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1.
铜(Ⅰ)—苯骈三氮唑络合吸附波的极谱研究与应用 总被引:4,自引:0,他引:4
本文在0.6mol/L NH3-NH4Cl缓冲溶液(pH=9.8)中,Cu(Ⅱ)在滴汞电极上还原生成Cu(Ⅰ),可与苯骈三氮唑(BTA)络合,产生一灵敏的络合吸附波,Ep=-0.73V(us,SCE)。苯骈三氮唑的浓度在0.40-10.0mg/L范围内与极谱波峰高呈线性关系,检测下限为0.40mg/L,相对标准偏差为1.4%-3.2%;回收率为97.5%-101.5%。 相似文献
2.
5,10,15,20—四(3—溴—4—磺酸苯基)卟啉高效液相色谱法测定河水中微量… 总被引:4,自引:1,他引:4
研究了新合成的显色剂5,10,15,20-四(3-溴-4-磺酸苯基)卟啉与Co(Ⅱ)、Zn(Ⅱ)、Cu(Ⅱ)形成配合物离子的反应,在ZORBAX ODS柱上,用含20mmol/L乙酸-乙酸钠(pH6.0)和10mmol/L四乙基碘化铵的乙腈-水(27:73,V/V)流动相洗脱,在420nm波长下检测。Co(Ⅱ)、Zn(Ⅱ)、Cu(Ⅱ)螯合物在9min内获得完全分离,检测限分别为0.2ng,0.05 相似文献
3.
研究了新合成的显色剂5,10,15,20-四(3-溴-4磺酸苯基)卟啉与Co(Ⅱ)、Zn(Ⅱ)、Cu(Ⅱ)形成配合物离子的反应,在ZORBAXODS柱上,用含20mmol/L 乙酸-乙酸钠(pH6.0)和10mmol/L四乙基碘化铵的乙腈-水(27:73,V/V)流动相洗脱,在420nm波长下检测。Co(Ⅱ)、Zn(Ⅱ)、Cu(Ⅱ)赘合物在9min内获得完全分离,检测限分别为0.2ng,0.05ng和0.09ng。该方法已用于河水样中钴、锌、铜的测定。 相似文献
4.
铂—钯共显色衍生络合物的高效液相色谱研究 总被引:1,自引:3,他引:1
研究了Pd(Ⅱ)和4,4'-二(二乙氨基)苯硫酮(BDPTK)共显色所生成的Pt(Ⅱ)络合物,于Nucleosil C8柱上,用含3×10^-3mol/L CSA和0.02mol/L HAc-NaAc(pH3.5)的乙腈-丙酮-水(72:5:23,V/V)作流动相(1.0ml/min)分离并检测。Pt的校正曲线的线性范围为0.2~3.0μg/ml,Pt检测限为0.7ng。此方法已应用于抗癌药物顺铂 相似文献
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肿瘤细胞中长春新碱的高效液相色谱法测定 总被引:10,自引:0,他引:10
长春新碱(VCR)为重要和常用抗肿瘤药物之一。肿瘤细胞耐药性是导致化疗失败的主要原因。为了筛选耐药细胞的逆转剂,建立了测定肿瘤细胞内VCR浓度的高效液相色谱法,色谱条件为:Zorbax-ODS反相柱25cm×4.6mmi.d.,流动相:0.02mol/LK2HPO4(pH6.6)∶CH3OH(20∶80,V/V),流速:1.0mL/min,检测波长:267nm。方法简单、快速、选择性好,在10~200mg/L范围内VCR浓度-峰高呈良好的线性关系(r=0.9998),仪器灵敏度为4ng。 相似文献
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用2—羟基—3—羧基—5—磺酸基苯重氮氨基偶氮苯流动注射分光光度法测定汞 总被引:7,自引:1,他引:7
研究了在乳化剂OP存在下,2-羟基-3-羧基-5-磺酸基苯重氮氨基偶氮苯(HCSDAA)-汞(Ⅱ)显色体系流动注射分光光度法。用PH10.0-10.5的Na2B4O7-NaOH缓冲溶液作载流,汞(Ⅱ)与HCSDAA和乳化剂OP的混合试剂反应形成红色络合物。用于测定汞时,方法的线性范围是0.05-1.0mg/L,检测限为0.016mg/L,进样频率为100样/h。直接应用于头发、自来水和废水中微量汞 相似文献
8.
吲哚乙酸与磷钼黄反应及其极谱分析的研究 总被引:1,自引:0,他引:1
在NH3-NH4Cl缓冲溶液中(pH=9.5),吲哚乙酸与磷钼黄的还原产物在滴汞电极上于-1.10V(vs.SCE)处产生一灵敏的极谱波,该波波高与吲哚乙酸的浓度在1.0×10-7-5.0×10-6mol/L范围内成线性关系,检测下限为5.0×10-8mol/L。如在上述还原产物中加入偶氮胭脂红B、孔雀绿、甲基紫等染料及聚乙烯醇,可使极谱波的灵敏度提高,使吲哚乙酸的浓度在5.0×10-8-1.0×10-6mol/L范围内与波高成线性关系,检测下限降低至1.0×10-8mol/L。 相似文献
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4—(6—甲基—2—苯并噻唑偶氮)间苯三酚反相高效液相色谱分离测定钒钴镍铬 总被引:2,自引:1,他引:2
作以新研制的4-(6-甲基-2-苯并噻唑偶氮)间苯三酚为柱前衍生试剂,用含10mmol/L的pH6.80的HAc-NaAc缓冲溶液,10mmol/L TBA.Br和1×10^-4mol/LEDTA的甲醇-水溶液(78:22,V/V)作流动相,在C18柱上,11min内反相HPLC分离测定了Cr(Ⅵ),V(Ⅴ),Co(Ⅱ),Ni(Ⅱ)。当S/N=3时,其检出限分别是V(Ⅴ)5.45ng,Co(Ⅱ) 相似文献
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反相高效液相色谱柱前衍生荧光法测定肠粘膜中的谷氨酰胺 总被引:1,自引:0,他引:1
以邻苯二甲醛及3-巯基丙酸为衍生试剂,50mmol/L磷酸缓冲液(pH7.0)-乙腈(94∶6,V/V)为流动相,在LichrosorbRP18(150mm×4.6mmi.d.,5μm)柱上,研究并建立了测定动物肠粘膜中谷氨酰胺(Gln)的柱前衍生荧光RP-HPLC法。样品与衍生剂按4∶1进行衍生反应,Ex=230nm,Em=389nm;流速为2.0mL/min。Gln的保留时间为3.158min,检测限为25μmol/L(S/N=3.5),线性范围为50~3200μmol/L,r=0.9996。 相似文献
11.
4-(S)-[2-(N-甲基)吗啉基 ]-5-(R )-(l-薄荷烷氧基 )-丁内酯结构分析 总被引:1,自引:0,他引:1
N-甲基吗啉对5-(l-薄荷烷氧基)-2(5H)-呋喃酮的光催化不对称共轭加生成了4-(S)-[2-(N-甲基)吗啉基]-5-(R)-(l-薄荷烷氧基)-丁内酯,在四氢呋喃(THF)对比实验、参比物^13CNMR对照及不同溶剂^13CNMR测定的基础上,该新化合物的结构用高分辨率的子核磁共振谱、碳核磁共振谱、质谱、红外光谱及元素分析、旋光度等数据进行了确证。 相似文献
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Introduction Pyrazole and its derivatives represent one of the most active classes of compounds possessing a wide spectrum of biological activities. During the past years, considerable evidence has been accumulated to demon-strate the efficacy of pyrazole derivatives including an-tibacterial,1 antifungal,2 herbicidal,3 insecticidal4 and other biological activities.5-7 Up to now, a great variety of these kind of compounds have been synthesized, among which some commercially pesticides have been… 相似文献
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Thierry Cassagne Henri‐Jean Cristau Grard Delmas Michel Desgranges Claude Lion Gilbert Magnaud liane Torreilles David Virieux 《Heteroatom Chemistry》2001,12(6):485-490
Reactions of O‐ethyl S‐(2‐diisopropyl‐amino)ethyl methylphosphonothiolate, VX 1 , were investigated with five oxidizing agents. In all the cases, the formation of the VX N‐oxide 7 was observed prior to the subsequent oxidation and hydrolysis into the nontoxic O‐ethyl methylphosphonate 2. Magnesium monoperoxyphthalate (MMPP) is probably one of the most active reagents to achieve the complete detoxification of VX 1 . The decontamination using MMPP was also extended with success to soman 13 , a G‐type agent. © 2001 John Wiley & Sons, Inc. Heteroatom Chem 12:485–490, 2001 相似文献
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Synthesis and Crystal Structure of Ethyl2—(2—Amino—3—ethoxycarbonyl—4H—benzopyran—4—yl)cyanoacetate 总被引:1,自引:0,他引:1
1 INTRODUCTION Inorganic solid supports as catalysts resulting in higher selectivity, milder conditions and easier work-up have been reported as useful catalysts for many reactions [1~3]. Recently, we have reported the Knoevenagel condensation catalyzed by KF-Al2O3[4]. In this paper, we discussed the crystal structure of the title compound synthesized by the reaction of salicylaldehyde and ethyl cyanoacetate in DMF using the catalyst KF-Al2O3 at room temperature KF-Al2O3. In or… 相似文献
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ZHANG Yanga HUANG Jiea SONG Ji-Rongb② REN Ying-Huia XU Kang-Zhena a 《结构化学》2008,27(2):195-199
4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data: C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309(3), b = 0.67682(6), c = 1.74237(19) nm, β = 114.744(3)°, V= 2.7106(5) nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F(000) = 1200, Z= 8, R= 0.0514 and wR= 0.1529. 相似文献
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4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine,potassium thiocyanate and methyl chloroformate in ethyl acetate.Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamidc at room temperature.The crystal structure was determined by X-ray diffraction analysis.Crystallographic data:C10H14N4O4S,Mr=286.31,monoclinic,space group C2/c with a=2.5309(3),b=0.67682(6),c=1.74237(19)nm,β=114.744(3)°,V=2.7106(5)nm3,Dc=1.403 g/cm3,μ=0.225mm-1,F(000)=1200,Z=8,R=0.0514 and wR=0.1529. 相似文献
18.
Andersen VF Ørnsø KB Jørgensen S Nielsen OJ Johnson MS 《The journal of physical chemistry. A》2012,116(21):5164-5179
Ethyl propionate is a model for fatty acid ethyl esters used as first-generation biodiesel. The atmospheric chemistry of ethyl propionate was investigated at 980 mbar total pressure. Relative rate measurements in 980 mbar N(2) at 293 ± 0.5 K were used to determine rate constants of k(C(2)H(5)C(O)OC(2)H(5) + Cl) = (3.11 ± 0.35) × 10(-11), k(CH(3)CHClC(O)OC(2)H(5) + Cl) = (7.43 ± 0.83) × 10(-12), and k(C(2)H(5)C(O)OC(2)H(5) + OH) = (2.14 ± 0.21) × 10(-12) cm(3) molecule(-1) s(-1). At 273-313 K, a negative Arrhenius activation energy of -3 kJ mol(-1) is observed.. The chlorine atom-initiated oxidation of ethyl propionate in 980 mbar N(2) gave the following products (stoichiometric yields): ClCH(2)CH(2)C(O)OC(2)H(5) (0.204 ± 0.031), CH(3)CHClC(O)OC(2)H(5) (0.251 ± 0.040), and C(2)H(5)C(O)OCHClCH(3) (0.481 ± 0.088). The chlorine atom-initiated oxidation of ethyl propionate in 980 mbar of N(2)/O(2) (with and without NO(x)) gave the following products: ethyl pyruvate (CH(3)C(O)C(O)OC(2)H(5)), propionic acid (C(2)H(5)C(O)OH), formaldehyde (HCHO), and, in the presence of NO(x), PAN (CH(3)C(O)OONO(2)). The lack of acetaldehyde as a product suggests that the CH(3)CH(O)C(O)OC(2)H(5) radical favors isomerization over decomposition. From the observed product yields, we conclude that H-abstraction by chlorine atoms from ethyl propionate occurs 20.4 ± 3.1%, 25.1 ± 4.0%, and 48.1 ± 8.8% from the CH(3)-, -CH(2)-, and -OCH(2)- groups, respectively. The rate constant and branching ratios for the reaction between ethyl propionate and the OH radical were investigated theoretically using quantum mechanical calculations and transition state theory. The stationary points along the reaction path were optimized using the CCSD(T)-F12/VDZ-F12//BH&HLYP/aug-cc-pVTZ level of theory; this model showed that OH radicals abstract hydrogen atoms primarily from the -OCH(2)- group (80%). 相似文献
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在溶液中,室温下对含有穴醚N8O3配体(H3L)的金属大环化合物[Na(H3L)](ClO4)3H2O(2)和[La(H3L)(OH)2](ClO4)3(3),作了1HNMR谱的测定,在化合物(2)-乙腈溶液中加入过量La(ClO4)3后的(2+La)和化合物(3)还作了13C和1H-1HCOSY(氢-氢相关二维谱)、1H-13CHMQC(氢核检测的异核多量子相干相关谱)及1H-13CHMBC(氢核检测的异核多键相关谱)的NMR谱测定,归属了所有1H,13C的谱线。对其配位行为通过1HNMR试验作了简单的讨论。 相似文献