The reaction of cis-2, 3-dimethylthiirane with hydrogen atom was investigated with a conventional discharge flow system at the pressure of 530 and 2130 Pa at 293 K. The main products were trans- and cis-2-butene. The trans/cis ratio was found to be independent of conversion, pressure and diluent gas. It was concluded that ( 1 ) the reaction proceeds via a stepwise (not simultaneous) fission of two C-S bonds and ( 2 ) the trans/cis ratio is controlled by a competition between the unimolecular decomposition and the rotation around the C-C bond of energized 2-mercapto-1-methylpropyl radical. The latter conclusion is supported quantitatively by the RRKM calculation.

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In order to study a NO-NH₃ reaction over a Cu-Al₂O₈ catalyst prepared by 112 reduction of Cu-Al₂O₃, the experiments were carried out by IR technique, adsorption measurements, an d kinetic studies. The results were compared with those of the preceeding paper on CuO-Al₂O₃catalyst.
It was found from IR measurements that NO adsorbed as N0^δ-- over Cu-Al₂O₃, and the adsorbed state of NH₃ over the catalyst was different from the case of CuO-Al₂O₃.The adsorption band of 1445cm^-1 observed during the reaction was ascribed to the intermediate proposed by Shelef et al. The reaction mechanism was proposed from the results of the kinetic studies. The rate of N₂ formation in NO-NH₃ reaction was controlled by the dissociative adsorption of NH₃ on Cu surface. On the other hand, N₂O was derived from the decomposition of NO occured at the same time in the reaction. Except for the rate determining step and N₂Oformation based on the decomposition of NO, this mechanism supports the conclusion of Shelef et al. which was obtained from the products distribution using ¹⁵N isotope in the same reaction system.

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The physical davelopment is a process which utilizes metallic deposition on latent image composed of tiny metallic nuclei. This process provides a powerful means of image amplification, but physical developers are, in general, chemically unstable and can not be stored long after preparation, because a metallic ion and a reducing agent are disolved together in it. This problem may be solved by activating the developer only for neccessary period by external energy such as heat, electricity, light, etc. We proposed a photoactivation type physical developer, which consisted of p-benzoquinone and silver nitrate in methanol-water solution. The developer was activated by UV light which convert p-benzoquinone into hydroquinone.
Fundamental parameters of the development such as the light intensity, th e cell thickness and the temperature were investigated. The light intensity affected the developing rate directly because the steady state concentration of hydroquinone was determined by the light intensity. But at the same time, the rate of homogeneous nucleation in the solution increased, too and the efficiency of silver utilization for image formation could not be improved by changing the light intensity. The cell thickness, or the depth of light absorption affected the developing rate, especially the induction period, to considerable extents. The concentra. tion of hydroquinone within the working region extended to a certain range from the latent image surface was found to be very important. Therefore, the developing rate dramatically increased by decreasing the cell thickness, under the conditions of constant total light absorption. The induction period was much shortened by increasing the temperature of the developer. Images with high contrast (transmission density, 4) were obtained under the following conditions; developing time 8 min, temperature 50°C, thickness of developer O.08 cm, concentration of p-benzoquinone 0.47 mol/l, concentration of silver nitrate 0.5 mol/l, light intensity 34 mW/cm².

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The reactions between TiP₂O₇ and CaCO₃ have been studied for the mixtures containing 10to 90 mol% CaCO₃. The mixtures were heated in air for 60 h at 900°C. Some of them were heated at 10°⋅Cmin^-1 to temperatures between 600 and 1400°C. The reaction products were quenched and subjected to X-ray diffractometry (CuK _αradiation).
The compounds formed by the reaction were CaTi₄( PO₄)₆, β-Ca₂P₂O₇, TiO₂ (Anatase and Rutile), 5TiO₂⋅2 P₂O₅, α- and β-Ca₃(PO₄)₂, C aTiO₃ and CaTiO(PO₄)₆(OH)_2-2xOx ( Figs.3 and 4). The double phosphate CaTi₄(PO₄)₆ was formed when the mixtures contained 10 to 60mol% CaCO₃. The double phosphate was isomorphous with MiTi₂(PO₄)₃ (Mr= Li, Na, K or Rb) (Table 1). Its lattice parameter (Hexagonal, a=8.3632±0.0002Å, c=22.0131±0.0007Å Z=3) was calculated. The formation of Ca. (PO₄)₆(OH)_2-2xOx was confirmed by the i nfrared spectrum (Fig.1). When a diffusion couple of CaCO₃ and TiP₂O₇ pellets was heated at 900°C, the reaction layer of CaCO₃ pellet consisted of Ca₃(PO₄)₂ and CaO while that of TiP₂O₇consisted of CaTi₄(PO₄)₆, 5TiO₂⋅2 P₂O₅ and TiP₂O₇ (Figs.5 and 6).

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The formation of fine TiO₂-Al₂O₃ powders by the vapor phase reaction of the TiCl₄-AlBr₃-O₂ system was studied at temperatures of 860 to 1400°C.
The phases produced were rutile-TiO₂, anatase-TiO₂, Al₂O₃, and β-Al2Ti05. The crystal type of TiO₂ became mainly rutile-form when the reaction temperature was above 1050°C and Al₂O₃ contents were above 10∼30 mol%. Although Al₂TiO₅ was formed when the reacti on temperature was above 1000°C and the Al₂O₃ contents were above ca.20 mol%, it was difficult to obtain it as single phase. In the reaction method where the TiCl₄-AlBr₃-N₂ gas mixture and O₂ gas were mixed at the low temperature zone of the reactor, the addition of AlBr₃ decreased the particle size of products from 0.1∼0.6 to 0.03∼0.3 μm and the crystallite sizes of TiO₂ from ca.0.17 to ca.0.03, μm. When the reactant gases were mixed at the center of high temperature zone, the products consisted of fine spherical particles with a narrow particlesizes distribution (0.02∼0.07μm). The formation of TiO₂-Al₂O₃ particles in the present reaction system was considered to occur by the preferential nucleation of Al₂O₃ and the growth through the codeposition of both TiO₂ and Al₂O₃ components. β-Al₂TiO₅ is formed as a metastable phase.

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The characteristics of the in-beam electron impact (IBEI) mass spectra of 20 5-dimethylamino1-naphthyl sulfonyl (dansyl) amino acids and 12 dansyl oligopeptides and their methyl esters (up to pentapeptide) compOsed of leucine and isoleucine are described. In the case of dansyl amino acids, the in-beam electron impact spectra measured under rapid heating of the samples over 200∼300°C gave abundant [M] ions as their molecular ions as compared with their conventional electron impact (DIEI) spectra. In the case of dansyl di- and tripeptide esters, the in-beam spectra also gave abundant [M] ions as their molecular ions as well as amino-acyl fragments. However dansyl peptides and dansyl pentapeptide ester exhibited abundant [M+1]⁺ ion peaks as their molecular ions and the spectral features were apparently a combination of those of the conventional electron impact spectrum and some peaks originating from the [M+1]⁺ions. As the peptide chains are lengthened, the fragment ion peaks corresponding to the conventional electron impact spectra of the cyclopeptide derivatives formed by thermal cyclization in the mass spectrometer were remarkably observed. The “sequencedetermining” peaks which are imoportant for the structural analysis were observed as the abundant and major peaks in all in-beam electron impact spectra of these dansyl oligopeptide derivatives. As the ionization mechanism by the in-beam electron impact, it was concluded that the [M+1]⁺ ions are derived from the ionization of associated molecules or molecular clusters upon electron impact in a vapour phase near the surface of the probe. In the measurment of the mass spectra of these substances, it was shown that the method by in-beam electron impact is more suitable than that by conventional electron impact.

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Four representative organic peroxidesdi-t-butyl peroxide, t-butyl perbenzoate, t-butyl 2-ethylperoxyhexanoate, and benzoyl peroxide were allowed to decompose adiabatically to investigate their thermal stabilities and the dangerous factors such as self-heat rate and pressure evolved were measured in addition to their kinetic data. Differential scanning calorimetry were also employed to compare the thermal data with those obtained by adiabatic accelerating rate calorimetry.
These organic peroxides began to evolve the heat at relatively lower temperature in the adiabatic system than in the DSC experiment. The decomposition proceeded exponentially with time to reach a violent explosion. Any autocatalytic reaction was scarcely indicated in these decompositions, and the self-heat rates were in good agreement with the calculated values, except in the region of the violent decomposition. The maximum self-heat rate and pressure for these ∼2g samples were 150∼440°C/min and 4.4∼9.4 MPa, respectively. On the other hand, little differences were found in the reaction kinetic data between the thermal analysis and the adiabatic method. The thermal analysis seem to be one of the effective method to evaluate the thermal hazard of unstable substances.

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The reaction of r-butyrolactone with N-(phenylthio)phthalimide in the presence of lithium diisopropylamide afforded a, α, α-bis(phenylthio)-γ-butyrolactone [2]in 81% yield. The oxidation of [2] followed by thermolysis gave 2-phenylsulfinyl-2-buten-4-olide [5] in a good yield. Further, Michael addition reaction of [5] with active methylene compounds and subseq. u, ent thermolysis gave 3-substituted 2-buten-4-olides. Similarly, the Michael addition reaction by the use of 2-phenylsulfinylated cyclopentenone and cyclohexenone, which were pregated from '2, 2 -bis(sulfenylated)derivatives, proceeded smoothly and subsequent pyrol ysis afforded 3-substituted 2-cyclopenten-1-one and 2-cyclohexen-1-one derivatives, respectively. -Thus; -a convenient method for the introduction of 'a substituent group to 3-position of 2-bu' teii-41-Olide and cyclic ienones was established.

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The acyl group in acylpolymethylbenzenes is transfered to arenes by the action of acids such as trifluoroacetic acid, trifluoromethanesulfonic acid, and aluminium chloride. Trifluoroacetic acid which does not induce the transfer of the methyl group is most excellent among the acids. The reaction of various acylpolymethylbenzenes with anisole in trifluoroacetic acid h as been examined. A typical reaction was carried out by heating a mixture of acetylpentamethylbenzene, anisole, and trifluoroacetic acid in a molar ratio of 1: 1: 50, respectively, under reflux to give p-acetylanisole and pentamethylbenzene. The reaction is considerd to proceed through two steps; the reaction of an acylpolymethylbenzene with trifluoroacetic acid gives a carboxylic trifluoroacetic anhydride and a polymethylbenzene, and then the reactive mixed acid anhydride reacts with an arene to give an acylarene and trifluoroacetic acid.

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Acylation reaction of aliphatic nitro compounds [1] with acetyl chloride in the presence of 1, 3 -disubstituted guanidines[2]afforded 3, 4-disubstituted 1, 2, 4 -oxadiazol-5(4H)-ones [3]in good yields. The reaction was carried out in N, N-dimethylacetamide (Method I ), or in benzene in the presence of 18-crown-6 as a catalyst (Method II). When nitroethane [1d]and 1, 3-diphenylguanidine [2a] were employed, 3, 4-diphenyl-1, 2, 4 -oxdiazol-5(4H)-imine [6e] and also 3, 4 -diphenyl-5-phenylimino-4, 5 -dihydro-1, 2, 4-oxadiazole [7e] were isolated from this reaction mixture. Thus the following reaction mechanism is proposed: Initially, the nitrile oxide [5]. icirmd as an intermediate in this acylation reacts with guanidine [2]to give and cycloadduct, oxadiazoline [9]and furthermore, [9]eliminates an amine or ammonia readily to give [6]or [7], respectively. Subsequent hydrolysis of [6] and [7] results in the corresponding oxadiazolone [3].
This one-pot reaction is more simple and useful than other methods for preparation of [3].

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Effects of diluents (steam, nitrogen, and helium) on the ethene pyrolysis rates in the temperature range 750∼890°C under atmospheric pressure have been studied. The pyrolysis was carried out by a flow method in a spherical quartz reactor of complete mixing type. Ethene was heated up by the sensible heat of heated diluents. The range of the residence time was 0.02∼0.65 s, and that of the partial pressure of ethene was 0.02∼0.8 atm. When dilu ted with steam, the reaction order was 1.3 with respect to ethene at the ethene partial pressure of 0.2 atm or higher, and 0.3 at the partial pressure of 0.02 atm. At the partial pressure lower than 0.02atm the reaction order decreased to zero (Fig.1). When diluted with nitrogen, the reaction order with respected to ethene was 1.3 in all the range of the partial pressure of ethene (Fig.2). The rates of ethene conversion in the presence of steam were high er than those in the presence of nitrogen at the low partial pressure of ethene (Figs.1 and 2). The rates in the presence of nitrogen and helium were almost equal.. -Temperature dependence of the over-all rate constants corrected to the ethene pressure of one atm was given as follows: k= 5.47×10¹⁰ exp[ (-58000±5000)/R(cal)T ] atm^-0.3⋅s^-1. The majorp roductsa t the low p arti4pressure of ethene in the presence of steam were acetylene and methane, whereas the product in the presence of nitrogen or helium was acetylene. The effects of steam, nitrogen, and helium were attributed to different states of the surface, quartz or carbon deposits,

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The oxidation of Goonyella (C 85.7% d. a. f. ), Amax (C 76.5% d. a. f. ), and Yallourn (C 64.1% d. a. f. ) coals was carried out in a hot aqueous alkaline nitrate solution to disclose th e optimum conditions of producing oxygenated compounds, the reduced form of the nitrate, possibility of nitration, and relation of the relative amount of benzenepolycarboxylic acids with reaction conditions. The oxidation to give oxalic acid and benzenepolycarboxylic acids was found to take place with a moderate rate at about 275°C for the lower ranked coals such as Amax and Yallourn coals. A similar reactivity could be found for the sample of higher ranked Goonyella coal when it was subjected to sufficient pre-oxidation with air at about 300°C. From Yallourn coal, maximal yield (40%) of oxalic acid could be reached by the oxidation at 275°C for 3 h with 30∼35 mol⋅kg^-1 (1200∼1400 g) NaOH/kg H₂O, 10 mol⋅kg^-1(850 g) NaNO₃/kg H₂O, and NaOH/coal wt. ratio of 4∼5. Maximal yields of oxalic acid and polycarboxylic acids from the similar oxidation of pre-oxidized Goonyella coal were about 40% and 20%, respectively. Nitro group was detected in the oxygenated products by the ir spectra. Relative amount of benzenepolycarboxylic acids in the oxidation products from both Goonyella and Amax coals was in the decreasing order: tri->tetra->penta->di-, whereas it was tetra->tri->penta-=di- from the lowest ranked Yallourn coal. Change in the reaction conditions including pre-oxidation of the sample did not alter the above sequences.

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The fractionation of dextran T-2000 (Pharmacia Fine Chemicals Co., Lot. No.8122) by gel filtration method was carried out using Sepharose gel CL-2 B (Pharmacia. Fine Chemicals Co. ). The experiments were repeated five times and the reproducibility of the fractionation was examined. The chromatogram of dextran T-2000 in gel filtration showed two peaks. The light scattering and viscosity measurements were carried out on each of the fractionated solutions. Then, the molecular weight, molecular size and intrinsic viscosity of the dextran fraction were directly determined. The order of molecular size of each fraction was always in agreement with elution order but the molecular weight was not always in agreement with elution order at the range of high molecular weight. It was thought to be due to the variety of the branching degree in dextran fraction.
The relationship between the weight average molecular weight, Mw, and the radius of gyration, R_G, obtained by the light scattering measurement of each fraction was R_G-M^0.5. Furthermore, the relationship between Mw and intrinsic viscosity, [η], was [η] Mw^3.37. The polydispersity parameter, Mw/Mn, calculated from the results of fractionation was 3.2for whole polymer T-2000.

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The polymerization of methyl methacrylate(MMA) by cobalt(II) complexes with polyamine was carried out in an aqueous solution containing a surfactant under a nitrogen atmosphere at 30°C. Polyamine used was ethylenediamine(en), diethylenetriamine(dien), triethylenetetramine(trien) or tetraethylenepentamine(tetren), Better yields of the polymer were achieved when the molar ratio of en or dien to cobalt was 2: 1 and that of trien or tetren was 1.: 1, respectively. The inhibition of the polymerization by addition of 2, 2-diphenyl-1-picrylhydrazyl suggested that the polymerization of MMA proceeded through a radical mechanism. It was considered that the polymerization was initiated with the donation of an electron from the complex to MMA.

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The rate of the reaction between Fe^II(edta) (NO) (2.6 mol/ms) and NaNa₂SO₃ (10 mol/m3) in aqueous solution was measured spectrophotometrically at temperatures ranging from 10 to 30°C and over the pH range of 5.74∼8.00. The Fe^II (edta) (NO) solution was prepared by introducing NO gas into a Fe^II (edta) solution. The ionic strength of the reaction mixture was adjusted to 0.2 with KCl and the pH of it was controlled with buffer solutions.

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For the purpose of removal of chromium(III) from an aqueous solution, the adsorption behavior of chromium(III) on some chelating resins was tested by batch and column methods. A macroreticulcahr elatingre sin(RMH) containing hydrazide groups was found to be useful for our purpose. In the batchm ethod, the RMH showeda good affinty for chromium(III) in the pH range of 5.8∼57. The adsorptioonf chromium(III) on the RMH was not influenced by the presenceo f Ca²⁺ over the concentration range of 0.01∼0.1 mol/l. In the column method, chromium(III) in an aqueous olution was favorablayd sorbed on the RMH, whent the chromium nitrates solution( pH3.8 ) containing either 1mg/l or 10mg/l of chromiim (III)was passed through the RMH olumn at the spacev elocity(SV) of 15h^-1. Chromium(III) adsorbed on the RMH column was effectively eluted by passing 20 bed volumes of 4 mol/l sodium hdiroxide solution overt he resinat the SV of 7.5h^-1.

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Kitakaname, Hiratsuka-shi 259-12 Japan The solubility of organic compounds in pure water was measured by means of TOC (Total Organic Carbon) method, and sufficient results were obtained. In the begining, a saturated solution of organic compounds was prepared, the TOC of the saturated organic compounds in water was measured, subsequently solubility of compounds was determined from the TOC values. The TOC values were measured by the use of a TOC measuring instrument (SHIMAZUTOC-10B).
Also, the method for the preparation of saturated solution at 20°C was established. In order to dissolve organic compounds in water, the shaking condition was studies (Fig.1-3). Moreover, when the solution that was shaken was allowed to remain in a stationary state, the variation of concentration of organic compounds as the stationary time increased was measured (Fig.4, 5). From the results of these experiments, it is found that following is the most desirable method to obtain the saturated solution. That is, after adding organic compounds in water at 50°C, the solution was shaken for 5 minutes, and the solution is permitted to stand for 48 h at 20°C. By the method described above, the solubility of organic compounds, that is above 10 μg/m/, was measured in a short time, directly, simply and very accurately and that is not necessary to use extraction and other complex procedures.

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The apparatus for easily measuring the compressibilities of liquids and solutions has been assembled by the combination of a standard type differential transformer and a glass cell of syringe type. With this apparatus, the compressibilities of water, hexane, ethylene glycol, and the aqueous solutions of 10 and 20 wt% sodium chloride have been determined at 298.15K and pressures up to 2000 kg⋅cm^-2. The results are in good agreement with the conventional data, indicating that the present apparatus is reliable and useful.

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The temperature dependence of the enantiomer-differentiating catalysis of the rhodium( I )chiral phosphine complex for the dehydrogenation of racemic 1-phenylethanol was studied in the range of 170∼195°C in the presence of various unsaturated compounds. An isokinetic relationship was observed between the activation parameters, ΔH^‡ and ΔS^‡, and further, it was found out that the difference, ΔΔH^‡, in the activation enthalpies between the (R)and the (S)-alcohol was proportional to the corresponding entropy difference, ΔΔS^‡. From these correlations, the enantio-selection mechanism was discussed.

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It was found that 1-bromo-3-chloropropane (BCP) was transformed on activated alumina into 1, 3-dibromopropane (DBP) and 1, 3-dichloropropane (DCP) and further that in this reaction the dehydrohalogenation of BCP into allyl bromide and allyl chloride also occurred. The degree of conversion of BCP increased with increasing the contact time at low temperatures, while it became almost constant at high temperatures. When a mixture of DBP and DCP was passed over activated alumina, a considerable amount of BCP was formed. These three compounds, BCP, DBP and DCP, were found to be in equilibrium. The results are interpreted by assuming that BCP is dissociated into a carbonium ion and a halide anion on the acidic sites of alumina, and that the halide anion attacks the BCP (S^N2 reaction).

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By considering material balance of chlorine and effects of concentrating ratio of chrominum (III) ion to chlorate ion in sulfuric acid solution, it was found that products of th e reaction between chlorate ion and chrominum(III) ion were chlorine dioxide, chlorine and chrominum (VI) ion. At various conc. ratios of chlorate ion to chrominum(III) ion in 8 mol/l sulfuric acid solution, the main reaction was represented by the equation (1) (Table 1).
6ClO₃- + 2Cr³⁺ + H20 = 6ClO₂ + Cr₂O₇^2- + 2H + (1)
Chlorine dioxide was reduced to chloride ion with chrominum(III) ion in sulfuric acid solution (Fig.1 and Table 2). The formation of chlorine could be explained by assuming that chlorine didxide first reduced to chloride ion and this chloride reacted with chlorate in sulfur ic acid solution (Table 3 and Table 4). It was found that Fe(III) ion in the presence of chrominum (III) ion promoted the formation of chlorine dioxide and depressed that of chlorine (Fig.2).

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In the growth of TiN whiskers from the TiCl₄-N₂-H₂ system, the addition of SiHCl₃ vapor or the predeposition of Si on substrate increased the whisker density and the growth rate in the r, adial direction but decreased the growth rate in the axial direction. In the case of TiC whiskers, the presence of SiHCl₃ vapor suppressed the whisker growth remarkably.

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A series of oxo- and sulfido-bridged dinuclear molybdenum(V) complexes, (a) M_O2O₂(μ-O, S) (dte)₂, (b) M_O2O₂(μ-S₃)(dtc)₃, (C) M_O2OS(μ-S₃) (dtc)₃ and (d) M_O2S₂(μ-S₂)(dct)₃ [dtc=S₂CN(n-Bu)₂] were synthesized: (a) by refluxing an aqueous solution containing molyb denum(V) chloride and sodium dibutyldithiocarbamate, (b) and (c) by the reaction among molybdenum(VI) oxide, sodium hydrogensulfide and dibutyldithiocarbamic acid, and (d) by the sulfurization of (a) with diphosphorus pentasulfide, respectively.
These complexes were separated by high-performance liquid chromatography employing a Zorbax SIL column (silica gel) with hexane-ethanol as an eluent and a Unisil C18 column (octadecylsilane) with water-methanol (Fig.1 and 2). Each molybdenum complex was successfully determined on a Zorbax SIL column with hexyl p-hydroxybenzoate as an internal standard hy use of a calibration curve drawn between the raios (Mo complex/standard) of weight and peak area. The coefficient of variation was 0.59∼2.21% and the limit of detection was about 2 ng for S/N=3.

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The metal ion concentration of the reaction mixture is monitored with an ion selective electrode, whose potential is compared with a reference voltage. A pump supplies the precipitant when the metal ion concentration is higher than a predetermined value, and another pump supplies the metal ion solution when the concentration is lower so as to keep the metal ion. concentration virtually constant throughout the precipitaion reaction. The apparatus is designed for small scale laboratory use. The performance was satisfactory on the tests of malachite and tengerite-type neodymium carbonate hydrate.

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Reaction products of mesityl oxide with phenol were analyzed by gas chromatography.4- (4-Hydroxypheny1)-2, 2, 4-trimethylchroman, bisphenol A and o, p'-bisphenol A were found. Since bisphenol A and o, p'-bisphenol A are not obtained by direct reaction of mesityl oxide with phenol, diacetone alcohol is proposed to be a key intermediate of the reaction. Bisphenol A is then formed by condensation of acetone and phenol.

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The uptake of Cd²⁺ and Cu²⁺ from aqueous solutions at 40°C was investigated on three slightly soluble calcium phosphates; hydroxyapatite (HAp), octacalciupm hosphate(OCP), and brushite (DCPD). The uptake of M²⁺ (Cd²⁺ or Cu²⁺) proceeded initially through an ion-exchange reaction Ca²⁺ _??_ M²⁺ and then through subsequent reactions accompanying the formation of either Cd₅H₂(PO₄)₄⋅4H₂O or, presumably, Ca²⁺-dissolving Cu₃(PO₄)₂⋅3H₂O. Exchange fractions of M²⁺ were estimated to be, at least, 10 mol% Cd²⁺ or 8 mol% Cu²⁺ for HAp, 4 mol% Cd²⁺ or 9 mol% Cu²⁺ for OCP, and 6 mol% M²⁺+ for DCPD. The reactivity was in the order of HAp<OCP<DCPD, and the Cu²⁺-uptake occurred more easily than the Cd²⁺-uptake.

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