氧化罗丹明6G褪色光度法测定微量锰

人体需要微量的锰,它能促进人体的发育且具有抗癌作用.目前,吸光光度法测定Mn(Ⅲ)的方法很多,其中二元体系褪色光度法也有报道,但高锰酸氧化罗丹明6G褪色光度法未见有报道.试验发现,在硫磷混酸介质中,高锰酸能氧化罗丹明6G使其褪色,利用溶液褪色前后的吸光度差值可测定微量锰,从而建立了一种测定锰的新方法.该法简便、快速,灵敏度高,应用于某些物质中微量锰的测定,结果满意.1 试验部分1.1 主要仪器与试剂UV-754型分光光度计Mn(Ⅶ)标准溶液:按常规方法配制0.01mol·L~(-1)的高锰酸钾溶液,用草酸钠标准溶液标定,使用时稀释成5μg·ml~(-1)Mn(Ⅶ)工作溶液.Mn(Ⅱ)标准溶液:称取1.0000g纯度为99.9%的金属锰(称量前用稀硫酸洗去表面氧化物)于250ml烧杯中,加硫酸溶液(1+4)10ml使其溶解,移入1L量瓶中,用水稀释至刻度,摇匀,配成1mg·ml~(-1)Mn(Ⅱ)标准溶液,使用时稀释成5μg·     

催化褪色光度法测定茶叶中痕量锰

锰 (Ⅱ )的光度法测定中 ,催化光度法测定已有报道[1～ 4 ] 。本文研究了在 pH 6 .3的KH2 PO4 Na2 B4 O7缓冲体系中 ,利用痕量Mn(Ⅱ )催化H2 O2氧化胭脂红的褪色来测定Mn(Ⅱ )的催化光度法。本法检出限为 1.1× 10 - 8g·L- 1,是测定Mn(Ⅱ )较灵敏的方法之一 ,其操作简便 ,试剂易得 ,灵敏度高 ,条件容易控制 ,选择性和重现性好。用本法测定茶叶样品中痕量锰 ,获得了满意的结果。1　试验部分1.1　主要仪器与试剂72 2型分光光度计pHS 3C型酸度计CS 5 0 1SP型超级数显恒温器Mn(Ⅱ )标准溶液 :1.0 0 0 0 g·L- 1,使用时稀释至 0 .5 …     

催化动力学光度法测定水中痕量锰

报道[1,2],但以高碘酸钾氧化胭脂红作为指示反应的方法还未见报道。本文研究发现,在氨水 NH4Cl介质中,锰能强烈催化高碘酸钾氧化食用色素胭脂红的褪色反应,在510nm波长处,其反应速度lg(A0/A)与锰的浓度之间符合动力学一级反应关系式:lg(A0/A)=KCMn,由此建立了一个高灵敏、高选择性的测定痕量锰的方法。该法检出限为8×10-9g·L-1,线性范围在0～5.0μg/25ml。用于水样中的痕量锰的测定,结果满意。1　试验部分1.1　主要仪器与试剂753B型分光光度计(上海分析仪器厂)锰标准溶液:1.0mg·ml-1,使用时稀释成1 0μg·ml-1。高碘酸钾溶液:0.01mo…     

表面活性剂存在下Mn(Ⅶ)氧化胭脂红的褪色反应及其应用

研究了表面活性剂十二烷基磺酸钠(SDS)存在下,锰(Ⅶ)氧化胭脂红的褪色反应。结果表明,在硫酸介质中,锰(Ⅶ)能够氧化胭脂红褪色,SDS可大幅度提高反应的灵敏度,且氧化褪色程度与锰(Ⅶ)的含量在一定的范围内符合比尔定律。据此建立了表面活性剂增敏、褪色光度法测定锰(Ⅶ)的新方法。锰(Ⅶ)的测定范围为0~4.0μg.mL-1,表观摩尔吸光系数为4.3×104L.mol-1.cm-1,应用于茶叶中锰的测定,结果满意。     

吸光光度法测定痕量锰

锰是人体及动物的必需元素[1 ] ,摄入超量会引起毒性 ,所以微量锰测定方法的探讨 ,在水质、食品等方面的测定中具有一定的实际意义[2 ,3] 。锰对于H2 O2 与邻氨基酚的氧化反应具有较好的催化作用。本文研究了在 p H 5.5的 HOAc- Na OAc介质中 ,以邻氨基酚氯仿为萃取剂 ,通过固定萃取时间 ,控制反应进行的程度 ,确定了最佳条件。用于水、食品及人发中痕量锰的测定 ,结果满意。1　试验部分1 .1　仪器与试剂GBC- UV( VIS) 91 6型紫外 -可见分光光度计Mn( )标准溶液 :用 Mn SO4· H2 O配制成1 .0 0 g·L- 1 储备液。过氧化氢溶液 :3…     

催化光度法测定粉煤灰中微量锰

粉煤灰作为电厂排放的废物在农业方面有广泛的应用。据文献 [1]介绍 ,粉煤灰中含有一些微量元素 (如锰 )对作物生长有利 ,但其含量如超过临界值会导致作物死亡 ,必须对其准确测定。目前锰光度法测定中 ,催化光度法测定锰已有报道[2～ 4 ] 。本文研究在ｐＨ 9.2 5的氨 氯化铵缓冲溶液中 ,利用痕量Ｍｎ(Ⅱ )催化Ｈ2 Ｏ2 氧化水杨醛肟 (ＳＡＯ)的显色反应测定锰。本法具有较高选择性和灵敏度 ,且操作较简便 ,可准确地测定粉煤灰样品中的微量锰。1　试验部分1.1　主要试剂与仪器Ｍｎ(Ⅱ )标准储备液 :1.0ｇ·Ｌ- 1,用时稀至 0 5 μｇ·ｍｌ- 1…     

氧化邻苯三酚红褪色光度法测定微量锰

高锰酸盐光度法是测定微量锰的常用方法[1,2 ] 。本文利用Ｍｎ(Ⅶ )在酸性介质中能氧化邻苯三酚红并使之褪色的反应 ,建立了测定锰的光度分析法。邻苯三酚红 (ＰｙｒｏｇａｌｌｏｌＲｅｄ) ,化学名称为连苯三酚磺酞 (ＰｙｒｏｇａｌｌｏｌＳｕｌｆｏｎｐｌａｌｅｉｎ) ,微溶于醇和水。其分子式为Ｃ19Ｈ12 Ｏ8Ｓ·Ｈ2 Ｏ ,分子量为 4 18 39,结构式如图 1。图 1　邻苯三酚红结构式在水溶液中酸性时为橙黄色 ,中性时为酒红色 ,碱性时为紫色。在酸性介质中Ｍｎ(Ⅶ )的强氧化性使邻苯三酚红醌基中的不饱和双键断裂而褪色。试验表明 ,在本法条件下…     

催化光度法测定痕量钒——钒（V）-溴甲酚紫-过氧化氢体系

催化光度法测定钒已有报道[1~3],在0.45 mol·L-1磷酸介质及加热条件下,过氧化氢氧化溴甲酚紫褪色反应非常缓慢,而痕量钒对此反应具有较高的催化活性,且在一定浓度范围内,钒量与褪色反应程度呈线性关系,据此可建立测定痕量钒的方法。方法的检出限为1.9×10-6g·L-1,测定范围为0·003~1.8 mg·L-1。方法操作简便,重现性好,用于钢样中痕量钒的测定,结果满意。1试验部分1.1仪器与试剂721型分光光度计LB801-2型超级恒温器钒(Ⅴ)标准溶液:1.000 0 g·L-1,称取偏钒酸铵0.229 7 g溶于热水中,冷却,定容于100 mL容量瓶中。溴甲酚紫(用R表示)溶液:…     

催化动力学光度测定茶叶中微量锰

锰是多种酶的激活剂 ,在许多生化中均起到一定作用 ,并可促进生长发育 ,人体内若缺乏锰 ,则会使生长停滞 ,骨骼畸形等 ,锰的测定方法很多 ,常见的有催化反应极谱法、吸光光度法、催化动力学法、高锰酸 甲基橙褪色反应吸光光度法[15 ]。本文在文献基础上 ,用二苯基碳酰二肼 (ＤＰＣ)作显色剂 ,以抗坏血酸中止反应的催化动力学光度法测定茶叶中微量锰 ,线性范围为 0 0 .6μｇ·ｍｌ- 1,测定波长为 490ｎｍ时 ,灵敏度高 ,重现性好 ,获得满意效果。1　试验部分1.1　仪器与试剂二苯基碳酰二肼 (ＤＰＣ) :0 .0 1ｍｏｌ·Ｌ- 1锰标准溶液 :1μｇ·…     

催化光度法测定井水和白葡萄酒中痕量锰

锰是人体必需的微量元素之一 ,适量的锰有利于身体健康 ,而含量过高或过低都会引起某些器官的病变而出现不适 ,因而准确测定痕量锰具有重要意义。锰的催化光度法测定已有不少报道 ,作者在试验中发现在乙酸 -乙酸钠介质中 ,锰对高碘酸钾氧化维多利亚蓝的褪色反应具有强烈催化作用 ,其褪色反应速率与 Mn( )的浓度在一定范围内呈良好的线性关系。本文研究了维多利亚蓝催化动力学光度法测定痕量锰的条件 ,建立了测定痕量 Mn( )的方法。方法检出限为 0 .1 3ng· ml-1,选择性较好。本法已用于井水和白葡萄酒中锰的测定。1　试验部分1 .1　仪器与…     

HEPT类化合物的QSAR研究

为定量结构／活性相关性研究提取了量子化学参数,拓扑指数Am,分子连接性指数^mxt及疏水性常数,同时应用正交变换和最佳变量子集算法（Leaps-and-Bonds)进行了变量压缩和选择,进而实施了多元回归分析,并由此结果进行了HEPT类化合物（1－[(2-hydroxyethoxy)methyl]-6-(phenylthio)-thymine derivatives)的结构／活性关系的理论解释,进行了人工神经网络法对于该类化合物的活性预测,其结构明显好于多元回归法。     

Effect of the pH of the medium on the chemical shifts in the PMR spectra and on the distribution of the π-electron density

The dependence of the chemical shifts of the ring protons on the pH of the medium for a number of 4-hydroxyquinoline derivatives was studied by means of PMR spectroscopy. The dipolar and uncharged hydroxy forms exist in equilibrium in aqueous solutions. The effect of intramolecular hydrogen bonding on the character of the dependence of the chemical shift on the pH of the medium in the case of 3-piperidinomethyl-4-hydroxyisoquinoline was investigated. The possibility of the separate protonation of the ring nitrogen and the side-chain nitrogen in 3-piperidinomethyl-4-hydroxyisoquinoline was established. The distribution of the -electron density in 4-hydroxyisoquinoline is in good agreement with its chemical behavior.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, pp. 1546–1549, November, 1971     

Effect of the pH of the medium on the chemical shifts in the PMR spectra and on the distribution of the π-electron density

The dependence of the chemical shift of the ring protons on the pH of the medium for a number of 3-hydroxyquinoline derivatives was studied by PMR spectroscopy. The regions of ionization of the molecules, which correspond to the ranges of acidic, neutral, and alkaline media, were found. In D₂O, 3-hydroxyquinoline is present only in the uncharged hydroxy form. The presence of intramolecular hydrogen bonding in 4-dimethylaminomethyl-3-hydroxyquinoline has a substantial effect on the character of the dependence of the chemical shift on the pH of the medium; the existence of separate protonation of the nitrogen atoms of the ring and the side chain of 4-dimethylaminomethyl-3-hydroxyquinoline was established. The distribution of the -electron density in the 3-hydroxyquinoline molecule is in good agreement with its chemical behavior during electrophilic substitution.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, pp. 1540–1545, November, 1971.     

液滴荧光传感与计算机联用技术在微量分析中的应用

通过在LS55型荧光-磷光-发光分光光度计上加装液滴产生及调节附件,采用计算机采集与分析处理数据,成功地研制了双通道液滴光化学传感装置.利用葡聚糖凝胶对复合维生素B中不同组分的选择性吸附来达到分离与同时检测的目的,并将其用于复合维生素B药片的分析,取得了满意的结果.     

On the theory underlying the Car-Parrinello method and the role of the fictitious mass parameter

The theory underlying the Car-Parrinello extended-Lagrangian approach to ab initio molecular dynamics (CPMD) is reviewed and reexamined using "heavy" ice as a test system. It is emphasized that the adiabatic decoupling in CPMD is not a decoupling of electronic orbitals from the ions but only a decoupling of a subset of the orbital vibrational modes from the rest of the necessarily coupled system of orbitals and ions. Recent work [J. Chem. Phys. 116, 14 (2002)] has pointed out that, due to the orbital-ion coupling that remains once adiabatic decoupling has been achieved, a large value of the fictitious mass mu can lead to systematic errors in the computed forces in CPMD. These errors are further investigated in the present work with a focus on those parts of these errors that are not corrected simply by rescaling the masses of the ions. It is suggested that any comparison of the efficiencies of Born-Oppenheimer molecular dynamics (BOMD) and CPMD should be performed at a similar level of accuracy. If accuracy is judged according to the average magnitude of the systematic errors in the computed forces, the efficiency of BOMD compares more favorably to that of CPMD than previous comparisons have suggested.     

From the Micro- to the Macro-: Managing the Conservation of the Warship,Vasa

Sweden's famous warship, Vasa, sank on her maiden voyage in August 1628, and remained on the bottom of Stockholm harbour for 333 years. Raised in 1961, she became the first large-scale wooden object to be treated with polyethylene glycol (PEG). In the summer of 2000 a number of acidic salt precipitations were noticed on the surface of the ship and on wooden artefacts in the storerooms. An international research project has been established to look into the causes of this problem and suggest possible re-treatments. Meanwhile projects are underway to monitor movements in the ship, to build a better support system, and to replace the thousands of iron bolts holding the structure together, while a sophisticated new climate system has recently been installed in the museum.