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85 巻, 2 号
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永嶋 仁, 佐藤 重臣, 岡野 三治, 望月 正, 吉岡 豊, 田野 学1999 年 85 巻 2 号 p. 85-90
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーAn X-ray fluorescence method using a semiconductor X-ray detector was investigated for rapid analysis of slag in steelmaking process.
Metallic rectangular solid was dipt in molten slag layer, and slag thin piece grew on the solid. Because this slag piece was rapidly solidified and was flat, it could be directly analyzed by X-ray fluorescence method.
Slag thin pieces obtained by large volume steel sampler were excellent as uniformity and representativity of slag component. These features gave excellent result for the determination of CaO, SiO2, Al2O3, Fe and MnO in steelmaking slag. In this method, the analysis time was shortened to 5 minutes. As the results, rapid and simple analysis of slag for steelmaking was established.抄録全体を表示PDF形式でダウンロード (979K) -
鈴木 章悟, 岡田 往子, 平井 昭司1999 年 85 巻 2 号 p. 91-96
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーTrace elements in high purity iron certified reference materials, JSS001-4 and JSS003-4, prepared by the Iron and Steel Institute of Japan were determined by instrumental neutron activation analysis (INAA).
Five or seven aliquots of each sample (ca. 130750 mg) were irradiated for a short time (2 min) at a thermal neutron flux of 1.5×1012n cm-2 s-1 (pneumatic transfer) and for a long time (6 h) at a thermal neutron flux of 3.7×1012 n cm-2 s-1 (cental thimble) in the Rikkyo University Research Reactor. The irradiated samples were measured by conventional γ-ray spectrometry using a coaxial Ge detector, and by anticoincidence γ-ray spectrometry with a coaxial Ge detector and a well-type Nal(Tl) detector.
The concentrations of 7 elements (Na, Cl, V, Co, Zn, As, W) in the JSS001-4 and 1 1 elements (Na, Al, V. Mn, Co, Ni, Cu, As, Mo, Sb, W) in the JSS003-4 were determined by these methods. The determined values were in good agreement with the certified and reference values. The lower limit of determination values for Sm, Ir, Au in the J55003-4 were 0.11 ng/g.抄録全体を表示PDF形式でダウンロード (1004K) -
中原 武利, 李 一木, 竹内 啓貴, 二村 実1999 年 85 巻 2 号 p. 97-101
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーAn annular-shaped high power nitrogen microwave induced plasma (N2-MIP) produced at atmospheric pressure by an Okamoto cavity in a surface wave mode has been used as a new and efficient excitation source for atomic emission spectrometry (AES). The results show that this kind of MIP source is more stable than conventional low power MIPs and remarkably tolerant to direct and continuous introduction of wet aerosols and molecular gases such as hydrogen, oxygen, air and gaseous hydrides because of its high input microwave power. Under the optimized experimental conditions, the best attainable detection limits at As(I) 228.812 and Se(I) 196.026 nm by use of N2-MIP-AES coupled with hydride generation technique were 2.99 ng As/ml and 0.86 ng Se/ml with a linear dynamic ranges of 5 to 10, 000 ng As/ml and 1 to 5, 000 ng Se/ml. The presence of several diverse elements has been found to cause more or less a depressing interference with the determination of arsenic and selenium by the present technique. Of the several pre-reductants potassium iodide has been found to be the most preferable to reduce As(V) to As(III) prior to hydride generation for the determination of total arsenic, i.e., As(III)+As(V). To the contrary, the heating of sample solutions, previously acidified in 5 M with hydrochloric acid, at 80°C for 20 min was the best way to pre-reduce Se(VI) to Se(IV) before hydride generation for the determination of total selenium, i.e., Se(IV)+Se(VI). The proposed method was applied to the determination of low concentrations of arsenic and selenium in carbon steels and stainless steels, respectively. The results obtained by this method were in good agreement with the certified values.抄録全体を表示PDF形式でダウンロード (1221K) -
石橋 耀一, 三角 武, 磯部 健1999 年 85 巻 2 号 p. 102-107
発行日: 1999/02/01
公開日: 2010/01/18
ジャーナル フリー(1)鉄分離原子吸光法の分析精度は直接原子吸光法よりも大幅に向上した.定量下限が直接原子吸光法では30～100ppmであったが,除鉄原子吸光法を用いると今回検討した10種類の金属元素では10ppmの定量下限が得られた.
(2)従来JIS法などでは残さ処理には二硫酸カリウムを用いていたが,硫酸イオンは200～300nmに分子吸収による化学干渉があるため微量成分を定量する場合は問題があることが分かった.このため微量域の金属元素を原子吸光法で定量するための分析試料処理には硫酸系試薬の使用を行わない方法とし,不溶解残さはふっ化水素酸,過塩素酸で処理し最終試料溶液は塩酸酸性とした.
(3)測定時のマトリックスの影響を取り除くため4-メチル2-ペンタノンによる除鉄操作を行ったが,4-メチル2-ペンタノン抽出でも完全には鉄を除去できず極微量ではあるが鉄が残存する.したがって,検量線作成時にも鉄を共存させた状態で試料処理操作を行い,原子吸光法で測定する際の残存鉄量による干渉の影響の補正を行って,分析精度(正確度)の向上を図った.
(4)確立した方法によれば,同一試料溶液から10元素の定量が可能であり,多元素同時定量型原子吸光装置などを用いると多元素同時定量が可能である.
(5)著者等の検討結果の一部は鉄鉱石中ビスマス定量方法として改訂JIS法の中に取り込まれている.抄録全体を表示PDF形式でダウンロード (1223K) -
藤本 京子, 志村 眞, 吉岡 啓一1999 年 85 巻 2 号 p. 108-113
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーThe analytical methods for Zn compounds in the dust recovered from the electric furnace dust have been investigated.
The recovered dust contains metallic Zn, ZnO, ZnS and trace amount of Zn(OH)2 as Zn compounds. The sample was dissolved in the FeCl3-citric acid solution at room temperature. During the dissolution, metallic Zn reduced Fe(III) to Fe(II) quantitatively. The amount of Fe(II) was determined by the titration with potassium dichromate, and converted to the amount of metallic Zn. The ZnS contained in the residue was dissolved in HNO3 (1 + 1), and the amount of Zn as ZnS was determined by ICP-AES. The amount of ZnO and Zn(OH)2 was obtained by subtracting the amounts of metallic Zn and ZnS from the amount of total Zn.
The electric furnace dust contained ZnO and ZnFe2O4, and the FeCl3-citric acid solution was used for the separation of ZnO from ZnFe2O4. Only ZnO was dissolved in the FeCl3-citric acid solution, and ZnFe2O4 contained in the residue was determined by ICP-AES after alkali fusion and acid dissolution.抄録全体を表示PDF形式でダウンロード (1347K) -
藤本 京子, 志村 眞, 吉岡 啓一1999 年 85 巻 2 号 p. 114-118
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーA rapid and high sensitive analytical method for the trace amounts of boron in high-purity steel and silicon material has been investigated.
Steel sample was dissolved in HCl-HNO3 mixture, and boron nitride in the sample was decomposed completely by treatment of H2SO4 H3PO4 fuming at 290°C for over 30 min. After masking of Fe by the addition of CyDTA, the pH value of the sample solution was adjusted at 8 by aqueous ammonia. The sample solution was passed through the column of anion exchange resin (Amberlite® IRA-743), and B was adsorbed selectively as boric acid on the resin. After washing the column for the removal of Fe and H2SO4H3SO4, B was eluted by small amount of 2M HCl, and was determined by ICP-MS.
The limit of detection (estimated by the 3σ of blank values) was 0.016 μg/g for steel, and 0.006 μ/g for silicon material.抄録全体を表示PDF形式でダウンロード (1097K) -
小熊 幸一, 加藤 宏治, 倉島 義博, 関 達也, 小野 昭紘, 石橋 耀一1999 年 85 巻 2 号 p. 119-123
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーNovel two methods for determination of trace metals in steel have been developed by combining ion-exchange separation and atomic spectrometry. Sample is decomposed with hydrochloric acid and hydrogen peroxide. For the determination of Mo of 0.01 m/m % level, the sample is loaded as dilute sulfuric acid solution on a column of anion-exchanger TEVA resin. Iron ion passes through the column and Mo ion retained on the column is then recovered by elution with nitric acid, followed by quantification by inductively coupled plasma atomic emission spectrometry (ICP-AES). For the simultaneous determination of Al, Mn, Ni and Co of 0.001 to 0.1 m/m % level, the sample is loaded as hydrochloric acid-oxalic acid-hydrogen peroxide solution on a cation-exchange resin Bio-Rad AG 50W column. Iron ion passes the column as oxalato-complexes, and Al, Mn, Ni and Co ions retained on the column are eluted with hydrochloric acid to be subjected to the simultaneous determination by ICP-AES (for metals of 0.01 to 0.1 m/m % level) or "one drop" flame atomic absorption spectrometry (for metals of 0.001 m/m level). The analytical results obtained for the steel certified reference materials are in good agreement with certified values and the precision (R.S.D.=1 to 8%) is satisfactory.抄録全体を表示PDF形式でダウンロード (1121K) -
小林 剛, 長谷川 信一, 吉岡 孝之1999 年 85 巻 2 号 p. 124-128
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーGraphite furnace atomic absorption spectrometry (GF-AAS) has been applied to the determination of trace amounts of arsenic, bismuth, cadmium, lead, thallium and zinc in the acidic solutions of iron and steels. The iron and steels were dissolved in nitric acid. After the solution (20 μl) was pipette into a L'vov platform furnace, it was ashed (600°C-30 s, hydrogen 5 ml/s) and then atomized by using argon as a purge gas and atomic absorption of each analyte was measured. The effect of iron concentration was suppressed by the use of peak area measurement. Synthetic calibration solutions were prepared by addition of standard solution of each analyte to iron or nickel matrix solution. For arsenic, bismuth, cadmium, lead, thallium and zinc, the limits of detection (3σ of blank values) were 0.05, 0.025, 0.002, 0.017, 0.025 and 0.003 ppm, respectively, when one gram of the specimen was used. The proposed method is able to be applied to other analyte in iron and steels.抄録全体を表示PDF形式でダウンロード (1163K) -
田中 龍彦, 佐藤 亨, 石山 高1999 年 85 巻 2 号 p. 129-134
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーA simple, rapid and reproducible method is described for the direct determination of arsenic at the, μg/g level in iron and steel based on differential pulse anodic stripping voltammetry without any separation of iron matrix. Electroinactive arsenic(V) was chemically reduced to arsenic(III) by potassium iodide prior to the stripping voltammetric determination. The interference of iron(III) was eliminated by reducing it with potassium iodide to iron(II). The generated iodine was reduced with L(+)-ascorbic acid. Arsenic(III) was electrodeposited from a 3 ml aliquot of the acid solution (0.3M HCl-0.1M HNO3-0.15M Kl-0.1M L(+)-ascorbic acid, pH=ca 0.1) containing 3 mg of a sample on a rotating gold-film electrode (gold plated on glassy carbon) at -0.5 V vs. SCE for 180 s. The deposit was then anodically stripped at a scan rate of 40 mV/s to +0.2 V vs SCE.
The calibration graph (peak height vs. concentration curve) prepared with standard arsenic solutions was linear in the range from 10 ng/ml to at least 40 ng/ml of arsenic and passed through the origin (correlation coefficient >0.998), with a sensitivity of ca. 0.2 μA/(ngAs/ml). Antimony(III), bismuth(III) and copper(II) interfered with the arsenic determination severely. The proposed method has been successfully applied to the determination of 50.4 and 448.8 μg/g of arsenic in iron and steel, with relative standard deviations of less than 2.4% (n=5), without any troublesome preconcentration steps using harmful chemicals. For a deposition time of 180 s, about 80% of arsenic(III) was accumulated and the detection limit (3 σ) was 1.0 μ/g. The time required for an analysis was within 40 min.抄録全体を表示PDF形式でダウンロード (1038K) -
今北 毅, 小縄 幸司, 中原 武利1999 年 85 巻 2 号 p. 135-137
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーFluoride separation-molybdosilicic acid blue spectrophotometry was applied to the determination of trace amounts of silicon in niobium and tantalum samples. After the sample was dissolved in hydrofluoric acid and nitric acid, the silicon was evolved by heating to 300°C in the presence of sulfuric acid. The liberated silicon tetra-fluoride was absorbed into the solution containing boric acid by sucking the evolved gas at a flow rate of 300 ml/min. Then the silicon in the absorbent was determined by Molybdenum Blue spectrophotometry. By this method, silicon at ppm level in commercially available metals was successfully determined. Recovery was 105% for niobium sample and the detection limit given by 3σ of blank value was 0.6ppm silicon in the metal sample.抄録全体を表示PDF形式でダウンロード (526K) -
安原 久雄, 志村 眞, 吉岡 啓一1999 年 85 巻 2 号 p. 138-142
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーRemoving the oxide film from the sample surface is an important process for analyzing trace oxygen in iron and steel.
The depth profiles of oxygen on the surface after electro-polishing in CH3COOH-HClO4, CrO3-H3PO4, and chemical polishing by HF-H2O2 were investigated.
As for the high-purity iron, thickness of the oxide layer after electro-polishing in CrO3-H3PO4was thicker than any other pretreatment methods. This is because Fe(III) hydroxide was formed on the surface of sample. This could be removed by rinsing with an acid after electropolishing.
As for the bearing steel, oxygen containing species were found around carbides on the surface of the sample after pretreatment except that the pretreatment was made by electro-polishing in CrO3-H3PO4. Those precipitates influenced the analysis of oxygen.
Analytical value obtained by conventional methods were 1 or 2 mass ppm higher than those obtained by charged particle activation analysis that is not influenced by surface contamination. This difference corresponds to the oxide layer formed on the sample surface.抄録全体を表示PDF形式でダウンロード (3153K) -
古主 泰子, 増田 正純1999 年 85 巻 2 号 p. 143-148
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリー100nm程度の多層酸化皮膜の成長挙動の解明のため,各種分光法による構造解析と,厚みおよび深さ方向の組成分析の組合わせを提案し,ラマン散乱分光法とGDSの併用法を用いて解析した.
(1)SUS304冷延板の短時間加熱時に生成する薄い酸化皮膜も長時間のものと同様に,スピネルとコランダムからなる.
(2)スピネルとコランダムの膜厚を推定し,その成長速度を求めた.
(3)スピネルよりコランダムの成長速度が温度依存性が大きい.
(4)スピネル成長速度は高Mnの方が大きく,コランダムの成長速度は逆に小さい.
(5)コランダムの成長速度の温度依存性は高Mnの方が大きい.抄録全体を表示PDF形式でダウンロード (4920K) -
槇石 規子, 山本 公, 吉岡 啓一1999 年 85 巻 2 号 p. 149-154
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーThe influence of backscattered electrons on the spatial resolution was investigated in the analysis of Auger electron spectroscopy. The size of the generation area of Auger electrons caused by backscattered electron generation was evaluated for Au/SiO2/Si and Ni/Fe specimens by measuring the line profile of O KLL and Ni LMM, respectively. It was shown that the size of the generation area, measured as the spread till the intensity becomes 5% of its maximum intensity, increased with accelerating voltage and exceeded 1 μ for the accelerating voltage of 20 kV. Cosequently, the accelerating voltage should be less than 5 kV for the sub-micron analysis. The sizes of the generation area were in good agreement with the values calculated from the theoretical equation proposed by Soejima. The quantitative analysis of carbon and boron in a borocarbide precipitate in steel was done under the analytical conditions determined for sub-micron analysis. The analytical errors were less than 3 atomic % when the relative sensitivity factors for carbon and boron obtained experimentally from Fe3C and Fe2B precipitates were used, respectively. On the other hands, when the relative sensitivity factors obtained from pure materials were used, the analytical accuracy was poor because of the influence of the change of spectrum shape due to the difference of chemical state.抄録全体を表示PDF形式でダウンロード (5506K) -
石黒 三岐雄, 高 世〓, 高田 九二雄, 花田 修治1999 年 85 巻 2 号 p. 155-159
発行日: 1999/02/01
公開日: 2010/01/19
ジャーナル フリーA method for separation and determination of TiC in in-situ TiC particle reinforced Fe3Al based alloys has been investigated. The results obtained are summarized as follows:
(1) When samples were dissolved in a 6N hydrochloric acid at 6080°C, TiC remained as a residue. TiC was separated from the acid solution by filtration.
Amount and composition of separated TiC could be determined quantitatively.
(2) Fe, Al and Cr in samples were detected as soluble elements in an acidic solution, while Ti was found in the insoluble residue (TiC). Mo was detected in both the acidic solution and insoluble residue.
(3) Two types of TiC particles were observed. Large ones with sizes of about 530 μ m have well developed facet structure, while small ones less than 1 μm in diameter have dendritic structure.
(4) Separation procedure along with the particle size was examined. Large particles were sedimented but small particles were dispersed in acetone, so they were able to be separated by filtration. Both large and small particles in samples are identified to TiC independent of the particle size.抄録全体を表示PDF形式でダウンロード (6541K) -
安原 久雄, 志村 眞, 鍋島 誠司1999 年 85 巻 2 号 p. 160-163
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーThe measurement of the particle size distribution of oxides in high carbon Si-Mn killed steel was achieved by extraction of oxides and the measurement with laser diffraction particle size analyzer.
The extraction method of oxide in steel by using nitric acid could not be applied to the present case because nitric acid decomposed the SiO2 formed in steel. On the other hand, bromine-methanol method was suitable for the extraction of these oxide. Otherwise, the dissolving reaction was disturbed because of high carbon content. Decarbonization of the samples in H2H2O atmosphere was found to be effective as a pretreatment of the bromine-methanol extraction in order to avoid the disturbance in the extraction procedure for high carbon content steel.
The bromine-methanol extracts the free carbon as well as the desired oxides. But the KMnO4 treatment with citric acid could dissolve only free carbon, and the oxides could be separated.
It was found that the amount of oxides at the surface area of bloom was greater than that at central area of bloom in case of both fine particle size of the oxides and large particle size of the oxides.抄録全体を表示PDF形式でダウンロード (5425K) -
河合 潤, 高橋 秀之, 林 好一, 岡崎 真也, 粟倉 泰弘1999 年 85 巻 2 号 p. 164-168
発行日: 1999/02/01
公開日: 2010/01/18
ジャーナル フリー電子プローブX線マイクロアナライザーや蛍光X線分光分析装置で,シンクロトロン放射光を用いるのと同様なX線吸収スベクトルの測定可能なことを,Mgの金属および酸化物について示した.今回の実験に用いたものと同じ使い方ができる電子プローブX線マイクロアナライザーや蛍光X線分光分析装置は,波長分散型といわれるものであるが,日本国内で数千台が現に使用されている.シンクロトロン放射光は,迅速で質の良いスペクトルが測定可能であるが,ビームタイムが限られており,また分析が必要な現場からは遠方にある.今回40μmφの局所のMgOのX線吸収スペクトルを150分で測定することができた.このような測定は,金属材料中の軽元素介在物の化学状態分析に応用可能と考えられる.介在物内ではMg,Al,Si等軽元素濃度が高いので,電子ビームを絞ることにより,S/Nの良いスペクトルが測定可能となるであろう.シンクロトロン放射光は,コスト的にも利便性の点でも,現時点では実用分析用にはほど遠いが,本報告のEPMAを用いたEXAFS法を用いればX線吸収分光実験がより一般化すると期待できる.
高エネルギー加速器研究機構物質構造科学研究所放射光研究施設北島義典氏にはシンクロトロン放射光によりMg化合物のXANESスペクトルを測定していただきました.抄録全体を表示PDF形式でダウンロード (995K) -
木村 正雄, 今福 宗行, 黒崎 将夫, 藤井 史朗, 森本 康秀1999 年 85 巻 2 号 p. 169-173
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーA new system has been developed for in situ obsevation of phase transformation at high temperatures. Changes in powder diffraction patterns from a heated specimen can be measured continuously by scanning an image plate located behind a slit. A heating system is designed for a sheet specimen (ca. 5×6 mm2) using Joule-heating, and it can heat the specimen up to 1100K at a rate up to 160K/sec, where effects of thermal expansion are minimized by a mechanism releasing stress.
This system was applied to Zn-coated steel. At temperatures higher than the melting point of Zn, different types of Fe-Zn intermetallics formed sequentially through rapid inter-diffusion. Changes in phase and crystallographic structure were monitored with a time resolution less than a few seconds. It has been found that an addition of a small amount of elements, such as P, into Fe changes an incubation time before the alloying reaction starts. This system has been shown to have the potential for application to in situ observation of other reactions at high temperatures.抄録全体を表示PDF形式でダウンロード (7787K) -
谷口 政行, 源内 規夫, 今北 毅1999 年 85 巻 2 号 p. 174-179
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーA new method for the observation of the macroscopic distribution images of light elements in metals by the charged particle activation-au-toradiography was developed by the use of the highly sensitive imaging plate (IP) instead of the conventional X-ray film.
Surfaces of metallic samples (max. size: about 120 mm×120 mm×5 mm) were irradiated by the 3He ion beam of cyclotron, and then were kept in contact with the IP's for appropriate exposure times. Light elements such as B, C and O were activated in higher yields compared with other coexistent elements and the macroscopic two dimensional distribution images of radionuclides produced from those elements (e.g.: 11C from B or C and 18F from O) were obtained by the above-mentioned IP-autoradiography.
The method developed was applied to observe the distribution images of C and O in steels and B and 0 in Al alloys. The results obtained were consistent with the results by chemical analysis. The method was considered to be useful especially for the evaluation of macroscopic defects in metallic materials such as segregations, inclusions or surface contaminations.抄録全体を表示PDF形式でダウンロード (9226K) -
今福 宗行, 黒崎 将夫, 川崎 宏一1999 年 85 巻 2 号 p. 180-183
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーIn order to study the dynamic phenomena of electrodeposition of metallic layers, we have newly developed in-situ X-ray diffraction system using an electrochemical cell and an image-plate detector. Electrodepositions of zinc layers on iron (100), (111) single crystals with current densities of 1.0×103 to 1.0×104 A/m2 were demonstrated. It was found that there were two stages for the preferred orientation of zinc layers. It was dominated by the crystallographic orientation of substrate material at the initial stage and the current density (i.e. overvoltage) at the next stage.抄録全体を表示PDF形式でダウンロード (2519K) -
今福 宗行1999 年 85 巻 2 号 p. 184-188
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーTexture mapping apparatus with energy dispersive X-ray diffraction method has been newly developed. A collimated white X-ray beam in the diameter of 0.1 to 2.0 mmφ was irradiated to a sample in a fixed incidence and the energy spectrum of diffracted X-ray was measured by solid state detector. In this apparatus, fast data transfer system from multi-channel analyzer to computer was adopted to reduce the total measuring time. Sample was mounted on X-Y stage and moved successively to obtain the intensity mapping of diffraction peaks. Some examples are demonstrated in order to show the performance of this apparatus. It is suitable for the analysis of local inhomogeneities of texture, such as colonies of grains in polycrystalline materials.抄録全体を表示PDF形式でダウンロード (9166K) -
藤岡 裕二1999 年 85 巻 2 号 p. 189-194
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーA new characterization method of skeletal structure for polycyclic aromatic hydrocarbons (PAHs) has been studied by the soft ionization mass spectrum. The soft ionization, such as field desorption (FD), mass spectrum gives molecular weights of PAHs in coal tars and pitches. PAL-Is are classified into two types skeletal structure groups. Type-I is the highest H/C group based on kata-type condensation. Type-II is the lowest H/C group based on pen-type condensation. The general rational formula of each structures are C4nr+2H2nr+4 (Type-I) and C6nr2H6nr (Type-II). In addition, relation between number of aromatic rings (Ra) and molecular weight (Mw), H/C atom ratio and Ra, H/C and Mw are expressed as follows. Ra and Mw Type-I: Ra=(Mw-28)/50, Type-II: Ra={4Mw-13(8Mw+1)1/2+109}/96. H/C and Ra, Type-I: H/C=(Ra+2)/(2Ra+1), Type-II: H/C=6/[{3(4Ra-1)}1/2+3]. H/C and Mw, Type-I: H/C=(Mw+72)/(2Mw-6), Type-II: H/C=24/{(8Mw+1)1/2-1}.
Coal tar pitch soluble in toluene and carbon black soluble in acetone are characterized by this method. The average molecular weight of the coal tar pitch soluble in toluene by the field desorption mass spectrum is higher than the carbon black soluble in acetone. But classified molecular ion peaks according to number of aromatic rings, carbon contents of each components of the coal tar pitch soluble in toluene are lower than the carbon black soluble in acetone. This example of the application disclose usefulness of the method for the characterization of polycyclic aromatic hydrocarbons in coal tars and pitches.抄録全体を表示PDF形式でダウンロード (1021K) -
齋藤 公児, 畠山 盛明, 松浦 慎, 加藤 健次, 古牧 育男1999 年 85 巻 2 号 p. 195-200
発行日: 1999/02/01
公開日: 2009/06/19
ジャーナル フリーA new carbonization process with high temperature preheating has been studied. A mechanism which improve the coking property was examined with coal properties by Solid State NMR and NMR imaging methods. It has been clarified that the molecular structure of coal has been relaxed by the rapid heating treatment and addition there is a close relation in hydrogen bond and relaxation of molecular structure of coal. Furthermore, the specimen of coal show the increase of mobile component by the rapid heat treatment using NMR micro imaging.抄録全体を表示PDF形式でダウンロード (5060K)
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