CID-ICP-AES检测煤中不同形态的硫

研究了CID-ICP-AES检测煤中硫酸盐和硫铁矿形态硫的方法。较现有国标方法快速、简便，常见元素不干扰，加标回收率在98．5％-103．0％之间，10次测定的RSD在0．76％-1．59％之间。     

The prediction of coal properties using compressed infrared data from osculating polynomials

Reduction of the representation of infrared spectra from coal samples by osculating polynomials of degree nine is discussed. The reduced representation contains polynomial coefficients of order zero to four. Mathematical models of the original spectra are obtained by linear combination of the coefficients. These compressed models are statistically correlated to coal properties, namely, volatile matter, fixed carbon, ash content, heating value, hydrogen, carbon, sulphur, nitrogen, and maximum vitrinite reflectance, and the results are compared with those previously obtained from second derivatives of the same spectra. The use of compressed data, while giving slightly better correlations for some of the properties, has the advantage of requiring less computational time.     

Thermal behaviour of ethynyl and ethenyl terminated imide resins

A series of ethynyl and ethenyl end-capped imide resins were synthesised by the reaction of 9,9-bis(4-aminophenyl) fluorene (BAF) with pyromellitic dianhydride (PMDA)3/3′, 4,4′-benzophenone tetracarboxylic acid dianhydride (BTDA)/2,2-bis(3,4-dicarboxy phenyl) hexafluoropropane dianhydride (6F) and 3-ethynyl aniline/maleic anhydride. Structural characterisation was done by infra red and elemental analysis. Thermal characterisation was done by differential scanning calorimetry and thermogravimetric analysis. The decomposition temperatures of cured resins were above 200°C in nitrogen atmosphere. Char yield at 800°C ranged from 59–65.5%.     

Fluorescence study of the solubilization of benzo[a]pyrene: application to its detection in coal washing waters

The solubilization of benzo[a]pyrene by organic solvents (dioxane, toluene and dichloromethane) and a surfactant (Triton X-100) was investigated. These media were successfully used for the determination of benzo[a]pyrene using fluorescence detection, with excellent limits of detection and large linear analytical ranges. Benzo[a]pyrene was detected in coal washing waters using liquid chromatography with fluorescence detection. The stability of this compound in dioxane was also examined.     

A new approach for fluorine determination by solid sampling graphite furnace molecular absorption spectrometry

This work deals with the determination of fluorine by solid sampling graphite furnace molecular absorption spectrometry. The molecular absorbance of aluminum monofluoride (AlF), which is produced in the vapor phase in the presence of Al³⁺, is measured at 227.5 nm, a non-resonant platinum line. A conventional graphite furnace program has been used with pyrolysis and vaporization temperatures of 800 and 2300 °C, respectively. Solutions of Ba²⁺ and Al³⁺ have been used to avoid fluorine losses during the pyrolysis stage and to produce AlF in the vaporization stage, respectively. Certified coal and alumina samples were analyzed using aqueous standards for calibration. The agreement between the found concentration and the certified value, or the value obtained by another method ranged from 92 to 105%, with a relative standard deviation less than 8.5%. The limit of detection and the characteristic mass was 0.17 μg g^− 1 and 205 pg, respectively.     

Donator-Acceptor Komplex Chromatographie Tetrachlorphthalimidopropylsilica,eine neue,chemisch gebundene Phase,geeignet zur Trennung von Kohleverflüssigungsprodukten und anderen technischen aromatischen Gemischen mit der Hochleistungsflüssigkeitschromatographie

Summary The preparation of a new tetrachlorophthalimidophase for HPLC is described. The capacity ratios (k) of about forty aromatics and twenty nitrogen-containing aromatics were determined. Most of the compounds used were alkylated. It was shown that the aromatics were eluted according to the number of rings, only slightly influenced by the substituents. A similar elution order was not observed with the heteroaromatics. The performance of the stationary phase is demonstrated, performing separations of coal liquids and other aromatic mixtures.

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Donator-Acceptor Komplex Chromatographie Tetrachlorphthalimidopropylsilica, eine neue, chemisch gebundene Phase, geeignet zur Trennung von Kohleverflüssigungsprodukten und anderen technischen aromatischen Gemischen mit der Hochleistungsflüssigkeitschromatographie

Zusammenfassung Es wird die Synthese einer neuen Tetrachlorphthalimid-Phase für die HPLC beschrieben. Anhand von Elutionsversuchen mit über vierzig Aromaten und zwanzig N-Heteroaromaten, die größtenteils alkyliert waren, konnte gezeigt werden, daß kondensierte Aromaten unabhängig vom Alkylierungsgrad streng nach der Zahl der aromatischen Ringe eluiert werden, was für die Heterocyclen nicht zutrifft. Die Kapazitätsverhältnisse (k) der untersuchten Verbindungen werden angegeben. Die Leistungsfähigkeit der Phase wird an der chromatographischen Trennung von Kohleverflüssigungsprodukten und anderen komplexen, aromatischen Gemischen demonstriert.

     

Effect of HF addition on the microwave-assisted acid-digestion for the determination of metals in coal by inductively coupled plasma-atomic emission spectrometry

The microwave-assisted acid-digestion for the determination of metals in coal by ICP-AES was investigated, especially focusing on the necessity of adding HF. By testing five certified reference materials, BCR-180, BCR-040, NIST-1632b, NIST-1632c, and SARM-20, it was found that the two-stage digestion without HF (HNO₃ + H₂O₂ was used) was very effective for the pretreatment of ICP-AES measurement. Both major metals (Al, Ca, Fe, and Mg) and minor or trace metals (Co, Cr, Cu, Mn, Ni, Pb, and Zn) in coal gave good recoveries for their certified or reference values. The possibility of ‘HF-memory effect’ was cancelled by the use of a set of vessels which had been never contacted with HF. Twenty-four Japanese standard coals (SS coals) were analyzed by the present method, and the concentrations of major metals measured by the present method provided very high accordance with those from the authentic JIS (Japanese Industrial Standard) method.     

Reactivity and characterisation of various rank turkish bituminous coal chars

A set of seven bituminous coal chars has been characterised by IR spectroscopy (FTIR), thermogravimetry (TG) and elemental analysis. FTIR study provided suitable information to establish differences between coal samples according to their chemical compositions. The reactivity of these samples was also studied and correlated with the coal parameters of mean vitrinite reflectance, fuel ratio and H/C ratio. The data suggest that reactivity as determined can be correlated with the mean vitrinite reflectance, fuel ratio and H/C ratio (0.90). The order of reactivity of samples were; Amasra (S1) (R _m= 0.65)>Azdavay (S4) (R _m=0.99)»Armutcuk (S2) (R _m=0.81)»Acenta (S3) (R _m=0.92)>Ac2l2k (S6) (R _m=1.11) Cay (S5) (R _m=1.03)>Sogutozu (S7) (R _m=2.14).     

Chromatographie par complexe de transfert de charge. Application à l'analyse d'hydroliquéfiats du charbon par HPLC

Résumé L'analyse de coupes lourdes (huile de distillation sous vide et huile issue du séparateur à chaud) provenant de l'hydroliquéfaction catalytique du charbon a été réalisée par mise en ouvre de différentes techniques chromatographiques. L'identification des principales structures résulte de l'application de la chromatographie par couplage de transfert de charge en mode HPLC et des spectroscopies UV et de masse.

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Donotor-acceptor complex chromatography —Application to analysis of coal liquefaction products by HPLC

Summary A Vacuum gas oil and the corresponding residue of a coal liquefaction product were investigated by means of HPLC and MS. Nearly a complete identification was performed by chromatographic, UV-spectroscopic methods and MS.

     

Utilization of flash chromatography for the fractionation of coal derived liquids

Summary The suitability of flash chromatography for the fractionation of coal liquids in compound classes has been studied. TLC data obtained from standards were used for establishing the sequence, composition and volume of eluents in order to collect the main components of coal liquids in six fractions of increasing polarity. The method was tested by the fractionation of a SCG coal extract and separations were evaluated by TLC, SEC, and IR and NMR spectroscopy.