Organic crystalline compounds with low melting points, e. g., cinnamic acid (mp 136°C), were hot-pressed and the whole contraction processes, starting from relatively loose packing, were observed. These processes were divided into four different steps, i. e., the initial step (I), the Bingham flow step (IV), the diffusive creep step (III), and the final diffusive step (IV). Equations for each step were proposed. A linear relationship between porosity, e, and logarithmic time, log t, was found in the initial step (I) (Fig.2), although its theoretical explanation is not yet possible. For the step (II), an equation was proposed by assuming Bingham solid with no surface tension effect but with driving force alone due to external pressure (Fig.8). A modified equation based on the Nabarrp-Herring creep model, in which the rate of deformation, e, is proportional to the effective stress, ce, was applied to the step (I1) (Fig.9). The final step (IV) was represented by the linear relationship hietween logarithmic shrinkage, log S, and log t, which is frequently used in sintering processes (Fig.11). The regions, in which each step appears, varied with different materials used and the. region, in which the steps (II) and (111) appeared, became narrower with increasing temperature and external pressure (Fig.13 and 14).

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The kinetics of the reactions between (dialkylamino)dimethylarsines or -stibines and ethylene carbonate have been studied by measuring with IR spectra the decrease in the amount of ethylene carbonate. The reactions followed the second-order kinetics.
The reactions of the aminostibines are much faster than that of the aminoarSines with the same N-substituents. This difference can be ascribed to the difference in polarity of the metal-nitrogen bonds. In both reactions, the reaction rates increased with increase in the electron donating ability of the N-substituents. It is found that there is no linear relationship between the logarithms of the reaction rate and the pK values of the nitrogen compounds. The correlations with Taft's equation were fairly good, but it seems that the additional contribution of a hyperconjugation effect exists in some cases. The reactions were not much accelerated in the polar reaction media. These results suggest that the nucleophilic attack of the nitrogen atom of the metal amides on the carbonyl carbon atom of ethylene carbonate is the rate determining step, where the interaction between the metal atoms and the ester oxygen is involved.

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Catalytic oxidation of propylene and surface oxidation-reduction processes on supported bimetallic catalysts which consist of Cu as substrate and small, amounts of Ag, Au, or Rh adhering to the substrate were examined.
The adhering components enhanced both rates of the reduction of preoxidized surface and the propylene oxidation (O₂STC) in the order Rh>>Au>Ag, but showed no effect on the oxidation rate of prereduced surface.
The reduction processes were kinetically divided into three stages as follows:
(1) the accelerating reduction rate period (ARP; x3) in which reduction ratio x increases in proportion to the 1.6 th power of time t, (2) the maximal reduction rate period (MRP; x#0.3∼O.8) in which dx/dt gives maximum, and x increases in proportion to log t, and (3) the decelerating reduction rate period (DRP; x=O.65∼0.95) in which dx/dt decreases in inverse proportion to log t.
For all catalysts, Arrhenius parameters of each reduction rate coefficient in the period MRP and DRP, and the (0₂STC)'s showed compensation effects
log A=E1(2.3 RTs) + log Cs
and gave the same T5, (615±9K). E for the initial reduction rate (k) of each catalyst was correlated with E of (0, STC) by
EK=E_(02STC) + (8.5±0.9) kcal/mol
The accelerating effects of the adhering components were observed in incubation period in the early stage of ARP. This indicates that small amounts of metal which is dispersed on the surface of Cu substrate and more difficult to be oxidized than Cu acts as the portholes of the spillover of the reductant gas, an, d as initiation nuclei for the surface reaction of oxygen.

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In optical communication systems with laser as a light source the optical fiber, used for optical waveguides, is required to have severe ultra-high purity characteristics for transition metal impurity contents. As a part of studies on ultra-high purification process in molten state, heating behavior of some transition metal nitrates in sodium nitrate, which is one of essential raw materials of multi-component glasses, were investigated by means of thermal analysis and Xray diffraction and solubilities of their pyrolysis products in molten sodium nitrate were measured by graphite furnace-atomic absorption spectrometry.
Results of thermal analysis of individual transition metal nitrates (Fig.2) and mixtures with sodium nitrate (Fig.3) showed that thermal decomposition products are their respective stable oxides (Table 1). Oxides of chromium and manganese, however, react with molten 'sodium nitrate to form sodium chromate and manganates (V, VT), respectively, both being soluble in molten sodium nitrate (Fig.4, 5).
Solubilities of individual transition metal oxides in molten sodium nitrate were measured in the temperature range from 350 to 550C (Fig.7-10). The solubility curves showed exothermic dissolution type in which the solubilities decrease slightly with increasing temperature. In general, the solubility decreased upon bubbling oxygen into molten salt, while it increased upon adding sodium peroxide to it (Table 2). Solubilities obtained in the former condition at 400C were as follows: Co, 2 ppb (ng-metal ionig-NaN0, ;); Mn, 4 ppb, Ni, 25 ppb and Cu, 80 ppb. I
It was found that transition metal impurities in sodium nitrate can be effectively removed by means of the filtration of thermally decomposed products in molten state.

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In the. presence of chlorate ion in a sulfuric acid solution, the electrode reaction of iron(II) ion proceeds by the following cyclic process:
The rate constant (k, ) of the reoxidation of iron(II) ion was calculated by Koutecky's equation from the ratio of limiting current, measured at +0.15 V vs. SCE by the D. C. polarographic method in the presence of chlorate ion, to that in the absence of it. The rate constant (kh) of the oxidation of iron(II) ion with chlorate ion in a sulfuric acid solution was determined by measuring the limiting current at +1.3 V vs. SCE by using a rotating platinum electrode.
The rate constants k, and le, in the solution (1.96 mol/l H, SO₄, /2=5.8molgadjusted by Na₂SO₄) at 45°C are 9.7 //molis, and 6.4 //mol. s, respectively; these values agree reasonably. Since the -reaction is of first-order with respect to the concentration of iron (II) and chlorate ions in a homogeneous reaction, and the chlorate ion reacts with iron(II) ion in the ratio of 1: 1 as shown by the gas analysis of chlorine dioxide, the rate constant measured by the above methods would be that of an elementary reaction of chlorate ion with iron (II) ion to form chlorine dioxide.

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Cadmium sulfide powder of uniform particles was prepared by heat treatment of precipitated cadmium sulfide with potassium iodide. The relation between the particle size and shape of the cadmium sulfide powder and the condition of preparation was studied through the analyses of X-ray diffraction pattern, electron microscopy, specific surface area, DTA and TG curves.
The dependence of the heat treatment temperature and the mixing ratio of KI/CdS on the size and shape of cadmium sulfide particles was found.
The cadmium sulfide powder of maximum particle size was obtained in the mixing ratio region of O.25∼0.75, heat-treated at 500°C for 2 hours (as shown in figures 1 and 2). The shapes of these powders varied irregular, spherical or granular with the mixing ratio of KI/CdS.
The uniform spherical particles of cadmium sulfide with particle size of 0.02 to 1.8 p were obtained by heat treatment of the mixture of KI/CdS with molar ratio of 0.5 at 300 to 500°C for 2 hours.
The contribution of cadmium iodide to the formation of spherical particles of the cadmium sulfide was confirmed. In the presence of potassium iodide, the formation of the cadmium iodide was confirmed with oxidizing of partial cadmium sulfide.

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Correlation among preheating temperature, hydrothermal' treatment of Shirasu-Na₂O mixture (Na₂O/SiO₂=1.3-2.0/1) and formation rate of faujasite was studied. The formation of faujasite was affected by the preheating temperature, Na₂O/SiO₂ molar ratio, temperature of hydrothermal treatment and H₂0/Na₂O molar ratio.
Sodium metasilicate and water soluble sodium aluminum silicate A were formed by evaporation of aqueous NaOH solution of Shirasu to dryness. With increasing temperature, sodium metasilicate changed to water soluble sodium aluminum silicates A, B and C. In the temperature range from 1000° to 1300°C, the preheating mixture of Shirasu-Na.20, whose Na₂0/SiO₂ molar ratio being in the range from 1.3 to 1.6, was glassy state. The amounts of faujasite by hydrothermal treatment of preheated mixture were in the following: glassy mixture, crystalline mixture, which contained water soluble sodium aluminum silicate, and evaporated mixture, which contained large amount of sodium metasilicate.
H₂O/Na₂O molar ratio affected the elution of SiO₂ from the preheated mixture and the SiO₂/ Al₂O₃ molar ratio in faujasite formed in solid phase. Na₂O/SiO₂ molar ratio affected the amount of eluted Si02 from the preheated mixture but did not affect appreciably the SiO₂/Al₂O₂ molar ratio in faujasite.
The amount of faujasite formed in solid phase was affected'by the relation between the SiO₂/ Al₂O₃ molar ratio in faujasite and that in solid phase. Under a certain condition of hydrothermal treatment, when the value of SiO₂/Al₂O₂ in faujasite was similar to that in solid phase, a large amount of faujasite was formed. Under other condition of hydrothermal treatment, when the value of SiO₂/Al₂O₂ molar ratio in faujasite differed from that in solid phase, the amount of fauiasite decreased.

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Conditions of formation for several ternary compounds in the Ln-Si-P systems were studied at the reaction temperature of 900°C changing Si/Ln atomic ratio and phosphorus vapour pressure (10^-2∼20 atm).
The following 4 types of phases were identified by X-ray diffraction technique. (1) P-type (CeSiPs, PrSiP, ), space group Pn2ia or Pnma, were formed under high phosphorus pressures. (2) X-type LaSiP₃ was only confirmed by its diffraction pattern of powdered sample which could not be indexed yet. (3) Needle-type compounds (LaSi₂P0, CeSi₂P₆, PrSi, P.) were formed under a high Si/Ln ratio and phosphorus pressure. (4) F-type compounds for Ln=La, Ce, Pr were formed as a X-ray diffractometrically pure single phase in the range of Si/Ln=1.0-- 2.0 under relatively low phosphorus pressures. This phase is structurally similar to P-type phase. There still remains some uncertainty about the existence of its non-stoichiometry.
Direct syntheses for the Si-P binary system at 900°C under constant phosphorus vapour pressures were tried and 3 types of compounds, SiP, an unknown phase and SiP2, were identified.

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A determination method based on the definite integral of a titration curve was applied to a potentiometric titration whose experimental curve does not show a sharp inflection point or a symmetric shape.
If the area, A, of the titration curve surrounded with E=Ea, E=Eb, and E-axis is measured, the concentration of the sample, cz, is given by the following relationship,
where V is the volume of the added titrant, E is the potential of an ion-selective electrode, Ex and Eb are set potentials chosen, and P and Q are constants and dependent upon both Ea and Eb. It was shown theoretically that the above equation was applicable to precipitation, complexformation, and acid-base titrations.
This method could be applied satisfactorily to F^--Ca²⁺, Ag^--CrO₄^2-, Ag⁺-edta^4-, and β-alanineNaOH systems with almost the same accuracy and precision as those obtainable with the potentiostatic method previously reported.

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In N, N-dimethylformamide (DMF) water media, debromination waves and a reduction wave of pyridine nucleus were observed for three bromopyridines at a dropping mercury electrode. The elimination wave of bromine corresponds to irreversible two-electron wave in DMF-water media. The reduction wave of pyridine nucleus corresponds to irreversible one-electron wave in DMF (0.1 vol% H₂O) and irreversible two-electron wave in water containing DMF (above 1∼2 vol% H₂O). The process of debromination was studied by controlled potential electrolysis and a number of electrons transferred during the electrolysis were determined.
The cumulative data indicate that mechanisms for the electrode reaction in DMF-water media are as follows;
The kinetic parameters of debromination process were determined by cyclic voltammetry. It was found that k3=(2.2∼3.7) X10^-6 cm/s and cy=0.2∼0.3. The ease of dehalogenation for pyridines with a different halogen at the same position (2-position) was evaluated by reduction potential and kinetic parameter. The larger the size of halogen atom, the easier becomes the elimination of halogen.

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Numerous metal chelates are separated and analyzed by gas chromatography. In such cases, metal chelates of acetylacetone and its derivatives, which form inner complexes, are mainly used because of their thermal stability and high volatility. Metal tropolonates similarly to metal j9-diketonates form inner complexes and are expected to evaporate in molecular form.
Thermal stability and volatility of copper tropolonate (Cu (trp), ) were investigated by means of thermogravimetric analysis (TGA) and by comparing IR spectrum of solid chelate before vaporization with that of vaporized one. The weight of Cu (trp), begins to decrease at 246°C and reaches 72% weight loss, while the weights of copper pivaloyltrifluoroacetonate, trifluoroacetylacetonate, dipivaloylmethanate, acetylacetonate and benzoylpivaloylmethanate (Cu (bpm), ) begin to decrease at 72, 93, 128, 155 and 222°C, respectively and reach almost 100% weight loss, except the weight of Cu(bpm)which reaches 93% weight loss. As for copper β- diketonates, IR spectra of vaporized chelates are the same as those of solid chelates before vaporization, while as for Cu (trp)besides its own absorption bands, bands of free ligand appear in vapor phase. On the basis of these results, Cu(trp), is less volatile and partially decomposes befdre sublimation.
Gas chromatographic behaviors of Cu (trp), were also investigated and compared them with those of copper chelate of β-diketone, Cu (bpm), . Typical gas chromatogram of Cu (trp), was obtained by using stainless steel column packed with silanized glass microbeads, to which Siljcone F-50 being applied and by programmed column temperature. Retention time of Cu. (trip), was 3.1 min, while that of Cu(bpm), was 1.1 min. On the basis of these results, it is difficult to elute copper tropolonate.

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Rhodium 2-thenoyltrifluoroacetonate Rh(tta)₃ was synthesized and ¹H NMR (60 MHz) and ¹⁹F NMR (56.4 MHz) studies on this were made in various solvents. In dimethyl sulfoxide, methyl isobutyl ketone and cyclohexanone, triplet and quartet were observed in ¹⁹F NMR spectra. These resonance lines were assigned by the peak area ratios and the investigation of the geometrical configuration of the isomers.
The relative content of isomers in the above three solvents could be determined by measuring the signal intensity ratios of CF, fluorines. The relative content of cis isomer was found to be less than 20 mold on-the synthesized sample. Equilibrium constants for isomerization of chelates in solvents were also evaluated at several temperatures ane the heats of isomerization were found to be roughly less than 5 kcal/mol.

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The catalytic hydrogenation of 1, 4-dimethyl-1, 3-cyclohexadiene (1a), 1-ethyl-4-methyl-1, 3- cyclohexadiene (1b), a-terpinene (1c)-t-butyl-4-methyl-1, 3-cyclohexadiene (1d) and 1, 4- diisopropyl-1, 3-cyclohexadiene Ciep has been studied using various kinds of catalyst in analcohol solution at ambient temperature and pressure. The product compositions were measured at 50% conversion of the dienes. Saturated hydrocarbons Ct-2, c-2D, I, 4-reduction products Cc-31 1, 2-reduction products [ 5 ], 3, 4-reduction products C 4 and dehydrogenation products C 6 were formed. Dependence of the selectivities on catalyst was estimated. The selectivity for monoolefin formation (Sm=100 x C3 + 4 + 5DI[2+3+4+5]) increased in the sequence: OsC, Ir-C<Ru-C, Rh-C, Pt <Pd-C, Fe (R), Co (R), Ni (R), Cu (R)=100. The selectivity for the 1, 4-addition of hydrogen (S4=100 x [ 3 ])I[3+4+5] increased in the sequence: Os-C, Ir-C < Ru-C, Rh-C, Cu (R), Fe (R), Ni (R) <Co (R), Pd-C, Pt. The selectivity for the 1, 2-addition of hydrogen to [R] and [id] (S₂=100 x 5 D/[4 + 5]) enhanced in the sequence: Os-C, Ir-C, RuC, Rh-C<Cu (R), Fe (R), Co (R), Ni(R) <Pd-C, Pt. The selectivity for dehydrogenation of the dienes (S.=100 X [ 6]IC₂+3+4+5+6D) decreased in the sequence: Ni(R), Pd-C>Rh-C, Fe(R), Pt>Co(R), Ru-C>Ir-C, Os-C, Cu (R)=0. From these results, a mechanism for the hydrogenation via 'r-adsorbed species CAD and conjugated diene adsorbed species [B] was proposed.

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2, 5, 6-, 2, 6, 7- and 2, 6, 8-Trihydroxy-1, 4-naphthoquinones which are unkown or not fully characterized among thihydroxy-1, 4-naphthoquinones in the literature have been synthesized. The NMR spectra of these quinones were compared with those of five known trihydroxy-1, 4- naphthoquinones. The NMR spectra of trimethoxy-1, 4-naphthoquinones, including new 2, 5, 6-, 2, 6, 7- and 2, 7, 8-trimethoxy compounds were analyzed by measurement of the nuclear Overhuser effect as well as by deuterium-labeling technique.

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In connection with the trans-t-butylation reaction, relative rates of de-t-butylation of 2-tbutylanisole derivatives having appropriate substituents on the m- or p-position (to the t-butyl group) have been measured by the competitive reaction technique.A good linear free energy relationship to the Brown's σ+ holds for the rate of the de-t-butylation. The ρ value for the debutylation reaction (-6.9) is quite similar to that obtained from trans-t-butylation of alkylbenzenes with 2, 4-di-t-butylanisole.

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The samples of activated carbon adsorbing iodine, p-nitrophenol, sodium dodecylbenzenesulfonate or Malachite Green oxalate by 0.03∼0.10 gig-carbon have been analyzed to investigate the adsorbed states on the carbon surfaces.
The micropores having radius below 15 Å seem to play the most important role in adsorption of these substances, since these volume is mainly decreased by adsorption (Fig.1, 2). Occupied micropore volume is 1.2∼2.4 ml per 1 ml of adsorbate.
The results from X-ray diffraction measurement of adsorbing carbons (Fig.4) show that the micropore is a kind of lattice defect and that adsorption means orientation of adsorbate molecules in the pore.

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Reduction of the title compound [1] to N, N-dimethyl-p-phenylenediamine [2] by representative metals (Al, Mg and Ca) and mineral acid was studied. It was found that a few times the theoretical amount of metal was necessary to obtain [2] in a high yield and increasing reaction temperature caused formation of by-products and a decrease in the yield of [2] . The optimum reduction condition was studied for each reduction system and the following results were obtained. Al-powder (1.5 times the theoretical amount) and hydrochloric acid gave [2] in 84% yield in water at 20C and Al-powder (2 times the theoretical amount) and sulfuric acid gave [2] in 68% yield in water at 40C. Mg-pow4er (2 times the theoretical amount) and hydrochloric acid gave [2] in 81% yield in water at 20C. Ca-granules (3 times the theoretical amount) and hydrochloric acid gave [2] in 46% yield and a considerable amount of by-products in ethanol at 60C.

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1-Chlorobutadiene-butadiene rubber (CB-BR) was prepared by using the emulsion-polymerization technique. From elemental analysis and infrared (IR) spectroscopy, CB-BR was found to contain hydroxyl group, carbon-carbon double bond, and chlorine as a functional group. By elemental analyses, oxygen was detected in CB-BR and the absorption attributable to hydroxyl group appeared at about 3400 cm^-1 in IR spectra of CB-BR. Furthermore, it was clarified from IR spectra that the amount of hydroxyl group in CB-BR increases upon treatment of CB-BR with 2-(dimethylamino)ethanol (DMAE). Thus, diisocyanate cure of butadiene rubber becomes feasible by using CB-BR. For example, CB-BR, compounded with diisocyanatotoluene (DIT), affords good vulcanizates by press-curing it at 70°C for 10 or 20 minutes. However, the rates of vulcanization are too high to control the diisocyanate cure, and sometimes scorching is observed. CB-BR is also cured by soaking in acetone solution of DIT. The cure rate is easily controlled by the vulcanization due to the soaking method, and tensile properties of the vulcanizates are superior to those of press-cured CB-BR. The tensile properties of the diisocyanate vulcanizates are improved by compounding DMAE to CB-BR, presumably because of an increase in hydroxyl content in terms of the Menschutkin reaction between DMAE and chlorine in CB-BR.

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In reverse osmosis, water flux.Jw is expressed as follows:
where A is a water permeation coefficient. Generally, the water permeation coefficient A is not constant, but it varies with applied pressure and feed concentration. This is due to "membrane compaction".
The purpose of this study is to investigate the effects of such membrane compaction phenomena, especially the effect of feed concentration on water permeation in cellulose acetate membranes.
Experimental data obtained and the values shown in the literatures were examined in detail, and a water permeation coefficient A was correlated to the following empirical equation which is analogous to the relation obtained by Kimura and Sourirajan for simple pressure compaction:
where A00 is a water permeability constant, a is a "pressure-induced compaction" factor, and b is a "salt-induced compaction" factor.
The effect of salt-induced compaction is more remarkably than that of pressure-induced compaction, and the value of "b" is greater than that of "a". The effect of salt-induced compaction was not recognized within the scope of this investigation.
And it was assumed that the salt-induced compaction is caused by the change in swelling pressure in the membrane.

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By deriving an experimental equation, IF=TθE, of intensity function (IF is essentially an estimate of the temperature required to attain a certain degree of thermal cracking with in the residence time of 1 sec), the product yield was estimated; the evaluation of exponential term "a" in the equation and the identification of the products with higher molecular weight, called heavy oils, were carried out.
Three kinds of dimers containing 2, 4-diphenyl-1-butene were found.
The degradation was roughly classified into following two steps.
(I) Decrease in heavy oils and increase in styrene monomer.
(II) Decrease in styrene monomer and increase in by-products.
As the steam dilution ratio is not important, operating factors were restricted to reaction temperature and residence time. For a given yield of the product, they were interchangeable.
IF is dependent only upon reaction temperature and residence time and 4, with reference to styrene monomer, is expressed by the following equations:
Difference in "a" value for the above two steps shows that the residence time is important during the degradation process of higher molecular weight materials and this method was suggested also to be applicable to the initial stage of degradation.
As IF correlates with product yields (as shown in Figs.9 and 10), the product yield can be successfully predicted by an appropriate choice of pyrolysis conditions.
IF in (I) will be applicable to the pyrolysis process to obtain styrene monomer.

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Adsorptivity and adsorption mechanism of strong acids, strong bases or their salts by commercial activated carbon, which was made from bituminous coal by steam activation at 950°C, were investigated, and pH of the solution with carbon suspension was studied with various method.
Hydrogen ion and' anions are adsorbed equally in the adsorption of acids (Fig.1, Table 2), and they are adsorbed mainly by carbonium ion mechanism. Hydroxide ion and cations are adsorbed equally in the adsorption of bases (Fig.3, Table 3), and hydroxide ion seemed to react with acidic oxidized groups of carbon surface. Anions are peculiarly adsorbed and cations are adsorbed to an electric double layer in the adsorption of salts, and pH of the solution increased with adsorption of hydrogen ion (Fig.5, Table 4). The distilled water, which was boiled with carbon and was separated from it, is neutral, but is alkali'ne without separation because of the adsorption of chloride ion from pH electrode. The city water, which was boiled with carbon and was separated from it, is alkaline because of the adsorption of salts in city water (Fig.6).

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The present paper deals with a spectrophotometric method for the determination of tetraphenylarsonium (TPA) salt or tetraphenylphosphonium (TPP) salt. The procedure was as follows Phosphate buffer solution (0.2 mol/l, pH 7) (5 ml) and potassium salt of tetrabromophenolphthalein ethyl ester solution (2 X 10^-3 mol/l in ethanol) (1 ml) were poured into a separatory funnel. After diluting the mixture to 25 ml with water, 10 ml of the aqueous solution of 1 X10^-6∼1 X 10^-5 mol/l salt was added (in the case of organic solution, 1 ml of the solution of 1, X 10^-5∼1 x 10^-4 mol/l salt was added). The solution was shaked for 1∼2 min with 10 ml of 1, 2-dichlaroethane. The absorbance of the extract at 615 nm was measured by using a reagent blank as. a reference.
The extraction of TPA or TPP was quantitative after 20 sec, coming to equilibrium, at pH 6∼11. About a 15-fold molar excess of the dye was required for the maximum and constant color development. Various inorganic anions and cations do not interfere with the reaction. The extracted gpecies was presumed to be a 1: 1 ion pair compound formed between the dye and TPA or TPP.

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Some problems were studied on usage of analogue integrator for measuring peak area of absorption signals in flameless atomic absorption spectrometry with graphite furnace atomizer.
For the convenience of determining optimum integration time constant, the conception of "effective atomization time", toff was introduced. The accuracy and precision of drawing for measuring peak area from integration curves were not affected by the base-line drift in original absorption signals. Two drawing methods were proposed for the measurement of peak area from integration curves considering the background signal. The effects of voltage setting in atomization stage on both peak height and peak area of absorption signals for copper were compared and it was found that peak area were almost independent of voltage setting while peak height was affected markedly.

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The ground products of condensed phosphates were separated and determined by highspeed liquid chromatography (HLC). The ground samples were chromatographed on a TSK-GEL LS 210 column with acetic acid-sodium acetate buffer solution. The area of the obtained chromatogram was measured. The analytical results agreed with those obtained by paper chromatography, iodometry and thermogravimetric analysis. This method is more rapid and simple than other methods.

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Di-t-butyl peroxide-induced addition of aromatic alcohols (benzyl alcohol [1a], ce-phenylethyl alcohol [1b], β-phenylethyl alcohol [1c]) to hexafluoropropene was carried out as a part of synthetic studies employing free-radical addition of aromatic compounds to fluoroolefins. These alcohols were oxidized readily by the peroxide. Thus [1a] gave phenyl-1, 1, 2, 3, 3, 3-hexafluoropropyl ketone [2] and 2, 2, 3-trifluoro-3-trifluoromethylindanone-1 [3], the same products as those obtained with benzaldehyde, and [1c] gave acetophenone. With [1c] the corresponding cyclic adduct [5] was obtained in 12.4% yield, together with [6] and [7], the products formed by the attack of benzyl radical.

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1-(Trifluoromethyl)-(1) and 2-(trifluoromethyl) naphthalene (2) were synthesized by the reaction of halogenonaphthalenes with trifluoromethyl iodide (3) in the presence of copper powder. Selection of the solvent was found to be important for increasing the yield of the desired product. In pyridine, the reaction of 2-iodonaphthalene with (3) afforded (2) in an excellent yield (86%), but in DMF, the yield of (2) was low (19%).
Similarly (1) was prepared by the reaction of 1-iodonaphthalene with (3) in a 63% yield. Activity of the halogenonaphthalenes decreased in the following order: iodonaphthalene>bromonaphthalene>>chloronaphthalene.

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Calcium methacrylate (monomer salt) is known to decompose at 450°C to give chiefly fivemembered cyclic ketones (2, 5-dimethy1-3-cyclopenten-l-one, 2, 5-dimethy1-1-cyclopentanone, etc.). These ketones are presumed to be formed as products of the thermal decomposition of the dimer salt which is developed from monomer salt by thermal dimerization below its decomposition temperature.
The authors confirmed the formation of dimers upon heating monomer salt in vacuo for 3 hours at 220°C. After heat treatment, the salt was acidified with hydrochloric acid and extracted with ether. The extract was esterified with diazomethane and distilled. A dimer ester fraction (bp 93∼94°C at 3 mmHg) was obtained in 30% yield. The fraction was identified as dimethyl α-methylene-δ-methyladipate (1) by the methods of NMR and IR, etc. Further reaction of (1) with diazomethane gives methyl 1-[3-(methoxycarbonyl) butyl]-1-cyclopropanecarboxylate (4).

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Fe₂(SO₄)₃-α-Fe₂O₃, catalysts used for the reduction of NO with NH, were prepared from the precipitation formed by the reaction of Fe, (SO₄), aq. with NH, aq. or by the addition of (NH₄) 2SO₄ to the precipitate formed by the reaction of Fe(NO, ), or FeCl, aq. with NH₃ aq.
The catalytic activity was studied by using a flow reactor (I. D.: 12.0 mm) under atmospheric pressure and at 250∼550°C.
The average diameter of the granular catalysts was 1, 0 mm. Inlet gas concentrations were 500 ppm NO-0-1000 ppm (mainly 0 ppm), SO^2-334∼2000 ppm (mainly 500 ppm), NH₃-0-10% (mainly 5%), 02-0-10% (mainly 10%) and H₂O-N₂ balanced; the total gas flow rate was 1000 Ncrnsimin toward 1.0 g of the catalysts.
It was proved that a small amount of (NH₄)2SO₄ contained in Fe (OH), after precipitation (Fe2(SO₄)3 + 6 NH₃ + 6 H₂O) 2 Fe(OH), + 3 (NH₄)25O₄ and washing or a small amount of (NH₄)2SO₄ added is decomposed to form SOx by the calcination of precipitate at 450∼750°C, which reacts with the precipitate to form Fe₂(SO₄)3 on α-Fe₂O₃ surface, and that this Fe₂(SO₄)3 gives an excellent activity and a selectivity (reduction rate of NO over Fe₂(SO₄)3-α-Fe₂O₃ catalysts calcined at 450∼650°C is ca.95% in the case of inlet gas of 500 ppm NO-500 ppmNH₃-5% O₂-10% H₂O-N₂ at 400∼450°C).

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The binary systems consisting of triethylenediamine or triethylamine and Mg (II) salt promote the carboxylation of active methylene compounds with carbon dioxide. Only monocarboxylic acids derived from the active methylene compounds are obtained in a good yield.

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