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Preparation of MnFe 2O 4/TiO 2 and Its Fenton⁃Like Photocatalytic Properties
Wang Xiaodi, Li Lihua, Zhang Jinsheng, Wu Xian, Ma Cheng
Abstract234)   HTML    PDF (1550KB)(102)      
MnFe2O4/TiO2 Fenton⁃like photocatalyst was successfully prepared by sol⁃gel method, the structure and morphology of the sample were characterized by XRD, SEM and UV⁃vis. MB was used as the target pollutant for degradation, and the photocatalytic properties of products with different doping amounts were investigated in visible light. The results show that: The degradation rate of TMF Fenton⁃like photocatalytic reaction to MB is up to 96.8%, under the optimum conditions, in the iodine⁃tungsten lamp with a light source of 300 W, the doping amount of MnFe2O4 to TiO2 is 2%, the mass of catalyst is 60 mg, pH=11, and the concentration of H2O2 is 8 mmol/L . Under the same conditions, compare with the undoped pure TiO2, the catalytic performance of MnFe2O4/TiO2 for MB under visible light is significantly improved.
2021, 41 (2): 32-36. DOI: 10.3969/j.issn.1672-6952.2021.02.007
Water Injection Optimization Technology in High Water Cut Period of Ultra⁃Low Permeability Reservoir in Fengfuchuan Oilfield
Ai Xiaofan, Zhang Jinghao, Chen Jing
Abstract519)   HTML    PDF (2703KB)(168)      
Fengfuchuan Oilfield is a ultra⁃low permeability reservoir, pilot experiment of pre⁃water injection in Chang 2 reservoir began in 2002. In 2003, the development of water injection in the whole area was basically realized. However, the development effect of the whole area was not ideal. The comprehensive water content increased from 25.0% in the initial period to 92.0% in 2015, and entered the stage of ultra⁃high water cut period.The main problems faced in this area are that the phenomenon of fractured water flooding and water channeling is more serious, the water content of the oil well rises obviously, the output of a single well is low, and the output of the oil field decreases rapidly. In this paper, the geological of the whole area was recognized again. On the basis of fine comparison of single sand bodies, improvement of injection⁃production well nets and improvement of the corresponding degree of small⁃layers, the first one was to propose a large⁃area water injection on the whole area, a partial slow and gentle water injection to supplement the stratigraphic energy; the second one was to adopt two sets of injection⁃production patterns to realize stratified injection, expanded the original well spacing, and solved the inter⁃layer contradiction; the third one was to improve the single well production efficiency and improved the single well production to improve the development of the whole area.
2020, 40 (3): 52-56. DOI: 10.3969/j.issn.1672-6952.2020.03.010
Ion Exchange Property of H2O2⁃Modified H1.07Ti1.73O4•H2O Layered Titanate
Zhang Jin, Zhou Wenli, Wang Xing, Kong Xingang
Abstract481)   HTML    PDF (4119KB)(284)      
In this paper, layered titanic acid H1.07Ti1.73O4•H2O (HTO) was treated with hydrogen peroxide solution to achieve the hydrogen peroxide intercalation and modification of HTO. The hydrogen peroxide molecules entered into the interlayer of TiO6 octahedral layer, forming a peroxytitanium coordination bond with Ti4+ in the layer, which increased the negative charge density of the TiO6 layers. XRD, SEM, TEM, XRF, FT⁃IR and other methods were used to characterize the samples before and after ion exchange. The ion exchange experiments show that compared with HTO, the ion exchange efficiency and ion exchange capacity of H2O2⁃modified HTO are greatly enhanced. And the main reason is that the introduction of H2O2 leads to the increase of negative charge of TiO6 octahedral layers.
2020, 40 (3): 1-7. DOI: 10.3969/j.issn.1672-6952.2020.03.001
Recent Advancement of Iron Oxide Photoelectrocatalytic Materials
Sun Cai, Gao Ying, Zhang Jing
Abstract663)   HTML    PDF (1297KB)(432)      
Photoelectrocatalytic technology can provide an energy conservation and environmental protection way for environmental governance and chemical production. High efficient photoanodes materials are one of the challenges in the practical application of photoelectrocatalytic technique, therefore, high performance photoanode materials have been designed and developed for enhancing the application efficiency of photoelectrocatalytic technique. Fe2O3 has become a hot spot in the field of photocatalysis because of its narrow band gap, high stability and low price. In order to develop the high performance Fe2O3 photoanodes materials, many studies focused on the energy band position, conductivity and photogenerated the hole diffusion length. This review summarized the preparation techniques (hydrothermal method, spray pyrolysis, chemical vapor deposition, atomic layer deposition, etc), modification methods (“junction” construction, doping, morphological control, ect) and modified hydrogen production of the Fe2O3 photoanodes materials, the challenges and opportunities in this promising research area were proposed.
2020, 40 (2): 30-37. DOI: 10.3969/j.issn.1672-6952.2020.02.006
Study on Foaming Agent System of Heavy Oil Foam Flooding
Ma Di, Pan Yi, Zhang Jinhui, Rassadkina Regina, Liao Songze, Zhang Ran
Abstract381)   HTML    PDF (790KB)(272)      
In the process of foam flooding in heavy oil fields, the performance of single foaming agent is unstable. In view of this difficult problem, a new foaming agent system for foam flooding is designed in this paper. The foam synthesis index and temperature and salt resistance are taken as the evaluation indexes by Waring⁃Blender agitation method four kinds of foaming agents such as betaine, CTAB, SDBS and SDS were selected. The best foaming agents were betaine and CTAB. Through the experimental selection of different proportion of foaming single agent, the oil washing ability test and sand filling tube simulation experiment of CTAB and betaine system with 2∶1 ratio were carried out. The results show that the foaming agent system have good temperature and salt resistance and strong oil washing ability. In the sand⁃filled pipe simulation experiment, the two displacement modes of steam flooding plus foam flooding and steam foam alternating injection flooding are compared. The results show that the oil recovery can reach 60.7% by alternately injecting steam and foam fluid into the reservoir, which has certain reference value.
2020, 40 (2): 11-15. DOI: 10.3969/j.issn.1672-6952.2020.02.003
Oxidation⁃Extraction Desulfurization of Visbreaking Diesel Fuel
Zhou Shixin, Zhang Jing, Qiao Haiyan, Han Dongyun, Cao Zubin, Shi Weiwei
Abstract395)   HTML    PDF (1146KB)(167)      
The oxidation⁃extraction process was used to desulfurize of the visbreaking diesel oil, O3 was used as oxidant, formic acid was used as catalyst, and polar oxides such as sulfoxide and sulfone were extracted and separated from diesel oil by polar organic solvent. The effects of oxidation time, oxidation temperature, ratio of extractant to oil and amount of formic acid on the desulfurization rate of diesel oil in the reaction system were investigated, and the optimum reaction conditions were determined. The results showed that the sulfur content of visbreaking diesel oil decreased from 4 980 μg/g to 490 μg/g and the desulfurization rate was 90%. By comparing the properties of visbreaking diesel oil before and after oxidation, it can be concluded that the oxidation⁃extraction method can also improve the chromaticity and acidity of visbreaking diesel oil.
2020, 40 (2): 6-10. DOI: 10.3969/j.issn.1672-6952.2020.02.002
Preparation of CdS Phase Junction by Solid Phase Method and Photocatalytic Performance
Wang Xin,Zhang Jing
Abstract535)   HTML    PDF (1050KB)(286)      
In this work, the cubic/hexagonal cadmium sulfide (c/h⁃CdS) heterojunction catalyst was successfully prepared by solid phase reaction with cadmium acetate and thioacetamide as raw materials.The synthesized catalysts were characterized by means of XRD, SEM and SPV. The activity of photocatalytic degradation of rhodamine B (RhB) was evaluated by using visible light as the light source. The effect of calcination temperature on the photocatalytic performance of CdS was investigated, and the mechanism of the degradation process was discussed. The results suggest that with the increasing of calcination temperature, c⁃CdS is gradually changing to h⁃CdS. The c/h⁃CdS phase junction formed in the phase transition shows a higher photocatalytic activity than the pure c⁃CdS and h⁃CdS, and the appropriate six⁃square phase content is more beneficial to improve the photocatalytic performance of the heterogenous sample. The results of surface photovoltage show that the formation of heterojunction can significantly improve the photoelectron⁃hole separation efficiency, thus promoting the photocatalytic performance of c/h⁃CdS phase junction. In the experiment of the sacrificial agent, the active species in the CdS photocatalytic reaction is ·O2-.
2019, 39 (3): 30-34. DOI: 10.3969/j.issn.1672-6952.2019.03.006
Metal⁃Loaded ZSM⁃5 Molecular Sieve Catalyzed Ozonation of Phenol Wastewater
Cui Fuxu,Zhang Jing,Zhang Bo,Yang Liangdong,Wang Yingying,Pan Liwei
Abstract415)   HTML    PDF (1668KB)(221)      
ZSM⁃5 molecular sieve was used as carrier, cerium (Ce), manganese (Mn), nickel (Ni) and copper (Cu) were used as active components to prepare metal⁃supported catalyst to catalyze ozonation treatment of phenol wastewater. The catalyst was prepared by impregnation method and characterized. The effects of active components, ozone dosage, catalyst concentration and pH on the treatment of phenol wastewater were investigated. The results showed that Ce⁃ZSM⁃5 had the best catalytic effect and COD removal rate under the conditions of pH=7, catalyst concentration of 1.00 g/L, ozone dosage of 44.0 mg/min and reaction time of 60 min. It is 85.74%. When Ce⁃ZSM⁃5 is added, about 80% of the ozone can be saved. It shows good stability which the COD removal ratio reached about 70% after the catalyst repeatedly used for 7 times.
2019, 39 (2): 10-14. DOI: 10.3969/j.issn.1672-6952.2019.02.002
Analysis of Oil & Gas Pipeline Transportation Leakage  and Its Emergency Management Mechanism
Zhao Donghui, Zhang Jinhui, Wang Zhipeng
Abstract445)      PDF (1421KB)(268)      
Based on the field investigation of the leakage of pipeline transportation and combining with the latest research direction of emergency management mechanism, it was found that the stochastic Petri net model suitable for this kind of problem was modeling. Taking the Huangdao oil pipeline leakage accident as an example, the data of emergency management flow of pipeline transportation leakage were collected and processed, and isomorphism Markov chain to study the change utilization rate and average delay time was used. The results of the study indicated that the coordinated treatment of pipeline leakage systems, protection of the affected areas and the transfer of the masses took the most time in emergency operations. Therefore, intensifying the cooperation between the central construction administrative agencies and the local construction administrative agencies and perfecting the mass transfer and resettlement system were reasonable measures to strengthen emergency management of pipeline leakage and minimize economic losses.
2018, 38 (04): 68-71. DOI: :10.3969/j.issn.1672-6952.2018.04.013
Preliminary Construction of the Safety Management System of Intelligent Marine Oil Spill
Zheng Jun,Bian Jiang,Wang Yujuan,Jin Shihao,Zhang Jingxiao,Gong Shuaihu,Jiang Wenming
Abstract636)      PDF (1765KB)(283)      
       In order to minimize the loss of life and property caused by sudden marine oil spills, it was necessary to apply intellectual technology to marine oil spills management system, combining human wisdom and the wisdom of computer technology, wisdom marine oil spill management system was established. The basic concepts and technology development were introduced and the wisdom and intelligence technology would be applied to marine oil spill management system. The wisdom marine oil spill management was initially established to reduce or even avoid the occurrence of oil spills at sea, to protect the marine environment, and to achieve sustainable and healthy development of marine and depot business.
2017, 37 (2): 22-26. DOI: 10.3969/j.issn.1672-6952.2017.02.005

Synthesis of CuS by DirectReaction and Their Thermal Degradation of Ammonium Perchlorate

Zeng Ying, Zhang Jing, Cheng Yun, Lai Junling, Luo Genxiang
Abstract710)      PDF (2007KB)(635)      
The flower-like CuS microspheres has been synthesized through elemental-direct-reaction at room temperture in the n (C5H14ONCl)/ n (EG)=1 2 based deep eutectic melt. The prepared CuS sample was characterized by XRD, EDS, SEM and so on, and the formation mechanism of flower-like CuS microspheres has been discussed. Meanwhile, the thermal decomposition of ammonium perchlorate (AP) has been investigated by DTA technique. The results show that: the flower-like CuS microspheres has a good catalytic effect on the thermal decomposition of ammonium perchlorate. The starting and ending decomposition temperature of ammonium perchlorate which added 2% CuS were decreased by 30 and 132 , respectively.
2016, 36 (2): 1-4. DOI: 10.3696/j.issn.1672-6952.2016.02.001
Research on Synthesis and the Photocatalytic Degradation of Rhodanmine B of MIL53(Fe)
Lu Yuanyuan, Zhang Dan, Zhang Jing,Gong Xiaojie, Song Jia
Abstract623)      PDF (2564KB)(498)      
In this paper, MIL53(Fe) was prepared by solvothermal method under different sythetic conditions. The phase structure of samples were characterized by XRD, the morphology and particle size of samples were obtained by SEM, the ultraviolet visible light absorption of samples were explored by UVvis and the band gap energy of samples were calculated from the absorption data. The photocatalytic activities of the samples on Rhodanmine B degradation were investigated. The results show different photocatalytic effects for the samples prepared under different synthetic condition. Accordingly, photocatalytic effect of samples can be controlled through the variation of different synthetic conditions.
2015, 35 (5): 1-4. DOI: 10.3969/j.issn.1672-6952.2015.05.001
Laboratory Study of the Composite OilWell Cement Early Strength Agent LL
Liang Lu, Li Lihua, Zhang Jinsheng, Wang Jing
Abstract497)      PDF (2164KB)(333)      
A chlorinefree composite as oilwell cement early strength agent named LL was developed. Combining organic acids A, alcohol amines B and nitrate compound C in a certain ratio, the compressive of cement stone in 6 h as the strength examining index can be designed in optimization test using the orthogonal method. The optimum formula determined by orthogonal was as follows: the weight of organic acids D is 1.0% based on cement,the weight of alcohols amines E is 0.04%,the weight of nitrates F is 4%. Under the optimum proportion, and the performance test of early strength agent LL was carried out after its addition of 2.5% in the cement. The ratio of the thickening time of early strength agent LL slurry to cement slurry is 0.436 less than 0.5, and the compressive strength of cement stone 6 h (39 ℃ and atmospheric pressure) is 11.0 MPa more than 4.0 MPa, they are all meeting the requirement of early strength agent industry standard SY/T5504.4—2008. And it has a good compatibility with the homemade retarders MAM, dispersants FASA and fluid loss AS.
2014, 34 (2): 33-36. DOI: 10.3696/j.issn.1672-6952.2014.02.009
 
Route Survey and Free Span Assessment for the Extended Service Subsea Pipelines in Bohai Bay
LI Chenggang,ZHANG Jing'an,ZHENG Hui,XIAO Zhiguo,XU Yongzhen
Abstract501)      PDF (2118KB)(215)      
 
Subsea pipeline is the lifeline of the offshore oil & gas field. More and more pipelines have reached their designed life with the increase of the service time. Geophysical equipment acquired the date of the free span, exposure and buried condition for the subsea pipelines. The subsea pipeline assessment system assessment the critical length and fatigue life of free span. By knowing of the condition of those lines in service, the operation risk was decreased and the safety of the subsea pipelines was increased. The support of maintenance for the owner of the subsea pipelines was also offered.
2013, 33 (4): 50-55.
Green Tea Differentiation Using Multistatistical Analysis  Based on Content of Mineral Elements
LI Lihua, ZHANG Jinsheng, WEI Linji
Abstract396)      PDF (1264KB)(327)      
The contents of eleven mineral elements(Mg,Al,Ca,Mn,Fe,Cu、Zn,K,Na,Co and Pb) in twentythree green tea samples from different areas were analyzed by microwave plasma torch atomic emission spectrometry (MPTAES). Then principal component analysis (PCA) and cluster analysis (CA) were applied to differentiate the geographical origins of these tea. The result indicated that This method can discriminate the geographical origins of these tea from AnHui、ZheJiang、SiChuan and JiangXi, the classification performance was clearly, the content of the mineral elements in teas were good chemical descriptors for differentiating their geographical origins.
2013, 33 (3): 12-15.
Laboratory Study on a New Accelerator WSA1 for Oil Well Cement
CAO Jie, ZHANG Jinsheng, LI Lihua, JIANG Weiwei,LIU Xiangdong
Abstract425)      PDF (1943KB)(214)      
As the cement slurry hydration speed is slow, the curing time is long and the increase of cement early compressive strength is slow in the low temperature cementing of conductor and surface casing, it is easy to result in oil, gas and water invasion which impairs cementing quality and operation safety. In view of the fact that the accelerator is lack in cementing of low temperature shallow formation currently at home, some accelerators have poor effectiveness and significant negative impact on slurry rheology etc, a new compound accelerator WSA1 was selected by laboratory study. The performance of slurry that mixed WSA1 was systematically evaluated. The result shows that the accelerator WSA1 can enhance the hydration of oil well cement, shorten the thickening time of cement slurry and significantly improve the early compressive strength of cementstones, which all accord with the requirement of the accelerator evaluation criterion. When WSA1 addition amount is 3%, the thickening time of cement slurry can be shortened more than 50%, the 6 h strength of cementstones enhanced from 3.2 MPa to 11.3 MPa and the 24 h strength of cementstones enhanced from 24.3 MPa to 46.1 MPa. Accelerator WSA1 is a kind of highperformance compound accelerator, which can be used in low temperature shallow formation and has no effect on the initial consistency and rheological parameter of cement slurry. 
2013, 33 (2): 20-23.
Hydrolysis of Corn Straw to Produce Reducing Sugar by Diluted Acid Over Ferrous Sulfate Under Microwave Radiation
ZHANG Jin-hui, WANG Shuo, ZHANG Qi-kai, LI Fei, DU Yun-chao
Abstract417)      PDF (718KB)(372)      
The corn straw was hydrolyzed by diluted acid via microwave radiation under the conditions of the metal salt ferrous sulfate as catalyst. The effect on the reducing sugar production rate was investigated by the concentration of ferrous sulfate, sulfuric acid content, ratio of liquid to solid, the microwave radiation power, time and pressure. The results show that the product yield can reach 38.5% under the best hydrolysis conditions: ferrous sulfate mass fraction of 3%, sulfuric acid mass fraction of 2%, mass ratio of liquid to solid 15, the microwave radiation power 187.5 W, the microwave radiation time 30 min and the microwave radiation pressure 0.3 MPa. Compared to the method without ferrous sulfate or without microwave radiation, this method shows higher yields by 1.1 and 2.8 times, respectively. 
2012, 32 (4): 13-16.
Evaluation of Uncertainty in the Determination of  Calcium and Magnesium in Milk by MPT-AES
YU Yong-qing, ZHANG Jin-sheng, LI Li-hua, ZHAO Wen-tao, 
Abstract452)      PDF (594KB)(323)      
The measurement uncertainty was estimated for the determination of calcium and magnesium in milk using microwave plasma torch atomic emission spectrometry (MPT-AES) and the uncertainty parameters were discussed and compared in detail. The results show that the "whole method" performance parameters, such as precision and recovery, and sampling are the three main contributors to uncertainty. In addition, the content of calibration solution is the main contributor to measurement uncertainty in the determination of magnesium. When coverage factor k=2 and confidence level approximately 95%, the expanded uncertainties were determined as 18.6 and 3.2 mg/L for Ca and Mg, respectively.
2012, 32 (4): 8-12.
Preparation and Characterization of Early Strength Accelerator
YANG Bo-yong, ZHANG Jin-sheng, LI Li-hua, WANG Guang-ying
Abstract347)      PDF (244KB)(364)      
AMPS, diethanolamine, and calium nitrate as materials of early-strength accelerator were prepared and characterized. Orthogonal experiment was utilized to optimize optimum content of early-strength accelerator. The samples were characterized with powder X-ray diffraction (XRD) and SEM. It is shown that when the weight of 5% early agents were introduced, the 1, 3 and 7 d of cement strength improved by 15.2%、14.3%、16.7%, respectively, which is also a further development in the high temperature.
2012, 32 (3): 29-32.
Synthesis and Evaluation of AS Fluid Loss Additive for Cement Slurry
WANG Guang-ying, ZHANG Jin-sheng, LI Li-hua, YANG Bo-yong
Abstract421)      PDF (206KB)(242)      
The AS fluid loss additive was formulated with sodium lignosulfonate and the copolymers obtained by radical polymerization with AMPS and AM as raw material. Orthogonal tests were designed for optimizing the synthetic process of the fluid loss additive AS, and the performance of this fluid loss additive was systematically evaluated. API filtration in saturated salt solution at 150 ℃ is 96 mL; API filtration can be controlled within 50 mL when adding AS between 3% and 8% (weight percentage) at 120 ℃; Meanwhile AS has good compatibility with other additives. Sodium bicarbonate was used to adjust the PH and discharge oxygen of device used in the synthesis process. No nitrogen was needed as protective gas, which simplified the synthesis process. The sodium lignosulfonate derives from the wastewater of paper mill, so it not only reduces the cost but also protects the environment.
2012, 32 (2): 38-42.
Performance of Thickening Agent on Water-Base Fracturing Fluid
ZHANG Jin-sheng, YU Wei-kun, LI Li-hua, WANG Guang-ying
Abstract391)      PDF (222KB)(250)      
The thickening agent of graft copolymer was synthesized by carboxymethyl starch (CMS) and acrylamide (AM) under the condition of initiator. The optimum synthesis conditions were investigated by orthogonal experiment design. The structure of the product which was obtained under the best reaction conditions was characterized by FT-IR, and the salt sensitivity and temperature stability, shear stability and anti-ageing of the graft copolymer solution in different slurry were measured by rotational viscometer. The results show that the viscosity can reach 280 mPa·s under the reaction conditions as follows: the reaction temperature 60 ℃, the reaction time 7 h, the mass ratio of CMS to AM 1∶6 and the initiator addition amount 0.9%. The CMS-AM graft copolymer in different slurry shows excellent the salt sensitivity and temperature stability, shear stability and anti-ageing, which can satisfy the needs of oil field fracturing fluid for thickening agent.
2012, 32 (2): 20-23.
Determination the Trace Elements in Wild Pine Tea by MPT-AES
ZHAO Wen-tao, ZHANG Jin-sheng, LI Li-hua, YU Yong-qing, LIN Jing
Abstract392)      PDF (178KB)(257)      
The method for the determination of copper, zinc, manganese, iron, magnesium, calcium in wild pine tea by microwave plasma torch-atomic emission spectrometry (MPT-AES) was developed. The effect of nitric acid concentration in the sample solution and co-ionized elements on the emission intensity of copper, zinc, manganese, iron, magnesium and calcium was investigated in detail. The experimental conditions were optimized and showed that the detection limits of metal Cu, Zn, Mn, Fe, Mg and Ca are 3.6, 7.7, 6.1, 14.1, 0.5 and 0.9 ng/mL, respectively, and the RSD of the method is between 1.05%~6.46%, the recoveries are 97.25%~103.37%. This demonstrated that the proposed method is simple, accuracy and efficient, providing a well-established analytical method.
2012, 32 (2): 8-11.
 
Determination of Flavonoids From Polygo-Num Avculare by Microwave-Assisted Extraction and Spectrophotometry
ZHANG Li-min, ZHANG Jin-sheng, LI Li-hua, LI Yan-nan
Abstract441)      PDF (143KB)(220)      
 
Flavonoids were extracted from polygonum avculare by microwave-assisted extraction, and its content was determined by spectrophotometry using the rutin as the quality control standard. The effect of extraction temperature, solid to liquid ratio, alcohol concentration and extraction time on content determination were investigated by orthogonal. The optimum conditions are as follows: extraction temperature 80 ℃, the solid to liquid 1∶40, the volume ratio of ethanol 85% and extraction time 7 min. Under the optimum conditions, the average content of flavonoids in polygonum avculare is 2.099 mg/g, average total flavonoids extract ratio is 3.481% , RSD= 0.304% (n=6), and their recovery rate measured are in the range of 94.17% ~99.50%.
2011, 31 (3): 28-30. DOI: 10.3696/j.issn.1672-6952.2011.03.008
Determination of Flavonoids From Codonopsis Pilosula With Spectrophotometer
WANG Qing-ming, ZHANG Jin-sheng, LI Li-hua, XUE Li-min
Abstract410)      PDF (195KB)(294)      
Flavonoids were extracted from codonopsis pilosula with microwave-assisted method, and its content was determined by spectrophotograpy. Two methods with NaNO2-Al(NO3)3 or AlCl3 as the chromogenic agent were performed and the precision, stability, reproducibility and recovery ratio of the two methods were studied. The results show that the AlCl3 colorimetric determination of flavonoids in codonopsis pilosula was simple, convenient, accurate and reliable as compared with the NaNO2-Al(NO3)3 colorimetric determination method.
2010, 30 (4): 4-07. DOI: 10.3696/j.issn.1672-6952.2010.04.002
Determination of Flavonoids From Codonopsis Pilosula by Microwave-Assisted Extraction and Spectrophotometer
WANG Qing-ming, ZHANG Jin-sheng, LI Li-hua, XUE Li-min
Abstract499)      PDF (209KB)(228)      
 
Flavonoids were extracted from Codonopsis pilosula by microwave-assisted extraction and its contents were determined by spectrophotometer. The extraction rate of flavonoids were investigated by single factor experiment included alcohol volume fraction, ratio of material to liquid, extraction temperature, and extraction time. The best conditions for procedure were as follows: extracting time is 15 min, extracting temperature is 85 ℃, the volume fraction of ethanol is 70%,  and material to liquid ratio is 1∶30. Under the optimal conditions, the amount of flavonoids in codonopsis pilosula was 2.87%, RSD=0.878%(n=5), and their recovery is between 99%~102%.
2010, 30 (2): 8-10. DOI: 10.3696/j.issn.1672-6952.2010.02.003
Extracting of Cucumber-Seed Oils by Soxhlet Method
GUO Zi-geng, LI Li-hua, ZHANG Jin-sheng
Abstract572)      PDF (182KB)(350)      
The cucumber seed oil was obtained by Soxhlet extraction with the seed as the raw material. Soxhlet extraction of oils from cucumber-seed was studied with single factor test, and the yield of cucumber-seed oils was the evaluation index. The influences of extracting solvent, extracting temperature, extracting time, the rate of raw material , and solvent on the yield of cucumber-seed oils were investigated respectively. The optimal conditions of Soxhlet method were obtained: extracting temperature is 68.5 ℃, extracting time is 8 h, the mass concentration of cucumber-seed oil is 0.071 g/mL, optimal extracting solvent is n-hexane. The oil yield reaches 40.38% under the optimal conditions.
2009, 29 (4): 27-29.
Determination of Cu、Zn and Ni in Waste Active Muddy Soil by Microwave Digestion-FAAS
ZHANG Jin-sheng, LI Li- hua, CHEN Yu-yan
Abstract277)      PDF (149KB)(187)      
The content of copper, zinc and nickel in waste active muddy soil were measured by microwave digestion-fire atomic absorption spectrometry(FAAS), and the optimization condition was studied. The results are compared with that of acid digestion at atmosphere. The results of the above two method are similar. The experiment results show that two steps are suggested in microwave digestion. Microwave power is 340 W, constant time is 10 min, and microwave pressure is 0.4 MPa and 0.45 MPa in each step, respectively. Linear range of copper, zinc, nickel is 0~20,0~12 and 0~25 mg/L respectively. Detection limit of copper, zinc, nickel is 0.300 0,0.030 7 and 0.010 6 mg/L respectively. Average recovery of copper, zinc, nickel in waste active muddy soil samples is 97.6%,98.9% and 96.5% respectively, and relative standard deviation is 1.74%,0.95% and 1.00% respectively.
2009, 29 (4): 24-26.
Determination of Copper and Iron in Gasoline by MPT-AES
LI Li-hua, ZHANG Jin-sheng, LU Ying-bing, GONG Xiao-jie
Abstract422)      PDF (180KB)(308)      
Microwave plasma torch is used as exaction power, and Argon is used as work gas. Contents of copper and iron in gasoline were determined by microwave plasma torch atomic emission spectrometry (MPT-AES) with pneumatic nebulization sample introduction system. The influence of microwave power, support gas flow rate, work gas flow rate, oxygen shielded gas on the contents of copper and iron were discussed and optimized. The experimental results show that the detection limits of copper and iron are 5.3 and 22.1 μg/L respectively; RSD of the method is less than 2.83%; the linear ranges of copper and iron are 0.05~60 and 0.1~100 mg/L respectively; the recoveries of sample are in the range of 95.1%~103.5%. The method has many features,such as high sensitivity, rapidity, less sample quantity, low maintenance cost and accurate.
2009, 29 (4): 12-14.
Biodiesel Preparation via Transesterification on Silica Sulfonic Acid Solid Catalyst
ZHANG Jing-yu, REN Li-guo
Abstract434)      PDF (216KB)(317)      
The silica sulfonic acid(SiO2-SO3H) sold acid catalysts was prepared with chlorosulfonic acid reacting with the silica prepared in sol-gel method. The catalyst was used for the transesterification of soybean and ethanol to form biodiesel. Experiments have proved that the yield of ethyl esters reached over 95.6% under the condition: treatment of catalyst at 120 ℃, molar ratio of ethanol and oil is 6∶1, the mass fraction of catalyst in oil 5.0%, the mass fraction of heptane in oil 30.0% and refluxe time 6.0 h. The results show that the catalyst so prepared has a better adaptability than the solid bases catalysts to the acidity of raw oil.
2009, 29 (3): 41-43.
Synthesis of Methyl Methacrylate With Single-Mode Focus Microwave Radiation
ZHANG Jin-sheng, HU Zhi-feng, LI Li-hua, LI Ling, WANG Yong-yan, SHAO Hai
Abstract290)      PDF (208KB)(232)      
The methyl methacrylate (MMA) was synthesized by precision microwave organic synthesis system and its single-mode focusing microwave radiation technology, synchronized Pneumatic gas cooling technology. In the experiment, 2-methyl acrylate and methyl alcohol were used as materials, sulphuric acid as a catalyst for esterification, and hydroquinone as a polymerization inhibitor. Under Discover precision microwave organic synthesis system standard mode, the mol ratio of reaction, the reaction power, the reaction time, and other factors were investigated. The experimental results show that the optimal conditions of microwave heating are as follows: The reaction temperature 70 ℃, the ratio of 2-methyl acrylate and methyl alcohol 1∶2, the power 100 W, the reaction time 30 min, the yield 88%.
2009, 29 (3): 37-40.