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N,N-二甲氨基乙酸盐酸盐的合成研究 被引量:2
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作者 熊燕 胡志勇 《应用化工》 CAS CSCD 2007年第1期72-73,共2页
以氯乙酸和二甲胺水溶液为反应原料,合成了N,N-二甲氨基乙酸(DMG),加入浓盐酸得到N,N-二甲氨基乙酸盐酸盐(DMGC)晶体,并通过IR对其结构进行了表征。同时考查了原料投料比、反应温度、反应时间对反应产率的影响。实验发现较优反应条件为... 以氯乙酸和二甲胺水溶液为反应原料,合成了N,N-二甲氨基乙酸(DMG),加入浓盐酸得到N,N-二甲氨基乙酸盐酸盐(DMGC)晶体,并通过IR对其结构进行了表征。同时考查了原料投料比、反应温度、反应时间对反应产率的影响。实验发现较优反应条件为:二甲胺和氯乙酸的摩尔比为3∶1,反应时间10 h,反应温度为70℃,此时收率能达到80%。 展开更多
关键词 氯乙酸 二甲胺 n n-二甲氨基乙酸盐酸 合成
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微波辐射合成N,N-二甲氨基乙酸盐酸盐的研究
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作者 王升文 高桂枝 +1 位作者 宋延卫 李丕高 《化学与生物工程》 CAS 2010年第7期31-33,共3页
在微波辐射下,以氯乙酸和二甲胺为原料合成了N,N-二甲氨基乙酸盐酸盐。采用单因素实验研究了原料配比、反应温度、微波辐射功率、微波辐射时间等因素对产物收率的影响,并用红外光谱对产物进行了表征。结果表明,在n(氯乙酸)∶n(二甲胺)=1... 在微波辐射下,以氯乙酸和二甲胺为原料合成了N,N-二甲氨基乙酸盐酸盐。采用单因素实验研究了原料配比、反应温度、微波辐射功率、微波辐射时间等因素对产物收率的影响,并用红外光谱对产物进行了表征。结果表明,在n(氯乙酸)∶n(二甲胺)=1∶3.0、反应温度为65℃、微波辐射功率为500 W、微波辐射时间为150 min的优化反应条件下,N,N-二甲氨基乙酸盐酸盐的收率达86.02%。 展开更多
关键词 n n-二甲氨基乙酸盐酸 微波辐射 氯乙酸 二甲胺
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首批盐酸西布曲明2个去甲基衍生物化学对照品的研制 被引量:2
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作者 吴先富 张娜 +1 位作者 马玲云 肖新月 《药物分析杂志》 CAS CSCD 北大核心 2013年第11期2005-2008,共4页
目的:建立供含量测定用的盐酸西布曲明两个去甲基衍生物(盐酸N-单去甲基西布曲明和盐酸N,N-双去甲基西布曲明)的首批化学对照品。方法:应用UV、IR、NMR和ESI-MS对盐酸N-单去甲基西布曲明和盐酸N,N-双去甲基西布曲明对照品进行结构鉴定,... 目的:建立供含量测定用的盐酸西布曲明两个去甲基衍生物(盐酸N-单去甲基西布曲明和盐酸N,N-双去甲基西布曲明)的首批化学对照品。方法:应用UV、IR、NMR和ESI-MS对盐酸N-单去甲基西布曲明和盐酸N,N-双去甲基西布曲明对照品进行结构鉴定,并采用HPLC法、醇中碱电位滴定法和高氯酸非水电位滴定法进行纯度分析和含量测定。结果:HPLC测得两者的纯度分别为99.15%和99.33%;醇中碱电位滴定法测得两者的含量分别为101.3%和101.2%;高氯酸非水电位滴定法测得两者的含量分别为101.2%和100.6%。结论:本文中建立的醇中碱滴定法简便、准确、无汞污染,适用于盐酸西布曲明2个去甲基衍生物的含量测定。盐酸N-单去甲基西布曲明和盐酸N,N-双去甲基西布曲明对照品的建立为减肥类保健食品中非法添加西布曲明衍生物的检测和监督提供有力支持。 展开更多
关键词 盐酸n-单去甲基西布曲明 盐酸n n-双去甲基西布曲明 对照品 结构鉴定 有关物质 醇中碱滴定 高氯酸电位滴定 含量测定
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NHD脱硫溶液中硫化物的测定——N,N-二甲基对苯二胺盐酸盐光度法
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作者 司朝辉 《大氮肥》 CAS 2008年第4期278-281,共4页
建立了NHD溶液中硫化物的N,N-二甲基对苯二胺盐酸盐光度法测定方法,研究了测定条件对测定结果的影响。结果表明,在恒温条件下,通过氮气汽提(吹气)的方法,N,N-二甲基对苯二胺盐酸盐光度法可以测定NHD溶液中硫化物,硫离子浓度线性范围为0... 建立了NHD溶液中硫化物的N,N-二甲基对苯二胺盐酸盐光度法测定方法,研究了测定条件对测定结果的影响。结果表明,在恒温条件下,通过氮气汽提(吹气)的方法,N,N-二甲基对苯二胺盐酸盐光度法可以测定NHD溶液中硫化物,硫离子浓度线性范围为0~1.0mg/L,摩尔吸光系数为1.69×104,用于实际样品的测定,其精密度和准确度符合要求。 展开更多
关键词 n n-二甲基对苯二胺盐酸 硫化物 测定
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阻挡层CMP中盐酸胍对铜和钽抛光速率的影响 被引量:7
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作者 李海龙 刘玉岭 +2 位作者 王辰伟 张宏远 高娇娇 《微纳电子技术》 CAS 北大核心 2013年第9期586-591,共6页
在铜互连超大规模集成电路(ULSI)中,由于铜和钽的物理化学性质的差异造成两者的去除速率不同,导致布线晶圆表面抛光后出现碟形坑等缺陷。针对该问题,研究了盐酸胍(CH5N3·HCl)对Cu和Ta去除速率选择性的影响。根据Cu和Ta的CMP机理,... 在铜互连超大规模集成电路(ULSI)中,由于铜和钽的物理化学性质的差异造成两者的去除速率不同,导致布线晶圆表面抛光后出现碟形坑等缺陷。针对该问题,研究了盐酸胍(CH5N3·HCl)对Cu和Ta去除速率选择性的影响。根据Cu和Ta的CMP机理,通过在有氧化剂和无氧化剂环境下的实验对比,以及不同质量分数的盐酸胍对Cu和Ta去除速率选择性的影响,对盐酸胍在钽CMP中的作用进行了定性和定量分析,确定并优化了盐酸胍及氧化剂的含量,使钽的去除速率快于铜的去除速率。应用上述抛光液对300mm布线晶圆进行阻挡层抛光实验,通过对碟形坑的检测,证明了该种抛光液能够高速、有效地修正碟形坑。 展开更多
关键词 盐酸胍(CH5n3·HCl) 化学机械抛光(CMP) 阻挡层 钽(Ta) 选择性 碟形坑
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Nitrate-Nitrogen Dynamics and Nitrogen Budgets in Rice-Wheat Rotations in Taihu Lake Region, China 被引量:3
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作者 ZHANG Jun-Hua LIU Jian-Li +2 位作者 ZHANG Jia-Bao CHENG Ya-Nan WANG Wei-Peng 《Pedosphere》 SCIE CAS CSCD 2013年第1期59-69,共11页
Nitrate-nitrogen (NO3-N) dynamics and nitrogen (N) budgets in rice (0ryza sativa L.)-wheat (Triticum aestivum L.) rotations in the Taihu Lake region of China were studied to compare the effects of N fertilizer... Nitrate-nitrogen (NO3-N) dynamics and nitrogen (N) budgets in rice (0ryza sativa L.)-wheat (Triticum aestivum L.) rotations in the Taihu Lake region of China were studied to compare the effects of N fertilizer management over a two-year period. The experiment included four N rates for rice and wheat, respectively: N1 (125 and 94 kg N ha-1), N2 (225 and 169 kg N ha-1), N3 (325 and 244 kg N ha-1), and NO (0 kg N ha-1). The results showed that an overlying water layer during the rice growing seasons contributed to moderate concentrations of NO3-N in sampled waters and the concentrations of NO3-N only showed a rising trend during the field drying stage. The NO3-N concentrations in leachates during the wheat seasons were much higher than those during the rice seasons, particularly in the wheat seedling stage. In the wheat seedling stage, the NO3-N concentrations of leachates were significantly higher in N treatments than in NO treatment and increased with increasing N rates. As the NO3-N content (below 2 mg N L-1) at a depth of 80 cm during the rice-wheat rotations did not respond to the applied N rates, the high levels of NO3-N in the groundwater of paddy fields might not be directly related to NO3-N leaching. Crop growth trends were closely related to variations of NO3-N in leachates. A reduction in N application rate, especially in the earlier stages of crop growth, and synchronization of the peak of N uptake by the crop with N fertilizer application are key measures to reduce N loss. Above-ground biomass for rice and wheat increased significantly with increasing N rate, but there was no significant difference between N2 and N3. Increasing N rates to the levels greater than N2 not only decreased N use efficiency, but Mso significantly increased N loss. After two cycles of rice-wheat rotations, the apparent N losses of N1, N2 and N3 amounted to 234, 366 and 579 kg N ha-1, respectively. With an increase of N rate from NO to N3, the percentage of N uptake in total N inputs decreased from 63.9% to 46.9%. The apparent N losses during the rice seasons were higher than those during the wheat seasons and were related to precipitation; therefore, the application of fertilizer should take into account climate conditions and avoid application before heavy rainfall. 展开更多
关键词 above-ground biomass crop uptake nitrate-nitrogen leaching nitrogen mineralization nitrogen transport
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Synthesis and Crystal Structure of Bis(nitrate)- bis(N,N'-dimethyl-N,N'-dibenzenyl-urea)uranyl(Ⅱ) 被引量:1
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作者 ZHU Li-Ming LI Bao-Long② CAO Zheng-Bai ZHANG Yong (College of Chemistry and Chemical Engineering, Suzhou University, Suzhou 215006, China) 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 北大核心 2003年第5期521-524,共4页
The new uranyl complex UO2(NO3)2[PhN(CH3)C(O)(CH3)NPh]2 was synthesized and its crystal structure has been determined by single-crystal X-ray diffraction. Crystal data: C30H32N6O10U, triclinic, space group P with a = ... The new uranyl complex UO2(NO3)2[PhN(CH3)C(O)(CH3)NPh]2 was synthesized and its crystal structure has been determined by single-crystal X-ray diffraction. Crystal data: C30H32N6O10U, triclinic, space group P with a = 7.772(1), b = 9.267(1), c = 12.644(1) ? a = 68.246(8), b = 73.871(9), g = 84.99(1)o, V = 812.4(2) ?, Mr = 874.65, Z = 1, Dc = 1.788 g/cm3, F(000) = 426, m = 5.062 mm-1, the final R = 0.022 and wR = 0.059 for 3571 observed reflections (I > 2s(I)). The central uranyl ion is coordinated by six oxygen atoms, two from the carbonyl groups of N,N-dimethyl-N,N-dibenzenyl-urea molecules and the other four from two nitrate groups. 展开更多
关键词 substituted urea uranyl complex synthesis crystal structure
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Industrial Synthesis of N-Methylhydroxylamine Hydrochloride by Electrochemical Reduction of Nitromethane 被引量:2
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作者 甘永平 张文魁 +2 位作者 黄辉 夏新辉 陈永胜 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2006年第5期649-653,共5页
An industrial electrolytic cell was designed for the electrochemical synthesis of N-methylhydroxylamine hydrochloride (N-MHA). Copper was used as the cathode, graphite as the anode, and a cation membrane as the sepa... An industrial electrolytic cell was designed for the electrochemical synthesis of N-methylhydroxylamine hydrochloride (N-MHA). Copper was used as the cathode, graphite as the anode, and a cation membrane as the separator. The results show that N-MHA with a high purity of 99% can be electrosynthesized directly from nitromethane in HC1 solution. Under a constant current of 1000-2500A.m^-2 in the temperature of 30-50℃, the average yield, current efficiency, and reaction selectivity were 65%, 70%, and 99%, respectively. Graphite electrode and membrane material can be used continuously in the preparative electrolysis for 5000h. Moreover, the effects of the electrode and membrane materials, current intensity, electrolyte temperature, and other associated parameters on the electrosynthesis results were investigated. The direct current power consumption was 8151.3kW-h-(1000kg N-MHA)^ -1. This method is a simple separation process with limited contamination and hence, is a new green synthesis method for the industrial production of N-MHA. 展开更多
关键词 n-methylhydroxylamine hydrochloride ELECTROSYnTHESIS nITROMETHAnE
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UPLC-MS/MS法快速测定减肥类中成药及保健食品中非法添加15种化学药的研究 被引量:31
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作者 詹淑玉 朱琦峰 +1 位作者 徐宏祥 傅应华 《中草药》 CAS CSCD 北大核心 2016年第17期3023-3031,共9页
目的建立一种快速、准确检测减肥类中成药及保健食品中非法添加15种化学药的方法。方法采用UPLC-MS/MS法,以Waters Acquity BEH-C18柱(100 mm×2.1 mm,1.7μm)为色谱柱,以0.1%甲酸甲醇溶液(A)-0.1%甲酸水溶液(B)为流动相,梯... 目的建立一种快速、准确检测减肥类中成药及保健食品中非法添加15种化学药的方法。方法采用UPLC-MS/MS法,以Waters Acquity BEH-C18柱(100 mm×2.1 mm,1.7μm)为色谱柱,以0.1%甲酸甲醇溶液(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱:0-3 min,33%-45%A;3-5 min,45%-55%A;5-7 min,55%-70%A;7-9 min,70%-80%A;9-10 min,80%-90%A;10-11 min,90%-33%A;11-13 min,33%A;体积流量0.2 m L/min;柱温40℃。选择ESI离子源、正离子扫描、多反应监测(MRM)模式测定15种临床常用的化学减肥药,通过比较MRM通道中样品峰与对照品峰的分子离子峰、二级碎片离子峰、色谱保留时间等信息确定添加的化学药物,并根据外标法以质谱峰面积计算添加药物的准确量。结果在上述色谱及质谱条件下,硫酸特布他林、盐酸麻黄碱、茶碱、咖啡因、多索茶碱、盐酸克仑特罗、盐酸妥洛特罗、盐酸班布特罗、盐酸芬氟拉明、呋塞米、吲达帕胺、酚酞、盐酸西布曲明、盐酸N-单去甲基西布曲明、盐酸N,N-双去甲基西布曲明等15种化学药物的分离良好,方法检测限(LOD)均在0.1-5.0 ng/g,定量限(LOQ)均在0.3-15.0ng/g,标准加样回收率均在91.8%-110.8%。在86批样品(包括胶囊、颗粒剂等不同基质类型)中检出74批添加了化学药,阳性率为86.0%,样品中主要检出盐酸西布曲明(39批)、呋塞米(20批)、酚酞(23批)、茶碱(1批)、咖啡因(15批),其中检出2种的22批,3种的1批。相较而言,未明确标示生产厂家的产品中非法添加更严重。结论方法简便、准确,灵敏度高,可作为减肥类中成药及保健食品中非法添加15种化学药的定性定量方法。 展开更多
关键词 UPLC-MS/MS 化学药物 中成药 保健食品 非法添加 硫酸特布他林 盐酸麻黄碱 茶碱 咖啡因 多索茶碱 盐酸克仑特罗 盐酸妥洛特罗 盐酸班布特罗 盐酸芬氟拉明 呋塞米 吲达帕胺 酚酞 盐酸西布曲明 盐酸n-单去甲基西布曲明 盐酸n n-双去甲基西布曲明
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N-methyl-2-(2-nitrobenzylidene) hydrazine carbothioamide——A new corrosion inhibitor for mild steel in 1 mol·L^(-1)hydrochloric acid
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作者 K.Krishnaveni K.Sampath +1 位作者 J.Ravichandran C.Jayabalakrishnan 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2015年第11期1916-1922,共7页
The corrosion inhibition of mild steel in 1 mol·L^(-1) hydrochloric acid by N-methyl-2-(2-nitrobenzylidene)hydrazine carbothioamide(MNBHC) was studied using weight loss and electrochemical studies.Results obtaine... The corrosion inhibition of mild steel in 1 mol·L^(-1) hydrochloric acid by N-methyl-2-(2-nitrobenzylidene)hydrazine carbothioamide(MNBHC) was studied using weight loss and electrochemical studies.Results obtained indicate that the inhibitor is effective in hydrochloric acid medium and the efficiency decreases with increase in temperature.Added halide additives improve the efficiency of the inhibitor.The AC impedance studies reveal that the process of inhibition is through charge transfer.Polarization studies indicate the mixed nature of the inhibitor.From the thermodynamic,spectral and surface analyses the nature of adsorption has been found out.The adsorption of the inhibitor on mild steel follows the Langmuir isotherm. 展开更多
关键词 Mild steelEISMass lossSEMAcid corrosion
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Evaluating the Validity of a Nitrate Quick Test in Different Chinese Soils
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作者 YUE Xian-Lu LI Fei +4 位作者 HU Yun-Cai ZHANG Huai-Zhi JI Hong-Jie ZHANG Wei-Li U. SCHMIDHALTER 《Pedosphere》 SCIE CAS CSCD 2012年第5期623-630,共8页
Because laboratory tests are expensive and time-consuming and may not be available to farmers, soil nitrate quick tests are required for optimal nitrogen management strategies in China to increase nitrogen use efficie... Because laboratory tests are expensive and time-consuming and may not be available to farmers, soil nitrate quick tests are required for optimal nitrogen management strategies in China to increase nitrogen use efficiency and to reduce nitrogen losses. A total of 328 soil samples were collected at different soil depths from 225 sites in China, which covered a wide range of climatic and geographic regions, soil types, croplands and soil textures, to evaluate the suitability of a quick reflectometer test method for analysing soil NO3-N in a wide range of soil NO3 concentrations, soil types and cropping systems in China, mainly by comparison of soil NO3-N assessed by a quick-test method (a reflectometer) and a standard laboratory method, i.e., high-performance liquid chromatography (HPLC). The reflectometer showed excellent agreement with the laboratory HPLC method with regard to soil nitrate contents for all analysed soil samples. The linear regression had slopes of 1 ± 0.08 and intercepts of ± 1.38 mg NO(-,3)-N L^(-1) among different soil types and croplands. Compared with the 1:1 lines, the regression analysis for each soil type showed statistically significant but small differences in slope; the relative difference between the values measured using the two analytical systems varied from -8% to 6%, and there were no differences in intercept except for paddy soil. The reflectometer showed adequate, statistically significant precision in determining soil nitrate contents, and it could therefore be directly used instead of the laboratory methods for soil NO(-,3)-N measurement in China. 展开更多
关键词 DILUTIOn n recommendation nitrate test strip REFLECTOMETER soil nO(3 -)-n
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季铵盐壳聚糖纳米荧光探针的制备及细胞渗入研究 被引量:5
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作者 刘璠娜 饶华新 张子勇 《功能材料》 EI CAS CSCD 北大核心 2008年第5期857-860,863,共5页
将异硫氰酸荧光素(FITC)接枝到N,N,N-三甲基壳聚糖盐酸盐(TMC)的侧基上,制备了荧光标记的壳聚糖衍生物TMC-g-FITC。其水溶液与羧甲基壳聚糖(CMC)水溶液经凝聚复合,制备了TMC-g-FITC/CMC纳米粒子荧光探针。用激光散射仪和透... 将异硫氰酸荧光素(FITC)接枝到N,N,N-三甲基壳聚糖盐酸盐(TMC)的侧基上,制备了荧光标记的壳聚糖衍生物TMC-g-FITC。其水溶液与羧甲基壳聚糖(CMC)水溶液经凝聚复合,制备了TMC-g-FITC/CMC纳米粒子荧光探针。用激光散射仪和透射电镜表征了该纳米荧光探针的粒径、粒径分布、Zeta电位值和形态结构。结果表明,纳米粒子的粒径在150-360nm范围,粒径分布约为0.10,Zeta电荷值为正值。用MTT法检测了其细胞毒性,发现纳米粒子对细胞的抑制作用较弱,在实验浓度下细胞的抑制率均低于7%。通过激光共聚焦显微镜研究了TMC-g-FITC/CMC纳米粒子荧光探针对HepG2细胞的渗透和迁移过程:纳米粒子先是在细胞周围富集,然后逐渐渗入细胞的内部,最后直至进入细胞核。 展开更多
关键词 n n n-三甲基壳聚糖盐酸 羧甲基壳聚糖 异硫氰酸荧光素 纳米粒子 荧光探针
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潘氨酸的一种合成方法
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作者 匡滨海 郭惠 张泉 《江西医学院学报》 2003年第6期13-13,共1页
关键词 潘氨酸 合成方法 n n-二甲基甘氨酸盐酸 元素分析
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3,5-二氯-2-戊酮的合成研究 被引量:2
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作者 陈明明 刘伟 +2 位作者 陈蒙慈 曾雪云 陈明 《精细化工中间体》 CAS 2015年第1期36-38,49,共4页
以α-氯-α-乙酰基-γ-丁内酯、固体光气为原料,N,N-二甲基哌啶盐酸盐为催化剂合成了3,5-二氯-2-戊酮。考察了催化剂种类、氮气通入速率、物料配比、滴加时间、滴加温度等因素对反应的影响。优化条件下,3,5-二氯-2-戊酮的含量94.0%,收率... 以α-氯-α-乙酰基-γ-丁内酯、固体光气为原料,N,N-二甲基哌啶盐酸盐为催化剂合成了3,5-二氯-2-戊酮。考察了催化剂种类、氮气通入速率、物料配比、滴加时间、滴加温度等因素对反应的影响。优化条件下,3,5-二氯-2-戊酮的含量94.0%,收率81.5%(以α-氯-α-乙酰基-γ-丁内酯计)。 展开更多
关键词 α-氯-α-乙酰基-γ-丁内酯 固体光气 n n-二甲基哌啶盐酸 3 5-二氯-2-戊酮 合成
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贝前列素钠(Beraprost)侧链中间体3-甲基-2-氧代-5-庚炔基磷酸二甲酯的合成
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作者 许程桃 张玉柳 +6 位作者 刘婷 余善宝 李辉 占莉 罗宇 汤杰 杨帆 《合成化学》 CAS CSCD 北大核心 2018年第11期859-862,共4页
报道了一种合成贝前列素钠(Beraprost)侧链中间体的新方法。以丙酸酐和N,O-二甲基羟胺盐酸盐为原料,经三步反应以总收率57%合成了贝前列素钠中间体3-甲基-2-氧代-5-庚炔基磷酸二甲酯,其结构经1H NMR,13C NMR和HR-MS(ESI)确证。并对反应... 报道了一种合成贝前列素钠(Beraprost)侧链中间体的新方法。以丙酸酐和N,O-二甲基羟胺盐酸盐为原料,经三步反应以总收率57%合成了贝前列素钠中间体3-甲基-2-氧代-5-庚炔基磷酸二甲酯,其结构经1H NMR,13C NMR和HR-MS(ESI)确证。并对反应条件进行了优化。 展开更多
关键词 贝前列素钠 丙酸酐 n O-二甲基羟胺盐酸 1-碘代-2-丁炔 药物合成
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