WATER-SOLUBLE FULLERENE DERIVATIVES, SYNTHESIS AND CHARACTERIZA

ＷＡＴＥＲ－ＳＯＬＵＢＬＥ　ＦＵＬＬＥＲＥＮＥ　ＤＥＲＩＶＡＴＩＶＥＳ，ＳＹＮＴＨＥＳＩＳ　ＡＮＤ　ＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮ　ＯＦ　β－ＡＬＡＮＩＮＥ　Ｃ＿（６０）　ＡＤＤＵＣＴＳＷＡＴＥＲ－ＳＯＬＵＢＬＥＦＵＬＬＥＲＥＮＥＤＥＲＩＶＡＴＩＶ...     

STUDIES ON THE SYNTHESIS OF SINULARIOL－D， SINULARIOL－A AND SINULARIC ACID－A．－SYNTHESIS OF （5R）－7，7－DIMETHOXY－5－［1－（2－TERT－BUTYLDIPHENYLSILOXYMETHYL）VINYL］－2－HEPTANONE

ＳＴＵＤＩＥＳＯＮＴＨＥＳＹＮＴＨＥＳＩＳＯＦＳＩＮＵＬＡＲＩＯＬ－Ｄ，ＳＩＮＵＬＡＲＩＯＬ－ＡＡＮＤＳＩＮＵＬＡＲＩＣＡＣＩＤ－Ａ．－ＳＹＮＴＨＥＳＩＳＯＦ（５Ｒ）－７，７－ＤＩＭＥＴＨＯＸＹ－５－［１－（２－ＴＥＲＴ－ＢＵＴＹＬＤＩＰＨＥＮＹＬＳ...     

THE NON－TEMPLATE SYNTHESIS OF MACROCYCLIC SCHIFF BASE DERIVED FROM THIOPHENE，AND ITS Ag（Ⅰ），Hg（Ⅱ） COMPLEXES

ＴＨＥ　ＮＯＮ－ＴＥＭＰＬＡＴＥ　ＳＹＮＴＨＥＳＩＳ　ＯＦ　ＭＡＣＲＯＣＹＣＬＩＣ　ＳＣＨＩＦＦ　ＢＡＳＥ　ＤＥＲＩＶＥＤ　ＦＲＯＭ　ＴＨＩＯＰＨＥＮＥ，ＡＮＤ　ＩＴＳ　Ａｇ（Ⅰ），Ｈｇ（Ⅱ）　ＣＯＭＰＬＥＸＥＳＴＨＥＮＯＮ－ＴＥＭＰＬＡＴＥＳＹＮＴ...     

MICELLE-SENSITIZED DERIVATIVE VARIASLE-ANGLE SYNCHRONOUS FLUORESCENCE FOR SIMULTANGOUS DETERMINATION OF 2,2 DIHYDROXYBEPHENYL AND 4-HYDROXYBIPHENYL

ＭＩＣＥＬＬＥ－ＳＥＮＳＩＴＩＺＥＤ　ＤＥＲＩＶＡＴＩＶＥ　ＶＡＲＩＡＳＬＥ－ＡＮＧＬＥ　ＳＹＮＣＨＲＯＮＯＵＳ　ＦＬＵＯＲＥＳＣＥＮＣＥ　ＦＯＲ　ＳＩＭＵＬＴＡＮＧＯＵＳ　ＤＥＴＥＲＭＩＮＡＴＩＯＮ　ＯＦ　２，２　ＤＩＨＹＤＲＯＸＹＢＥＰＨＥＮＹＬ...     

PARAMAGNETIC AND DIAMAGNETIC DICOPPER（Ⅱ） COMPLEXES WITH DI－SCHIFF BASE DERIVED FROM 2－HYDROXY－1－NAPHTHALDEHYDE AND1，3－DIANINO－2－PROPANOL

ＰＡＲＡＭＡＧＮＥＴＩＣＡＮＤＤＩＡＭＡＧＮＥＴＩＣＤＩＣＯＰＰＥＲ（Ⅱ）ＣＯＭＰＬＥＸＥＳＷＩＴＨＤＩ－ＳＣＨＩＦＦＢＡＳＥＤＥＲＩＶＥＤＦＲＯＭ２－ＨＹＤＲＯＸＹ－１－ＮＡＰＨＴＨＡＬＤＥＨＹＤＥＡＮＤ１，３－ＤＩＡＮＩＮＯ－２－ＰＲＯＰＡＮＯＬ...     

ZEOLITE－CATALYZED FRIEDEL－CRAFTS ACYLATION OF AROMATICS∶Ⅲ．SYNTHESIS OF 4－ACYL ANISOLE WITH USY CATALYST

ＺＥＯＬＩＴＥ－ＣＡＴＡＬＹＺＥＤＦＲＩＥＤＥＬ－ＣＲＡＦＴＳＡＣＹＬＡＴＩＯＮＯＦＡＲＯＭＡＴＩＣＳ：Ⅲ．ＳＹＮＴＨＥＳＩＳＯＦ４－ＡＣＹＬＡＮＩＳＯＬＥＷＩＴＨＵＳＹＣＡＴＡＬＹＳＴ￥ＹｕＤａｏＭＡ；ＱｉＬｏｎｇＷＡＮＧ；ＸｉｎｇＤｏｎｇＪＩ；Ｃ...     

ZEOLITE－CATALYZED FRIEDEL－CRAFTS ACYLATION OF AROMATICS：I》．SYNTHESIS OF 4－ACYL ANISOLE WITH A HY CATALYST

ＺＥＯＬＩＴＥ－ＣＡＴＡＬＹＺＥＤＦＲＩＥＤＥＬ－ＣＲＡＦＴＳＡＣＹＬＡＴＩＯＮＯＦＡＲＯＭＡＴＩＣＳ：Ｉ．ＳＹＮＴＨＥＳＩＳＯＦ４－ＡＣＹＬＡＮＩＳＯＬＥＷＩＴＨＡＨＹＣＡＴＡＬＹＳＴ￥ＱｉＬｏｎｇＷＡＮＧ；ＹｕＤａｏＭＡ；ＸｉｎｇＤｏｎｇＪＩ；Ｈ...     

PREPARATION OF DI－GRIGNARD REAGENTS MEDIATED BY THE TRANSITION METAL CHLORIDES

ＰＲＥＰＡＲＡＴＩＯＮＯＦＤＩ－ＧＲＩＧＮＡＲＤＲＥＡＧＥＮＴＳＭＥＤＩＡＴＥＤＢＹＴＨＥＴＲＡＮＳＩＴＩＯＮＭＥＴＡＬＣＨＬＯＲＩＤＥＳＰＲＥＰＡＲＡＴＩＯＮＯＦＤＩ－ＧＲＩＧＮＡＲＤＲＥＡＧＥＮＴＳＭＥＤＩＡＴＥＤＢＹＴＨＥＴＲＡＮＳＩＴＩＯＮＭ...     

以混合模板剂合成TS—1分子筛及其性能研究

以四丁基溴化铵（ＴＢＡＢｒ）＋四乙基氢氧化铵（ＴＥＡＯＨ，ｎ（ＴＢＡ＾＋）／ｎ（ＴＥＡ＾＋）＝１）或以四丙基溴化铵（ＴＰＡＢｒ）＋ＴＥＡＯＨ为模板剂，钛酸四丁酯和正硅酸乙酯为原料，于１７０℃水热合成出ＴＳ－１分子筛。对合成的ＴＳ－１样品进行了ＸＲＤ，ＦＴ－ＩＲ，ＳＥＭ和ＢＥＴ比表面积分析，证实了样品中钛已进入Ｓｉｌｉｃａｌｉｔｅ－１骨架。选择戊烷氧化为探针反应，考察了ＴＳ－１的催化活性。结果表明以     

SYNTHESIS OF 5－SUBSTITUTED－2－CHLORO－6－METHYL－4， 7－DIOXOBENZOTHIAZOLE DERIVATIVES

ＳＹＮＴＨＥＳＩＳ ＯＦ ５－ＳＵＢＳＴＩＴＵＴＥＤ－２－ＣＨＬＯＲＯ－６－ＭＥＴＨＹＬ－４， ７－ＤＩＯＸＯＢＥＮＺＯＴＨＩＡＺＯＬＥ ＤＥＲＩＶＡＴＩＶＥＳ￥ＣｕｉＨｕａＬＩＵ；ＢｉｎＬＵ；ＪｉｎｇＬｉｎｇＺＨＡＮＧ（Ｉｎｓｔｉｔｕｔｅｏｆｏｒｇ...     

Ultrasensitive determination of gold in geogas by laser excited atomic fluorescence spectrometry

Ultratrace gold (Au) in geogas samples has been determined by means of laser excited atomic fluorescence spectrometry combined with graphite electrothermal atomization and time-gate technique. Gold atoms were excited from the ground state to the 6p²P_3/2 state by a pulsed laser beam with a wavelength of 242.8 nm. Fluorescence photons with a wavelength of 312.3 nm were measured by a photon-counting unit. The time-gate technique was used to reduce the background radiation caused by the furnace. This method has proved to be highly sensitive with minimal background interference. Eighty-two geogas samples were analysed and the Au contents obtained were in the range of 0.002–0.182 ng l⁻¹. The study of Au concentration of geogas in soil is of great interest in prospecting gold deposits.     

Determination of Ultratrace Metal Elements in Natural Samples by Laser-induced Fluorescence with Time-gate Technique

The determination of ultratrace metal elements is of great important in geochemistry, chemical exploration and many other fields. The laser-induced fluorescence (LIF) with time-gate technique is an extremely efficient method for the determination of ultratrace concentrations of elements. This paper reports on the high sensitive detection researches in our laboratory, included lead in Antarctic ice-snow samples, gold in geogas, gold and palladium in seabed sediment samples, gallium and indium in rock and sediment samples, based on laser-induced fluorescence combined with graphite electrothermal atomization and time-gate technique.     

全反射X射线荧光光谱法同时测定地气样品中锰、镍、铜、锌、铅、铷和锶

论述了利用自行研制的有３个反射体的全反射分析装置，用钼靶Ｘ光管激发，以Ｓｅ为内标，同时测定了地气样品中Ｍｎ、Ｎｉ、Ｃｕ、Ｚｎ、Ｐｂ、Ｒｂ和Ｓｒ等元素。对纳克级元素含量，方法的精密度为７．２％．绝对检出限为１０－１０～１０－１１。其分析结果的准确度与无火焰原子吸收相符。     

Separation of gold on a selective chelating ion exchanger and in situ determination by gamma-spectroscopy

For the separation and determination of low gold concentrations in the sub g g^–1 range in ore and sediment samples an analytical technique has been developed, based on the selective adsorption of gold on the chelating resin, Srafion NMRR, and the in situ determination of the retained gold by instrumental neutron activation analysis (INAA), using the 411.8 keV line of the isotope¹⁹⁸Au. In the case of higher gold concentrations Au could be directly determined in the ore by the technique of loss-free counting in spite of the high radioactivity of the investigated samples. By the described procedure it was possible to determine Au amounts in the range of ng g^–1 sediments.     

Determination and distribution of gold in Greek bauxites of the Parnassos-Ghiona area by gamma-spectroscopy after ion exchange separation

For the determination of gold in Greek bauxites from the Parnassos-Ghiona area, an analytical technique was used based on the selective adsorption of gold on SRAFION NMRR chelating anion exchanger resin, after leaching the bauxites with aqua regia in a teflon-autoclave at 120 °C, and the determination of the retained gold directly on the resin by instrumental neutron activation analysis (INAA), using the 411.8 keV line of the ¹⁹⁸Au isotope. The procedure allowed to determine Au in concentrations down to ng/g. The obtained data were used to examine the distribution of Au in the profiles of a group of different bauxites from the upper or the called third bauxitic horizon of the Parnassos-Ghiona area in Greece. Especially in the basement of some bauxite deposits unexpected high concentrations of Au up to 2 mg/g have been found. Furthermore, the correlation of Au with other trace elements, found in the bauxitic samples, was investigated.     

Determination of tin in environmental samples by graphite furnace atomic absorption and inductively coupled plasma-mass spectrometry

Summary Methods for the determination of total Sn in environmental samples (waters, animal tissue, plant material, sediments and coal fly ash), by graphite furnace atomic absorption spectrometry (GFAAS) and inductively coupled plasma mass spectrometry (ICP-MS) have been developed and evaluated.Noble metals (Ag, Au, Pd, Pt, Rh) under reducing conditions were studied as matrix modifiers for the determination of Sn by GFAAS. The maximum ashing temperature (1400°C), highest sensitivity and the best absolute detection limit (4 pg) were achieved when Pd was used in the presence of hydroxylamine hydrochloride. The achievable sensitivity depended strongly on the chemical composition of the matrix.Both GFAAS and ICP-MS appeared to be equally sensitive techniques for the direct determination of Sn in waters, though ICP-MS was a more convenient and sensitive technique for the determination of Sn in digested biological and geological materials.

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Bestimmung von Zinn in Umweltproben durch Graphitrohr-AAS und ICP-MS

     

Pt and Au analysis by delayed X-ray spectrometry after fast neutron activation

A novel technique for the determination of Pt and Au at low concentrations is described. The method involves /K/ X-ray spectrometry preceded by fast neutron activation of the stable isotopes of the elements of interest. A full appraisal of the technique is presented for the analysis of small powdered samples. The sensitivity was optimized by employing a detector that was particularly effective at energies below 150 keV. The investigation formed the basis of a feasibility study which was utilized to establish if the application could be developed for the routine off-line determination of Pt and Au. We show that the method does not necessarily depend on the sample matrix, and that it proves to be a strong rival to conventional activation analysis.     

Determination of iodine in diverse botanical and dietary matrices by pre-irradiation combustion followed by neutron activation analysis

Summary The method chosen for determination of iodine in this investigation is an extension of an existing analytical technique to food samples which was developed for environmental samples. The method is based on pre-irradiation combustion of the sample to liberate iodine, trapping the iodine on charcoal, and quantitating the element by neutron activation analysis (NAA). Existing botanical and dietary reference materials were used to check the validity of the method. Several mixed diet samples with high fat content from the U.S. Total Diet Study and composites of cereals with both low and high iodine content were analyzed. This method of pre-irradiation combustion followed by NAA has been shown to be a viable technique for the determination of iodine in dietary samples. However, with a detection limit of about 50 ng of iodine, large amounts of sample (>1 g) are typically required for each determination.     

电感耦合等离子体质谱法测定地质样品中铂、钯、钌、铑、铱和金

研究Ｔｅ共沉淀分离富集、ＩＣＰ－ＭＳ铂族元素和金测定方法。方法检出限 １～９ ｐｇ／ｇ;回收率≥９０％。国标ＧＢＷ０７２８８－ＧＢＷ０７２９４、加拿大ＷＧＢ１及南非铂矿ＳＡＲＭ７等标样分析表明：结果满意,方法可靠。     

Sugar determination via the homogeneous reduction of Au salts: A novel optical measurement

A novel optical assay for sugar determination based on the catalytic and biocatalytic growth of gold nanoparticles (AuNPs) is presented. The reaction of carbohydrates with these Au salts in alkaline media generates AuNPs at room temperature (RT) without the need for Au seeds in the solution or fibrous mesh. The optical properties of the resulting AuNPs relates to the total reducing sugar content of the samples analyzed. The development of such inexpensive optical assay was evaluated qualitatively and quantitatively on food beverages and honey samples. Its application can be of help to control the glucose content of the diet or easily extended in a host of industrial, biomedical and clinical fields.