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Volume 37, Issue 11
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Yoshimi KITADA, Michiko SASAKI, Yutaka YAMAZOE, Yumie MAEDA, Masatoshi ...1988 Volume 37 Issue 11 Pages 561-565
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and rapid method for the determination of 8 water soluble vitamins, sodium benzoate and caffeine in beverages was developed by means of HPLC. Nicotinic acid, nicotinamide, calcium pantothenate, thiamine hydrochloride, riboflavine 5'-phosphate sodium, riboflavine, pyridoxine hydrochloride, cyanocobalamine, sodium benzoate and caffeine were separated on a Nucleosil 7C18 column (4.6 mm i.d. × 25 cm) by using acetonitrile-water-triethylamine (9 + 90.5 + 0.5 v/v) solution containing 5 mM sodium heptanesulfonate (pH 2.8 adjusted with phosphoric acid), and detected at 210 nm with 0.05AUFS. One ml of sample was added 2 ml of 100μg/ml acetanilide solution as an internal standard and diluted to 10 ml with the mobile phase. The relative standard deviations of reproducibility of 10 compounds at the level of 60600 μg/ml were less than 2.5%.View full abstractDownload PDF (645K) -
Kozo HIKIDA, Nobuchika ISHII, Yoshimasa INOUE, Yosuke OHKURA1988 Volume 37 Issue 11 Pages 566-569
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn automated method for the determination of ampicillin in serum was developed by means of columnswitching HPLC with UV detection (235 nm). The TSK precolumn BSA-ODS and Ultra-sphere ODS are used in the sample preparation column and analytical column, respectively. Serum samples (20μl) are directly applied onto the sample preparation column. The recovery of ampicillin from human serum is complete (approximately 100%) with good reproducibility (R.S.D., less than 2%). This method can be successfully used for the determination of ampicillin in sera from humans and dogs receiving oral doses of bacampicillin preparations.View full abstractDownload PDF (510K) -
Shizuho NODA, Hiroko KANAI, Toshiyuki OSHIMA, Kazuhiko SAGARA, Tsuguch ...1988 Volume 37 Issue 11 Pages 570-574
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn HPLC for the determination of lysozyme in pharmaceutical preparations was studied. A reversed-phase chromatographic system consisting of an ODS column and a linear gradient elution system (1%/min) of 10% acetonitrile solution containing 0.1 % trifluoroacetic acid (TFA) and 50% acetonitrile solution containing 0.1% TFA was used. By the HPLC method, a good peak pattern and linearity in calibration curves were obtained. In addition, good consistency between the official assay method and HPLC was obtained in the analysis of the lysozymes denatured by heat and pepsin. Therefore, the HPLC method seems to be suitable for routine analysis in quality control of lysozyme in pharmaceutical preparations.View full abstractDownload PDF (639K) -
Yuji ITO, Kazuyoshi YOSHIDA, Mitsuichi HANDA, Nobuo YUNOKI, Tsuguchika ...1988 Volume 37 Issue 11 Pages 575-579
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSStandardization of analytical procedures for OTC (over-the-counter) drugs using reversed-phase HPLC was studied in order to improve the efficiency of quality control. As commercial ODS packings have pronounced differences in elution behavior among manufacturers and among lots, the standard test method for obtaining a packing material having a constant elution behavior was established by testing the elution behavior of ingredients involved in anti-cold drugs. Then, extraction conditions for the simultaneous determination of anti-cold drugs were investigated. As a result, good recoveries were obtained by using a methanol-water-phosphoric acid mixture (700 : 300 : 1) as the extraction solvent and ultrasonication. HPLC conditions for determining the active ingredients in anti-cold drugs, antipyretic analgesics, vitamin preparations and antivertigo drugs were as follows : 1 : a mixture of acetonitrile-water-phosphoric acid (510 : 490 : 1) containing 0.5% SDS, 2 : a mixture of water-acetonitrile-50 mM TBA (pH 6) (17 : 2 : 1), 3 : a mixture of water-acetonitrile-phosphoric acid (700 : 300 : 1) containing 0.5% SDS. Analytical results under the above mentioned extraction and HPLC conditions, showed good recovery and reproducibility. The efficiency of quality control was improved by this procedure.View full abstractDownload PDF (559K) -
Masakazu HORIE, Kouichi SAITO, Youji HOSHINO, Norihide NOSE, Yasuo SHI ...1988 Volume 37 Issue 11 Pages 580-584
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and rapid method for the determination of components of spiramycin in phamaceutical preparations has been developed by HPLC. Spiramycin, a member of the macrolide group of antibiotics, consists of a mixture of three major components such as spiramycin I (SPM-I), spiramycin II (SPM-II) and spiramycin III (SPM-III) and three minor components such as neospiramycin I (NSPM-I), neospiramycin II (NSPM-II) and neospiramycin III (NSPM-III). The SPM-I, SPM-II and SPM-III were purified from the pharmaceutical preparations by using preparative HPLC. The NSPM-I, MSPM-II and MSPM-III were obtained by acidic treatment of the corresponding purified SPM-I, SPM-II and SPM-III, respectively. These purified components were confirmed with secondary ion mass spectorometry. The HPLC separation was carried out on a Chemcosorb 5-ODS-H column (25 cm×4.6 mm i.d.) using 0.05 M sodium dihydrogenphosphate (pH 2.5)-acetonitrile(73 : 27) as the mobile phase with a flow rate of 0.5 ml per minute, and detected at 232 nm with 0.08 AUFS. The content of SPM-I in the pharmaceutical preparations by the presented method was about 70%.View full abstractDownload PDF (645K) -
Tsuneo KAWAMURA1988 Volume 37 Issue 11 Pages 585-588
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method has been established for the determination of ppb levels of U and Th in Mo by ICP-MS. The detection limits (3σ) for U and Th in 1 M nitric acid solution were 0.006 ng/ml and 0.009 ng/ml, respectively. Signal suppression of both elements was observed with solutions containing more than 0.1 mg/ml of Mo. The effect became more marked as the Mo concentration increased. So, an ion-exchange technique was applied for the separation of the analytes from Mo matrix. A sample was dissolved with aqua regia, evaporated to dryness and dissolved in a mixed acid solution (1 M HF-0.5 M HCl). The solution was passed through an anion exchange column. The effluent was evaporated to dryness, dissolved in 1 M nitric acid and analyzed by ICP-MS. The recoveries of U and Th were more than 90%. The method was applieds to the determination of U and Th in high purity Mo metals. At the 1 ppb level, the relative standard deviations of the U and Th determinations were 25 and 19%, respectively.View full abstractDownload PDF (536K) -
Kazukiyo SUGIMOTO, Takanori AKIYOSHI, Takaaki KONDOU1988 Volume 37 Issue 11 Pages 589-594
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSQuick determination of carbon in pig iron is required to control carbon concentration in pig iron and steel. The X-ray intensity of carbon is affected by the sample structure. This reproducibility of carbon analysis is better for white pig iron than for gray pig iron. Therefore, good samples of white pig iron for reference materials were obtained using a high frequencies induction melting-centrifugal casting machine. A new disk sampler for routine analysis was developed. Factors of analytical error by XRF are: (1) contamination of the vacuum chamber by oil from the vacuum pump, (2) degree of evacuation, (3) temperature of the sample, (4) sample preparation (polishing and cleaning). The reproducibility of carbon analysis by XRF was 0.050% (σM), and accuracy was 0.083% (σd) for 3.54.7% concentration range.View full abstractDownload PDF (5165K) -
XRF determination of major elements in rocks using glass bead method with synthetic standard samplesAkira YOSHIOKA, Takao SEKINE, Hidemistu YOSHIDA, Koichi NOMURA1988 Volume 37 Issue 11 Pages 595-600
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and rapid method for the determination of major elements in rocks by XRF using the glass bead technique has been investigated. Calibration curves were made by using synthetic standard glass bead samples. The preparation of the synthetic standard samples was as follows. High-purity compounds containing desired concentrations of elements were mixed well and then heated at 1000°C in air. A sample (0.500 g) was fused with Li2B4O7 (5.500 g) in a Pt-5% Au crucible at 1100 °C for 3 min. A small amount of monobromtrifluoromethane gas (CBrF3) was sprayed on the melt to remove air bubbles and to allow the melt to be removed readily from the crucible. The synthetic standard glass bead smples had a good reproducibility and linear calibration curves were obtained without matrix correction. The proposed method was applied to the determination of Si, Ti, Al, Fe, Mn, Mg, Ca, Na, K and P in various rock samples. The analytical results of rock standard samples showed good agreement with the recommended values.View full abstractDownload PDF (792K) -
Akira NARUKAWA, Isao ODA1988 Volume 37 Issue 11 Pages 601-606
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA computer controlled automatic sample preparation and analysis system for laboratory automation is described. The system is based on XRF analysis with grinding and pressing techniques. The apparatus consists of the weigher, disc mill, press, conveyers, simultaneous XRF spectrometer, ignition loss determinator and realtime computer. The consecutive analysis of various kinds of materials differing in chemical composition has been achieved by this system without any contamination. In automatic analysis of raw materials, raw mixtures and ceramics, the system has provided precise and accurate analytical results. The relative standard deviation was ±0.15% for major elements and ±0.5% for minor elements.View full abstractDownload PDF (913K) -
Kazumi MIZUKAMI, Shigeo KASAI, Naoki KASAI, Kazuhiko AMAKAWA1988 Volume 37 Issue 11 Pages 607-611
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIt is important to analyze the chemical composition of iron ore sinter, rapidly and accurately, for stable operation of the blast furnace. In this report, the effect of the magnesioferrite state of sinter on XRF analysis (briqutte sample use) and its relation to raw material particle size and sintering process were described. Sinter samples (fine samples) which contained fine serpentine (dominent MgO source) produced relatively lower intensities of magnesium-characteristic X-rays than those containing coarse serpentine. In order to clarify this problems, the analytical data obtained by wet chemical and XRF analysis were compared, size distribution was examined and state analysis of the magnesium oxide compound was performed. Electron probe micro analysis (EPMA) made it clear that the fine samples contained much more magnesioferrite than coarse samples and the difference in the quantity of magnesioferrite affected the intensities of magnesium-characteristic X-rays. The glass beasd sample preparation method was applied to the XRF analysis in order to solve this problem and good agreement between the wet chemical analysis and the XRF analysis was obtained.View full abstractDownload PDF (746K) -
Tadayosi YOSHIMURA1988 Volume 37 Issue 11 Pages 612-618
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAutomated odor-sensing system based on plural semiconductor gas sensors and computerized pattern recognition techniques has been developed. Odor signals are detected by using eight TGS sensors which have different sensing properties for gases. But, there are control points of interest such as the signal acquisitions, the air steady level and heater voltages of TGS sensors. These problems have been solved by the use of air brush and computerized techniques.View full abstractDownload PDF (734K) -
Yuji FUJIOKA, Keiichi TANIKAWA1988 Volume 37 Issue 11 Pages 619-622
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAdditives in cold rolling oils were analyzed by HPLC using an infrared detector (IRD). Animal and vegetable oils, synthetic esters, fatty acids and other compounds are added to cold rolling oils to improve their lubricity. These components can not be monitored by an UV detector because of their low sensitivity compared with that of the mineral oil and are also difficult to determine accurately by a differential refractive index detector due to interference by the mineral oil. The IRD can selectively detect the additive components in samples and five components were successfully determined in cold rolling oils in a short time with this method. The HPLC-IRD method was found to be capable of analyzing the oil deposits left on the surface of cold strip after rolling because of its high sensitivity. The values obtained closely reflected the correlative changes in the chemical composition of the rolling oil bath. The HPLC-IRD method is rapid and simple, and is considered to be fully applicable to the process control of rolling oils.View full abstractDownload PDF (588K) -
Hirofumi KURAYASU, Yasuo INOKUMA1988 Volume 37 Issue 11 Pages 623-627
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDifferential pulse anodic stripping voltammetry (DPASV) was applied to the determination of 0.12 mg/l of Tl, Pb, Cd, In, Sn, Cu, Bi and Sb in zinc plating solution. Tl gave a DPASV peak without interference in the solution containing Pb, Cd, In and Sn with added EDTA. After the oxidation of Sn(II) to Sn (IV) by H2O2, Pb and Cd gave DPASV peaks in the solution containing H3PO4 which masked In and Sn. If the sample contained Tl, peak heights of Pb and Cd were corrected by subtracting the overlap of the Tl peak. Indium gave a DPASV peak in the solution containing HCl. If the sample contained Tl or Cd, the peak height of In was corrected by subtracting the overlap of the respective Tl or Cd peak. After the oxidation of Sn(II) to Sn(IV) by H2O2, Sn gave a DPASV peak in the solution containing HCl. If the sample contained Tl or Pb, the peak height of Sn was corrected by subtracting the overlap of the Tl or Pb peak. After the oxidation of Sb(III) to Sb(V) by H2O2, Cu and Bi gave DPASV peaks. After the reduction of Sb(V) to Sb(III) by ascorbic acid, Sb gave a DPASV peak in the solution containing Cl-. If the sample contained Bi, the peak height of Sb was corrected by subtracting the overlap of the Bi peak. An automatical on-line voltammetric analyzer was developed for process control. The analyzer was able to determine Pb, Cd and Cu in plating electrolytes and Ni in the wash water of the plating bath with a 3% relative standard diviation.View full abstractDownload PDF (675K) -
Izumi KUBO, ISAO KARUBE1988 Volume 37 Issue 11 Pages 628-632
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA microbial alcohol sensor consisting of immobilized trichosporon brassicae and a dissolved oxygen electrode For fermentation process control was developed. This sensor coupled with a membrane sampler was applied to the fermentation process and on line monitoring of ethanol was performed selectively and precisely. The sensor gave a linear response in the 245 mM range and was reusable 1200 times. The microbial ammonia sensor consists of immobilized nitrifying bacteria, a gas permeable membrane and an oxygen electrode. At pH 10 a linear lerationship was observed between the response of the sensor and the concentration of ammonia in the range of 0.11.2 mM. The sensor was applied to waste water monitoring.View full abstractDownload PDF (488K) -
Noriko KATORI, Nobuo AOYAGI, Yasushi TAKEDA1988 Volume 37 Issue 11 Pages 633-635
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA laboratory robot system was applied to content uniformity test and weight variance test of several commercial sugar coated tablets containing 50 mg of ajmaline. The system was composed of robot, balance, stirrer, ultrasonic washer, pipetting module and HPLC system. HPLC was used for determining ajmaline in the tablets and R.S.D.(relative standard deviation) was 0.18%. The system showed good precision; the R.S.D. of weighing tablets was 0.2% and that of dispensing 0.5 and 1.0 ml of water was 0.4 and 0.1%. All samples passed the content uniformity criteria for the Japanese pharmacopoeia, and the variability of the ajmaline contents was from 1.24 to 4.28% of R.S.D. and that of the weights was from 1.30 to 6.05%. In conclusion, the system showed good suitability for these tests.View full abstractDownload PDF (391K) -
Mitsuhiro YAMAZAKI, Hiroshi MIYAZAKI, Soei SATO1988 Volume 37 Issue 11 Pages T121-T127
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTo establish the suitable conditions for separating sugars in prepared foods, their separation behavior on TLC was examined. The relationship between the Rf values and the type of sugars (difference in molecular weight and chemical structure) was also discussed. Sugars used in this experiment are various sugars of about 30 kinds such as mono, di and tri saccharides, glucose oligomers (linear type and cyclic type), sugar alcohols, acidic sugars, amino sugars and glycosides. Good separation of these sugars was achieved by using suitable solvent systems according to the composition of sugars, as follows: (1) for the separation of samples containing mono-, di-and tri-saccharides, and glycosides, CHCl3-CH3OH-H2O (30 : 20 : 4 v/v); (2) for the mutual separation of glucose and fructose, CHCl3-CH3OH-H2O (30:15:3 v/v) ; (3) for the separation of oligosaccharides, iso-C3H7OH-CH3COOH-H2O (4 : 1 : 1 v/v); (4) for the separation of samples containing acidic sugars, sugar alcohols and amino sugars, n-C4H9OH-CH3COOH-H2O (8: 3: 2 v/v). On the other hand, when several sugars were positioned close together, the color development of the spot could be also used for identification. This chromatographic method was applied to the separation and identification of mono-, di-, tri-and oligosaccharides in the prepared foods such as milk preparations and alimentary foods containing various sugars with good results.View full abstractDownload PDF (781K) -
(I) Rapid assay of cefaclor in mixed powdersHiroshi OYA, Masumi NAGAI, Minoru SAWADA, Yoshikiyo KANAYA1988 Volume 37 Issue 11 Pages T128-T132
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid, assay method for process control of cefaclor capsule manufacturing was established by application of near-infrared spectrophotometry to determination of cefaclor. Procedure is as follows: Second derivatives of absorbances, d2A at 1140 nm and 1198 nm are obtained by the irradiation of near-infrared beams (1100 2500 nm) to a sample. Absorbance A is the negative logarithm to the base 10 of the reflectance. The wavelength at which concentration of cefaclor has linear relationship to d2A is not 1198 nm, but 1140 nm. The former is useful to monitor any disturbance of d2A caused by different particle sizes of cefaclor. Determination of cefaclor is given by Cefaclor (%) = a + b[d2A (1140 nm)/d2A (1198 nm)], in which a, b are parameter estimated by least square method. The accuracy was 99101% and the repeatability was 0.3% (n=6). The time expended on assay was 2 min per 1 sample.View full abstractDownload PDF (461K) -
Harumi NIMBE, Masao KUROSAKI, Sigeo KASAI1988 Volume 37 Issue 11 Pages T133-T137
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSRecently, there is a graet demand for rapid analysis of molten steel in order to control the dynamic steel refining process. For this purpose, an on-site type emission spectrometer with some modification was installed in a control room at a production site. The use of a disk-type sampler and a milling-cut sample preparation made it possible to reduce analysis time. A high energy pre-spark discharge was adopted to avoid the effects of heterogeneous structure of the sample. The total analysis time was reduced to 150 s from 370 s and the precision was almost the same as that of the conventional emission spectrometry.View full abstractDownload PDF (588K) -
Kunio SHIRATORI, Norio SHIRATA, Akio TANAKA, Kengo SENOO1988 Volume 37 Issue 11 Pages T138-T141
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA computer data processed spectrophotometric analyser has been developed for determination of small amounts of phosphorus (less than 100 ppm) in steel samples. The analyser performs automatically and continuously all the photometric procedures after sample preparation by acid dissolution. The spectrophotometric absorbances are automatically measured and are corrected by smoothing drift, discard of abnormal signal by Grubbs and Dixon verification using a data processing computer system. Certificated steel samples containing 2 ppm and 11 ppm of phosphorus were determined for 6 min with a relative standard deviation of 9% and 2%, respectivelyView full abstractDownload PDF (490K) -
Akihiro ONO, Masahiro MIDORIKAWA1988 Volume 37 Issue 11 Pages T142-T147
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIt is important to control the concentration of Fe(II) and Fe(III) ions in galvanizing solution for process control of Zn-Fe alloy electroplating. On-line titrimetric determination system of Fe(II) and Fe(III) ions has been developed. Fe(II) (76 g dm-3) was determined by KMnO4 titrimetric method in 120 s for a single measurement with 0.7% R.S.D. (relative standard deviation). Fe(III) (13 g dm-3) was determined by TiCl3 titrimetric method in 90 s for a single measurement with 0.5% R.S.D. Interference by Zn(II), H2SO4, citric acid, SrCO3 powder were not significant in the proposed method.View full abstractDownload PDF (915K) -
Takashi SHIMANUKI, Isamu INAMOTO1988 Volume 37 Issue 11 Pages T148-T151
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the determination of C and S in ferrosilicon, the infrared absorption method and the combustion method of the sample for induction furnace were investigated. The experiments were carried out with the cross check tests of 58 laboratories. The results of C determinations were compared with those obtained by coulometry or conductometry using the resistance furnace for combustion of the sample, which has been specified by JIS as the standard method. With the induction furnace, satisfactory results were obtained when Fe and W or Fe, W and Sn were used as the flux for combustion of the sample. The results of S determinations were compared with those obtained by Methylene Blue spectrophotometry after decomposition of the sample with acids as in the standard method. In the combustion method, satisfactory results were obtained when Fe, W and Sn were used as the flux for combustion of the sample. Moreover, the precision and determination limits for each method were calculated from these results.View full abstractDownload PDF (584K) -
Kiyoshi IWASAKI, Komei HIYOSHI1988 Volume 37 Issue 11 Pages T152-T156
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSCentrifugal casting method was applied to the sample preparation for the XRF analysis of bronze castings in order to reduce the structural difference between samples and standards. The bronze sample was remelted and then quenched into a disk shape. In the disk thus obtained, lead present heterogeneously in the original sample was homogeneously dispersed as fine particles. Consequently, the intensity of Pb Lα line for the recast bronze increased compared with that for the original material, while the intensity of Cu Kα line decreased. The effect of recasting on the intensity of Sn Kα line was negligibly small, but significant effect was found for zinc. The intensity of Zn Kα line decreased due to the loss of zinc by vaporization during the remelting of the sample. It is important, therefore, to minimize such loss by controlling the procedure and time of remelting. About 30 g of the sample in small cubes of 45mm in size was prepared and melted for 3540 s by using a high frequency induction furnace in the stream of argon. The melt was cast in a rotating copper mold under an applied centrifugal force, and then a solid disk was obtained. Finally, the surface of the disk was made up to flat by lathe machining for XRF analysis. The standard samples for calibration were also prepared by the same procedure as applied to the samples to be analyzed.View full abstractDownload PDF (2439K) -
Yoichi ISHIBASHI, Yutaka YOSHIOKA, Shigeomi SATOH1988 Volume 37 Issue 11 Pages T157-T162
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe analysis of pig iron and steel composition for production control has been automated to answer the demand for time and labor saving in the steel making process. A fully automatic spectrochemical analyzing system has been developed consisting of an automatic sampling system, a sample transfering system, an automatic analyzing system and a transmission system of analytical values. The procedure is fully automatic from sampling of molten steel and reception of samples at the laboratory to transmission of analytical values.The most suitable conditions for automatic analysis were established.View full abstractDownload PDF (2717K) -
Tosihisa HATO, Minoru AOKI, Takehisa TSUCHIDA1988 Volume 37 Issue 11 Pages T163-T170
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA rapid analytical system for metal from the conveter process, and an automated analytical system for metal samples from the iron refining and continuous casting process were developed at No. 3 Steel-making plant in Yawata Works. The former involved a partial omission and simplification in sample preparation, made possible by development of an improved type of capsule. The latter was a tracking and matching system from sample identification to the transmission of analytical data by automating and systemizing the devices and establishing continuity between them. The more effective operation and quality control concerning with steel-making and some decrease in number of analyst were completed.View full abstractDownload PDF (2673K) -
Hiroshi SHIMIZU, Manabu MURAKAMI1988 Volume 37 Issue 11 Pages T171-T175
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSRecently, a rapid analysis is especially required for the process control of production lines. FIA is often suitable for the process control of liquid line. We have applied FIA method for the process control of a wet non-ferrous metal refinement, which was operated manually by a line operator. The FIA method proposed were as follows; (1) Determination of Cu in the ashes treatment flow by spectrophotometry with Cu(II)-TAMSMB complex (absorbance at 585 nm). (2) Determination of Fe(II) and Fe(III) in the ashes treatment flow by spectrophotometry with Fe(III) chloro complex (absorbance at 440 nm). (3) Determination of Cd in the wastewater by spectrophotometry with Cadion chelate (absorbance at 477 nm).(4) Determination of Ga in the process flow by spectro-fluorescence with lumogallion complex (λex: 485 nm, λem : 560 nm)View full abstractDownload PDF (560K) -
Kuniaki KAWATA, Osamu SUZUKI, Tatsuo UEMURA, Fumio SHIRAI1988 Volume 37 Issue 11 Pages T176-T180
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSRound robin tests were carried out to investigate the precision of determinations of volatile chlorinated hydrocarbons in water by the solvent extraction/GC method and the head-space GC method which are prescribed by the Japanese Ministry of Health and Welfare. Four samples of waters with added trichloroethylene, tetrachloroethylene and 1, 1, 1-trichloroethane were analyzed by 15 different laboratories: 14 laboratories measured concentrations of the three compounds by the solvent extraction/GC method and 13 laboratories, by the head-space GC method. The results show that intralaboratory precision was better than interlaboratory precision. Although the precision of the results by the solvent extraction/GC method was better than those by the head-space GC method in many cases, there were no significant differences between the results obtained by the two methods.View full abstractDownload PDF (639K) -
Koji YAMAGAKI, Tadashi TAKAHASHI, Keio YAMADA, Michinao YOSHII, Toshio ...1988 Volume 37 Issue 11 Pages T181-T186
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method has been investigated for the simultaneous determination of six elements in sludges by solvent extraction/ICP-AES using DDTC or [APDC+HMAHMDC (hexamethyleneammonium hexamethylenedithiocarbamate)]. The combination of APDC and HMAHMDC as a chelating reagent was superior for reducing Fe amounts in the sample solution. The interference by Fe on the Cd determination (226.5 nm) was reduced to about 16% by using the solvent extraction.View full abstractDownload PDF (680K) -
Kazuhiko TANAKA, Riichi KUROKAWA, Ryozo NAKASHIMA1988 Volume 37 Issue 11 Pages T187-T191
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIon chromatography (IC) with conductivity detection for determining anions and ion-exclusion chromatography (IEC) with conductivity detection for determining cations were investigated. Both techniques were applied to the establishment of the optimal conditions for the simultaneous removal of thiosulfate, acetate, and ammonium ions by a batchwise activated sludge process. The process consists of the combination of aerobic and anaerobic biological treatment processes by a sequential automatic process control system equipped with pH, DO, and ORP sensors as process control parameters. The optimal conditions for the pH, DO, and ORP levels required to control automatically the entire process were established using the relationship between the biodegradation behavior of the above ions and the DO, pH, or ORP in the respective process water obtained by the application of IC and IEC.View full abstractDownload PDF (842K) -
Motohisa MATSUMOTO, Masao KAWAMORITA, Akira SHIGEFUJI, Etsuko KASE1988 Volume 37 Issue 11 Pages T192-T195
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWe have determined the concentrations of these benzidine-derivatives in the air of azo-pigment plants based on the official method (absorptiometric method) of analysis for a long time. However, abnormal data, plus error, were recognized at times. The result of our investigation showed that the error was caused by the coloring of the collected liquid by minute particles of pigment dust. We have been studying an HPLC analytical method to replace the absorptiometric method. Our new HPLC method is not only uninfluenced by pigments, but is also superior to the absorptiometric method in repeatability, and equal to it in regard to sensitivity. Conditions of the HPLC method were as follows; Column : reversed phase ODS series; Eluent : 40% (v/v) water/methanol & 55%(v/v) 0.01 mol/l diammonium hydrogenphosphate aq./methanol; Detector : UV284 nm & 303 nm etc.View full abstractDownload PDF (589K) -
Akira NARUKAWA, Isao ODA1988 Volume 37 Issue 11 Pages T196-T201
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA laboratory information mangement system (LIMS/CA) aimed at laboratory automation for chemical analysis is described. A super-minicomputer with relational database connected to realtime computers for each piece of analytical equipment has been developed, namely the LIMS/CA. The system has centralized the management of the analytical information for the routine analysis work from sample log-in to final report. LIMS/CA has improved the response and relaiability of the routine analysis by increasing sample throughput, removing ilde time, and reducing transcription errors.View full abstractDownload PDF (919K) -
Masaru HAYASHI, Hiroshi ENDO1988 Volume 37 Issue 11 Pages T202-T204
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAluminium nitride (0.3 g) was decomposed with hydrochloric acid in a Teflon pressure vessel at 200°C for 3 h. The sample solution was diluted to 250 ml with water. Aluminium was determined by titration method with EDTA. Nitrogen was determined by acid-base titration method after separation by steam distillation. Impurity metals were determined by ICP-AES. The analytical results of aluminium agreed with those by conventional Na2CO3-H3BO3 fusion method. NBS SRM 194 (Ammonium Phosphate) was used to test recovery of the nitrogen analysis method and the measured results agreed well with the certified value. Impurity metals were determined accurately without matrix interferences.View full abstractDownload PDF (389K) -
Akira OKADA, Naoyuki HIRATE1988 Volume 37 Issue 11 Pages T205-T208
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination of trace amounts of U and Th in semiconductor materials by ICP-AES with a tungsten-boat vaporizer was studied. Optimum conditions for vaporizing temperature, carrier gas flow rate and analytical lines for ICP-AES were established. Epoxy resin, SiO2 filler and Sb2O3 flame retardant used for encapusulating plastic package, and Mo and W metals used for the electrodes were decomposed with acids. U and Th were separated from the matrix by anion and cation exchange method. U and Th could be determined to the level of 0.05 ng and 0.02 ng respectively.View full abstractDownload PDF (483K) -
Kazuo KUGA, Hiromitsu MATSUNO, Katsuyuki HOSOYA1988 Volume 37 Issue 11 Pages T209-T214
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFluorescent lamp characteristics depend critically on the state of interface between the thermionic emitter (alkaline earth oxide) and the base metal (tungsten) of the thermionic emitting electrode. Consequently, for lamp quality control, determination of trace amounts of alkaline earth tungstate and tungsten oxide is performed by micro-chemical analysis. Our procedure was as follows;(1) The emitter oxide was removed from the interface with 10 ml of 5 % acetic acid solution for each electrode sample (In this procedure a percentage of tungstate dissolves simultaneously; therefore, it is necessary to make a correction for it.). (2) The separation of alkaline earth tungstate and base metal tungsten was performed with 10 ml of 10% EDTA-NH2 solution (containing 5% acetic acid) for an electrode sample (tungstate content, 0.11 mg). The process was repeated 2 times. (3) The separetion of tungsten oxide and base metal tungsten was done with 10 ml of 10% EDTA-NH2 solution containing 5% aqueous ammonia per electrode sample. Determination of tungsten was performed with thiocyanate absorption spectrometry or ICP-AES. Interfrence from the dissplving reagent (EDTA-NH2 solution) was almost negligible compared with the former technique (alkali containing solution).View full abstractDownload PDF (743K) -
Hideki MATSUNAGA, Naoyuki HIRATE1988 Volume 37 Issue 11 Pages T215-T217
Published: November 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA sensitive and accurate determination method for detecting metallic impurities in semiconductor films such as SiO2 and Si3N4 has been investigated by using vapor phase decomposition and graphite furnace AAS. The decomposition apparatus is constructed with a sealed container, a storage container for generating hydrofluoric acid vapor, a film supporter such as a wafer carrier, and a resolved solution receptacle. The semiconductor films are resolved completely by hydrofluoric acid vapor. Each resolved solution is collected with a micropipette, and finally impurity concentrations are measured by graphite furnace AAS. This method was found to be highly effective for preventing contamination from the reagent and the surroundings. The detection limits were Na : 0.2 pg/cm2, K, Fe : 0.1 pg/cm2, and Cr : 0.05 pg/cm2.View full abstractDownload PDF (502K) -
Hisashi MORIKAWA, Yoshinori UWAMINO, Yasuo IIDA, Akira TSUGE, Toshio I ...1988 Volume 37 Issue 11 Pages T218-T221
Published: November 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSICP-AES was applied to the determination of impurities (Al, Ca, Cr, Fe, Mg, Mo, Na, Si, Ti, and V) in boron nitride (BN) samples. BN was digested by either acid pressure decomposition with hydrofluoric acid-hydrochloric acid for the determination of the 9 elements excepting Si or fusion with Li metaborate for that of Si. The matrix effects on the emission intensities and the background levels of the elements were compensated by using the matrix-matched standard solutions for calibration. The analytical results show that the proposed method is useful for the quality control of BN samples.View full abstractDownload PDF (577K)
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