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Volume 35, Issue 9
Displaying 1-16 of 16 articles from this issue
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Adsorption of copper-nitroso R-salt complex on solid adsorbent with assistance of alkylammonium saltAtsushi YOSHINAGA, Yohichi GOHSHI1986 Volume 35 Issue 9 Pages 789-794
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new type of the preconcentration techniques of trace metal ions in solution with solid adsorbent was performed. By adding alkylammonium cation, an anionic metal complex, Cu-nitroso R-salt, was adsorbed on XAD-2 resin of low polarity. The length of alkyl carbon chains and the substitution numbers of alkylammonium cations influenced the adsorption-assisting effect. In this study, n-octylamine showed the highest assistant effect and the Cu-complex could be quantitatively recovered with an enrichment factor of 1000. Because the adsorption tendency of this method was different from that of anion exchanger, it was concluded that the adsorption of alkylammonium ions to XAD-2, which will give anion exchangability to the adsorbent, does not occur prior to the ionic association of alkylammonium ions with the complex. On the other hand, the adsorption of free-nitroso R-salt, which doesn't contribute to the complex formation, was reduced in the same way by the presence the Cu-complex for all alkylammonium ions tested. This fact was inconsistent with the assumption of ion association of alkylammonium ions with the complex. On the basis on the results, it was concluded that the adsorption mechanism for this method is neither ion exchange of the anionic Cu-complex with another anion which is attracted to alkylammonium on the adsorbent, nor the nonionic adsorption of the ion pair of alkylammonium cation and the anionic complex.View full abstractDownload PDF (997K) -
Kunihiro WATANABE, Izuo AOKI1986 Volume 35 Issue 9 Pages 795-801
Published: September 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe fluorometric determination of magnesium with bissalicylidene-ethylenediamine (BSED) in the mixed solvent was studied in the presence of large amounts of amine or amino acid. BSED was hydrolyzed in the aqueous solution to liberate salicylaldehyde, which reacts with large amounts of amine to form a Schiff base corresponded to the amine. The Schiff base reacts with magnesium in the range of pH 1012 to form a complex, which has a yellow fluorescence with ultraviolet exciting. The diamines and triamines, which have two methylene groups between two amino groups, were superior to other amines discussed in respect of fluorescence intensity. Mono amine reacts magnesium not to form a Schiff base complex. Amino acid enhanced the value of reagent blank. Magnesium-Schiff base complexes were not hydrolyzed in the aqueous solution. Therefore the fluorescence intensity of the complexes was stable. However, the intensity of fluorescence was very weak, because the free reagent decreased the fluorescence intensity of the complex due to self-absorption. The organic solvent suppressed the self-absorption by changing the exciting and emission spectra of the free Schiff base reagent as an anion. The recommended procedure is as follows: Take 17ml of a sample solution containing from 0.05 to 15 μgMg, add 2ml of buffer solution(diethylenetriamine: 0.5M HCl=1:1), 15ml of dioxane, and 1ml of 0.1% BSED dioxane solution to the sample solution. Then adjust the volume to 25ml with water, and stand for 10min. The fluorescence intensity of the complex at 430nm is measured at an excitation wavelength 350nm against the reference of 0.050.5 μg/ml quinine sulfate solution.View full abstractDownload PDF (1205K) -
Michiko ITO, Mika SATO, Nobuyuki SHIBATA, Shigeo SUZUKI1986 Volume 35 Issue 9 Pages 802-806
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn investigation for the quantitative determination of cadmium in foods containing large amounts of sodium chloride was made by adopting the coprecipitation method with zirconium hydroxide and AAS. Fifty ml of an acidified test solution was added to 1ml of a 7.06% zirconium oxychloride solution (containing 20mg of zirconium), and the pH was adjusted from 5.0 to 11.0 with diluted ammonia water or 4M sodium hydroxide. After stirring for 10min, the precipitate was separated by centrifugation and dissolved in hot 2M hydrochloric acid and the solution was diluted to 20 or 50ml of total volume with 2M hydrochloric acid. The cadmium was then determined by flame AAS. The optimum pH needed to obtain a complete recovery was 10.0 with 4M sodium hydroxide.The relative standard deviation was found to be 1.14%. Various foreign ions as K+, Ca2+, SO42-, PO43-, Fe3+, Mg2+, Cu2+, Zn2+, Mn2+, Al3+, Ni2+ and Pb2+ did not interfere with the analysis. The method was applied to the determination of cadmium in soy sauce and bean paste, and the analytical values agreed well with those of other methods involving extraction processes with organic solvents.View full abstractDownload PDF (785K) -
Hiroki OHURA, Toshihiko IMATO, Yasukazu ASANO, Sumio YAMASAKI, Nobuhik ...1986 Volume 35 Issue 9 Pages 807-813
Published: September 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe highly sensitive flow analysis of disaccharides (maltose, lactose, cellobiose and melibiose) was proposed by using a potential buffer solution and an oxidation-reduction potential(ORP) electrode. The analysis was based on the detection of the change in a composition of the buffer solution with the ORP electrode in a redox-reaction of the disaccharide with a hexacyano-ferrate (III) ([Fe(CN)6]3-)-hexacyanoferrate (II) ([Fe(CN)6]4-) potential buffer solution (containing sodium hydroxide). The sample(140μl) injected into a water stream was merged with the stream of the buffer solution ([Fe(CN)6]3--[Fe(CN)6]4-; 5×10-51×10-2mol dm-3) containing sodium hydroxide(0.6mol dm-3). The reaction was complete for 4.5min when the sample flows through the reaction tube(0.5mm i.d., 20m long) kept at 85°C. The potential change of the ORP electrode was detected as a peak-shaped, and a linear relationship between the peak height and the concentration of disaccharides was observed in the wide range of 1×10-61.5×10-3mol dm-3. The lower detection limit was 2.5×10-7mol dm-3. Sampling rate for determination was about 60 per hour. The relative standard deviation was 1.72.9% for analysis of 5×10-6mol dm-3 maltose at sampling rates of 2060h-1.View full abstractDownload PDF (1121K) -
Shoichiro TAGAMI, Yukiko MORI, Chikage MATSUURA1986 Volume 35 Issue 9 Pages 814-818
Published: September 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSResponse characteristics of the potential of alkylamine (ethylamine, dimethylamine, diethylamine, trimethylamine and n-amylamine) electrodes prepared of a body of a commercial ammonia electrode has been described, in which 0.05M alkylamine hydrochloride solutions were used as an inner solution instead of ammonium chloride. These electrodes have been applied to the determination of N-ethylnicotinamide and N, N-diethylnicotinamide. The Nernstian slopes of these elecrodes in the concentration range of 10-510-2M alkylamine were -58.4-59.6mV, and the correlation coefficients were 0.9971.008. The response time required for the electrode potential to reach a steady value in 10-210-4M alkylamine solutions was 310min and the continuance time was 210min. The effect of pH on the Nernstian slope was examined. in the concentration range of 10-510-2M diethylamine. At pH 12.18, a linear calibration curve was obtained in the concentration range of 10-510-2M diethylamine, while the similar curves were obtained in 10-510-3M at pH 11.9 and in 10-510-4M at pH 11.58. N-ethylnicotinamide or N, N-diethylnicotinamide decomposed into nicotinic acid and ethylamine or diethylamine on refluxing 6M hydrochloric acid for 4or 5h. After neutralization with sodium hydroxide to pH6, the ethylamine or diethylamine was determined with the ethylamine or diethylamine electrode. The mean recoveries of N-ethylnicotinamide and N, N-diethylnicotinamide were found to be 99.65% and 99.73%, respectively.View full abstractDownload PDF (728K) -
Suwaru HOSHI, Norimitsu TAKAHASHI, Sadanobu INOUE, Mutsuya MATSUBARA1986 Volume 35 Issue 9 Pages 819-822
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe complex formation of zinc(II), cadmium(II), lead(II), copper(II) and mercury(II) with diacetyl bis(4-phenyl-3-thiosemicarbazone) (DBS) was studied in 80v/v% N, N-dimethylformamide-water mixture, and reversed phase partition chromatography with a spectrophotometric detection was applied to the separation of metal-DBS complexes by using a ODS column (6mm i.d.×250mm in length). The elution peaks of Cd-DBS and Pb-DBS, and of Ni-DBS and Cu-DBS on their chromatogram were not separated successfully by using a methanol-water and a acetonitrile-water as mobile phases. The resolved separation of Zn, Cd, Pb, Ni, Cu and Hg-DBS was achieved by using a 67.5v/v% acetone-water mobile phase containing 0.01mol dm-3 sodium acetate(apparent pH 8.8). The calibration curves of the peak area for Cd-DBS and the peak hights for others were linear in concentration ranges of (0.22.0)×10-5 mol dm-3 for Zn and (0.44.0)×10-5mol dm-3 for others (0.04 absorbance unit full-scale at 425nm, injected volume 25mm3). All the relative standard deviation (sample size concentration of 1.0×10-5mol dm-3 for Zn and 2.0×10-5mol dm-3 for others, n=5) was better than 1.9%.View full abstractDownload PDF (609K) -
Tomoko SAKAGUCHI, Yoshihiko OHYAGI1986 Volume 35 Issue 9 Pages 822-824
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSCopper(I)iodide, silica powder and calcium sulfate (CaSO4·1/2H2O) were mixed and made into tablet as dried Hg-absorbing agent. Absorbing ability was tested in several composition by AAS using silver amalgam. Mixing ratio of each chemicals that showed superior absorbing ability was 1:1:1 in weight. As mercury(I) iodide shows vermilion color, the absorbing ability can be observed easily by surface color change. This tablet can be more easily handled than potassium permanganate-sulfuric acid solution absorbent in wet state.View full abstractDownload PDF (566K) -
Temperature, time and absorbance at the peakSusumu NAKAMURA, Yoshinori KOBAYASHI, Masaaki KUBOTA1986 Volume 35 Issue 9 Pages 824-826
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTemperature, time and absorbance at the peak of an absorbance signal in electrothermal AAS were calculated for Cu using mathematical models of atom formation mechanism and temperature-time relationship reported previously. Values calculated agreed well with those obtained by experiments within experimental error. The models enable us to predict temperature, time and absorbance at the signal peak for an analyte under a selected heating rate.View full abstractDownload PDF (582K) -
Kunio NAGASHIMA, Shigetaka SUZUKI1986 Volume 35 Issue 9 Pages 826-828
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new sensor for continuous monitoring of hydrogen was developed by using a silver sulfide and silver iodide solid electrolyte. The sensor is expressed as Pt/Ag2S/Ag2S+AgI/AgI/Ag, and can be formed easily into a form of small disk with a die and press. Silver powder, silver iodide, mixture of silver sulfide and silver iodide, silver sulfide and a platinum gauze were placed in layers in the die, and 600kg/cm2 of pressure was applied. The diameter and thickness of the disk were 13mm and 2.1mm, respectively. The cell was then transferred in a heating air bath held at 350°C, and a constant voltage of 3μV was applied.When the sample gas containing hydrogen was impinged on the platinum anode of the sensor, an electrolytic current flowed through the external circuit of the sensor. The current was proportional to the concentration of hydrogen at a constant bath temperature and constant flow rate of the gas. The calibration curve for hydrogen was rectilinear between 1001000ppm, and the relative standard deviation in this range was within 5.0%. The detection limits of hydrogen at the flow rate of 50cm3/min was 50ppm, and the response time was about 13min for 500ppm hydrogen. When hydrogen (500ppm H2/N2) was impinged on the sensor for about 6h/d, the sensitivity after 33 days exposure decreased to about 80% of the original value.View full abstractDownload PDF (475K) -
Shukuro IGARASHI, Akira OBARA, Hiroaki ADACHI, Takao YOTSUYANAGI1986 Volume 35 Issue 9 Pages 829-831
Published: September 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSimultaneous determination of small amounts of Cu(II), Zn(II), Co(II) and Mn(II) with α, β, γ, δtetrakis(4-carboxyphenyl) porphine (TCPP) by HPLC was developed. The metal-TCPP complexes were quantitatively formed within 20min at room temperature in the presence of Hg(II) and pyridine([Hg2+]Total≥10-6mol dm-3 and [Pyridine] Total≥10-2mol dm-3) over the following pH ranges of 7.0?11.2(Cu), 7.0?10.9(Zn), 8.2?10.2(Co) and 7.8?10.7(Mn). Pyridine not only acted as an accelerator for complexation, but also as a selective modifier, as seen by the retention behavior of the Co complex in the chromatogram. Recommended procedure: Prepare a sample solution containing up to 1.6μg of Cu(II), Zn(II), Mn(II) and Co(II) in a 25cm3 amber-colored-volumetric flask, to which add 2cm3 of 1×10-4mol dm-3 TCPP, 0.25cm3 of 1mol dm-3 pyridine solution, 0.5cm3 of 0.1mol dm-3 sodium tetraborate pH buffer solution(pH 9.3), and 1cm3 of 1×10-4mol dm-3 mercury(II) solution. Leave to stand at room temperature for 30min and dilute to 25cm3 with water. Inject 0.1cm3 of the mixture into the HPLC system [mobile phase: 50w/w% mixture of acetonitrile and aqueous acetic acid-sodium acetate solution(pH 3.5), flow rate 0.5cm3/min, column: Merck CGC glass cartridge LiChrosorb RP-18 (5μm: 3.2 mm i.d.×150 mm)], and measure the absorbance at 420nm. The molar absorptivities (ε/cm-1mol-1 dm3) of Cu-, Zn-, Mn- and Co-complexes at 420nm were 2.35×105, 5.81×105, 5.25×104 and 6.46×10-4, respectively. The peak height calibration curves of these metal ions were linear over the range of 4×10-8 to 1×10-6mol dm-3, and the relative standard deviation (5 determinations) at the center of the calibration range were 3.6%(Cu), 3.3%(Zn), 1.6%(Co) and 4.3%(Mn). Up to 100μg of alkali metal ions (Na+, K+), alkali earth metal ions (Mg2+, Ca2+, Ba2+, Sr2+), and anions (Cl-, Br-, NO3-, SO42-, ClO4-. CH3COO-) did not interfere with the determination.View full abstractDownload PDF (525K) -
Jun-ichi TÔEI, Nobuyuki BABA1986 Volume 35 Issue 9 Pages 832-835
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA titration method utilizing an anion exchange Table 2 Effect of HCl column (8mm i.d.×10mm length; TSK-Gel SCX 10μm) and a low volume mixer has been developed for the determination of salt concentration of brines by flow injection system. Samples are pumped through the column and alkalinised. The alkalinised samples are mixed with a reagent (phenolphthalein) and sent to a detector. And the peak width is observed. This method gives wide dynamic range (0.0010.4M) with low sample volume (20μl). Precision of the method is better than 1.5 % R.S.D. (n=10) at the 0.01M level for sodium chloride and the sampling rate is 120 samples/h. This method was successfully applied to the analysis of isotonic saline solutions.View full abstractDownload PDF (700K) -
Koji MATSUSAKI, Masaaki MOMOI, Minoru FUJIMOTO1986 Volume 35 Issue 9 Pages 835-837
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTap water always contains more than 0.1ppm chlorine for disinfection. The residual chlorine was determined with 2, 7-fluorenediamine(FDA) spectro-photometrically. Ten ml of the sample water, which contained less than 1.5ppm chlorine, was transferred to a 15ml test tube with a ground stopper. One ml of 2M nitric acid and 1ml of 40mg/l FDA solution were added and shaken. After 3min the absorbance was measured at 422nm. The calibration curve showed a straight line which passed through the origin and the molar extinction coefficient was 5.1×104l mol-1 cm-1. Coexisting cations and anions in tap water did not interfere with the determination.View full abstractDownload PDF (374K) -
Hisatake NARASAKI, Takashi OGAWA, Ikuyo MATSUSHIMA1986 Volume 35 Issue 9 Pages T73-T75
Published: September 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTrace arsenic and selenium in copper and nickel powders were determined, after separation with Muromac chelating ion exchange resin which is composed of networks of styrene-divinylbenzene copolymers with attached iminodiacetate groups, by hydride-generation AAS in the prresence of masking agents. The powders dissolved in nitric acid were evaporated to dryness and then redissolved in hydrochloric acid. After the pH of the solution had been adjusted to 3.5 by adding 1ml of 4% potassium hydrogen phthalate solution, arsenic and selenium were separated with Muromac resin (2050 mesh). When determing selenium, the effluent concentrated to approximately 5ml was heated with 5ml of concentrated hydrochloric acid in a boiling water bath. When arsenic and selenium in copper powder were determined, 1ml of 2% thiourea, and of 4% neocuproine solutions were added, respectively. When nickel powder was taken as a sample, 1ml of 2% 1, 10-phenanthroline solution was added to the effluent. Accuracies checked with an NBS Standard Reference Material Unalloyed Copper (SRM 454) were within the certified values. Arsenic and selenium in copper and nickel powders of chemically pure grade were determined by the proposed method.View full abstractDownload PDF (419K) -
Hideo HARA, Toshio HASHIMOTO, Shinichi FUJIE, Yohichi GOHSHI1986 Volume 35 Issue 9 Pages T76-T79
Published: September 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA powdered (agate pot and vibrating mixer mill is used) sample (0.2g) is decomposed with a mixed acid solution (15ml of hydrochloric acid +1ml of hydrofluoric acid) in a Teflon bomb. When the resultant solution is diluted directly with water, large quantities of precipitates (consisting of titanium, zirconium and lead compounds etc.) are observed. To avoid this, the following procedure is employed; The solution is transferred into a polyethylene beaker containing 1.5g of citric acid. After pH adjustment to 89, most of the precipitates can be dissolved by the addition of 2.0g of EDTA·2Na. The remaining LaF3 precipitate is dissolved by heating with 1.5g of boric acid and 20 ml of nitric acid. After cooling, this solution is used for rinsing the bomb, and is transferred into a 250ml volumetric flask. An aliquot of 25ml is diluted four times with water and analysed by ICP-AES. The procedure described here provides a rapid and precise (R.S.D.<3%) determination for all elements (Ti, Zr, Pb, Nb, Sr, La, Cr, Mn and Mg) without erosion of glassware and quartzware (plasma torch, nebulizer etc.).View full abstractDownload PDF (703K) -
Hideaki TOYODA, Hiroshi UCHIDA, Jun-ichi TAKAHASHI1986 Volume 35 Issue 9 Pages T80-T85
Published: September 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSimultaneous multielement analysis of human hair has been investigated by ICP-AES. Half a gram of hair sample was rinsed in water and acetone, and left in nitric acid in room temperature for 16h. Then, the sample was digested with nitric acid and hydrogen peroxide in a volumetric flask at 80°C for 5h, or evaporated to dryness with perchloric acid in a Teflon tall beaker at 180190°C after digestion with nitric acid at 80°C for 6h. The digested sample was finally diluted to 10 or 5ml, respectively, with the addition of yttrium (20μg ml-1) as the internal standard. Hydride generation system was used for the determination of Se, As and Hg, and the other 18 elements were determined in direct nebulization. Emission and background spectra and also the precision in the determination about the samples solutions obtained from both digestion methods were compared with each other. Both methods were available for the determination of the elements above 1μg g-1, and the digestion with perchloric acid seems to be suitable for trace elements below 1μg g-1. However, the contamination caused by reagents used and/or the atmosphere was observed in the latter case. Further, Se, As and Hg were determined by the flask digestion without any loss of the amounts. Proposed method was applied to the analysis of certified reference material “Hair”, and the results were well agreed with certified and reference values.View full abstractDownload PDF (1051K) -
Rokuro KURODA, Fumiyasu TAKEKAWA, Koichi OGUMA1986 Volume 35 Issue 9 Pages T86-T89
Published: September 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method was described for the determination of traces of copper in standard silicate rocks by fusion with a lithium carbonate-boric acid mixture followed. by graphite furnace AAS. About 200mg of powdered sample was fused with a mixture of 250mg each of lithium carbonate and boric acid. The cake was dissolved in 1M hydrochloric acid and diluted to exactly 50ml with the same acid. A 2.5ml aliquot was taken and diluted with 1M hydrochloric acid to 10ml. Ten μl of the solution was injected into the furnace. A Shimadzu AA-646 atomic absorption/flame spectrophotometer equipped with a Shimadzu GFA-4 graphite furnace atomizer and a deuterium-arc background corrector was used for the absorbance measurements. Wavelength, band width and current of the copper hollow cathod lamp were 324.7nm, 0.38nm and 7mA, respectively. The optimum program consisted of drying for 30s at 150°C (ramp mode), ashing for 20s at 250°C (step mode), atomization for 4s at 2300°C (step mode) and cleaning for 3s at 2800°C (step mode). Calibration solutions contained the same concentrations of hydrochloric acid and flux as used for the sample preparation. The results obtained for thirteen USGS and two GSJ standard rock samples are in excellent agreement with the recommended values. The relative standard deviations (n=35) were less than 10% (av. 4.1%) except those (1528%) for two ultramafic rocks.View full abstractDownload PDF (571K)
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