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钨-镍-铜高比重合金烧结时液相凝固机理的探讨
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作者 周国安 赖和怡 《兵器材料科学与工程》 CAS CSCD 北大核心 1989年第5期21-24,20,共5页
本文通过对烧结合金W-Ni-Cu液相凝固过程的研究,发现液相凝固类似于熔融合金的凝固,亦有形核和在温度梯度为负时的枝晶生长,不同之处是已有一个末溶的颗粒存在,从而,末溶相往往可以作为新相的核心,长大就依靠烧结时溶解-沉淀过程而长大。
关键词 烧结合金 合金 液相凝固
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基于漂浮有机液滴凝固液相微萃取的黄酮类化合物分配系数及含量测定 被引量:5
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作者 张茜 陈璇 白小红 《高等学校化学学报》 SCIE EI CAS CSCD 北大核心 2011年第2期269-274,共6页
利用漂浮有机液滴凝固液相微萃取(SFODLPME)技术对中药中的黄酮类化合物进行富集,建立了SFODLPME-HPLC快速测定中药材样品中低丰度黄酮类化学成分含量的方法.讨论了黄酮类化合物的富集倍数与浓度及与供相体积之间的关系,定义并阐述了... 利用漂浮有机液滴凝固液相微萃取(SFODLPME)技术对中药中的黄酮类化合物进行富集,建立了SFODLPME-HPLC快速测定中药材样品中低丰度黄酮类化学成分含量的方法.讨论了黄酮类化合物的富集倍数与浓度及与供相体积之间的关系,定义并阐述了富集倍数(EF1μg/mL)及其物理意义,计算了漂浮有机液滴凝固相体积及黄酮类化合物的表观分配系数.在优化的SFODLPME条件下,结合高效液相色谱测得8种黄酮类成分的线性范围均为0.01~10.00μg/mL;检出限为1.0~0.01 ng/mL;精密度RSD〈7.0%;药材中分析物的回收率为96.0%~104.2%.当加入的萃取溶剂体积为40μL时,形成的漂浮有机液滴凝固相体积为(52±14)μL;8种黄酮类成分的表观分配系数在44.8~243.9之间. 展开更多
关键词 漂浮有机液滴凝固液相微萃取 表观分配系数 富集倍数 黄酮类化合物
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超分子有序聚集凝固液相微萃取及其对五味子中木脂素类化合物的测定及质量评价 被引量:2
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作者 薛雪 张红芬 +1 位作者 白小红 岳媛 《高等学校化学学报》 SCIE EI CAS CSCD 北大核心 2012年第5期942-947,共6页
通过分析比较漂浮有机液滴凝固液相微萃取(SFODLPME)对木脂素类化合物萃取前后紫外光谱的变化,提出了超分子有序聚集凝固液相微萃取(SSMOALPME)机理;建立了简单、快速、灵敏的SSMOALPME高效液相色谱法(HPLC)同时测定中药五味子中5种低... 通过分析比较漂浮有机液滴凝固液相微萃取(SFODLPME)对木脂素类化合物萃取前后紫外光谱的变化,提出了超分子有序聚集凝固液相微萃取(SSMOALPME)机理;建立了简单、快速、灵敏的SSMOALPME高效液相色谱法(HPLC)同时测定中药五味子中5种低丰度木脂素类化合物含量的方法,并对不同产地五味子的质量进行比较和评价.在最佳的SSMOALPME条件下,测得五味子醇甲、五味子酯甲、五味子甲素、五味子乙素和五味子丙素的线性范围分别为2.48×10-3~6.21,2.27×10-3~28.5,2.31×10-3~28.8,2.27×10-3~5.69和1.05×10-3~5.25μg/mL;检出限分别为0.4,0.4,0.4,0.08和0.08 ng/mL;日内及日间精密度RSD<9.7%;药材中分析物的回收率为91.9%~104.7%;SSMOALPME对5种分析物的富集倍数分别在39~529倍之间.本法测定结果与药典法测定结果相比无显著差异(P=95%).SSMOALPME方法的提出为液相微萃取的理论研究奠定了基础,为反映中药多成分、多靶点及协同作用的特性,建立科学的质量控制方法提供了理论依据和实验基础. 展开更多
关键词 漂浮有机液滴凝固液相微萃取 超分子有序聚集 富集倍数 五味子 木脂素
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Al-Cu-Fe准晶相的液相面与邻近晶体相液相面的交线投影图 被引量:5
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作者 赵东山 瞿文榜 +3 位作者 王仁卉 沈宁福 石广新 桂嘉年 《金属学报》 SCIE EI CAS CSCD 北大核心 2004年第1期14-19,共6页
采用金相(OM)、X射线衍射(XRD)、扫描电子显微术(SEM)和透射电子显微术(TEM)等方法,研究了在不同温度长时间保温后水淬的Al_(48-60)Cu_(33-50)Fe_(0-10)系列合金的凝固组织及相组成,结果表明,Gayle等报道的Alcu-Fe三元相图的单变量线(... 采用金相(OM)、X射线衍射(XRD)、扫描电子显微术(SEM)和透射电子显微术(TEM)等方法,研究了在不同温度长时间保温后水淬的Al_(48-60)Cu_(33-50)Fe_(0-10)系列合金的凝固组织及相组成,结果表明,Gayle等报道的Alcu-Fe三元相图的单变量线(液相面交线)投影图中β相的液相面应当划分为β+φ两个区域,新增的四相反应为包共晶反应U_8∶L+β→IQc+φ,反应温度约为800℃,X射线能谱(EDXS)分析表明,Ni_2Al_3结构的φ相的成分范围是Al_(47.3-50.6)Cu_(45.4-48.1)Fe_(4.5-5.2),而其成分中心是Al_(47.9)Cu_(47.1)Fe_(5.0)。 展开更多
关键词 单变量线(液相面交线)投影图 凝固组织 二十面体准晶相 Ф相
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SFOD-LPME-HPLC法测定白酒中甘草酸、甘草次酸
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作者 黄媛 洪丽 +3 位作者 黄何何 潘城 胡朝阳 蔡小明 《中国酿造》 CAS 北大核心 2023年第9期217-222,共6页
建立漂浮有机液滴凝固液相微萃取联合高效液相色谱法(SFOD-LPME-HPLC)测定白酒中甘草酸(GA)和甘草次酸(GTA)。取2 mL白酒经95℃热水浴脱醇,20 mL水溶液复溶后进行微萃取,以40μL正十二醇作为萃取剂,50μL四氢呋喃作为分散剂,以酸性体系... 建立漂浮有机液滴凝固液相微萃取联合高效液相色谱法(SFOD-LPME-HPLC)测定白酒中甘草酸(GA)和甘草次酸(GTA)。取2 mL白酒经95℃热水浴脱醇,20 mL水溶液复溶后进行微萃取,以40μL正十二醇作为萃取剂,50μL四氢呋喃作为分散剂,以酸性体系作为萃取供相,加入1.0 g氯化钠,在40℃条件下萃取15 min。在最优萃取条件下,甘草酸及甘草次酸在2.50~50.0 ng/mL的质量浓度范围内线性关系良好,相关系数R2>0.999,检出限为0.004 mg/L,定量限为0.01 mg/L,样品加标回收率在89.2%~105.0%之间,精密度试验结果相对标准偏差(RSD)在1.59%~5.57%。该方法快速准确,绿色环保,适用于白酒中甘草酸、甘草次酸的检测。 展开更多
关键词 漂浮有机液滴凝固液相微萃取 高效液相色谱 甘草酸 甘草次酸 白酒
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Rapid solidification of Cu_(60)Co_(30)Cr_(10) alloy under different conditions 被引量:2
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作者 郭晋波 曹崇德 +6 位作者 弓素莲 宋瑞波 白晓军 王建元 郑建邦 文喜星 孙占波 《Transactions of Nonferrous Metals Society of China》 SCIE EI CAS CSCD 2013年第3期731-734,共4页
Metastable liquid phase separation and rapid solidification in a metastable miscibility gap were investigated on the Cu60Co30Cr10 alloy by using the electromagnetic levitation and splat-quenching.It is found that the ... Metastable liquid phase separation and rapid solidification in a metastable miscibility gap were investigated on the Cu60Co30Cr10 alloy by using the electromagnetic levitation and splat-quenching.It is found that the alloy generally has a microstructure consisting of a(Co,Cr)-rich phase embedded in a Cu-rich matrix,and the morphology and size of the(Co,Cr)-rich phase vary drastically with cooling rate.During the electromagnetic levitation solidification processing the cooling rate is lower,resulting in an obvious coalescence tendency of the(Co,Cr)-rich spheroids.The(Co,Cr)-rich phase shows dendrites and coarse spheroids at lower cooling rates.In the splat quenched samples the(Co,Cr)-rich phase spheres were refined significantly and no dendrites were observed.This is probably due to the higher cooling rate,undercooling and interface tension. 展开更多
关键词 Cu-Co-Cr alloy rapid solidification metastable liquid phase separation electromagnetic levitation splat-quenching
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SFOD-LPME-HPLC测定白芷中香豆素类活性成分 被引量:1
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作者 李卫霞 于智慧 白小红 《中国继续医学教育》 2018年第25期139-141,共3页
目的建立漂浮有机液滴凝固液相微萃取-高效液相色谱(SFOD-LPME-HPLC)法测定白芷中香豆素类成分含量的方法。方法以20μl十二醇为萃取剂,萃取30 min,转速600 r/min,样品相体积7 ml,盐浓度15%(w/v),在此优化条件下,测定白芷中香豆素类成... 目的建立漂浮有机液滴凝固液相微萃取-高效液相色谱(SFOD-LPME-HPLC)法测定白芷中香豆素类成分含量的方法。方法以20μl十二醇为萃取剂,萃取30 min,转速600 r/min,样品相体积7 ml,盐浓度15%(w/v),在此优化条件下,测定白芷中香豆素类成分的含量。结果在SFOD-LPME最佳条件下,测得5种香豆素类成分的富集倍数为52~250倍;线性范围均为0.005~2μg/ml(R2=0.998 9~0.999 6);检测限为0.01~0.5 ng/ml;日内精密度和日间精密度分别为RSD<1.53%和RSD<1.69%;回收率为98.9%~102.1%。结论 SFOD-LPME-HPLC具有操作简单、速度快、高富集倍数、高灵敏度、有机溶剂用量少等优点,可做中药样品前处理技术。 展开更多
关键词 漂浮有机液滴凝固液相微萃取 高效液相色谱法 白芷 香豆素类化合物 富集倍数 含量测定
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漂浮有机凝固液相微萃取-高效液相色谱法测定食品中米酵菌酸 被引量:3
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作者 黄媛 梁敏 +5 位作者 陈言凯 蔡小明 吴少明 叶梦薇 吴丽倩 李燕妹 《食品科技》 CAS 北大核心 2022年第4期342-347,共6页
建立漂浮有机液滴凝固液相微萃取法联合高效液相色谱测定食品中米酵菌酸。方法经过系统的优化后,确定了最佳萃取条件:以30μL十二醇作为萃取溶剂、300μL丙酮作为分散剂,供相溶液pH值为2,在室温下萃取时间为15 min。在最佳萃取条件下,... 建立漂浮有机液滴凝固液相微萃取法联合高效液相色谱测定食品中米酵菌酸。方法经过系统的优化后,确定了最佳萃取条件:以30μL十二醇作为萃取溶剂、300μL丙酮作为分散剂,供相溶液pH值为2,在室温下萃取时间为15 min。在最佳萃取条件下,米酵菌酸在0.5~10 ng/mL的浓度范围内线性良好,相关系数R^(2)大于0.999,最低检测限为1.00μg/kg,样品加标回收率为83.5%~98.6%,富集倍数约达200倍。该方法快速准确、绿色环保,适用于食品中米酵菌酸的检测。 展开更多
关键词 漂浮有机液滴凝固液相微萃取 高效液相色谱 米酵菌酸 食品
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Effect of gap size on microstructure of transient liquid phase bonded IN-738LC superalloy 被引量:4
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作者 Vahid MALEKI Hamid OMIDVAR Mohammad-reza RAHIMIPOUR 《Transactions of Nonferrous Metals Society of China》 SCIE EI CAS CSCD 2016年第2期437-447,共11页
In order to investigate the microstructure evolution and gain complete isothermal solidification time, transient liquid phase (TLP) bonding of IN-738LC superalloy was carried out using powdered AMS 4777 as the fille... In order to investigate the microstructure evolution and gain complete isothermal solidification time, transient liquid phase (TLP) bonding of IN-738LC superalloy was carried out using powdered AMS 4777 as the filler metal. The influence of gap size and bonding time on the joints was investigated. For example, complete isothermal solidification time for 40μm gap size was obtained as 45 min. In the case of lack of completion of isothermal solidification step, the remained molten interlayer cooled in the bonding zone under non-equilibrium condition andγ–γ′ eutectic phase formed in that area. The relationship between gap size and holding time was not linear. With the increase in gap size, eutectic phase width became thicker. In the diffusion affected zone, a much larger amount of alloying elements were observed reaching a peak. These peaks might be due to the formation of boride or silicide intermetallic. With the increase in gap size, the time required for bonding will increase, so the alloying elements have more time for diffusion and distribution in farther areas. As a result, concentrations of alloying elements decreased slightly with the increase in the gap size. The present bi-phasic model did not properly predict the complete isothermal solidification time for IN-738LC-AMS 4777-IN-738LC TLP bonding system. 展开更多
关键词 IN-738LC superalloy transient liquid phase (TLP) bonding gap size complete isothermal solidification
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Role of interlayer composition in microstructure and mechanical properties during TLP bonding of GTD-111/IN-718 superalloys 被引量:2
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作者 Ali IZADI GHAHFEROKHI Masoud KASIRI-ASGARANI +2 位作者 Kamran AMINI Mahdi RAFIEI Reza EBRAHIMI-KAHRIZSANGI 《Transactions of Nonferrous Metals Society of China》 SCIE EI CAS CSCD 2022年第3期908-926,共19页
An investigation was carried out to assess the applicability of transient liquid phase bonding of two dissimilar super-alloys with different interlayers. The effect of using three types of interlayer such as BNi-2, BN... An investigation was carried out to assess the applicability of transient liquid phase bonding of two dissimilar super-alloys with different interlayers. The effect of using three types of interlayer such as BNi-2, BNi-3, and BNi-9 on microstructure and mechanical properties was studied in the GTD-111/IN-718 system at 1100 ℃ for different bonding time. To determine the compositional changes and microstructure in the joint region, field emission scanning electron microscopy equipped with energy dispersive spectroscopy was utilized. The formation of Ni_(3)B in the athermally solidified zone(ASZ) is controlled by the B content and, accordingly, the morphology of Ni_(3)Si is governed by the Si content. The Cr content might impede the relocation of B from the interlayer into the base metal and the formation of CrB inside the ASZ is dominated by the Cr content. The high micro-hardness of the eutectic compounds is originated from the formation of boride matrixes such as Ni or Cr boride. The shear strength of the joint using BNi-9 after the completion of isothermal solidification is lower compared that that using BNi-3 and BNi-2, which could be related to the absence of Si in the filler metals constituent and the significant presence of Cr in BNi-9. 展开更多
关键词 transient liquid phase bonding Ni-based superalloy isothermal solidification Ni-B compounds
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New insights into microstructural changes during transient liquid phase bonding of GTD-111 superalloy 被引量:2
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作者 Javad ASADI Seyed Abdolkarim SAJJADI Hamid OMIDVAR 《Transactions of Nonferrous Metals Society of China》 SCIE EI CAS CSCD 2021年第9期2703-2715,共13页
The effects of joining temperature(TJ)and time(tJ)on microstructure of the transient liquid phase(TLP)bonding of GTD-111 superalloy were investigated.The bonding process was applied using BNi-3 filler at temperatures ... The effects of joining temperature(TJ)and time(tJ)on microstructure of the transient liquid phase(TLP)bonding of GTD-111 superalloy were investigated.The bonding process was applied using BNi-3 filler at temperatures of 1080,1120,and 1160℃ for isothermal solidification time of 195,135,and 90 min,respectively.Homogenization heat treatment was also applied to all of the joints.The results show that intermetallic and eutectic compounds such as Ni-rich borides,Ni−B−Si ternary compound and eutectic-γcontinuously are formed in the joint region during cooling.By increasing tJ,intermetallic phases are firstly reduced and eventually eliminated and isothermal solidification is completed as well.With the increase of the holding time at all of the three bonding temperatures,the thickness of the athermally solidified zone(ASZ)and the volume fraction of precipitates in the bonding area decrease and the width of the diffusion affected zone(DAZ)increases.Similar results are also obtained by increasing TJ from 1080 to 1160℃ at tJ=90 min.Furthermore,increasing the TJ from 1080 to 1160℃ leads to the faster elimination of intermetallic phases from the ASZ.However,these phases are again observed in the joint region at 1180℃.It is observed that by increasing the bonding temperature,the bonding width and the rate of dissolution of the base metal increase.Based on these results,increasing the homogenization time from 180 to 300 min leads to the elimination of boride precipitates in the DAZ and a high uniformity of the concentration of alloying elements in the joint region and the base metal. 展开更多
关键词 TLP bonding joint GTD-111 superalloy isothermal solidification MICROSTRUCTURE HOMOGENIZATION
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SFOD-LPME-HPLC测定金线莲中对羟基苯乙酮和香草乙酮 被引量:2
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作者 杨晓灵 廖小英 +2 位作者 黄媛 潘清清 黄丽英 《中国医院药学杂志》 CAS CSCD 北大核心 2016年第24期2156-2161,共6页
目的:建立漂浮有机液滴凝固液相微萃取-高效液相色谱(SFOD-LPME-HPLC)法测定金线莲中对羟基苯乙酮和香草乙酮含量的方法。方法:利用SFOD-LPME技术对中药材金线莲中低峰度组分对羟基苯乙酮和香草乙酮进行富集,最后运用HPLC进行分析。优... 目的:建立漂浮有机液滴凝固液相微萃取-高效液相色谱(SFOD-LPME-HPLC)法测定金线莲中对羟基苯乙酮和香草乙酮含量的方法。方法:利用SFOD-LPME技术对中药材金线莲中低峰度组分对羟基苯乙酮和香草乙酮进行富集,最后运用HPLC进行分析。优化后的萃取实验条件:60μL的十二醇为萃取溶剂,1 000μL的四氢呋喃为分散溶剂,15 mL样液加入氯化钠4.50 g,pH为4.0,40℃水浴,以1 500 r·min^(-1)转速搅拌萃取40 min。色谱条件:色谱柱:Agilent TC-C18(4.6 mm×250mm,5μm);流动相:甲醇-0.1%乙酸(25∶75);流速:1.0mL·min^(-1);柱温:31.5℃;检测波长:275 nm。结果:对羟基苯乙酮和香草乙酮的线性范围均为2~24 ng·mL^(-1),检测限分别为0.06 ng·mL^(-1)和0.17 ng·mL^(-1),富集倍数分别为166和140,测得福建南靖组培金线莲中对羟基苯乙酮和香草乙酮的含量分别为1.69μg·g^(-1)和0.72μg·g^(-1),回收率在95.29%~104.30%之间。结论:该法具有集富集、净化于一体的特点,可成为简单、可靠、快速的中药质量控制前处理和测定方法。 展开更多
关键词 漂浮有机液滴凝固液相微萃取 高效液相色谱 金线莲 对羟基苯乙酮 香草乙酮 富集倍数
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