单扫描示波极谱法连测铅锌

铅和锌极谱测定方法很多 ,有在碱性介质中测定 ,也有在强酸性介质中测定。铅和锌连测有时也有报道[1,2 ] ,但测定范围局限于微量及半微量分析。本法特点是在同一份溶液中连测铅和锌 ,测定范围扩至常量 ,干扰少 ,重现性好。铅的回收率为 95%～1 0 0 % ,锌的回收率为 97%～ 99% ,适合于铜矿及铅锌矿中铅和锌的分析。1　试验部分1 .1　主要试剂与仪器铅 [3]和锌 [4 ]标准溶液 :均为 2 mg·ml-1抗坏血酸溶液 :1 0 0 g· L-1硫氰酸钾溶液 :50 g·L-1HOAc- Na OAc缓冲溶液 [5] :p H4.5明胶溶液 :2 .5g· L-1试剂均为分析纯JP3- 1型示波仪 ,三…     

全固态铅离子选择性电极测定人发中微量铅

提出了用全固态铅离子选择性电极测定人发中微量铅的方法。在 1.5 g·L- 1抗坏血酸 1g·L- 1三乙烯四胺 0 .0 5mol·L- 1高氯酸钠 ,pH 4.85 .5的条件下 ,采用格氏作图法可准确测定人发中微量铅。方法简便、准确度高 ,回收率 95 % 10 6% ,相对标准偏差小于 5 .3 %。     

同时测定中草药中痕量铅和汞的氢化物原子荧光法

提出了同时测定痕量铅和汞的氢化物发生原子荧光法 ;采用断续流动氢化物发生器 ,以碱性铁氰化钾为氧化剂 ,在柠檬酸介质中产生铅烷和汞蒸气 ;讨论了氧化剂和络合剂对铅烷和汞蒸气生成的作用机理 ,考察了共存元素的干扰情况;在选定最佳工作条件下 ,测得铅和汞的检出限(3σ)分别为0.21μg·L-1 和0.026μg·L-1,相对标准偏差(对20μg·L-1Pb和2μg·L-1Hg,n=11)分别为1.2 %和0.71 % ;该法应用于中草药中痕量铅和汞的同时测定 ,结果令人满意     

微分电位溶出法连续测定饮料中的铜铅镉锌

建立了微分电位溶出法连续测定饮料中痕量铜、铅、镉、锌的新方法。在HAc- Na Ac( p H4 .5)～ 3.5× 1 0 -2 mol·L-1KCl～ 2 .6× 1 0 -5 mol· L-1Hg2 +介质中测定锌 ,然后调节底液为 0 .0 1 mol·L-1HCl,连续测定铜、铅、镉。铜、铅、镉、锌 ,检出限分别为 4 ,0 .1 ,2 ,4 μg· L-1,线性测定范围 Zn2 +:0～ 30 0 μg·L-1,Cu2 +、Pb2 +、Cd2 +:0～ 2 2 0μg· L-1,回收率为 83.4 %～ 1 0 3.3% ,RSD<3.4 % ( n=7)。该法较好解决了金属互化物的影响 ,样品不需消化便可直接测定。     

微分电位溶出法快速测定全血中铅

提出了在硝酸 (1+ 9)中 ,旋涡振荡提取 ,离心沉淀分离的微分电位溶出法快速测定全血中铅的方法。全血中铅的最低检出浓度为 5 .0 μg·L-1,RSD均小于 6 .8% ,线性范围为 5 .0～ 2 5 0 .0 μg·L-1。采用单点标准加入法对 7份CDC血铅标样进行了测定 ,结果与标准值相符     

氢化物发生原子吸收光谱法测定食品中铅

采用微波溶样,以盐酸铁氰化钾硼氢化钾反应体系,将标准液及食品中铅氧化为Pb4+,利用连续流动注射氢化物发生器,以15g·L-1硼氢化钾在酸性条件下产生的氢自由基,与Pb4+生成的PbH4(铅烷)气体从反应体系中逸出,导入电热石英原子化器,采用高性能空心阴极灯作光源,进行原子吸收光谱检测。方法的灵敏度为0.065μg·L-1/1%A,检出限为0.070μg·L-1,线性范围在0～14μg·L-1之间,相关系数为0.9991,RSD小于3%,加标回收率为97%。     

抗坏血酸为阻断剂肾上腺素法测定微量元素对SOD活性的影响

Vitamin阻断法测定了不同浓度Se、Mn、F- 对SOD活性的影响。结果显示 :①Se浓度由0 0 0 μg·L- 1增加到 40 0 μg·L- 1时 ,SOD活性由 5 1 0 0u·mg- 1上升到 5 40 0u·mg- 1;Se浓度继续增加到 60 0 μg·L- 1,SOD活性下降至 5 1 40u·mg- 1;②Mn浓度由 0 0 0 μg·L- 1增加到 40 0 μg·L- 1,SOD活性由 5 1 0 0u·mg- 1上升到 5 90 0u·mg- 1;Mn浓度继续增加到 5 0 0 μg·L- 1,SOD活性下降到 5 2 0 0u·mg- 1;③F- 浓度由 0 0 0 μg·L- 1增加到 1 0 0 μg·L- 1,SOD活性由 5 1 0 0u·mg- 1上升至 5 2 80u·mg- 1,继续增加F- 浓度到 2 0 0 μg·L- 1,SOD活性下降为 5 1 70u·mg- 1,再增加F- 浓度到 40 0 μg·L- 1,60 0μg·L- 1,80 0 μg·L- 1,SOD活性基本维持在 5 2 0 0～ 5 1 80u·mg- 1之间     

氢化物发生-原子吸收光谱法测定蔬菜中痕量铅

采用微波消化、氢化物发生-原子吸收光谱法测定蔬菜中痕量铅。研究了硼氢化钾用量、酸介质及其酸度对铅的测定影响,采用铁氰化钾-草酸体系可消除金属元素对铅测定的干扰。检出限为0．023μg·L-1,回收率为97．8％～105．6％,RSD为0．8％～1．8％,线性范围为0～40μg·L-1。     

铅基合金的溶解及铅的快速测定

铅基轴承合金因为磨擦阻力小、贴服性优良、铸造性能好等优点广泛用于中小负荷机械设备的轴瓦上。然而铅基合金在用酸溶解[1] 、稀释时极易产生沉淀 ,给分析带来困难。本文研究了用盐酸 硝酸混合酸溶解试样 ,加一定量的氯化钠防止铅析出 ,用NaCl+HCl稀释液稀释 ,在微酸性溶液中 ,用EDTA容量法[2 ] 测定铅的含量。该铅基制备液还可同时测定其中的锡、铜。1　试验部分1.1　主要试剂酒石酸溶液 :30 0 g·L- 12 ,4 二硝基酚指示剂 :2 g·L- 1的乙醇溶液六次甲基四胺缓冲溶液 :称此试剂 4 0 g溶于10 0ml水中 ,加浓盐酸 10ml,调至 pH≈ 5 .…     

铅(Ⅱ)-DBONBF-CTMAB吸光光度法测定铅

邻硝基苯基荧光酮属于三羟基荧光酮显色剂,已用于多种元素的光度分析[1]。本文对其衍生物4,5 二溴邻硝基苯基荧光酮(DBONBF)与铅(Ⅱ)的反应进行了研究。试验表明,该反应的灵敏度较高(ε可达1.6×105L·mol-1·cm-1),体系的选择性与稳定性较好,可用于工业废水中铅的测定。1　试验部分1.1　试剂与仪器铅标准溶液:1.0g·L-1,10μg·ml-1DBONBF乙醇溶液(AR级):0.4g·L-1CTMAB溶液:2g·L-1NH3 NH4Cl缓冲溶液:pH9.6721型分光光度计(上海第三分析仪器厂)1.2　试验方法于25ml容量瓶中加入含10μg铅的标准溶液,再依次加入DBONBF乙…     

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.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

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.     

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.     

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.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

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.