金属材料分析方法的选择和施行——第六讲 金属材料中稀土元素的测定（续）

2．7．1．1偶氮胂ⅢС.Б.Саввин于1959年合成了偶氮胂Ⅲ,其化学学名为2,2’-[1,8-二羧基-3,6-二磺酸-2,7-萘双偶氮]二苯胂酸。为暗红色粉末,溶于水中呈紫红色溶液,易溶于氢氧化钠及碳酸钠等碱性溶液中,不溶于浓酸及乙醇、乙醚、丙酮等有机溶剂中。在稀的无机酸如硫酸、硝酸及盐酸中有一定的溶解度,但当浓度较高时,如在2 mol·L-1或更浓的盐酸中,将因     

锡酸钾对流动锌酸钾碱液中锌沉积/溶解的影响

研究了在流动的高浓度锌酸钾溶液中锡酸钾添加剂对锌负极沉积/溶解行为的影响. 循环伏安测试结果表明, 扫描速度为1 mV/s时, 随着添加锡酸钾浓度的增加, 阴极分支更早出现沉积, 溶解峰的峰值逐渐减小; 随着扫描速度的增加, 这种规律变得不明显. 利用SEM观测电沉积500 s的沉积物形貌发现, 向基础溶液中添加锡酸钾有利于晶种的产生和晶粒的生长. EDS测试结果表明含锡酸钾的锌酸钾溶液中沉积层含有锌和锡. 自放电测试结果表明, 基础电解液加入锡酸钾后自放电现象得到了明显的改善, 充满电静置12 h后加入0.1 mol/L锡酸钾的电池放电库仑效率从基础溶液的60.0%提高到81.1%.     

非完全消化-火焰原子吸收光谱法测定润滑油中钙锌

在低温加热的条件下,油样用浓硝酸消化,所得试液中加入适量Triton X-100及Tween 80使乳化从而得到均匀的透明或半透明的呈橙黄色或黄绿色的试样溶液,供火焰原子吸收光谱法(FAAS)测定钙及锌.对非完全消化所用的酸和乳化剂的选择和FAAS测定中的化学干扰、背景干扰以及空白溶液及试样溶液粘度的一致性等分析务件进行了试验和优化.钙及锌两元素的线性范围依次为0～12 mg·L-1和0～1.6 mg·L-1,检出限(3σ/s)依次为0.14 mg·L-1及0.018 mg·L-1.此方法应用于润滑油实样分析,所得两元素分析结果的RSD(n=6)值均小于5%,回收率均在100.0%～102.1%之间.     

非完全消化-火焰原子吸收光谱法测定水果中铜铁锌

用非完全消化法处理杏、油桃和草莓样品,即在低温下用浓硝酸-高氯酸(3+1)混合酸消解样品,再加入乳化剂TX-10溶解消化过程中所产生的油脂,将所得橙红色的均匀透明溶液用火焰原子吸收光谱法测定其中铜、铁和锌元素的含量.对样品处理条件、混合酸中杂质及共存TX-10的干扰进行了试验.铜、铁和锌的检出限(3s/k)分别为0.019,0.145,0.009 mg·L-1.用此法测定水果实样中铜、铁和锌的含量,所得结果与灰化法测定结果相一致.     

电感耦合等离子体原子发射光谱法测定杨树叶中铜锌铅镍

研究了电感耦合等离子体原子发射光谱法(ICP-AES)的仪器工作参数,溶液提升速率为2.4 mL.min-1,雾室压力为2.07×105Pa,观测高度为16 mm。用浓硝酸1 mL作样品的消化剂。用此方法测定杨树叶标准物质(GBW 07604)中铜、锌、铅、镍,相对误差在0.54%~9.3%之间,加标回收率在97.9%~101.0%之间。     

酚酞指示剂在酸中的颜色问题

酚酞指示剂在稀碱溶液显玫瑰红色,在浓碱溶液先显玫瑰红色,然后褪为无色,这是大家熟悉的。至于酚酞指示剂在浓酸中的颜色问题,由于中学化学老师的询问,我们做了一些实验,结果如下。     

壳聚糖浓溶液流变学性质研究-溶剂性质的依赖性

用不同pH值的HCOOH, CH~3COOH, HCl,0.1mol.dm^-3CH~3COONa+0.2mol.dm^-3CH~3COOH水溶液为溶剂, 进行了壳聚糖浓溶液的流变学性质研究。实验结果表明, 溶剂pH值相同时, 壳聚糖在各种酸中的溶解性和溶液沾度差别较大。同一种酸中, 在可溶范围内, pH值增加, 溶剂变劣, 粘度-浓度的幂律方程指数α增大。外加盐使溶剂变劣程度增加。在任何一种酸中, 浓溶液粘度都随存放时间的延长而下降, 流动指数n减小, 流动活化能基本不变。     

玻碳电极阳极溶出法测定高纯铝中PPb级杂质锌

高纯铝中ppm级锌杂质的测定,现都采用酸分解试样后转化成pH约3.5的三氯化铝溶液,而后直接用悬汞电极或铂球镀银沾汞电极阳极溶出伏安法进行测定。在该底液中测定锌,氢离子浓度控制甚严,否则将干扰锌的测定。特别对于高纯铝中ppb级杂质锌的测定,即使底液中微量的氢离子存在,亦使锌波波底平直不易测量,产生严重的干扰。本试验利用玻璃碳电极导电性好、灵敏度高和氢的超电势高等优点,用二硫腙-四氯化碳溶液萃取分离铝基体及试样中共存的干扰杂质元素,同时对锌进行富集,而后在乙酸钠底液中用阳极溶出伏安法进行测定,解决了在一般     

含胺或非质子溶剂的醇钠-醇溶液的酸性函数

自1932年,Hammett 等人对于浓强酸溶液的酸度采用该溶液供给质子于中性溶质(指示剂)的能力来表示以后,提出了 Hammett 酸性函数。并对不同类型的酸溶液进行了系统地研究和测量。在五十年代,酸     

铅锌矿中铅锌的连续络合滴定

于pH5.5—6的乙酸-乙酸钠缓冲溶液中,先以EDTA络合滴定铅锌合量,再将此溶液调至pH6—6.5,以邻二氮菲(Phen)从Zn-EDTA络合物中夺取锌使成Zn-Pben,定量释放出EDTA,继以硝酸铅滴定,从而测得锌量。经试验表明,1.2克Phen可从Zn-EDTA中夺取1毫克锌。铜、铁有干扰,若加入10毫升8%硫脲溶液,则允许共存20毫克铜。加入Phen后再补加约1克固体硫脲,可使锌的滴定终点更敏锐;加入15毫升4%氟化钠溶液,且缓冲液中乙酸钠浓度达40%时,即使共存40毫克铁也不影响铅的测定。方法应用于铅锌矿中铅锌的测定,结果满意。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Effect of the Method of Modification of Zeolite X on Selectivity of Catalytic Methylation of Toluene

Theoretical and Experimental Chemistry - The effect of the method of modification of catalysts based on zeolite X by cesium and magnesium cations (ion exchange and impregnation) on the selectivity...     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Synthesis of tetrabenzoporphins of the basis of isoindoline

Chemistry of Heterocyclic Compounds -