standard GB/T21198.4-2007 and Thermo IRIS Intrepid Ⅱ ICP spectrometer were analyzed and discussed.The interference problems in the gold matrix were compared. After comprehensive study of spectral line intensity, sensitivity, standard curve correlation coefficient, light intensity value, interference line position and other factors, 212.681 nm has been confirmed as the best spectral line for testing Ir element in gold jewelry by this model of ICP spectrometer.

Analysis of Rope Fiber by PY-GC/MS

YANG Ben, LV Yin-ni, SHI Xiao-fan

2017, 23(2): 106-113. doi: 10.16495/j.1006-3757.2017.02.007

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9 polyester rope samples of different origins and different specifications were identified by the pyrolysis gas chromatography-mass spectrometry(PY-GC/MS). Firstly, through optimization, the experimental conditions were determined:the pyrolysis temperature was 550℃and the pyrolysis time was 6 s, the column temperature was programed from 50℃(1 min) to 250℃(10 min) at a speed of 20℃/min. Under these conditions, the characteristics of polyester pyrolysis products can be displayed. Pyrolysis analysis results showed that there were 13 main cracking products of polyester fiber, and the characteristics of the product were benzoic acid (relative intensity 100%), vinyl benzoate, biphenyl, benzene etc. Although the 9 polyester ropes had the same cracking characteristics, but the individual pyrolysis products and the relative contents of each characteristic product of were different. It can be used as the basis for the analysis and identification of polyester ropes in different specifications and different regions.

Determination of Flavonoids in Anoectochilus Roxburghii (wall) Lindl Cultivated with Different Modes by HPLC

HUANG Qing-zuo, YANG Xiao-ling, ZHAO Hui-xian, HUANG Li-ying

2017, 23(2): 114-119. doi: 10.16495/j.1006-3757.2017.02.008

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Three flavonoid compounds(quercetin, kaempferol and isorhamnetin)in Anoectochilus roxburghii cultivated with four different modes were determined by HPLC. The above metioned compounds were extracted by ultrasonic-microwave synergistic extraction method and the quantitative and qualitative analysis were separately analyzed by HPLC and HPLC-ESI-MS. Quercetin, kaempferol and isorhamnetin had good linear relationship in the range of 0.25~20.0(r=0.999 2), 0.25~20.0(r=0.999 5), and 1.0~80.0(r=0.999 0), respectively. The contents were within 151.8~240.0、47.2~88.2、16.8~29.8 μg/g, respectively. The method is a simple, accurate and fast method for the quality evaluation of A. roxburghii cultivated with different modes. The contents of three flavonoid compounds increased effectively in A. roxburghii with the addition of nitrogen, phosphorus, potassium(NPK) compound fertilizer in cultivation and decreased 2.3%, 17.2% and 18.8% respectively in A. roxburghii with the addition sulfur-phosphorus(SP) compound fertilizer, this finding provides scientific guidance for planting A. roxburghii.

High Frequency Infrared Carbon Sulfur Analyzer Determinate Sulfur Trioxide in Gypsum Mines

WANG Na

2017, 23(2): 120-123. doi: 10.16495/j.1006-3757.2017.02.009

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In this paper, a method for the determination of the contents of sulfur trioxide in gypsum mines by high frequency infrared carbon sulfur analyzer with satisfactory results was established. The detection limit of the method was 0.003 0%. The proposed method was applied to the analysis of certified reference materials of gypsum (GBW03109a, GBW03110), and obtained results in consistent with the certified values, the RSD(n=9) was 0.32%~0.81%. By the analysis of the certified reference material of gypsum (GBW03111), there was no significant difference between this method and the routine gravimetric method of BaSO₄. Recovery rates obtained by standard spike method were in the range of 96.4%~104.0%.

Opening Use and Management of X-ray Photoelectron Spectroscope

MIAO Li-jing, JIANG Ke-min, LU Huan-ming

2017, 23(2): 124-126. doi: 10.16495/j.1006-3757.2017.02.010

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X ray photoelectron spectroscopy (XPS) is one of the most important methods for the qualitative and semi quantitative analysis of surface elements. It is an essential tool for the scientific research in surface analysis. How to improve the efficiency of the use of the instrument is a thorny problem. The opening and sharing of large-scale instrument to optimize the test efficiency has been proposed. In this paper, the experience of the opening usage of XPS is summarized.

Common Failure Phenomena and Troubleshooting Method for Sample Chamber of ZSX PrimusⅡ X-Ray Fluoresence Spectrometer

LIU Jiang-bin, ZHU Jian-guo

2017, 23(2): 127-129. doi: 10.16495/j.1006-3757.2017.02.011

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In the paper, a general introduction of sudden faults and the corresponding troubleshooting for sample chamber of RIGAKU ZSX Primus Ⅱ X-ray fluorescence spectrometer in use, and the requirements for regular maintenance of this instrument are described.

Elimination of 180° Nonuniqueness of ZnO Diffraction Pattern

TANG Ming-hua, CHEN Mu-zi, ZHU Xing, GUO Jun, YAN Chun-hui

2017, 23(2): 130-134. doi: 10.16495/j.1006-3757.2017.02.012

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In the determination of electron diffraction pattern of crystal involving interface, dislocation and other defects of crystallography properties, to eliminate the problem of 180° nonuniqueness is needed. In this article, using the precise specimen stage of transmission electron microscope (FEI, Tecnai G² F20) the systematic tilting of crystals can be accomplished, and by the analysis and study of the changes of electron diffraction pattern, the selection of the right index of crystalline plane and index of zone axis, the elimination of 180° nonuniqueness of ZnO diffraction pattern can be achieved.

Quality Assurance of Determination of Heavy Metals in Soils

YU Xiu-juan, FAN Ji-peng, WEI Xiao-pei, WANG Yang

2017, 23(2): 135-137. doi: 10.16495/j.1006-3757.2017.02.013

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Quality control measures were discussed in the process of proficiency testing of heavy metals in soils, in order to provide the reference for guarantee the accuracy of the proficiency testing results, and raise the level of laboratory testing technology unceasingly.

2017 No. 2

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