离子色谱法间接检测原油中的硫化氢含量

原油中的硫化氢（H2S）经氮气吹脱，碱性双氧水吸收转化为SO4^2-离子色谱法测定SO4^2-含量，从而间接得到H2S的含量。通过正交实验优化了氮气吹脱-双氧水吸收氧化的实验条件，发现吸收液中双氧水浓度租氮气流量对转化效率影响显著。当双氧水含量为3，0％（φ）、氮气吹脱流量为0.2L／min、吹脱时间为30min、NaOH浓度为0．1mol／L时，H2S转化为SO4^2-的效率最高。方法的RSD为1．18％，原油中硫化氢的加标回收率为89％-111％，检出限为0．042μ／g。该法不受油样粘度和色度影响，适用于原油及其馏分油中硫化氧含量的测定。     

矿石中锇和钌的分离与测定

矿样经过氧化钠熔融,用硫酸酸化,加高锰酸钾蒸馏。用0.1％盐酸-4％乙醇-2M硫酸溶液吸收钌。锇进入第二吸收管,用亚砷酸的硫酸溶液吸收。吸收液分别作锇和钌的催化测定。提出了新的蒸馏器设计,从而使蒸馏分离与催化测定得到较好的结合。     

平台原子吸收法测定血清中铝

本文采用国产仪器建立了血清铝的平台原子吸收测定方法。通过对基体组成的改身,抑制了基体效应,使得方法灵敏度、线性范围等统计指标都有所改善,从而可用铝的水溶液工作曲线代替血清工作曲线。方法的灵敏度为63×10~(-12)Al/1％吸收,检出限(3(?))为68×10~(-12)g,相对标准偏差为10％,回收率10.02％,线性范围为0—600μgAl/L。     

硝酸铋共沉淀—火焰原子吸收法测定蒸馏酒中痕量铅

蒸馏酒中铅的测定方法,常用消化样品-双硫腙比色法或稀释样品-火焰原子吸收光度法。前者操作复杂,重现性差,且用剧毒药品氰化钾。后者灵敏度不高,不能测定含铅量低的酒样。本文报道了用硝酸铋作共沉淀剂分离富集、火焰原子吸收光度法测定蒸馏酒中痕量铅的方法。该方法操作简便,灵敏度高(95％置信度的检出限为0.005mg·L~(-1)),线性范围宽,基体没有干扰。相对标准偏差为2.2％～4.5％。回收率为100.2％～103.2％。对样品进行测定,结果与双硫腙比色法一致。     

间接原子吸收法测定葡萄籽提取物中的原花青素

提出了间接测定葡萄籽提取物中原花青素的原子吸收光谱法。它是基于原花青素能与醋酸铜发生络合反应,生成难溶于水的棕黄色沉淀,经离心分离后,用原子吸收法测定上清液中过量的铜离子,可间接测定原花青素的含量。方法线性范围为3．0-30．0mg／L;RSD为1．1％-1．2％;回收率为98.9％-102.0％。     

绿茶及其饮料中总黄酮的分析

以绿茶及其饮料为分析对象采用三波长-光谱法测定绿茶及其饮料中黄酮的含量，有效地消除了吸收峰不对称给定量分析造成的影响，并校正了基于干扰组分(饮料中添加剂)的吸收光谱具有线性吸收产生的基线倾斜。本法的回收率为93％～106％，相对标准偏差小于0．48％。     

FAAS法测定ZYSP喷金料中高含量锡

用盐酸(1+1)和硝酸(1+1)混合液溶解ZYSP喷金料,并采用富火焰原子吸收法在锡的次灵敏线286.3nm处对样液中高含量的锡进行直接测试。线性范围0～250mg·L~(-1),其灵敏度为3.10mg·L~(-1)/1％吸收,回收率为100.1％～103.7％,相对标准偏差不大于3.5％,并用标准加入法进行对照。     

原子吸收分光光度法测定生物样品中的游离脂肪酸

本文研究了用原子吸收分光光度法间接测定生物样品中游离脂肪酸(FFA)的方法,用氯仿-正己烷-甲醇混合液萃取样品中FFA,用铜溶液与FFA形成“铜皂”,进入有机相,未反应的Cu~(2+)进入水相,用原子吸收法测定有机相中铜,间接求得游离脂肪酸含量。本法线性范围为10～100nmol,对血浆测定结果的相对标准偏差为<6.59％,回收率为96％～102％。本法的测定结果与比色法的结果基本一致。     

紫尿酸双波长叠加光度法测定水中微量铁

在碱性介质中,铁（Ⅱ）与紫尿酸发生显色反应形成一种蓝色配阴离子,该配阴离子具有两个吸收峰,分别位于630nm和350nm,吸光度A630,A350之和△A与铁（Ⅱ）的含量在0-2μg／mL范围内线性关系良好,据此建立了测定微量铁的紫尿酸双波长叠加光度法,该法用于水中微量铁的测定,测定结果与火焰原子吸收法（FAAS）相吻合,加标回收率为98％-102％,测定结果的相对标准偏差为1．2％-2．9％（n=5）。     

离子色谱法测定乙烯中微量氨

用稀硫酸吸收,离子色谱法测定乙烯中微量的氨,对吸收瓶、吸收溶液的浓度进行选择,同时对方法的吸收效率、加标回收率、检出限、精密度进行测试。该方法快速、简便,不需要复杂的样品前处理,完成一次测定只需16min。该方法检出限为0．003mg／L,当采样体积为100L时,最低检出浓度为0．003mg／m^3。样品测定结果的相对标准偏差为2．8％（n=4）,加标回收率为93．8％-109％。     

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%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

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.     

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.     

Microwave-assisted copper-catalyzed stereoselective ring expansion of three-membered heterocycles with α-diazo-β-dicarbonyl compounds

Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular S_N2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively.     

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.     

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%).