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961.
The present work describes a metallic hydride atomizer for atomic absorption spectrometry, by evaluating the performance of the Inconel 600® tube. For this purpose, stibine was used as the model volatile compound and antimony determination in river and lake sediments and in pharmaceutical samples was carried out to assess the metal furnace performance. Some parameters are evaluated such as those referring to the generation and transport of the hydride (such as KBH4 and acid concentrations, carrier gas flow rate, injected volume, etc.), as well as those referring to the metal furnace (such as tube hole area, flame composition, long-term stability, etc.). The method presents linear Sb concentration from 2 to 80 μg L−1 range (r > 0.998; n = 3) and the analytical frequency of ca. 140 h−1. The limit of detection (LOD) is 0.23 μg L−1 and the precision, expressed as R.S.D., is less than 5% (40 μg L−1; n = 10). The accuracy is evaluated through the reference materials, and the results are similar at 95% confidence level according to the t-test. 相似文献
962.
Masataka Hiraide Kennich Ishikawa Zuo Sheng Chen Hiroshi Kawaguchi 《Mikrochimica acta》1994,117(1-2):7-13
Coprecipitation first with magnesium hydroxide, next with tin(IV) hydroxide is developed for the determination of traces of beryllium in sea-water. To a 200-ml sample is added a sodium hydroxide solution to form magnesium hydroxide at pH 11.5, on which beryllium is quantitatively coprecipitated. The precipitate is separated by centrifugation and dissolved in 2 ml of 12 mol/l hydrochloric acid. The resulting solution (ca. 10 ml) is mixed with 2 mg of tin (IV) carrier and the pH is adjusted to 5.0 to collect the beryllium on tin (IV) hydroxide, leaving magnesium ions in the solution. The tin (IV) hydroxide is centrifuged, dissolved in 0.1 ml of 5 mol/l hydrobromic acid, and then diluted to 1 ml with water. Magnesium is so added as to be 500 g/ml for increasing the sensitivity about four times, and the beryllium in the solution is determined by graphite furnace atomic absorption spectrometry. The experiments with synthetic seawater samples showed that pg — g amounts of beryllium can be coprecipitated on the metal hydroxides and beryllium at the low ng/1 level can be determined with reasonable precision (RSD < 10%). The detection limit of the proposed method is 0.5 ng/l of beryllium in seawater. 相似文献
963.
全反射X—射线荧光光谱的原理和应用 总被引:9,自引:2,他引:9
本文综述全反射-X射线荧光光谱分析的进展,原理,仪器和应用。参考文献67篇。 相似文献
964.
W. Mikenda F. Pertlik E. Steinwender 《Monatshefte für Chemie / Chemical Monthly》1993,124(8-9):867-875
Summary X-ray structural data are reported for 2-hydroxy-benzhydrazide(monoclinic; P21/n-C
2h
5
;a=10.569(2) Å,b=11.264(2) Å,c=6.074(1) Å, =98.80(1)°;Z=4;R=0.054) and 2-hydroxy-thiobenzhydrazide (monoclinic; P21/n-C
2h
5
;a=14.598(6) Å,b=5.975(2) Å,c=9.286(4) Å, =107.80(3)°;Z=4;R=0.044). In both compounds the phenolic OH groups are intramolecularly hydrogen bonded to the (thio)carbonyl oxygens and sulfurs, respectively; the basic intermolecular association patterns consist of closed six-membered hydrogen bonded dimers which are connected via N-H ... NH2 hydrogen bonds. The spectral characteristics of the intramolecular O-H...O/S hydrogen bonds (solid state
(OH)=2800/2700 cm–1, CCl4 solution
(OH)=3035/3100 cm–1, CDCl3 solution (OH)=11.62/10.56 ppm) are similar to those of corresponding primary and secondary amides. The solid state IR spectra are consistent with hydrogen bonded NH groups and free NH2 groups, the solution IR spectra indicate free NH2 as well as free NH groups.
Wasserstoffbrückenbindung in 2-Hydroxy-benzhydrazid und 2-Hydroxy-thiobenzhydrazid. Strukturelle und spektroskopische Untersuchungen
Zusammenfassung Es werden Röntgenstrukturdaten für 2-Hydroxy-benzhydrazid (monoklin; P21/n- C 2h 5 ;a=10.569(2) Å,b=11.264(2)Å,c=6.074(1)Å, =98.80(1)°;Z=4;R=0.054) und 2-Hydroxy-thiobenzhydrazid (monoklin; P21/n - C 2h 5 ;a=14.598(6)Å,b=5.975(2)Å,c=9.286(4)Å, =107.80(3)°;Z=4;R=0.044) berichtet. In beiden Verbindungen bilden die phenolischen OH-Gruppen intramolekulare Wasserstoffbrücken mit den Carbonyl-Sauerstoff-, bzw. den Thiocarbonyl-Schwefel-Atomen. Das intermolekulare Assoziationsmuster wird durch N-H...NH2 Wasserstoffbrücken bestimmt, die jeweils zwei Moleküle über sechszählige Ringe zu Dimeren verbinden. Die IR- und NMR-spektroskopischen Charakteristika der intramolekularen O-H...O/S Wasserstoffbrücken (kristallin: (OH)=2800/2700 cm–1, CCl4-Lösungen: (OH)=3035/3100 cm–1, CDCl3-Lösungen: (OH)=11.62/10.56 ppm) sind sehr ähnlich zu denen entsprechender primärer und sekundärer Amide. Die Festkörper-IR-Spektren stehen in Einklang mit assoziierten NH- und freien NH2-Gruppen, während die Lösungs-IR-Spektren auch auf das Vorliegen freier NH-Gruppen schließen lassen.相似文献
965.
钌—钛金属氧化物涂层电极的电子能谱分析 总被引:1,自引:0,他引:1
用X-光电子能谱分析了Ru-Ti金属氧化物电极的组成、结构和元素价态。结果表明,电极表面不同于体内,讨论了表面和体内Ti的价态区别对Ru-Ti阳极活性和寿命的影响,指出掺杂Ir和Pd后会提高电极活性。 相似文献
966.
Nigel T. Lucas Marie P. Cifuentes Lam T. Nguyen Mark G. Humphrey 《Journal of Cluster Science》2001,12(1):201-221
The new phosphines Ph2PC6H4-4-CCR [R=SiMe3 (1), H (2)] have been used to prepare Ru3(CO)9(Ph2PC6H4-4-CCSiMe3)3 (4) and Ru(CCC6H4-4-PPh2)(PPh3)2(-C5H5) (3), respectively, the latter with a pendent phosphine. Reaction of 4 with carbonate or fluoride affords Ru3(CO)9(Ph2PC6H4-4-CCH)3 (5) with pendent terminal alkynyl groups, the identity of which was confirmed by a structural study. Reaction of 5 with [Ru(NCMe)(PPh3)2(-C5H5)]PF6 or reaction of Ru3(CO)12 with 3 gives Ru3(CO)9{(Ph2PC6H4-4-CC)Ru(PPh3)2(-C5H5)}3 (6). Complexes 3–6 have been studied by cyclic voltammetry. Proceeding from Ru3(CO)12 to 4 or 5 shifts the cluster-centred reduction to more negative potential and affords facile cluster-centred oxidation. Proceeding from 4/5 and 3 to 6 results in similarly-located cluster-centred reduction and peripheral ruthenium-centred oxidation, but results in a lack of observable cluster-centred oxidation. Crystal data for 5·C6H14: space group P¯1, a=12.760(1) Å, b=17.077(1) Å, c=17.924(2) Å, =108.656(5)°, =96.344(5)°, =93.523(5)°, V=3658.4(6) Å3, Z=2, R=0.078, Rw=0.105 for 5008 reflections [I>2.00(I)]. 相似文献
967.
The decomposition of N2O in a 13.56-MHz parallel-plate system was studied usingin situ Fourier transform infrared (FTIR) spectroscopy. Areas of two infrared absorption bands of N2O recorded at 8 cm–1 resolution were used to estimate relative gas-phase dissociation as a function of rf power and flow rate at 500 mT. Flow rate was found to strongly affect band areas over the range of powers investigated (10–90 W). The effect of rf power on band areas diminished above 40 W, probably due to poor plasma confinement. Distortion of the band shapes by the plasma permitted rotational temperatures to be estimated. Rotational temperature increased essentially linearly with power at constant flow rate, reaching 450 K at 80 W, but was independent of flow rate at constant power. Rotational temperatures were also found to depend on the temperature of the electrodes, which were heated by plasma exposure. No infrared-active product species were observed even under batch conditions where all N2O was irreversibly dissociated. This lack of detectable products and a 50% pressure rise observed in a batch study suggest that N2 and O2 are the primary stable discharge products. 相似文献
968.
Moreno-Cid A Yebra MC Cancela S Cespón RM 《Analytical and bioanalytical chemistry》2003,377(4):730-734
Iron was extracted on-line from solid meat samples by a simple and rapid continuous ultrasound-assisted extraction system (CUES). The CUES is connected to a flow injection manifold, which allows the on-line flame atomic absorption spectrometric determination of iron. A Plakett–Burman design was used for the optimisation of the CUES. The method achieved a total sampling frequency of 11 samples per hour with a relative standard deviation for the complete procedure of 0.4%. The detection limit was 0.6 g g–1 (dry mass) for a sample amount of 30 mg. Accurate results were obtained by measuring the certified reference materials BCR-186 (pig kidney) and BCR-184 (bovine muscle). The analytical procedure was applied to different real meat samples with satisfactory results. 相似文献
969.
Kim WS Park M Lee DW Moon MH Lim H Lee S 《Analytical and bioanalytical chemistry》2004,378(3):746-752
Fly ash has been regarded as hazardous because of its high adsorption of toxic organic and/or inorganic pollutants. Fly ash is also known to have broad distributions of different chemical and physical properties, such as size and density. In this study, fly ash emitted from a solid waste incinerator was pre-fractionated into six sub-populations by use of gravitational SPLITT fractionation (GSF). The GSF fractions were then analyzed by sedimentation field-flow fractionation (SdFFF) and ICP–AES. SdFFF analysis showed the fly ash has a broad size distribution ranging from a few nanometers up to about 50 µm. SdFFF results were confirmed by electron microscopy. Inductively coupled plasma–atomic emission spectroscopy (ICP–AES) analysis of the GSF fractions showed the fly-ash particles contain a variety of inorganic elements including Ca, Si, Mg, Fe, and Pb. The most abundant in fly ash was Ca, followed by Si then Mg. No correlations were found between trace element concentration and particle size. 相似文献
970.
Hamdi N. Feutelais Y. Yagoubi N. de Girolamo D. Legendre B. 《Journal of Thermal Analysis and Calorimetry》2004,76(3):985-1001
Indomethacin is known to exhibit polymorphism and solvates, the different forms obtained do not exhibit the same solubility
and their bioavailabilities are different. It is of a prime importance to identify the various polymorphic and solvated forms.
This study was carried out by: DSC (different scanning calorimetry), TG (thermogravimetric analysis), X-ray diffraction and
thermomicroscopy. Seven solvates, with acetone, benzene, dichloromethane, tetrahydrofurane, propanol, chloroform and diethylether,
were isolated and studied. Their formulae have been determined by thermogravimetric analysis and their X-ray patterns on powder
are presented, by DSC their behaviour after desolvation is recorded, the temperature and the enthalpy of fusion are measured
and by this way the form obtained is deduced.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献