Determination of trace-level haloacetic acids in drinking water by ion chromatography-inductively coupled plasma mass spectrometry

A new method for the determination of nine haloacetic acids (HAAs) with ion chromatography (IC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) was developed. With the very hydrophilic anion-exchange column and steep gradient of sodium hydroxide, the nine HAAs could be well separated in 15 min. After suppression with an ASRS suppressor that was introduced in between IC and ICP-MS, the background was much decreased, the interference caused by sodium ion present in eluent was removed, and the sensitivities of HAAs were greatly improved. The chlorinated and brominated HAAs could be detected as 35ClO and 79Br without interference of the matrix due to the elemental selective ICP-MS. The detection limits for mono-, di-, trichloroacetic acids were between 15.6 and 23.6 microg/l. For the other six bromine-containing HAAs, the detection limits were between 0.34 and 0.99 microg/l. With the pretreatment of OnGuard Ag cartridge to remove high concentration of chloride in sample, the developed method could be applied to the determination of HAAs in many drinking water matrices.     

From D-glucose to biologically potent L-hexose derivatives: synthesis of alpha-L-iduronidase fluorogenic detector and the disaccharide moieties of bleomycin A2 and heparan sulfate

A novel and convenient route for the synthesis of biologically potent and rare L-hexose derivatives from D-glucose is described. Conversion of diacetone-alpha-D-glucose (14) into 1,2:3,5-di-O-isopropylidene-beta-L-idofuranose (19) was efficiently carried out in two steps. Orthogonal isopropylidene rearrangement of compound 19 led to 1,2:5,6-di-O-isopropylidene-beta-L-idofuranose (27), which underwent regioselective epimerization at the C3 position to give the L-talo- and 3-functionalized L-idofuranosyl derivatives. Hydrolysis of compound 19 under acidic conditions furnished 1,6-anhydro-beta-L-idopyranose (35) in excellent yield, which was successfully transformed into the corresponding L-allo, L-altro, L-gulo, and L-ido derivatives via regioselective benzylation, benzoylation, triflation and nucleophilic substitution as the key steps. Applications of these 1,6-anhydro-beta-L-hexopyranoses as valuable building blocks to the syntheses of 4-methylcoumarin-7-yl-alpha-L-iduronic acid and the disaccharide moieties of bleomycin A(2) as well as heparan sulfate are highlighted.     

Micellar effects on the electrochemistry of dopamine and its selective detection in the presence of ascorbic acid

The electrochemistry of dopamine (3-hydroxytyramine) was studied by cyclic voltammetry at a glassy carbon electrode in the presence of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) micelles at different pH. The anodic peak potential (E(pa)) and peak current (I(pa)) were found to be remarkably dependent on the charge and the concentration of the surfactant. The E(pa) and I(pa) change abruptly around the critical micellar concentration (CMC) of the surfactants and reach a plateau above the CMC. The E(pa) at the plateau shifts to more positive values in the cationic CTAB micellar solution, e.g. from 180 mV vs SCE in aqueous solution at pH 6.8 to 410 mV in CTAB micelle, whilst it shifts to less positive values in the anionic SDS micellar solution, e.g. 150 mV at pH 6.8. Therefore, the overlapped anodic peaks of dopamine and ascorbic acid in the mixture of the two compounds in aqueous solutions can be separated in CTAB micelles since the micelle shifts the E(pa) of ascorbic acid to less positive values. The two peaks are separated by ca. 400 mV at pH 6.8 in CTAB micelle, hence dopamine can be determined in the presence of 100 times excess of ascorbic acid. In SDS micelle and in the presence of ascorbic acid, the I(pa) of dopamine is greatly enhanced due to the catalytic oxidation of the latter that enables quantitative determination of both compounds.     

通过密度函数理论表征炭质吸附剂的孔径分布

通过密度函数理论（DFT-DensityFunctionalTheory）对炭质吸附剂的孔径分布进行了表征。该法以多孔固体上N2吸附分子模型为依据，用一种方法对多孔固体的孔径分布从微孔到大孔范围进行确定。本文用该法对自制的聚丙烯腈活性炭纤维、国产煤质活性炭及日本产活性炭微球等六种炭质吸附剂的孔径分布进行了表征。     

Detection of 8-hydroxy-2'-deoxyguanosine in deoxyribonucleic acid by the 32P-postlabeling method.

Using synthesized 8-hydroxy-2'-deoxyguanosine 3'-monophosphate as a marker, the 32P-postlabeling method was adapted with minimum modifications for the analysis of 8-hydroxy-2'-deoxyguanosine (8-OH-dG) content in deoxyribonucleic acid (DNA). This method allows the analysis of one 8-OH-dG per 10(4) DNA nucleotides with only 10 pmoles of nucleotides required. The amounts of 8-OH-dG in DNA detected by the postlabeling method correlated well with the electrochemical detection method but were consistently lower.     

A new route to semirigid poly(amide-ester)s with ordered structure

Four novel semirigid poly(amide-ester)s having the same ordered amide-amide-ester-ester (-AAEE-) and the same or the different phenyl structure were synthesized from the various combination of active acylamide of benzotriazole (HBT) such as 1,1′-(isophthaloyl)bisbenzotriazole (IPBBT) and 1,1′-(terephthaloyl)bisbenzotriazole (PBBT) with diols such as N,N'-bis(2-hydroxyethyl)isophthamide (HEIPA) and N,N'-bis(2-hydroxyethyl)terephthamide (HEPTA) which prepared from the selective N-acylation of IPBBT or PBBT with aminoethanol in excellent yield at room temperature. Before the preparation of diol monomers, a model reaction of selective N-acylation was also completed from active monoacylamide of benzotriazole, 1-benzoylbenzotriazole with aminoethanol. The ordered structure of poly(amideester)s were characterized by infrared (IR) and NMR spectra. On the bases of different reactivity between selective N-acylation and O-acylation of active acylamide of benzotriazole, poly(amide-ester)s having the ordered AAEE and the same phenyl structure were also readily synthesized from the IPBBT or PBBT with aminoethanol under mild conditions by one-bath process.     

A theoretical study of electronic excited states of photosynthetic reaction center in Rhodopseudomonas viridis

The electronic singlet vertical excited states of photosynthetic reaction center (PSRC) in Rhodopseudomonas (Rps.) viridis were investigated by ZINDO and INDO/S methods. The effects of the interactions of pigment-pigment and pigment-protein on the electronic excitations were examined. The calculation results showed that the interactions of pigment-pigment and pigment-protein play an important role in reasonably assigning the experimental absorption and circular dichroism (CD) spectra of PSRC in Rps. virids. By comparing the theoretically computed excited states with the experimental absorption and CD spectra, satisfactory assignments of the experimental spectroscopic peaks were achieved.     

31P and 1h NMR as probes of domain alignment in a rigid crystalline surfactant mesophase

A viscous reverse hexagonal surfactant mesophase containing bis(2-ethylhexyl) sodium sulfosuccinate (AOT) and alpha-phosphatidylcholine (lecithin), with comparable volume fractions of isooctane and water, was characterized by Fourier transform (31)P and (1)H NMR spectroscopy. Shear alignment was reflected through both (31)P NMR and (1)H NMR spectra. A complicated (31)P spectrum was observed as a result of superposition of chemical shifts according to the distribution of crystalline domains prior to shear. The initially disordered samples with polydomain structures become macroscopically aligned after Couette shear. (31)P NMR chemical shift anisotropy characteristics are used to elucidate orientation of the hexagonal phase. Interestingly, (1)H NMR spectra exhibit spectral changes upon shear alignment closely corresponding with that of (31)P NMR spectra. These observations complement the findings of mesophase alignment obtained using SANS and imply that (31)P and (1)H NMR spectroscopy can be used as probes to define microstructure and monitor orientation changes in this binary surfactant system. This is especially beneficial if these mesophases are used as templates for materials synthesis.     

MH—Ni电池封口化成及其性能

在硼氢化钾碱性溶液中对金属氢化物（ＭＨ）电极的表面进行化学还原处理，提高了ＭＨ电极的放电容量、活化性能和电催化活性．用其为负极组装的ＡＡ型ＭＨ－Ｎｉ电池进行了封口化成，电池放电容量达到１１５０ｍＡｈ，５Ｃ下电池的放电容量达到０．２Ｃ下容量的８０％以上，电池在１Ｃ１００％ＤＯＤ（放电深度）充放电条件下，循环寿命由原来的１００次左右提高到２００次以上     

高富勒烯的提取,分离和分析

采用二硫化碳重结晶富勒烯混合物或二硫化碳二次抽提烟灰以提取高富勒烯（ｈｉｇｈｅｒｆｕｌｅｒｅｎｅｓ，Ｃｎ，ｎ＞７０）。产物经高效液相色谱分析，高富勒烯的含量从１％分别提高到４％和６％；经激光飞行时间质谱证明，产物中除含主要成分Ｃ６０和Ｃ７０以外，还含有Ｃ７６、Ｃ７８、Ｃ８２、Ｃ８４以及更高碳原子的富勒烯。