Pulse polarographic determination of trace amounts of cobalt (II) by complex formation with calcon

Some aspects of the polarographic reduction of sodium 1-(2-hydroxy-1-naphthylazo)-2-naphthol-4-sulphonate (trivial name: calcon or Eriochrome Blue Black R), as observed when using differential pulse polarography (d.p.p.) and alternating current polarography (a.c.p.), are described, as well as the polarographic behaviour of this compound in the presence of some metal ions. The peak that appears in the d.p.-polarogram due to the reduction of the cobalt (II) complex is the basis of a method for the determination of very small trace amounts of cobalt(II). The proposed procedure is rather selective (Ni(II) interferes, Mn(II) does not) and has a limit of detection of 7 g 1^–1 (minimum amount which can be determined 0.6 g Co(II)).     

硫脲对块体纳米晶工业纯铁在盐酸溶液中的缓蚀行为

采用电化学阻抗谱(EIS)研究了硫脲对室温下1 mol•L－1盐酸溶液中粗晶和纳米晶工业纯铁的腐蚀行为的影响.从EIS的拟合结果得知,在1 mol•L－1盐酸溶液中,块体纳米晶工业纯铁比粗晶工业纯铁腐蚀倾向小.基于纳米晶和粗晶工业纯铁在添加有硫脲的1 mol•L－1盐酸溶液中阻抗谱随浸泡时间的变化关系,观察到以下现象,当浸泡时间短至5 min时,对应不同浓度(50、100、150、500 mg•L－1)的缓蚀剂添加量,在粗晶工业纯铁的阻抗复平面图上出现一感抗弧,而在纳米晶工业纯铁的阻抗复平面图是一圆心下偏的容抗弧.随着浸泡时间的延长,两种样品的容抗弧半径增大,在150 mg•L－1的浓度时,电荷传递电阻(Rct)出现极值,这表明硫脲是一种吸附型缓蚀剂.抗盐酸腐蚀性能的提高和没有感抗弧的出现, 归因于体纳米化的结果,这与体纳米化的制备技术密切相关.     

Inclusion Compounds — possibility of their combination and use in different branches of chemistry

Hofmann-type and related compounds, a natural zeolitic material of the clinoptilolite type, and cyclodextrins have been studied. Different products, useful in the separation of organic mixtures, used with fertilizers and insecticides in agrochemistry, perfumes, and in the detoxication of raw materials, have been prepared by combinations of the inclusion compounds studied. In the Hofmann-type compounds and cyclodextrins the original guest is substituted; in the zeolite the original sorbate, as well as some part of the zeolitic host is substituted. The physical mixtures of the starting materials differed from the products in their thermal, spectral and diffractographic characteristics. Field test results and other supporting evidence are added.     

气提吸附／热脱附／气相色谱－质谱法分析污水中的痕量有机物

采用气提吸附／热脱附／气相色谱－质谱法对齐鲁公司所处地区工业污水进行分析。方法采用Ｔｅｎａｘ－ＧＣ吸附剂对样品进行气提吸附，脱附时样品直接进入色谱仪汽化室，一次进样即可完成全组分分析，共检测出含四氯丙醚在内的４０种有机组分，测定了各组分的程序升温保留指数。气相色谱－质谱法测定出四氯丙醚三个异构体的结构。     

分子筛基NH3吸附材料的制备与性能研究

通过对分子筛原粉添加黏结剂,制备出了适宜作为吸附材料的成型分子筛颗粒.随后对成型分子筛颗粒进行活性组分的负载,并采用氮气吸附等温线对不同样品的比表面积和孔径分布进行了分析表征.通过考察样品对氨气的动态吸附能力,对活性组分的种类和含量进行筛选和优化,最终确定以质量分数为8%的H_2SO_4作为分子筛基氨气吸附材料的配比组成.通过与活性炭吸附材料的对比发现,在低湿度和高湿度2种条件下,分子筛基防护材料对NH3的防护性能均优于活性炭.     

Bridging the Gap between Industrial and Well‐Defined Supported Catalysts

Many industrial catalysts contain isolated metal sites on the surface of oxide supports. Although such catalysts have been used in a broad range of processes for more than 40 years, there is often a very limited understanding about the structure of the catalytically active sites. This Review discusses how surface organometallic chemistry (SOMC) engineers surface sites with well‐defined structures and provides insight into the nature of the active sites of industrial catalysts; the Review focuses in particular on olefin production and conversion processes.     

工业污泥中铜含量的不同测定方法对比

采用火焰原子吸收分光光度法（AAS）和快速碘量法对工业污泥中铜含量进行测定,并对结果做了对比分析.结果表明两种方法的准确性和可操作性均较好,回收率在91.0%~99.0%之间,相对标准偏差均低于7%.碘量法分析简单,结果准确可靠,但不适合分析大批量的样品.火焰原子吸收分光光度法分析速度较快,灵敏度高,可以同时进行大批量的样品分析.     

Organometallic Homogeneous Catalysis—Quo vadis?

Homogeneous catalysis is the success story of organometallic chemistry. Otto Roelen's initial discovery of hydroformylation in 1938 not only entailed large-capacity production plants but was later followed by systematic research into the catalytic chemistry of the ever-growing class of organometallic compounds. Further developments in industrial chemistry towards clean, low-temperature, low-pressure, and economic processes—in feedstock or in the fine chemicals and polymer area—clearly depend on improved catalysts. Molecularly defined, tailor-made structures are the safest prerequisites for chemical selectivity; hence, organometallic compounds with their overwhelming variety of compositions and structures offer the most promising approach. Wilkinson's catalysts [HRh(CO){P(C₆H₅)₃] and [ClRh{P(C₆H₅)}₃}₃] are outstanding examples. On the other hand, process technology has to be considered also (for example catalyst-product separation and hear-exchange problems). The following review attempts to critically assess the future trends and present demands in the applied area of orgnometallic catalysis–a “gentle art” that is far from being a mature field.     

Indirect determination of free cyanide in water and industrial waste water by flow injection-atomic absorption spectrometry

A simple and rapid flow injection system is proposed for indirect determination of cyanide by flame atomic absorption spectrometry. It consists of a microcolumn of immobilized salen (N,N′-bis(salicylidene)ethylenediamine) on sodium dodecyl sulfate (SDS)-coated alumina saturated with silver ion and a carrier of dilute solution of sodium hydroxide (10⁻⁵ mol L⁻¹). The micro-column was located between the injection valve and nebulizer of atomic absorption spectrometry. Injection of 250 μL of aqueous cyanide standard or sample solution at pH range of 9–11 cause elution of silver as silver cyanide complexes, which was then measured by flame atomic absorption spectrometry. The absorbance was proportional to the concentration of cyanide in the sample. The graph of absorbance (as peak height) vs. cyanide concentration was linear over the concentration range of 0.1–10 mg L⁻¹ of cyanide, and the detection limit was 0.06 mg L⁻¹. The relative standard deviation at 1 and 3 mg L⁻¹ of cyanide concentration were 4.1 and 4.7%, respectively. The method was successfully applied to determination of cyanide in water and industrial waste waters, and the accuracy was examined through independent analysis by accepted method of pyridine-barbituric acid.     

工业用水中铁含量的双光束FIA光度法

工业用水中铁含量的双光束ＦＩＡ光度法赵珍义（辽宁大学化学系沈阳１１００３６）李淑凡（辽宁武警总队医院）流动注射分析（ＦＩＡ）具有取样量少、分析速度快、精密度好等优点而被广泛用于分析测试之中［１，２］。目前，ＦＩＡ光度法均采用单光束而开展的研究工作。尚...