流动注射多功能溶液处理装置在原子吸收光谱分析中的应用

使用本实验室研制的流动注射多功能溶液处理装置，通过比较流动注射在线离子交换、在线液－液萃取火焰原子吸收光谱法测定铅和资金的效果，评价了该装置的性能。     

用DDTC-Zn作载体流动注射在线共沉淀预富集火焰原子吸收法测定人发和水样中的痕量铅

提出了在高酸度下流动注射在线共沉淀预富集－火焰原子吸收法测定痕量铅的新体系。在０．５ｍｏｌ／ＬＨＣｌ介质中痕量铅与ＤＤＴＣ－Ｚｎ螯合物产生共沉淀。在线生成的沉淀物收集在编结反应器中，用甲基异丁酮溶解沉淀并直接引入火焰原子化器中进行测定。经４０ｓ富集，检测限为２．７μｇ／Ｌ。测定含量为２００μｇ／Ｌ的铅时，相对标准偏差为１．３％。建立的方法已成功地应用于人发标准参考物中和水样中痕量铅的测定     

微柱流动注射在线预浓集与电热原子吸收光谱法的全自动联用

研究了一种流动注射在线预浓集、分离与电热原子吸收光谱全自动联用的最新技术，在最优化条件下，采用９μＬ微柱预浓集，８０μＬ甲醇洗脱剂可将吸附于微柱上的待测物定量洗脱并全部自动导入石墨炉原子化器。富集倍数高达６４，进行了河和海水标准参考物质中痕量铅的测定，无基体干扰，不必使用基体改进剂，结果满意，检出限４．５ｎｇ／Ｌ，回收率９７－１０４％，相对标准偏差为２．９％。     

流动注射-导数火焰原子吸收光谱测定植物油中的镍、锰、铬和铅

提出了流动注射－导数火焰原子吸收光谱测定植物油中微量镍、锰、铬和铅的新方法，流动注射进样技术克服了常规火焰原子吸收法耗样量大和基体干扰严重的缺点，导数技术应用于火焰原子吸收可提高方法的灵敏度和信号的选择性，流动注射与导数技术相结合应用于火焰原子吸收成功地测定了常规火焰原子吸收法和流动注射－火焰原子吸收法难以测定的植物油中微量镍、锰、铬和铅。镍、锰、铬和铅的特征浓度（μg/mL)，分别为0.0054、0.0034、0.0067、0.025，相对标准偏差在0.3%-2.8%的范围内。     

流动注射在线吸发离预浓集冷蒸气原子吸收法测定痕量镉

研究了IRC－718离子交换树脂、122螯合树脂和MuromacA-1树脂对镉 的预浓集条件,建立了超痕量镉的流动注射在线吸着分离预浓集冷蒸气发生原子吸收光谱测定方法,在每小时进样60,60和45次速度下检出限（3σ）分别为3．0,3．0和2．4ng/L,线性范围0－0．3μg/L,对0．2μg/L镉测定的相对标准偏差为2．0％－2．6％（n=11),。讨论了用这3种离子交换树脂微柱进行分离预浓集时条件参数的优化、抗干扰能力以及对天然水样的回收率,并分别进行了水样的测定。     

痕量铅的在线SHA离子交换预浓度流动注射原子吸收测定

采用羟基磷灰石微型柱的流动注射系统与火焰原子吸收光谱联结对工业废水中铅进行预浓集测定。在进样时，被分析物沉积在羟基磷灰石微型柱上，并通过注射半胱氨酸（碱性条件下）予以洗脱。该方法成功地应用于工业废水的分析。通过回收实验，标准物质分析等方法评价了准确度。４ｍｌ样品体积的检测限：为４μｇ／Ｌ（４ｍＬ／ｍｉｎ），进样时间１ｍｉｎ，２μｇ／ｍＬ和０．２μｇ／ｍＬ含量测定的相对标准偏差分别为１．５％和２．２     

用流动注射在线预浓集－原子吸收光谱法测定痕量镉

研究了以巯基苯骈噻唑和８－羟基喹啉为复合萃取剂、活性硅胶为载体制成的色谱柱对镉离子吸附的条件，建立了痕量镉的流动注射在线预浓集－原子吸收光谱测定的新方法，变异系数１．３％，检出限０．０１ｍｇ／Ｌ．用于环境水分析，获得满意结果．     

流动注射在线沉淀共沉淀预分离富集与原子光谱联用的进展

综述流动注射在线沉淀共沉淀预分离富集与原子光谱联用技术的进展.重点评述了流动注射在线沉淀预分离-火焰原子吸收间接法测定无机阴离子和有机化合物的方法和流动注射在线无滤共沉淀预富集-火焰或电热原子吸收法测定痕量金属离子的方法.共引用文献35篇.     

用流动注射在线预浓集——原子吸收光谱法测定痕量镉

研究了以巯基苯骈噻唑和８－羟基喹啉为复合萃取剂、活性硅胶为载体制成的色谱柱对镉离子吸附的条件，建立了痕量镉的流动注射在线预浓集－原子吸收光谱测定的新方法，变异系数１．３％，检出限０．０１ｍｇ／Ｌ，用于环境水分析，获得满意结果。     

流动注射在线分离富集-火焰原子吸收光谱法测定硫酸镍电解液中的微量铅

采用微型分离柱流动注射在线分离富集火焰原子吸收法测定硫酸镍电解液中的铅。用本法分析含铅量为１．３３ｍｇ／Ｌ的试样,相对标准偏差（ｎ＝１０）为３．４％,检出限为０．０３ｍｇ／Ｌ。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.