分离富集-原子吸收光谱法测定锌锰电池中铅和镉

对用原子吸收光谱法测定锌锰电池中铅和镉结果的可靠性进行了研究。对于典型的4R25电池,试液中主要成分锌和锰总量超过40 g.L-1,直接用普通稀释法得不到准确的结果。采用CL-7301萃淋树脂微色谱柱将电池试液中铅和镉与基体快速分离,用火焰原子吸收光谱法测定铅和镉,当铅和镉的含量较高时,可以将样品预稀释后采用在线稀释技术直接测定铅和镉。     

ABS工程塑料中铅、铬(Ⅵ)、镉及汞含量测定

用浓硫酸与浓硝酸(1 5)的混合酸消解ABS工程塑料试样,消解过程中铅(Ⅱ)以PbSO4形式沉淀,用乙酸铵溶解PbSO4沉淀后在乙酸盐缓冲溶液中用火焰原子吸收光谱法(FAAS)测定铅,检出限为0.088 mg·L-1.溶液中镉(Ⅱ)也用FAAS法测定,其检出限为0.074 mg·L-1,溶液中汞采用氢化物发生,冷原子蒸气-原子吸收光谱法测定,其检出限为0.64 μg·L-1.六价铬采用二苯基羰酰二肼光度法测定,检出限为0.039 mg·L-1.对方法的精密度及回收率作了试验,测得相对标准偏差(n=7)均小于3.5%,回收率在91.8%～106.0%之间.     

湿法磷酸中钾、钠、钙、镁的原子吸收光谱法测定

在湿法磷酸生产过程中,为了对生产流程和产品质量进行控制,有必要对湿法磷酸中微量的钾、钠、钙、镁含量进行分析。用火焰原子吸收光谱法测定湿法磷酸中钾、钠、钙、镁受基体和背景以及溶液粘度的影响很大,特别是对钙含量的测定,干扰最严重[1]。为此本文提出用离子交换树脂分离     

硝酸-过氧化氢消解试样-MIBK-APDC萃取分离FAAS法测定酱油中铅

铅是一种对人体极为有害的重金属元素,由于环境及食品污染,酱油也不可避免地从原料、加工及储运过程中引入铅,国家食品卫生标准严格规定:酱油中铅的含量≤1.0 mg·kg-1[1];对酱油中铅的分析常采用火焰原子吸收光度法[2],由于酱油基体较复杂,酱油中铅的含量一般较低,并且存在高达15%的氯化钠,给原子吸收直接测定带来困难。文献[3]报道了用活性炭富集火焰原子吸收光谱法测定酱油中铅,但误差大,在实际工作中难于应用;吴士定等[4]提出了加入基体改进剂后,直接用石墨炉原子吸收测定,效果较好。但由于使用的仪器较贵重,实际应用受到了一定限制…     

火焰原子吸收光谱法测定工业废水中铅锌镉

火焰原子吸收光谱法测定微量铅、锌、镉的报道较多,该法用于工业废水的测定,可实现连续分析,成本低、操作简单,能快速准确地得到测定结果,可及时有效地进行监控。经石灰、片碱处理后的工业废水中含高钠、钙等碱土金属、碱金属等离子,用火焰原子吸收光谱法直接测定此废水中铅、锌、镉的报道不多。     

原子吸收光谱法测定植物叶中微量重金属

用浓硝酸与高氯酸混酸消解植物叶，其中铜、锌及锰含量较高，可直接用火焰原子吸收光谱法测定；铅、镉及铬含量较低，用石墨炉原子吸收光谱法测定；铅和镉含量甚微，受基体及共存元素干扰严重，用标准加入法消除干扰。     

原子吸收光谱法同时测定铅钙锡铝合金中钙和锡

铅钙锡铝合金广泛用于全密封免维护铅蓄电池极板的生产。合金中微量钙的测定有汞分离ＥＤＴＡ容量法[1] ,氯化铅 铜试剂分离ＥＤＴＡ容量法[2 ] ,原子吸收光谱法[3 ] 。锡的测定通常采用邻苯二酚紫 十六烷基三甲基溴化铵吸光光度法[4 ] 。而用原子吸收光谱法测定铅钙锡铝合金中钙和锡的方法还未见报道。科研所研制生产的铅钙锡铝合金中含钙0 0 75 %～ 0 .12 % ,含锡 0 .4 %～ 0 .6 % ,含铝 0 .0 2 %～ 0 .0 3% ,余量为铅。本文用原子吸收光谱法同时测定其中的钙和锡 ,吸收波长分别为 4 2 2 .7和2 86 3ｎｍ。为了防止铅钙锡铝合金中锡水…     

原子吸收光谱法测定丹参及其近缘种中痕量元素

丹参及其近缘种样品用硝酸-高氯酸混合酸(体积比4比1)浸泡过夜,加热消解.在优化的仪器工作条件下,用火焰原子吸收光谱法测定所制得样品溶液中钙、镁、铁、锰、铜和锌的含量,并用石墨炉原子吸收光谱法(GFAAS)测定其中的钼、铅、铬及镉的含量.测定铅及镉时,用磷酸二氢铵作基体改进剂,而测定铬时,用抗坏血酸作基体改进剂.10种元素的检出限(3S/N)均小于0.26μg·g-1,测定钙、镁、铁、锰、铜和锌时,测得其回收率在99.0%～103.6%之间,其相对标准偏差(n=5)在0.54%～1.77%之间;测定钼、铅、铬和镉时,其回收率在100.O%～108.0%之间,相对标准偏差(n=5)在0.02%～1.9%之间.     

火焰原子吸收光谱法测定锡锌合金丝中的镉

<正>锡锌合金丝属于软钎焊料,是金属化薄膜电容器端面喷金的一类电子焊接材料。电子设备热喷涂用锌和锌合金丝标准规范ASTM B943-2009要求镉的质量分数不大于0.005%。对于纯锡和锡基合金中镉的标准分析方法有邻菲啰啉光度法[1]和火焰原子吸收光谱法[1-3],对于纯锌和锌基合金中镉的标准分析方法有火焰原子吸收光谱法[4-6]。锡锌合金中镉的原子吸收光谱法国内鲜见报道。本工作采用火焰原子吸收光谱法测定锡锌合金     

铬(Ⅵ)-二乙基二硫代甲酸钠共沉淀-原子吸收光谱法测定环境水样中铁、锰、锌、镉

提出了以二乙基二硫代甲酸钠螯合铬(Ⅵ)作为载体共沉淀富集水体中铁、锰、锌和镉的方法。沉淀经离心分离,甲基异丁酮溶解后,以微量进样300μL火焰原子吸收光谱法测定铁、锰、锌,以石墨炉原子吸收光谱法测定镉。用水样10.0 mL,在pH 4.6的邻苯二甲酸氢钾缓冲介质中加入20 g.L-1重铬酸钾溶液150μL,20 g.L-1DDTC溶液1.0 mL可达到完全共沉淀分离,所得沉淀经离心分离后用甲基异丁酮2.0 mL溶解,并用于AAS分析。在优化的条件下,铁、锰、锌和镉的检出限(3σ)分别为9.0,6.8,1.8,0.03μg.L-1,相对标准偏差(n=6)在1.8%~3.8%之间。方法用于实际水样的测定,用标准加入法测得回收率在93.7%~105.0%之间。     

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。     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

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.     

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。     

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.     

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.