用三元络合物萃取-火焰原子吸收法测定食品中痕量镉

建立了一种测定食品中痕量镉的新方法.以茜素黄R和邻菲罗啉为螯合剂,以甲基异丁基甲酮为萃取剂,直接以有机相进样测定,提高了测定的选择性和灵敏度.考察了介质酸度、缓冲溶液及螯合剂的用量等对测定的影响,优化了测定条件.详细研究了常见元素对镉元素测定的干扰情况,用酒石酸钾钠做掩蔽剂,可以消除大量共存组分的影响.在最佳工作条件下,镉离子质量浓度在3.0×10-3 ～0.25 μg·mL-1范围内线性关系良好,方法的检出限为1.7×10-3 μg· mL-1,对0.2 μg· mL-1的镉标准溶液进行9次平行测定,相对标准偏差为1.1％,检出限低,重现性好.该法用于食品中镉的测定,结果满意.     

Pheromone specificity inEriocrania semipurpurella (Stephens) andE. sangii (Wood) (Lepidoptera: Eriocraniidae) based on chirality of semiochemicals

The fifth abdominal segment of femaleEriocrania semipurpurella (Stephens) andE. sangii (Wood) contains a pair of exocrine glands. Hexane extracts of this segment were prepared from both species and analyzed by gas chromatography with simultaneous flame ionization and electroantennographic detection (EAD). For both species, the EAD active peaks were identified as nonan-2-one, (Z)-6-nonen-2-one, and (Z)-6-nonen-2-ol by means of mass spectrometry and comparison of retention indices with those of synthetic standards. Enantiomeric separation of chiral alcohols from the female extracts was achieved by gas chromatographic analysis on a cyclodextrin column. InE. semipurpurella, a mixture of (2S,6Z)-nonen-2-ol and (2R,6Z)-nonen-2-ol (2: I) was found, whereas inE. sangii (2S,6Z)-nonen-2-ol was the predominant enantiomer and only traces of theR enantiomer were indicated by the antennal response. In field tests, a blend of the three compounds was not attractive to conspecific males. A subtractive assay showed that the alcohol in various enantiomeric mixtures was the only attractive compound, whereas addition of (Z)-6-nonen-2-one to the alcohol completely inhibited the attraction of both species. A trapping experiment including a wide range of ratios between theR andS enantiomers showed that baits containing 95–100% of theS enantiomer were attractive to maleE. sangii, whereas males ofE. semipurpurella were attracted to all tested ratios of the enantiomers. However, the response profiles of maleE. semipurpurella differed between populations from southern Sweden, south Finland, and the Kola Peninsula in Russia. In south Sweden males were maximally attracted to a racemic mixture of the alcohols. At the Kola PeninsulaE. semipurpurella was attracted to baits containing 95–100% of theR enantiomer. In south Finland all tested ratios between 0 and 100%R enantiomer trappedE. semipurpurella, but the trap catches appeared to be bimodally distributed with peaks around 15 and 70%R enantiomer. The trapping results suggest the existence of pheromone races or sibling species among the specimens identified asE. semipurpurella.Dedicated to Prof. H. J. Bestmann on the occasion of his 70th birthday.     

Synthesis and photo-induced solution properties of new rigid-rod polyimides

A series of new, substituted pyromellitic dianhydrides were synthesized from 1,2,4,5-tetramethylbenzene. New soluble rigid-rod polyimides were obtained from the dianhydrides and 2,2′-bis(trifluoromethyl)-4,4′-biphenyl (PFMB) in phenolic solvents in the presence of isoquinoline as a catalyst. The polyimides are soluble in N-methyl-2-pyrrolidone (NMP), N,N-dimethylacetamide (DMAc), m-cresol and other solvents, in spite of having no bending in their rigid structures.

UV irradiation changed color of the polyimide solutions and also their viscosity. We observed new absorbance in the 700-nm region and an ESR signal by UV irradiation. The new visible absorbance and the ESR signal are derived from the same origin. They are attributed to the anion radical of the diimide moiety in the polyimide as deduced from the hyper fine structure of the ESR signal. In addition, UV irradiation diminishes the solution viscosity.     

X射线荧光光谱法测定连铸保护渣的化学成分

根据连铸保护渣成分及试样特点,对试样预处理、试样熔融条件、熔制程序及干扰校正等进行试验研究,运用X射线荧光光谱法测定连铸保护渣中主要化学成分的含量。测定结果显示,各成分校准曲线相关系数大于0.999,相对标准偏差小于0.5%,与化学法对照结果无显著差异。     

家用冰箱储藏室内挥发性有机物检测及分析

为研究家用冰箱储藏室中挥发性有机化合物(VOCs)的释放量及主要来源,采用气相色谱–质谱法对工作状态下冰箱储藏室的VOCs含量进行检测;利用傅里叶变换红外光谱仪对冷藏室的物料进行成分分析,同时用密封舱法探究冷藏室不同物料对VOCs含量贡献。结果表明,冰箱冷藏室物料中发泡聚苯乙烯风道泡沫释放的总挥发性有机化合物(TVOC)、正戊烷及异戊烷最多,是造成异味的关键性物料,而正戊烷、异戊烷是冰箱异味的主要成分。聚氯乙烯门封条对异味的贡献也较大,通用聚苯乙烯抽屉体贡献的VOCs种类最多;在工作状态下,随着密闭时间的增加,冰箱储藏室的VOCs的种类及含量增加,但苯、甲苯、二甲苯、TVOC及戊烷类的含量均未超过国家标准。储藏室异戊烷含量较高,是冰箱的异味的主要来源。     

热裂解气质联用鉴别PA56、PA66和PA6

采用热裂解气质联用（Py-GC/MS）方法鉴别聚酰胺56（PA56）、聚酰胺66（PA66）和聚酰胺6（PA6）及其共混物。结果表明,在550 ℃裂解温度下,PA56与PA66相对丰度100 %的峰为环戊酮,分别具有特征裂解产物1,8-二氮杂环十三烷-2,7?二酮和1,8-二氮杂环十四烷-2,7-二酮,PA6相对丰度100 %的峰为己内酰胺;此方法可用于快速鉴别PA56、PA66和PA6的工业初级品,并成功检出了PA6/PA56共混物、PA6/PA66改性共混物与改性PA66。     

321不锈钢钝化膜孔蚀破坏的原子吸收光谱研究

采用原子吸收光谱方法测定不锈钢局部破坏后各种元素的析出量，研究了３２１不锈钢在ＮａＣｌ水不溶液中钝化膜孔蚀破坏的特征。研究结果表明：ＡＡＳ可有效地用于不锈钢孔蚀动力学的研究。     

Microstructure of a nitrided steel previously decarburized

In this study the effects of a surface-controlled decarburization on the structure of a nitrided steel are analyzed. Samples of a quenched and tempered 42CrMo4 steel were decarburized by heating in air at different depths and submitted to gaseous nitriding. After decarburization and nitriding, the microstructure of surface layers was investigated by optical microscopy (OM) and scanning electron microscopy (SEM). The nitrogen and carbon profiles in the diffusion layers were determined by SEM equipped with a wavelength dispersive spectrometer (EPMA-WDS) and by glow discharge optical spectrometry (GDOS). The effect of nitriding was determined by microhardness measurements. Our results indicate that a previous decarburization only slightly affects the surface hardness, but reduces the conventional nitriding depth. The decarburization also favors the nitrogen take-up and produces increased nitrogen concentrations in the compound layer and in the narrow zone beneath it.     

Morphological and microchemical phenomena in the high-temperature oxidation of binary Al-Li alloys

The high-temperature oxidation behavior of binary Al-Li alloys has been characterized by scanning electron microscopy and secondary ion mass spectrometry in order to understand the mechanism of rapid oxidation in these alloys and to correlate the oxide morphology to its microchemistry. The oxide scale developed on polished specimens during short exposures in air at 530°C shows characteristic nodules that usually nucleate at grain boundaries. Examination of the alloy surface after removal of the oxide layer shows that the initial growth of the oxide nodules occurs laterally in addition to thickening normal to the oxide/alloy interface. Microchemical analysis of the oxide film with a scanning ion microprobe reveals a thick Li-oxide layer at the oxide/gas interface indicating preferential oxidation of Li at the free surface; the rest of the oxide film is composed of both Al- and Li-rich oxides, probably Li₂O and LiAlO₂ The presence of trace impurities (K, Na, F, and Cl) in the oxide scale was also detected. A microstructural model for the development of the oxide film in the Al-Li system is presented on the basis of both morphological and microanalytical data obtained in this study; this new model is compared with existing models.     

Synergistic influence of alloy grain size and Si content on the oxidation behavior of 9Cr−1Mo steel

The synergistic influence of prior-austenite grain size and silicon content of 9Cr–1Mo steel on the resistance to scale spallation has been studied in air at 773 K (for 500 hr) and 973 K (12 hr). Two steels, irrespective of their grain size and Si content, did not show spallation during oxidation at 773 K. Spallation occurred at 973 K, and fine-grain steels exhibited less spallation resistance than coarse-grain ones (in low-as well as high-Si steels). Among the four possible combinations of grain size ans Si content, the steel with low Si and fine grains showed least resistance to spallation, while the steel with high Si and coarse grains showed the best resistance. Spallation was found to initiate in the areas adjoining the oxide ridges formed at the alloy grain boundaries. Oxide scales at the ridges and within the grains were analyzed by scanning electron microscopy (SEM/EDX) and secondary-ion mass spectrometry (SIMS). These analyses suggest depletion of silicon from the areas adjoining grain boundaries, resulting in thicker scaling that triggers spallation in such areas. For similar grain-size materials, the necessary thickness for spallation was attained earlier with low-Si steel rather than in high-Si steel.