Pore size distribution in porous substances has so far been analyzed on the conventional assumption that each pore is isolated from other pores. This paper proposes a three-dimensional network structure (TNS) model for a more realistic analysis of the distribution taking account of pore structure. The TNS pore system comprises cylindrical unit pores, which are of various sizes and are randomly distributed on each site of an appropriate lattice model (Table 1).
It was confirmed experimentally that variation in the thickness of sorbed layers could be neglected in a first approximation (Figs.1-4). This finding allows us to describe the state of a sorbate in terms of the sorbed layer on the pore wall and the condensate on the layer.
The condensation of the sorbate in unit pores in the TNS system can proceed in three rou-tes (reversible route I, irreversible n, and intermediate III). The route and the vapor pres-sure for condensation in a unit pore depend not only on the pore size but also on the environ-ment, i. e., whether the adjacent unit pores have already been filled with liquid or not. Based on the TNS model, the process of capillary condensation with increasing vapor pressure was simulated by a digital computer (Figs.5, -7). The results revealed that more than half of unit pores, particularly, most of larger ones were filled via route I (Figs.8, 9, and Table 2). Accordingly, it was concluded that for a practical analysis of pore size distribution, not a cylindrical meniscus but a spherical one should be assumed with respect to the adsorption branch of isotherms regardless of the mode of network structure.

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The kinetics of NO_x removal from N₂-NO and N₂-0₂-NO mixtures under irradiation with high energy electron beam (1.2 MeV) has been studied. The concentrations of NO and N₂0 were monitored in an essential tirnd by means of the newly devised molecular absorption spectrometry. The decreasing rate of NO became lower gradually with increasing irradiation time. This decrease in rate became more significant with decreasing NO content and increasing temperature. The initial decreasing rate of NO was higher in the presence of 0₂ than that in the absence of 0₂, but a decrease in rate at a later stage became significant. These findings are quantitatively explained in terms of the knowledge of the radiation chemistry of N₂ and of the rate of the subsequent reactions. The employed G values were: G(N₂⁺) =2.3, G(N⁺) =0.6, G(e) =2.9, G (N (⁴S)) =1.5, and G(N(²D)) =1.0. The main reactions concerning the reduction of NO were: N+NO→ N₂+0, and 0+NO+M→ NO²+M. N (₂D) reacted with 0₂ to produce NO_x in the presence of O₂. A possible role of electronic-excited nitrogen molecules was also discussed in terms of the observation made on N₂0 formation in N₂-0₂ mixtures.

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Hydrogenation of benzene to give cyclohexylbenzene over potassium-graphite lamellar com-pound catalysts (C_nK, n=8 or 24) was investigated at 200-250° C and under 50-100 kg/cm²-H₂. By-products were cyclohexane and dicyclohexylbenzenes. To produce cyclohexylbenzene catalyzed by CK was found to be due to a characteristic property of lamellar compound cata- lysts C_nK because in the above case catalyzed by the physical mixture of potassium and graphite, cyclohexane was almost selectively obtained. Furthermore, higher ratio of cyclohexylbenzene/ cyclohexane was obtained with Ca, K than that with C8K and these ratios were 7 and 0.4, respectively at 200° C and under 100 kg/cm²-H₂.
X-ray analysis of C_2CK during the initial stage of hydrogenation suggested that absorbed benzene occupied the space of CI, K-layers without being replaced by hydrogen. On the other hand, Cal< changed into somewhat complex species of catalyst, which seemed to be produced by the interaction of C8K-hydride with benzene. Selectivity of CK catalysts to produce cyclohexylbenzene or cyclohexane was discussed in terms of the absorption of benzene or hy- drogen by CnK-layers. Results of hydrogenation of some related hydrocarbons such as toluene and biphenyl were also described.

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Effects of aliphatic polyamines, ethylenediamine (en), propylenediamine (pn), diethylene-triamine (dien), triethylenetetramine (trien) and tetraethylenepentamine (tetren), on the electrodeposition of zinc from zincate bath were investigated by cathodic polarization curves, polarography, current efficiency measurements and electronmicrophotography. The reaction mechanism proposed by Gerisher, Zn (OH) ₄^2- Zn (OH) ₂ + 2 OH-, Zn (OH), ₂ + 2 e- Zn + 2 OH-, was employed for the interpretation of experimental results. The following results were obtained:
(1) Addition of trien and tetren to the zincate bath was very effective for the zinc plating, but no effect was found for en, pn, and dien.
(2) The polarograph and cathodic polarization curves showed that the stability of Zn-amine complexs increased in the order en< pn< dien< trien< tetren. The amount of amine required for producing each Zn-amine complex was determined from the complete dissolution of Zn (OH)₂.
(3) It was proposed that on cathodic polarization added amines react with the intermediate compound Zn(OH)₂ produced from Zn(OH)₄^2- ion to form a Zn-amine complex and thus cathodic polarization is increased and the amount of codeposited Zn(OH) ₂ decreases in the zinc deposit.

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Fibrous calcium vanadate crytals in the system CaO-V₂0₅-H₂O were hydrothermally synthesized over the temperature range of 200 to 600° C and pressure of 20 to 350 atm. The reaction lasted up to one month. Chemicals used as starting materials, V₂O₅ and Ca (OH)₂were of reagent grade. Techniques involving X-ray diffraction, microscopy and differential thermal analysis were applied for the examination of vanadate crystals. The pH of the solution after the reaction was also recorded. The calcium vanadate fiber tended to increase in length with increasing temperature and pressure. The fiber also grew in a different way according to the reaction time at a given pressure (200 atm); up to 320° C it tended to lengthen with increasing reaction time, but at 400° C it decreased in length with the time involved. The best result was yielded by treating the reaction mixture for 1 hr at 450° C under a pressure of 300 atm. The length of fiber was also dependent on the pH of the solution for the reaction conditions involving temperature of 250, 320 and 400° C-pressure of 200 atm-treatment time of 2 days. Within the temperature range given about the same length of fiber was grown, as far as the pH was held constant. The pH 4 was found to yield the longest fiber after the reaction. According to X-ray diffraction measurements smerwoodite became a stable phase below about 320° C, while above 400° C both hendersonite and simplotite grew together. An unknown phase with a platy crystal habit was produced together with smerwoodite at temperature range above 500° C. DTA and TG curves indicated that a large peak near 645° C for the endothermic reaction should be attributed to the release of bonded water. A fiber (smerwoodite) having a maximum length of 3.4 mm and 10 μ m in diameter was synthesized in this way, which exhibited a light brown color and flexibility.

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The reaction between ZrP₂O₇ and MgO in the solid state has been studied for the compressed mixtures in various concentrations ranging from 10 to 90 mol% MgO and for the ZrP₂O₇-MgO diffusion couple. The mixtures were heated at 1200° C for 24 hr or at elevated temperatures up to 1400° C(heating rate: 10° C. min^-1) in air. After the reactions had completed, the samples were quenched to room temperature and subjected to X-ray powder diffractometry.
The reactions between ZrP₂O₇ and MgO yielded the following compounds; MgZr₄(PO₄)₆, Mg₂(PO₄)₂, Mg₂P₂O₇, Mg (PO₃)₂, ZrO₂ (monoclinic and tetragonal) and (ZrO)₂P₂O₇. The double phosphate, formed in the reaction, was isolated from the reactant of the mixture containing 50 mol% MgO. Chemical analysis and IR spectrum revealed that the formula of the substance corresponds to MgZr₄(PO₄)₆. It was confirmed that the formation reaction of MgZr₄(PO₄)₆ proceeded via inter-diffusion of MgO and P₂O₅. In addition, the mixture of ZrP₂O₇ and MgO with MgO contents ranging from 0 to about 60 mol% gave the MgZr₄(PO₄)₆ upon the solid state reaction.

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Nitriding of Ti powder, Ti and V plates with N₂ (1 atm) has been carried out at 900-1440 ° C, to obtain fundamental information for the nitriding of Ti-V alloys. The process of nitriding was Investigated by gravimetric method, X-ray diffractometry, X-ray microprobe analysis and microscopic observation. Two stages were observed in the nitriding of Ti; (1) the solution of nitrogen in α -Ti, (2) formation and increase of TiN layer on the surface of α -Ti phase, after the disappearance of the concentration gradient of nitrogen in α -Ti phase. In the nitriding of V, VN and V₃N were observed on the surface of metal and V₃N developed in the inner part of metal saturated with nitrogen. The solution of nitrogen in the V metal proceeded so rapidly that the nitrogen concentration gradient was not observed. The initial rate of nitriding followed the parabolic law, and the diffusion of nitrogen in metal phases was rate-determining. The rate constants of this reaction were as follows for Ti and V, respectively.
The apparent diffusion coefficients of nitrogen in α -Ti and TiN were calculated by using-the nitrogen concentration in each phase boundaries obtained from Ti-N equilibrium phase diagram.

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The method to prepare K-substituted β'' -alumina from MgO-stahilized Na⁺-β'' -alumina was established by treating the β''-alumina in a aqueous solution of potassium ion.
Since the ion exchange of sodium ion in Na₊-β'' -alumina by other alkali ions with the treatment of alkali aqueous solution tended to be hindered by the water adsorbed on the crystal surface, sodium ion was first replaced by H₃0⁺ ion through the immersion of Na⁺β'' -alumina powder in a concentrated sulfuric acid at 220-240° C for 15-30 minutes, and then, the replacement of H₃0⁺ ion in H₊-β ''-alumina by alkali ion was tried through the immersion of H⁺-β'' -alumina powder into a concentrated alkali aqueous solution.
The replacement of H₃O⁺ ion by potassium ion was made through the immersion of H⁺-β'' - alumina into a concentrated aqueous solution of potassium hydroxide at 150-400° C for several hours. On the other hand, the replacement of H₃O⁺ion by lithium ion was not successful under the present experimental conditions because of the formation of reaction by-products such as lithium aluminate from the reaction of H⁺-β''-alumina with a concentrated aqueous solution of lithium hydroxide.
The H⁺- and alkali-substitute β''-aluminas obtained by the above exchange reactions were examined by DTA, TGA and X-ray diffractometry.

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A number of copper (II) complexes with 1-(p-substituted phenyl)-1, 3-butanediones (HL, L=p-RC₆H₄COCHCOCH₃, R=NO₂)[1], COOH[2], COOCH₃[3], Br[4], Cl[5], H[6], NHCOCH₃[7], C₂H₅[8], CH₃[9], OCH₃[10]and OH[11] were synthesized. From the elemental analyses, thermal analyses and molecular weight measurements, the complexes were found to have a 1: 2 molar ratio of copper (II) to ligand, all being anhydride except for [ 2 ] and [11], which were mono- and dihydrate, respectively. The spectra of complexes which exhibited the magnetic moment of 1.88-1.93 BM in the solid state and in chloroform were characteristic of the square planar structure, and the ligand field bands appeared at about 18 and 16 x 10³ cm^-1. The spectra of complexes which exhibited the moment of 2.0-2.2 BM in pyridine and DMSO were characteristic of the distorted octahedral structure, and the ligand field bands were observed at about 15.5 and 13-10 x 10³ cm^-1. Both bands about 18 and 16 X 10₃ cm^-1 shifted linearly to the higher frequency side as the substituents become more electron donative. The main IR absorption bands of the chelate ring were assigned, and the stability of these complexes was discussed in relation to the shift of and as caused by the substituent effect.

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Sodium, chlorine, manganese and strontium in fresh shells of pecten collected from the Enoshima-Bay, Miyagi Prefecture were determined by nondestructive neutron activation analysis to study changes in statistical distribution of chemical elements of shells by diagenesis. Samples of the fresh shell consist of three groups, i. e., different parts of the same growth stage in the same disc (group A), different parts of the same disc along a central radial rib (group B), and similar parts of different discs (group C). In order to compare with the fresh shell, data of the Recent shells reported in the previous works were also examined as leached shells (group D). Samples of group D consist of similar parts of different discs, but their locality and buried period were not the same.
Geometric means of sodium, chlorine, manganese and strontium contents in each group were calculated, and the fitting of lognormal distribution to data for manganese and strontium was illustrated. Each element in group A exhibited the least relative standard deviation. These values were much the same as the experimental errors of γ -ray spectrometry. Medium variations observed in groups B and C may be reflections of environmental and individual variations of living shells, respectively. On the other hand, group D showed large variations in contents of all the elements. Large differences in the distribution of elements between the fresh shells (groups A, B and C) and the leached shells (group D) are perhaps due to the versatility in diagenesis in the latter. These results seems to be of importance for the study of paleoenvironment by trace elements in fossil shells, because similar phenomena may also have happened among fossil shells during the process of fossilization.

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A method for the determination of vanadium in plants and biological materials by a com-bined solvent extraction-carbon furnace atomic absorption spectrometry was described. N-cinnamoyl-N-(2, 3-xylyl)hydroxylamine (CXA) was used as a selective and sensitive chelating reagent for the extraction of vanadium. This reagent was superior in terms of selectivity and sensitivity to other chelating reagents for vanadium. The pyrolytic-graphite-coated tube was used in order to avoid the soak of the vanadium chelate into the carbon tube as well as the formation of vanadium carbide. The proposed method achieved the enhancement of absorbance by about 12 times as large our previously reported method which involved the extraction with N-benzoyl-N-o-tolylhydroxylamine and use of conventional carbon tube.
Procedure: Digest sample(plants and biological materials: 1-10 g, blood: 10 ml, urine 50 ml) with a mixture of nitric acid and perchloric acid. Dilute to 20-40 ml with distilled water, and then transfer to a separatory funnel. For oxidation of V(IV) to V (V), add 0.02 mol/l potassium permanganate solution dropwise until the pink reagent color persists for 5 min, and then 1 ml of O.1% CXA in carbon tetrachloride solution. Adjust the resulting solution to ca.6 N in hydrochloric acid. Extract vanadium by shaking the mixture for 3 min into the carbon tetrachloride. Apply a 20 μ l aliquot of the extract on the carbon tube by means of a micro-syringe. Proceed according to the experimental conditions given in Table 1.
Under this condition, vanadium in plants and biological samples could be determined with an average recovery of 94%. The coefficient of variation was as low as 14%. The sensitivity (1% absorption) was estimated to be 4 x 10^-11 g (2 ng/ml)

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Micro amounts of polycyclic aromatic hydrocarbons (PAH) in sea bottom sediments were determined successfully by combination of open column, thin layer, and high performance liquid chromatography.
A dried sedimental mud was extracted with a dimethyl sulfoxide (DMSO) by using an ultra-sonic apparatus. PAH in DMSO solution to which added 15% NaCl aqueous solution were extracted reversely with a hexane and this solution was condensed with an evaporator. The extract was placed on the top of a clean-up column containing silica gel. PAH fraction was collected by passing a benzene through the column after aliphatic hydrocarbons eluted with the hexane. The benzene solution was evaporated gently and reduced to 1.00 ml at lower than 40° C.
Pre-fractionation of PAH was accomplished by developing the solution spotted on an one dimentional dual thin layer plate (Kieselguhr G, 20%-O-acetylated cellulose) with methanol-ether-water (4: 4: 1, v/v) solvent. PAH developed on the thin layer plate were divided into four fractions according to each R_f values. PAH in each fraction was scraped off and extracted with the benzene. These solutions were condensed with the evaporator under the mild conditions.
A liquid chromatographic separation of each fraction was carried out by introducing 1-10 μ l portions of this fraction on a LiChrosorb RP-18 column and by using methanol-acetonitrile- water as mobile phase with gradient elution method and a UV-254 nm photometric detector. PAH was identified by using the retention time, the fluorescence and excitation spectra, and determined quantitatively with a peak height method.
Isomeric PAH such as benzo[ e ]pyrene and perylene, benz[a ]anthracene and chrysene which were difficult to separate on the ODS column could be separated and identified successfully by this method. And a low detection limit below ng order could be obtained. Fifteen substances of PAH in sea bottom sediments were detected by this method.

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The response of electron capture detector (ECD) derived from the kinetic theory by Wentworth was studied in various pulse conditions. In the case of applying the pulses corresponding to each plateau of the background current-pulse width (I_b-t_w) curves (Fig.1), the electron concentration in the ECD increased with increasing pulse period (t_P) and reached the equilibrium at t_P = 2000 μ sec (Fig.2). The linear dynamic ranges of the response improved with increasing t_P and became more than 10³ at t=2000 μ sec (Fig.3). This result may be attributed to the fact that the steady state conditions assumed by Wentworth for many rate equations of the kinetic model are best assured when the electron concentration reaches the equilibrium. In the case of applying several pulses corresponding to each shoulder of the (tw⁰) curves, it was recognized that there was an optimum pulse width (tw⁰) achieving the maximum linearity and that the value of tw⁰ increased with increasing t_P: the linear dynamic ranges of the respose became more than 10³ at tw⁰ = 0.5 μ sec in t_P=100 μ sec, tw⁰ = 0.7 μ sec in t_P= 500 μ sec and tw⁰= 0.9 μ sec in t_P= 1000 μ sec (Fig.5-7). These results suggest that the electron concentration attains the equilibrium at tw⁰ in each t_P.

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The polished surface of cyrindrical steel (NT 70 H, Fe: 95.97 at%, C: O.56 at%, diameter: 5 cm, length: O.5 cm) was nitrided in (I) flowing gas atmosphere of ammonia (2 NH₃ → 2 N+3 H₂), in (II) fused bath of potassium cyanate and potassium cyanide, or by (III) nitrogen ion produced by electric discharge (N₂+ H₂ 2N⁺ + 2 H⁺), and chemico-physical states of iron nitride formed at the surface were analyzed layer by layer.
The surface was ground to the desired depth utilizing the fine powder of SIC 500 and CEMS' of the exposed layers were measured by detecting the resonantly scattered conversion and Auger electrons. The ground thickness was monitored through weighing of nitrided specimen. Gas nitrided steel at 790 K has 4 distinct layers on the surface. The uppermost surface material is attributed to ε -Fe₂N, the thickness of which is more than 10 μ m. Then, ε -Fe_2-3N austenite layer, the distorted Fe_3-xN (0≤ x≤ 1) layer and the γ '-Fe₄N martensite layer exist. The distorted Fe₄N layer, having split six peaks with the intensity ratio 3: 4: 1: 1: 4: 3, appeared above the α -Fe substrate.
The crystal structure of α -iron phase close to the γ '-Fe₄N is distorted to a considerable extent by the intrusion of nitrogen atoms into the lattice.
The surface of tufftrided steel is composed of ε -Fe₃N, the intermediate phase of ε -Fe₃N and γ '-Fe₄N, γ '-Fe₄N and α -Fe layers.
The ion nitrided steel has 3 layers on the surface, i. e., γ ₁'-Fe₄N, γ ₂'-Fe₄N and α -Fe phases. CEMS appeared to be feasible in characterizing the surface layer, elucidating clearly the distorted intermediate phase and magnetic property of the specific layer.

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Reaction of 1-methyl-9-fluorenone [ 1 ] with a variety of Grignard reagents or organolithium compounds gave 9-substituted 1-methyl-9-fluorenols [ 4].9-Alkoxy-9-ary1-1-methylfluorenes [6 ] were obtained by refluxing the solution of 9-bromo-1-methylfluorenes [ 5 ] in alcohol which in turn were prepared from C 4 J with HBr in acetic acid. Reduction of [ 4 ] with HI in acetic acid gave 9-substituted 1-methylfluorenes [ 7 ] (e. g., 9- (2-methylpheny1)- [7 e], 9- (3- methylpheny1)- [7 f], 9- (4-methylphenyl) - [7 g], 9- (1-naphthyl) [7 h], and 9- (2-methyl-1-naphthyl)-1-methylfluorene [7 i]).
The restricted rotation around the C_sp3-C_sp2 single bond in [ 7 ] has been investigated by means of the DNMR method. Rotational barriers around the C_sp3-C_sp2 bond in [7 e] (Δ G_115c=19.6 kcal/mol) and [7 h] (Δ G_160o=21.4 kcal/mol) were found to be 2-3 kcal/mol higher than those of 9- (2-methylphenyl)fluorene and 9- (1-naphthyl) fluorene, respectively.

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The products of the reactions between chloro-p-benzoquinones and Na₂S0₃ in aqueous buffer solution (50% EtOH) were examined by means of polarographic and spectrophotometric methods. Redox reaction proceeded in strongly acidic region (Eq. (1)); the rate became low at pH < 2 and the reaction was subjected to steric hindrance by the chloro groups in the case of tetra-chloro-p-benzoquinone.
Addition (Eq. (2)) and replacement (Eq. (3)) reactions proceeded competitively in the region from weakly acidic to neutral solution. XPQ + HS0₃^- + H₂O = XH₂Q + SO₄^2- H+ (1) XPQ + HS0₃-=XH₂QS^- (2) XPQ + HS0₃-=XPQS- X^-+11⁺ (3)
Where XPQ, XH₂Q, XH₂QS^- and XPQS^- represent chloro-p-benzoquinones, chlorohydro-quinones, chlorohydroquinonesulfonates, and chloro-p-benzoquinonesulfonates, respectively.
It was confirmed from these observation that HS0₃^- ion attacked carbonyl carbon atom in quinone ring in strongly acidic solution and attacked 2, 3, 5 and 6 positions in the above ring in weakly acidic or neutral solution.

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The liquid phase ammonolysis of phenol and/or cyclohexanone catalyzed by palladium supported on charcoal was studied. The ammonolysis of phenol alone did not occur substantially. On the other hand, the ammonolysis, of cyclohexanone took place easily to form aniline, cyclohexylamine, N-cyclohexylaniline, and dicyclohexylamine as main products. The aniline/ cyclohexylamine ratio(ca.1: 2) suggested that these two products appeared upon disproportion-ation of cyclohexanimine, an intermediate formed from cyclohexanone and ammonia. N-Cyclohexylaniline and dicyclohexylamine were considered to be formed by the condensation between aniline and cyclohexylamine, and between two molecules of cyclohexylamine, respectively.
When a mixture of phenol and cyclohexanone was allowed to react with ammonia in the presence of palladium catalyst, phenol reacted as well as cyclohexanone to form aniline in high Yield. The other main products were found to be cyclohexylamine and N-cyclohexylaniline. The conversion of phenol and the amount of aniline increased with increasing temperature, reaction time, and amount of palladium catalyst, while the conversion of cyclohexanone was always 100% and the yield of cyclohexylamine was almost unchanged.
The following ammonolysis reaction mechanism for the binary system was put forward from these results: Cyclohexanone reacted with ammonia to form aniline and cyclohexylamine, and next phenol was converted into aniline because of the presence of cyclohexylamine.

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In the course of a study on essential oils of the cyperaceae, essential oils from roots of Onigayatsuri (Cyperus pilosus Vahl) was studied. The yields of the oils were 0.023-0.339%, and the oils were separated into individual compounds by means of combination of elution chromatography and distillation or of gas chromatography (GC). The structure of a new compound separated was determinded based on chemical and spectral evidence. The new compound was dimethyl ester of a novel terpenic dibasic acid [ 1], dimethyl (2 E, 6 E, 10 E)-3, 7, 11-trimethyl-2, 6, 10-dodecatrienedioate, and the oils contained 41.1-69.1% of [1].
On the other hand, identification of the known compounds was performed based on comparison of the retention time of GC and of mass spectra with those of the authentic specimens. Main components were cyperene, β -selinene, α -cadinol, (2 E, 6 E)-farnesol, methyl (2 Z, 6 E)- farnesate, methyl (2 E, 6 E)-farnesate, new ester [ 1 ], and normal alkanes (C₁₉H₄₀, C₂₁H₄₄, C₂₂H₄₆, C₂₈H₄₈). Minor ones were caryophyllene, juniper camphor, (2 E, 6 E)-farnesyl acetate, methyl parmitate, and normal alkanes (C₁₇H₃₆, C₁₈H₃₈, C₂₀H₄₂, C₂₄H₅₀ and C₂₅H₅₂).

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The heat treatment of poly (a-chloroacrylonitrile) (PCAN) was carried out at lower temper-ature than 200° C in nitrogen and its effect was investigated.
When PCAN was heat-treated isothermally at higher temperature than 170° C in a differential thermal analyzer, an exothermic reaction, due to polymerization of cyano groups, was observed. Samples with different extent of polymerization of cyano groups could be prepared by varying the heat-treating temperature and time. Their degrees of dehydrochlorination and degradation were determined mainly by chlorine and IR analyses, respectively. The following conclusions were obtained from the above data. (1) At an early stage of heat treatment, dehydrochlori-nation and polymerization of cyano groups occurred in separate repeating units. (2) The final percentage of the repeating units, which were subjected to polymerization of cyano groups, became more than 30%. (3) Although the moiety, subjected to polymerization of cyano groups, was easily dehydrochlorinated, its dehydrochlorination was not completed before the end of exothermic reaction, if the heat-treating temperature was lower than 190° C. (4) An increase in degree of degradation after the end of exothermic reaction would bring about the formation of α, β-unsaturated cyano groups, derived from dehydrochlorination, but not the polymerization of cyano groups. Consequently, it was proved that, when PCAN was heat-treated, two different dehydro-chlorinations occurred until the moiety, subjected to polymerization of cyano groups, was completely dehydrochlorinated.

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Eight different poly-Schiff bases were prepared by the polycondensation of p-phenylenediamine or benzidine, with p-benzoquinone, 1, 4-naphthoquinone, anthraquinone and anthanthrone as raw materials in 116% polyphosphoric acid. The structures of the polymers were verified by the comparative study with synthesized model compounds based on elemental analysis, IR and UV spectra. The polymers were stable up to 310-500° C in air and 400-650° C in nitrogen. The specific conductance of the polymers was found to be 1.0 x10^-5 to 3.8 x 10^-7 Ω ^-1 cm^-1 at 200° C.

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A method of calculating breakthrough curves with only data of bach adsorption tests was investigated for liquid phase adsorption at nonlinear equilibrium. Adsorption tests of an aqueous solution of sodium p-dodecylbenzenesulfonate or p-methylbenzenesulfonate in the column of granular activated carbon were carried out at 20° C. The experimental data were compared with the breakthrough curves calculated from a mass transfer equation derived under the several assumptions given in Table 4.
The adsorption isotherms were found to be given by the Freundlich equation, and the change of the intraparticle diffusivity (D₁') with the concentration of the solution (C) to be shown by the equation: D₁'=aC^b + D₂. The experimental data were not in agreement with the breakthrough curves calculated by the conventional method. The data were, howevere, in good agreement with the calculated breakthrough curves when D₁' was corrected for each cal-culating concentration of solution, and the equation k_sa_v=60 D₁'p_b/d_p² was used for the relation between mass transfer coefficient and diffusion coefficient (Figs. 5-8).

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V₂O₅-Al₂O₃ and Fe₂O₃-Al₂O₃ catalysts were effective for the reduction of NO_x in a waste gas from a sintering furnace. In this paper, the techniques of regeneration are discussed on the basis of the results oftained by ion microanalyzer, X-ray fluorescence diffractometer, and X-ray diffraction spectrometer.
In general a heat treatment was effective to regenerate the catalysts, deactivated merely by SO_x in A dust free flue gas. However, the catalysts used in a waste gas from a sintering furnace could not be recovered by a heat treatment (Figs.4, 9). This is due to the adhesion of the dust components such as K, Ca, Na, Fe, and Si to the catalysts (Figs.5, 10). Among the dust components, K mostly lowered the catalytic activity for NO_x reduction. Therefore, the studies were made on the behavior of accumulated K on the catalysts surfaces and to establish the effective techniques to remove K from the catalysts.
In the case of V₂O₅-Al₂O₃ catalyst, K was concentrated on the outer surface of the catalyst particle (Fig.2); it could be removed by washing with hot water (Fig.7). An effective recovery of the catalytic activity was attained by washing (Fig.6). On the contrary, in the case of Fe₂O₃-Al₂O₃ catalyst, K permeated in an inner part of the catalyst particle (Fig.3) and the removal of K from the catalyst by washing was difficult. Potassium, permeated in the catalyst, migrated and concentrated on the outer surface of the catalyst particle by heating in air at' 550° C (Fig.10). Therefore, K could be removed from the catalyst, by washing with hot water (Figs.13, 14) after heating in air at 550° C. The catalytic activity was well recovered by this method.

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The removal of mercury (II) chloride (HgCl₂), methylmercury (II) chloride (CH₃HgCl), and phenylmercury(II) acetate (PhHgCH₃COO) from aqueous solutions by the char, prepared by carbonization of scrap tire at 500-800° C in a stream of nitrogen, was studied.
The rate of removal of mercury compounds was so high as that of its adsorption on activated carbon (Fig.2). Removal equilibrium data obeyed the Freundlich type isotherms over the concentration range 2-80 mg-Hg/l (Figs.4-6). The char carbonized at 600° C showed higher removal capacity than that carbonized at other temperatures (Fig.7). The effect of treatment with hydrochloric acid (10_-3, 10_-1, or 12 N) on the char was also studied. For HgCl₂ and CH₃HgCl, the removal capacities of the char treated with 10_-3N hyrdrochloric acid were nearly equal to or less than that of untreated ones, while the removal capacity for PhHgCH₃COO increased by the same treatment (Figs.9, 10). With increasing concentration of hydrochloric acid, the removal capacities of HgCl₂ and CH₃HgCl decreased appreciably, because zinc sulfide in the char was eluted by the acid treatment. The char contained approximately 10% ash, about 4% of which was zinc sulfide; zinc ion was eluted at the removal of HgCl₂and CH, . HgCl. The atomic ratio of eluted zinc to removed mercury has been found to be about O.6 for HgCl₂ and 0.4 for CH₃HgCl, respectively (Fig.13). In the case of PhHgCH₃COO, however, elution of zinc ion was not observed. In conclusion, despite HgCl₂ and CH₃HgCl₂ were removed by the absorption and the chemical reactions (1) and (2), PhHgCH₃COO was considered to be removed merely by the absorption.

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Fine crystals of several organic compounds were sintered under pressure at temperatures several degrees below the respective melting points, and the temperature dependence of the hardness of the sintered bodies were measured by an indentation method.
Sudden change in the temperature dependency of the hardness was observed for all of these 'bodies at temperatures several tens degrees below the melting points. The same behavior in the temperature dependency was also observed in the hot-press processes of these compounds used in the above experiments.
The ratio of the temperature of the singularity to the respective melting point on the absolute temperature scale was 0.89± 0.03.

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Preparation of a uniaxial oriented barium ferrite magnet using lamellar oxalate coprecipitate without pressing in a magnetic field was investigated. Anisotropic grades of pressed core (PC) were improved by the shape effect of the lamellar oxalate coprecipitate (molar ratio: Fe²⁺/Ba²⁺= 11), which allows the [010] to be aligned with the applying uniaxial pressure. The sintered barium ferrite core was obtained by the heat treatment of the PC at 1000° C in air for one hour. The grains of the sintered barium ferrite core were oriented uniaxialy along the [0001]. The topotactic relation between the coprecipitate and the barium ferrite should be responsible for the orientation along the [0001] of particle grains of the barium ferrite. Magnetic properties of the sintered core along the direction of the [0001] were as follows; (BH)_max=2.5 MGOe. B_r=3550 G and _BH_c=2600 Oe.
Excellent barium ferrite magnet was prepared in this way by means of a simple process and heat treatment in a lower temperature than was the case for the usual method.

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Methoxy-, methyl-, fluoro-, chloro-, and bromonaphthalenes were iodinated by using iodine-iodic acid, and the resulting iodo compounds were converted into the corresponding trifluoromethyl derivatives by treatment with trifluoromethyl iodide in the presence of copper powder. The iodination proceeded in the yield of 11-95%; the order of their reactivities was OCH₃> CH₃> F> Cl> Br, decreasing with less electron-donative effect of the substituent. The trifluoro-methylation reaction proceeded smoothly in the yield ranging from 72 to 81%, except for the bromoiodo compoud (1-bromo-4-iodo); besides which iodo (trifluoromethyl) naphthalene, his (trifluoromethyl)naphthalene, and bromo(trifluoromethyl)naphthalene were obtained.

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The reaction of o- and p-iodophenetoles [1] and [2] with an excess of 80-96% sulfuric acid at the temperatures of 20-100° C has been investigated. Both iodophenetoles readily underwent disproportionation, giving 2, 4-diiodophenetole [3] and a mixture of phenetolesulfonic acids and iodophenetolesulfonic acids. Dealkylation leading to the formation of diiodo- and triiodopheols[4]and[5]wasalsoobservedtosmallextentsinthesulfonationof[1]butalmostnotin, thecorrespondingreactionof[2].Interconvertionbetween[1]and[2]occurredslowlyevenin80%sulfuricacidat20-60°C, but, undertheseconditions, dispro-portionationscarcelytookplaceandtheyieldsofsulfonicacidswerequitesmall.SomephysicalPropertiesarereportedfornewamino, iodo, andnitroderivativesofphenetole-2-and4-sulfonicacids.

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Effects of reactant ratios and steam dilution on the formation of fluoroethylenes (chloro-trifluoroethylene, tetrafluoroethylene and 1, 2-dichloro-1, 2-difluoroethylene) by the copyrolysis of chlorodifluoromethane(R 22) and dichlorofluoromethane(R 21) have been investigated. A flow method in the tubular reactor was employed at 700° C under atmospheric pressure.
Formation of by-products other than the fluoroethylenes was inhibited by the presence of an excess of steam. The relative amount of the fluoroethylenes obtained agreed favorably with the values calculated by assuming the formation of the fluoroethylenes via a simple collision of: CF₂ and: CFC1 which would be formed by the pyrolysis of R 22 and R 21.

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Hydrolysis of (+)-8-hydroxy-1-p-menthen-9-yl acetate [ 2 ] which in turn was obtained from limonene [1] by oxidation with lead tetraacetate gave (+)-1-p-menthene-8, 9-diol [3]. Dehydration of [ 3 ] was improved to give (+)-1-p-menthen-9-al [ 4 ] in 64% yield by the use of potassium hydrogensulfate, thionyl chloride and oxalic acid as dehydrating agents. (+ )- 1, 8-p-Menthadien-9-ol [ 5] was obtained in a quantitative yield under another condition.

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The conductivity and stability of 7, 7, 8, 8-tetracyanoquinodimethane (TCNQ) salts consisting of polycations as shown in formulas ( I ) and (II) were measured. The resistivities of both TCNQ simple and complex salts are high, when the mole fraction of quarternized 4-vinylpyridine (x) is 0.04. However, the resistivities of simple and complex salts are 10⁸-10⁹ and 10⁴(Ω. cm), respectively, when x is larger than O.133. The conductivities agree with those of poly (1-methyl-4-vinilpyridinium)-TCNQ salts. The stability of TCNQ salts increased with decreasing x, which shows that the stability is influenced by the polycation structure. Thus, it is possible to improve the stability without decreasing the conductivity by introducing styrene or methylmethacrylate units.

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