含氨茂铁异核金属配合物合成和性质研究

Ｐｄ（Ⅱ）、Ｐｔ（Ⅱ）ＤＭＡＦ配合物已合成，并已定结构。本文采用ＭＸ２（Ｍ－Ｎｉ（Ⅱ），Ｃｏ（Ⅱ），Ｚｎ（Ⅱ）、Ｃｕ（Ⅱ）；Ｘ＝Ｃｌ，Ｂｒ，Ｉ）在ＣＨ２Ｃｌ２中和ＤＭＡＦ作用合成［ＭＸ２．２ＤＭＡＦ］型配合物。由ＮｉＣｌ２．２ＤＭＡＦ．Ｃ７Ｈ８晶胞参数推知属于对称链状四配位结构。ＩＲ谱表明，该化合物化学式为ＭＸ２．２ＤＭＡＦ。ＣＶ表明配合物中Ｍ（Ⅱ）和Ｆｅ（Ⅱ）存在。由于金属离子互相影响。Ｅｐ／２     

A NOVEL REACTION BETWEEN Ge－Ge AND Fe－Fe BONDS IN COMPLEX （Me_2GeGeMe_2）［（η~5－C_5H_4）Fe（CO）］_2（μ－CO）_2 AND CRYSTAL STRUCTURE OF THE PRODUCT

ＡＮＯＶＥＬＲＥＡＣＴＩＯＮＢＥＴＷＥＥＮＧｅ－ＧｅＡＮＤＦｅ－ＦｅＢＯＮＤＳＩＮＣＯＭＰＬＥＸ（Ｍｅ_２ＧｅＧｅＭｅ_２）［（η~５－Ｃ_５Ｈ_４）Ｆｅ（ＣＯ）］_２（μ－ＣＯ）_２ＡＮＤＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＯＦＴＨＥＰＲＯＤＵＣＴ￥ＸｉｕＴ?..     

尾式卟啉铁（Ⅲ）电化学性质研究──Ⅱ．二甲胺基／二乙胺基尾式卟啉铁轴向效应的循环伏安行为

本文用循环伏安法研究了一类新型生物模型化合物－氯化－间－［邻－（４－二甲胺基／二乙胺基丁酰胺基苯基）三苯基］卟啉铁（Ⅲ）在不同抗衡阴离子、ＮＯ及轴向含Ｎ有机碱存在下的电化学行为．结果表明：（１）抗衡阴离子对电对Ｆｅ（Ⅲ）／Ｆｅ（Ⅱ）半波电位的影响顺序为Ｃｌ＞Ｂｒ＞ＯＡｃ＞ＣｌＯ４．对电对Ｆｅ（Ⅱ）／Ｆｅ（Ⅰ）的影响则相反．（２）ＮＯ的配位改变了尾端叔胺的配位状态，由于ＮＯ与铁卟啉配位而被活化．（３）由于含Ｎ有机碱的轴向配位，使Ｆｅ（Ⅲ）／Ｆｅ（Ⅱ）和Ｆｅ（Ⅱ）／Ｆｅ（Ⅰ）电对的半波电位发生了很大的位移，位移的变化不仅通过轴向配位，而且通过配位还原来实现．本文还简要地讨论了尾端叔胺的电位调谐作用．     

A NOVEL SYNTHETIC METHOD FOR THE CLUSTERS FeCo_2（CO）_9－（RCCR）（R＝MeO_2C，EtO_2C）．X－RAY CRYSTAL STRUCTURE ANALYSES OF THE CLUSTERS FeCo_2（CO）_9（MeO_2CCCCO_2Me）andCo_4（CO）_（10）－（EtO_2CCCCO_2Et）

ＡＮＯＶＥＬＳＹＮＴＨＥＴＩＣＭＥＴＨＯＤＦＯＲＴＨＥＣＬＵＳＴＥＲＳＦｅＣｏ_２（ＣＯ）_９－（ＲＣＣＲ）（Ｒ＝ＭｅＯ_２Ｃ，ＥｔＯ_２Ｃ）．Ｘ－ＲＡＹＣＲＹＳＴＡＬ　ＳＴＲＵＣＴＵＲＥ　ＡＮＡＬＹＳＥＳ　ＯＦ　ＴＨＥ　ＣＬＵＳＴＥＲＳ　ＦｅＣｏ_２（?..     

低压离子色谱仪的原理及应用

本介绍了一种新型的离子色谱仪，它可以在１．９６－２．９４×１０＾５Ｐａ（约２８－４３Ｐｓｉ）的低压下，分析Ｃｕ＾２＾＋，Ｚｎ＾２＾＋，Ｎｉ＾２＾＋，Ｃｏ＾２＾＋，Ｆｅ（Ⅲ），Ｃｄ＾２＾＋，Ｍｎ＾２＾＋，Ｆｅ＾２＾＋，Ａｌ（Ⅲ），Ｚｒ（Ⅲ），Ｃｒ（Ⅲ），Ｃｒ（Ⅵ）等金属阳离子。中介绍了该仪器的原理及应用。     

反相色谱法分离和间接光度法测定无机阴离子

在化学键合固定相ＯＤＳ柱上,用Ｆｅ（Ｐｈｅｎ）_３~（２＋）作流动相添加剂分离并用间接光度法检测无机阴离子。探讨了主要因素（如流动相中Ｆｅ（Ｐｈｅｎ）_３~（２＋）浓度、有机溶剂浓度、ｐＨ值和离子强度等）对阴离子保留和检测灵敏度的影响。Ｃｌ~－,Ｂｒ~－,ＮＯ_３~－和Ｉ~－具有良好的分离度;间接光度检测波长为Ｆｅ（Ｐｈｅｎ）_３~（２＋）的最大吸收波长５１０ｎｍ。测定这４个离子的校正曲线的线性范围为１～１６０ｍｇ／Ｌ（Ｃｌ~－,Ｂｒ~－,ＮＯ_３~－）和２～３２０ｍｇ／Ｌ（Ｉ~－）;相关系数均达０．９９６。     

含氮茂铁异核金属配合物的合成和性质研究

Ｐｄ（Ⅱ）、Ｐｔ（Ⅱ）ＤＭＡＦ配合物已合成，并已定结构［１］．本文采用ＭＸ２（Ｍ＝Ｎｉ（Ⅱ），Ｃｏ（Ⅱ），Ｚｎ（Ⅱ），Ｃｕ（Ⅱ）；Ｘ＝Ｃｌ，Ｂｒ，Ⅰ）在ＣＨ２Ｃｌ２中和ＤＭＡＦ作用合成［ＭＸ２·２ＤＭＡＦ］型配合物．由ＮｉＣｌ２·２ＤＭＡＦ·Ｃ７Ｈ８晶胞参数推知属于对称链状四配位结构．ＩＲ谱表明，该化合物化学式为ＭＸ２·２ＤＭＡＦ．ＣＶ表明配合物中Ｍ（Ⅱ）和Ｆｅ（Ⅱ）存在．由于金属离子互相影响，Ｅｐ／２随Ｍ（Ⅱ）性质呈规律性变化．     

用Mo（Ⅲ）络合物分裂N_2分子

用Ｍｏ（Ⅲ）络合物分裂Ｎ_２分子麻省理工学院的Ｃ．Ｅ．Ｌａｐｌａｚａ和Ｃ．Ｃ．Ｃｕｍｍｉｎｓ用配位数为３的Ｍｏｔ（Ⅲ）络合物Ｍｏ（ＮＲＡｒ）３［Ｒ＝Ｃ（ＣＤ３）２ＣＨ３；Ａｒ＝３，５－Ｃ６Ｈ３Ｍｅ２（Ｍｅ，－ＣＨ３）与Ｎ２反应，实现了将Ｎ２分子裂开还?..     

SYNTHESIS AND CHARACTERIZATION OF NEIV PICKET FENCE CROWN－PORPHYRIN AND ITS Zn（Ⅱ），Fe（Ⅲ） COMIPLEXES

ＳＹＮＴＨＥＳＩＳＡＮＤＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮＯＦＮＥＩＶＰＩＣＫＥＴＦＥＮＣＥＣＲＯＷＮ－ＰＯＲＰＨＹＲＩＮＡＮＤＩＴＳＺｎ（Ⅱ），Ｆｅ（Ⅲ）ＣＯＭＩＰＬＥＸＥＳ￥ＹａｎｇｄｅＷＵ，ＦａＣｈｅｎｇＱＩＡＮ，ＬｉａｎＦａｎｇＳＨＥＮａ（Ｄｅ...     

Eu^3＋,Bi^3＋Me2Y8（SiO4）6O2中的发光特性与取代格位

在紫外光激发下，Ｅｕ＾３＋和Ｂｉ＾３＋在Ｍｅ２Ｙ８（ＳｉＯ４）６Ｏ２基质（Ｍｅ＝Ｍｇ，Ｚｎ，Ｃａ，Ｓｒ）中分别发射红光（＾５Ｄ０－＾７Ｆ２）和蓝光（＾３Ｐ１－＾１Ｓ０）．Ｅｕ＾３＋发光的红橙比随着激发波长和Ｍｅ＾２＋的不同而变化。荧光拉曼光谱表明，Ｅｕ＾３＋在四种基质中同时占据了４ｆ格位和６ｈ格位。依据Ｂｉ＾３＋发光的Ｓｔｏｋｅｓ位移推断，当Ｍｅ＝Ｃａ，Ｚｎ时，Ｂｉ＾３＋主要占据４ｆ格位，而当Ｍｅ     

单一阴离子交换柱同时分离有机酸和无机阴阳离子

研究了用乙二胺四乙酸（ＥＤＴＡ）作淋洗液时，性质迥异的有机酸、无机阴离子和碱土金属离子（Ｃａ＾２＋、Ｍｇ＾２＋）在同一阴离子交换柱上的同时分离以及保留机理，结果表明，在离子交换机理之外，非离子交换机理对有机酸及钙镁的ＥＤＴＡ络阴郭的保留行为起一定的辅助作用，９种有机酸和无机阴阳离子在１０ｍｉｎ内得到了较好的分离。各离子的电导检测灵敏度在１０＾－９至１０＾－１１ｍｏｌ，能满足环境和食吕分析的要求。     

Rapid high-performance liquid chromatography of nucleic acids with polystyrene-based micropellicular anion exchangers

Nucleic acids were separated by ion-exchange chromatography on 30 x 4.6 and 100 x 4.6 mm columns packed with a micropellicular anion exchanger made of 3-microns rigid polystyrene-based non-porous microspheres with a covalently bound hydrophilic layer and DEAE functional groups at the surface. The stationary phase particles showed negligible swelling in methanol according to permeability measurements with water and methanol. Nucleic acids and their fragments including synthetic single-stranded oligonucleotides, linear, nicked and supercoiled DNAs as well as DNA restriction fragments were separated in less than 5 min, a time scale that is much smaller than that of conventional high-performance liquid chromatographic analysis for such samples. When only buffer and sodium chloride were used in the eluent for the separation of double-stranded DNA restriction fragments pGEM-3Z/Taq I, electrophoretic analysis of the effluent revealed the presence of smaller fragments in the bands of the larger ones. Upon addition of ethylenediaminetetraacetic (EDTA) salt to the eluent, however, such contamination by shorter fragments was no longer observed. In the absence of EDTA, magnesium chloride in the eluent at a concentration of 1 mM precluded the separation of the restriction fragments under otherwise identical chromatographic conditions.     

Simultaneous determination of serum uremic toxins, cations and anions and urea determination by post-column colorimetry using immobilized enzyme

A column-switching method which combines ion-exchange and ion-pair reversed-phase chromatography was developed for the determination of serum uremic toxins, cations and anions. Serum urea, which was poorly separated by reversed-phase chromatography, was analyzed using an immobilized-urease column and detected by post-column colorimetry. Apart from the simultaneous analysis, anion analysis using ion-pair reversed-phase chromatography on an ODS column was also developed. The origin of the system peak observed in anion analysis with an eluent containing phthalate has been clarified.     

在线预处理对乙二胺四乙酸二钠离子色谱分离的影响及其应用

1引言乙二胺四乙酸二钠(EDTA-2Na)作为食品添加剂,能够对原料中的微量金属离子进行络和,防止金属离子对产品质量的缓慢破坏作用[1],常用在果蔬罐头、八宝粥等食品中,同时也可作为蛋白洗涤液中的添加剂,既增加舒适度又提高溶液杀菌能力。但是含量过高,会刺激皮肤和粘膜,引起哮喘等疾病,国家标准规定食品中最高限量为     

Simultaneous determination of arsenic species by ion chromatography-inductively coupled plasma mass spectrometry

Six arsenic species, arsenite, arsenate, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine and arsenocholine, were separated by coupled column ion chromatography using carbonate and nitric acid as eluents, and were detected by inductively coupled plasma mass spectrometry. Coupling of an anion column with a cation column made the simultaneous determination of both the cationjic and the anionic arsenic species possible by ion chromatography. Extremely low detection limits, below 0.2 μg/1 (as arsenic), were obtained for all the species studied.     

Determination of organic and inorganic mercury compounds by reverse-phase high-performance liquid chromatography after extraction of the compounds as their dithizonates

A sensitive and selective method is described for the simultaneous determination of inorganic and organic mercury compounds. The mercury compounds are extracted into toluene or chloroform with dithizone, and the dithizonates are separated by liquid chromatography on an ODS column. Complete resolution was obtained between methylethyl-, phenyl- and inorganic mercury with a mobile phase of THF/methanol (2:1) with 0.05 M acetate buffer pH 4 (62 + 38), containing 50 μM EDTA. The mercury chelates were detected spectrophotometrically at 475 nm. The detection limits were at the subnanogram level. The method is applicable to human urine, tap water and tomatoes.     

Separation selectivity of some ethylenediaminetetraacetic acid and cyclohexane-1,2-diaminetetraacetic acid complexes in column and ion electrokinetic chromatography

The complexes of Mn²⁺, Cd²⁺, Fe³⁺, Pb²⁺, Ni²⁺, Co²⁺, Zn²⁺ and Cu²⁺ with EDTA and cyclohexane-1,2-diaminetetraacetic acid (CDTA) were separated and detected in column and ion electrokinetic chromatography with suppressed conductivity and direct UV detection, respectively. In column ion chromatography (IC) these complexes were separated on an IonPac AS4A anion-exchange column (Dionex, USA). Parameters of carrier electrolyte, which were examined in the ion electrokinetic chromatography (IEKC) mode, include polymer and sulfate concentrations. In IEKC separation selectivity of complexes with poly(diallyldimethylammonium) cation as modifier is similar as for an IonPac AS4A column both for EDTA and CDTA chelates. It was shown that the ion-exchange capacity of the electrokinetic system is more than 100-times lower than the capacity of the IC column for the same peak resolution. In comparison with column main advantages of electrokinetic version are high separation efficiency (220 000–390 000 theoretical plates) and the absence of the analyte interaction with the sorbent matrix.     

Speciation of vanadium in oilsand coke and bacterial culture by high performance liquid chromatography inductively coupled plasma mass spectrometry

A simple and sensitive method for the speciation of vanadium(III), (IV), and (V) was developed by using high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICPMS). The EDTA-complexed vanadium species were separated on a strong anion exchange column with an eluent containing 2 mM EDTA, 3% acetonitrile, and 80 mM ammonium bicarbonate at pH 6. Each analysis was complete in 5 min. The detection limits were 0.6, 0.7 and 1.0 μg L⁻¹ for V(III), V(IV), and V(V), respectively. The method was applied to coke pore water samples from an oilsand processing/upgrading site in Fort McMurray, Alberta, Canada and to Shewanella putrefaciens CN32 bacterial cultures incubated with V(V). In the coke pore water samples, V(IV) and V(V) were found to be the major species. For the first time, V(III) was detected in the bacterial cultures incubated with V(V).     

高温二维液相色谱系统的构建及其评价

在二维液相色谱中, 第二维的分离速度是制约其发展的重要因素. 升高色谱柱温度可以有效降低流动相粘度, 加快溶质在两相间的传质速率, 有效加快分析速度. 以离子交换色谱法(WAX)为第一维分离模式和反相色谱法(RP)为第二维分离模式, 十通阀和两个捕集柱为接口, 通过将第二维色谱柱温度升高到80 ℃和提高流量到3 mL/min, 构建了高温WAX/RP二维液相色谱系统. 以4种标准蛋白的酶解物为样品评价系统的分离性能, 第一维共有33个馏分被捕集并导入到第二维分析, 高温二维液相色谱系统识别出187个色谱峰.     

Thermodynamic and Raman spectroscopic speciation to define the operating conditions of an innovative cleaning treatment for carbonated stones based on the use of ion exchangers--a case study

Thermodynamic and Raman spectroscopic speciation was used to define the operating conditions for an innovative cleaning treatment of the decayed carbonate-based stones using ion exchange technology. The conditioning process of the Lewatit OC1071 anion exchanger with EDTA (Y) was monitored by ionic chromatography. Characterisation of the initial (R-Cl) and the final (R2-H2Y) forms of the ion exchanger was carried out by dispersive Raman microprobe spectroscopy. The subtraction spectrum obtained between the chloride and the EDTA forms of the ion exchanger shows Raman bands at 1403, 1324, 1223, 1122, 932, 908, 591, 431 and 350 cm(-1), which agree with bands showed in the spectrum of the standard solution of the H2Y(2-) species. Therefore, this seems to be the EDTA species which takes part in the cleaning treatment performed by using resin poultices on black crusted limestone samples from an historical building.