Gas Phase Addition of Rare-earth Fullerenes with Benzene

Gas phase adduct of endohedral rare-earth fullerenes Nd@C-S2 with the ion system of benzene-[Nd@C-S2-C6H6](+) was observed for the first time by ion-molecular reaction under chemical ionization condition. The possible reaction passageway and molecular structures of this gas phase adduct were discussed and a parallel "reversed umbrella" pi-pi interaction complex of the [C6H6](+) ion reacting with the neutral rare-earth fullerenes Nd@C-S2 was considered to be much reasonable. The experimental result indicated that endohedral rare-earth fullerenes has relatively active reactivity and aromatic properties similar towards benzene molecular ion in gas phase.

High-yield extraction of endohedral rare-earth fullerenes

The technique of high-temperature high-pressure extraction with pyridine has been successfully utilized to extract a wide variety of endohedral rare-earth fullerenes of the type Ln@C-2n (Ln = La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb). Ln@C-80, Ln@C-82, and Ln(2)@C-80 for most of the rare-earth metals can be produced with high-yield and selectively extracted from the carbon-are evaporation soot. Metallofullerenes containing Sm, Eu, and Yb (which could have +2 oxidation states) are especially difficult to extract. Some possible reasons for the high-yield extraction are discussed. The laser desorption mass spectrometric characterization results indicate a relationship between the extraction yields of metallofullerenes and the oxidation states and ionic radii of the rare-earths.

Mass spectral study of extractable La- and Lu-containing fullerenes

Mass spectra of LaxC2n (x = 1,2), well known endohedral metallofullerenes, and Lu2C2n (2n = 76-112), new members of extractable metallofullerenes, were studied. Positive-ion laser desorption/ionization (LDI) and electron impact (EI) mass spectra indicated that lutetium is a special lanthanide that prefers to form dilutetium fullerenes by the are-burning method. However, the signals for Lu2C2n become very weak in negative-ion LDI-MS, this is different from La-2@C-80, which has close relative abundances in positive- and negative-ion MS. The distinction between Lu2C2n and La-2@C-80 in the negative-ion LDI mass spectra may be due to the different structures of La- and Lu-containing fullerenes. (C) 1997 by John Wiley & Sons, Ltd.

Effect of F- axial coordination on the electrochemistry of (TPP)Co

The axial coordination effect of F- on the redox behavior of (TPP)Co was investigated and spectroeletrochemistry in dichloroethane. It was verified that mono(F-) axial adduct (TPP)Co(II)(F-) could be reduced at 0.1 V(SCE). and bis(F-) axis adduct (TPP)Co(II)(F-)(2) formed with added F- molar ratio>1 could be reduced at the potential <-0.6 V(SCE). The equilibrium between (TPP)Co(II)(F-) and (TPP)Co(II)(F-)(2) was demonstrated.

High-yield synthesis and extraction of endohedral metallofullerenes Dy@C-2n

The successful encapsulation of dysprosium(Dy) into fullerene cages by activating the Dy2O3 containing graphite rods in situ, ''back-burning'' carbon-arc evaporation with a high-yield of pyridine extraction technique is reported.

Gas-phase ion-molecule reactions of C-60 and theoretical studies of [C60C2H3O](+) adduct cations

Gas-phase ion-molecule reactions of buckminsterfullerene (C-60) with the acetyl cation CH3-C-+=O (m/z 43) and formylmethyl cation (CH2)-C-+-CH=O (m/z 43, or oxiranyl cation), generated from the self-chemical ionization of acetone and vinyl acetate, respectively, were studied in the ion source of a mass spectrometer. Adduct cations [C60C2H3O](+) (m/z 763) and protonated C-60, [C60H](+) (m/z 721), were observed as the major products. AM1 semiempirical molecular orbital calculations on the possible structures, stabilities and charge locations of the isomers of the adducts [C60C2H3O](+) were carried out at the restricted Hartree-Fock level. The results indicated that the sigma-addition product [C-60-COCH3](+) is the most stable adduct for the reaction of C-60 with CH3-C-+=O rather than that resulting from the [2+2] cycloaddition. The [2+3] cycloadduct and the sigma-adduct [C60CH2CHO](+) might be the most possible coexisting products for the reactions of C-60 with (CH2)-C-+-CH=O or oxiranyl cation. Other [C60C2H3O](+) isomers are also discussed. (C) 1997 by John Wiley & Sons, Ltd.

High-temperature, high-pressure extraction of metallofullerenes Gd@C-2n

A high-temperature, high-pressure extraction technique with toluene and pyridine were employed for the extraction of metallofullerenes Gd@C-2n, A series of Gd@C-2n for 2n from 70 to 96 were effectively extracted by toluene. Gd@C-74 was shown to be a new stable soluble metallofullerene species. Pyridine was found to be more useful for the extraction of Gd@C-82 and Gd-2@C-80 from empty fullerenes and other metallofullerene species.

Formation and special solubility of endohedral thulium metallofullerenes

Endohedral metallofullerenes Tm@C-2n were synthesized with the carbon-arc discharge method of activating the Tm2O3-containing graphite anode in situ and back-burning technique, Toluene soxhlet extraction, toluene and pyridine high-temperature and high-pressure extraction technique were employed for the effective extraction of Tm@C-2n. The formation of Tm@C-2n was confirmed by LD-TOF and DEIMS characterization. The mass spectrometric results indicate that Tm@C-2n have a better solubility in toluene and worse solubility in pyridine than other metallofullerenes.

Instrumented impact testing of phenolphthalein polyether ketone

The Charpy impact fracture behaviour of unnotched specimens of phenolphthalein polyether ketone (PEK-C) was studied over a temperature range from room temperature to 220 degrees C by using an instrumented impact tester. The load-time and energy-time curves of PEK-C at different temperatures were recorded. From these curves, some important parameters, such as the maximum impact load, the maximum stress, the total impact energy, the crack initiation energy, the crack propagation energy etc., were obtained and their temperature dependences of PEK-C were investigated. The point of 100 percent maximum load on the load-time trace was shown to be the yield point. Two parameters, the ductile ratio (D.R.) and the ductility index (D.I.) were applied to characterize the ductility of PEK-C and their relationships to the relaxation processes were discussed.

Synthesis and characterization of novel polyimides from alicyclic dianhydride

New alicyclic Polyimides (PIs) were prepared from asymmetric alicyclic dianhydride, 5-(2,5-dioxotetrahydrofuryl)-3-methyl-cyclohexane-1,2-dicarboxylic anhydride (DOCDA) and the corresponding aromatic diamines such as p-phenylenediamine, m-phenylenediamine and oxydianiline etc. by the polycondensation in N-methyl-2-pyrrolidone (NMP) followed by chemical imidization as well as one step polyimidization in m-cresol in the presence of isoquinoline as a catalyst. The resulting PIs with glass transition temperatures ranging from 220 to 328 degrees C had the inherent viscosities within the range of 0.25 similar to 1.42 dL/g. These polymers were readily soluble in aprotic polar solvents such as NMP, dimethylacetamide (DMAc), dimethylesulfoxide (DMSO), etc. Furthermore, some of the polymers showed good solubility properties to common organic solvents like tetrahydrofurane and chlorform. Also, all of these polyimide films were tough, almost colourless, and transparent.

Two-step-method extraction of endohedral metallofullerenes

A new and efficient extraction method of endohedral metallofullerenes, especially of rare-earth elements encapsulated metallofullerenes, has been reported in this paper. Soxhlet-extraction of raw soot with toluene was used in the first step to wash away most accompanying C-60, C-70. Then pyridine was chosen as solvent to obtain high-temperature and high pressure extract. Two kinds of extract were analysed by DEI-MS and LDI-MS, the results indicate that this two-step method can provide the extract which has the highest fraction of endohedral metallofullerenes. So it will greatly simplify the following separation and purification processes of metallofullerenes.

Synthesis and extraction of lanthanofullerenes and its DEIMS, ESR characterizations

The synthesis for lanthanofullerenes was studied by activating the La2O3 containing graphite rod in situ and back-burning the carbide-rich cathode deposite, La@C-2n are efficiently extracted in high temperature toluene, among them, La@C-74 as a new species is added into the soluble lanthanofullerenes, The toluene extraction is first characterized by desorption electron impact (DEI) mass spectrometry, The ESR spectrum of the extraction at room temperature is also discussed.

Influence of the fold surface of the lamellae on radiation effects - Research on irradiated polyamide-1010 containing heterogeneous nuclei

Irradiated polyamide-1010 (PA1010) and PA1010 containing 0.5% (wt) heterogeneous nuclei were studied by ESR, WAXD, DSC and the determination of gel fractions. The fold surface of the lamellae plays an important role in the effects of radiation on crystalline PA1010. The results show that the direct radiation effects on both samples vary, while after being heated to 220 degrees C, the final radiation effects are identical, regardless of the difference in the amount of the fold surface of the lamellae. The post-radiation effects result predominantly from the fold surface.

High-yield Synthesis and Extraction of Gd@C-2n

Endohedral metallofullerene Gd@C-2n were synthesized with high-yield using the carbon-arc discharge method of activating the Gd2O3-containing graphite anode in situ and back-burning technique. A series of Gd@C-2n for 2n from 70 to 96 were effectively extracted by toluene at high-temperature and under high-pressure condition. Gd@C-82, Gd@C-74 were considered to be fairly stable and soluble metallofullerene species.