XRF法在聚乙烯微量金属分析中的应用

探讨了用Ｘ射线荧光光谱分析法（ＸＲＦ法）测定聚乙烯中所含的微量金属Ｆｅ、Ｔｉ、Ａｌ的方法，简 分析条件及实验方法。     

Measurement of zeolite,silicate, and phosphate in laundry detergent products by inductively coupled plasma atomic emission spectrometry

This paper reports the development of a method for simultaneously measuring zeolite, silicate, and phosphate in laundry detergent products by inductively coupled plasma atomic emission spectrometry. A sample is decomposed under alkaline oxidative conditions to decompose zeolite, silicate, phosphate, and organic substances. Then hydrochloric acid is added to the decomposed solution to dissolve aluminum hydroxide precipitate before analysis. This sample preparation procedure was investigated by using a total organic carbon analyzer and was confirmed to be applicable to simultaneous measurements of zeolite, silicate, and phosphate. Relative standard deviation for the analysis is less than 2.1%, recovery is more than 99.0%, and the calibration curve gives a correlation coefficient ofR=1.000. The detection limit of this method for aluminum and silicon is 0.1%, and for phosphorus, 0.2% by weight in the product. This method is applicable to various laundry detergent products that contain zeolite, silicate, or phosphate and is five times faster than the three wet chemical methods.     

Synthesis, isolation, spectroscopic and electrochemical characterization of some calcium-containing metallofullerenes

A few Ca-containing mono-metallofullerenes, i.e. Ca@C₇₆, Ca@C₈₈, Ca@C₉₀ (I, II), were synthesized by an improved DC arc discharge method and isolated by a multi-stage HPLC method for the first time. These isomer-separated metallofullerenes were characterized by LD-TOF MS and UV-vis-NIR spectrometry. Their HOMO-LUMO band gaps and possible molecular geometries are discussed according to the absorption spectra in this report. In addition, the cyclic and differential pulse voltammetry of Ca@C₇₆ was conducted in MeCN/C₆H₅CH₃ (1:4 v/v). The voltammograms of Ca@C₈₂ (II, III) and Ca@C₈₄ (II) were also recorded. Their electrochemical behaviors are discussed compared with those of corresponding ytterbium metallofullerenes. The features of the Ca metallofullerenes’ electronic structures are also discussed.     

悬浮液进样-火焰原子吸收光谱法测定茶叶中的微量铬

将茶叶悬浮于琼脂胶体中制成悬浮液 ,直接喷入空气 -乙炔火焰 ,用火焰原子吸收光谱法测定茶叶中的微量铬 ,方法简便、快速、灵敏度和精密度高、测定结果与用灰化法处理样品一致 ,检验表明 ,两种样品前处理方法之间无显著性差异。相对标准偏差为 3.4 %～ 6 .1% ,加标回收率为 95 .7%～ 10 3.8 %。     

Characterization of the TAG of peanut oil by electrospray LC-MS-MS

A study of processed peanut oil was undertaken to assess the utility of HPLC combined with tandem MS to obtain data easily regarding the number of TAG of fats and oils and their FA composition. Mass chromatograms and spectra corresponding to only TAG of a single M.W. were obtained for the full range of TAG in the sample. Analysis of the mass spectra allowed the identification of more than 160 TAG in the sample by their FA composition. In addition, it was possible to estimate relative abundances of the TAG and suggest the position of the FA on glycerol for a limited number of cases. This technique greatly simplifies the task of assigning FA to coeluting TAG and facilitates identification of TAG present in trace quantities in mixtures, with possible application in circumstances where such trace TAG could be significant markers. Results are quickly obtained without extensive sample preparation or prefractionation of the sample.     

The influence of an intermediate MoO3 layer on the solid state reaction of cobalt oxide withγ-Al2O3

In view of the importance for Co_xO_y,-MoO₃/-Al₂O₃ hydrodesulphurization (HDS) catalysts, the reactivity of cobalt oxide layers towards cobalt aluminate formation was investigated on both MoO₃-covered and bare -Al₂O₃ substrates. Co₃O₄/MoO₃/-Al₂O₃ and Co₃O₄/-Al₂O₃ systems were prepared by vapour-deposition of MoO₃ (12 × 10¹⁵ Mo atoms/cm²) and Co (400 × 10¹⁵ Co atoms/cm²) layers onto a -Al₂O₃ substrate, followed by oxidation of the Co layer to Co₃O₄. After annealing at 800°C for 40 h, the interfacial reaction to cobalt aluminate was assessed using Rutherford backscattering spectrometry. The presence of molybdenum oxide appeared to enhance cobalt aluminate formation. The Mo atoms, which spread out over the entire cobalt-containing layer, presumably caused a high defect density, which explains the observed higher reaction rate. The amount of MoO₃ was much too low to stabilize all cobalt atoms by cobalt molybdate formation.     

Identification of nine acetylenic fatty acids, 9-hydroxystearic acid and 9,10-epoxystearic acid in the seed oil ofJodina rhombifolia hook et arn. (Santalaceae)

In addition to some usual fatty acids, the seed oil ofJodina rhombifolia (Santalaceae) contains nine acetylenic fatty acids [9-octadecynoic acid (stearolic acid) (1.1%),trans-10-heptadecen-8-ynoic acid (pyrulic acid) (20.1%), 7-hydroxy-trans-10-heptadecen-8-ynoic acid (2.3%),trans-10,16-heptadecadien-8-ynoic acid (0.7%), 7-hydroxy-trans-10,16-heptadecadien-8-ynoic acid (0.1%),trans-11-octadecen-9-ynoic acid (ximenynic acid) (20.3%), 8-hydroxy-trans-11-octadecen-9-ynoic acid (12.2%),trans-11,17-octadecadien-9-ynoic acid (1.5%), 8-hydroxy-trans-11,17-octadecadien-9-ynoic acid (1.3%), 9-hydroxystearic acid (<0.1%) and 9,10-epoxystearic acid (0.7%)]. The fatty acids have been analyzed by gas chromatography/mass spectrometry of their methyl ester and 4,4-dimethyloxazoline derivatives. The hydroxy fatty acid methyl esters have been examined also as trimethyl-silyl ethers. Furthermore, the fatty acid methyl esters (FAME) have been fractionated according to their polarity (FAME-A: nonhydroxy; FAME-B: hydroxy fatty acids) and to their degree of unsaturation (FAME-A1/A2; FAME-B1/B2) by preparative thin-layer chromatography and argentation chromatography, respectively. All of these fractions have been analyzed by ultraviolet and infrared spectroscopy, and the fractions FAME-A and FAME-B have been analyzed further by nuclear magnetic resonance (¹H,¹³C, 2D H/C, attached proton test) spectroscopy and gas chromatography/mass spectrometry. This work is dedicated to the 65th birthday of Prof. Dr. K. Pfeilsticker, Institut of Food Science, University Bonn (Germany).     

Transient analysis of the release and reduction of NOx using a Pt/Ba/Al2O3 catalyst

The release and reduction of NO_x in a NO_x storage-reduction (NSR) catalyst were studied with a transient reaction analysis in the millisecond range, which was made possible by the combination of pulsed injection of gases and time resolved time-of-flight mass spectrometry. After an O₂ pulse and a subsequent NO pulse were injected into a pellet of the Pt/Ba/Al₂O₃ catalyst, the time profiles of several gas products, NO, N₂, NH₃ and H₂O, were obtained as a result of the release and reduction of NO_x caused by H₂ injection. Comparing the time profiles in another analysis, which were obtained using a model catalyst consisting of a flat 5 nmPt/Ba(NO₃)₂/cordierite plate, the release and reduction of NO_x on Pt/Ba/Al₂O₃ catalyst that stored NO_x took the following two steps; in the first step NO molecules were released from Ba and in the second step the released NO was reduced into N₂ by H₂ pulse injection. When this H₂ pulse was injected in a large amount, NO was reduced to NH₃ instead of N₂.

A only small amount of H₂O was detected because of the strong affinity for alumina support. We can analyze the NO_x regeneration process to separate two steps of the NO_x release and reduction by a detailed analysis of the time profiles using a two-step reaction model. From the result of the analysis, it is found that the rate constant for NO_x release increased as temperature increase.     

填充玻璃纤维滤膜基钛酸锶钡的手控注射式富集器对水中锌的富集性能

以多孔玻璃纤维滤膜基钛酸锶钡（BBST）为吸附材料,制备了手控注射式富集器;考察了该富集器对水中Zn2＋的吸附富集性能.结果表明：当介质的pH值为3-7时,多孔玻璃纤维滤膜基钛酸锶钡对水中的Zn2＋具有很强吸附能力,其静态吸附容量为24.30 mg/g;制备的富集器可实现对Zn2＋的动态吸附,被吸附的Zn2＋可用2.0%的EDTA溶液动态洗脱回收,其浓集因子可达500.提出了手控注射式钛酸锶钡富集器富集,火焰原子吸收光谱法测定水中痕量Zn2＋的新方法.方法检出限为0.09μg/L.应用于一次蒸馏水和纯净水中痕量Zn2＋的富集,用火焰原子吸收法测定,回收率为93.0%-102.0%.