Tadashi Mochizuki

Flow-injection analysis of silicate rocks for total iron and aluminium.

A flow-injection method is described for the spectrophotometric determination of total iron and aluminium in silicate rocks. Rock samples are opened up by fusion with a mixture of lithium carbonate and boric acid, the melt is taken up in 1M hydrochloric acid and the resulting solution is used for the determination of both iron and aluminium. The flow system for the determination of iron needs no particular reagents, involving simply measurement of the absorbance of the chloro-complex of iron(III) at 335 nm. The system for aluminium consists of the reduction of iron(III) to iron(II), colour development with Xylenol Orange (XO), destruction of XO-chelates other than that of aluminium by addition of EDTA and subsequent measurement of the absorbance of the aluminium-XO complex at 506 nm. The systems permit semi-automatic, rapid analysis of silicate rocks for iron and aluminium. Results obtained for standard rocks were in good agreement with the recommended values. The precision ranged from 0.1 to 0.9% for iron and from 0.3 to 0.7% for aluminium.

Application of slurry nebulization to trace elemental analysis of some biological samples by inductively coupled plasma mass spectrometry

SummaryThe application of slurry nebulization/inductively coupled plasma mass spectrometry (ICP-MS) to trace elemental analysis of biological samples has been investigated. Three standard samples of the National Institute of Standards and Technology (NIST) were dispersed in 1% aqueous Triton X-100 solution by grinding with a planetary micronizing mill. The resulting slurries were nebulized into an ICP without any additional treatments. The 1% (m/v) slurry of the NIST bovine liver showed no significant influence on cone blockage and signal suppression/enhancement. Detection limit, precision and accuracy were discussed for the determination of 24 elements of interest in bovine liver, rice flour and pine needles. Detection limits ranged from 0.0001 μg g−1 for U to 0.52 μg g−1 for Zn at the effective integrating time of 10 s. For high mass elements, low blank values were obtained, yielding excellent limits (<0.01 μg g−1). Acceptable accuracy and precision were obtained for most of the elements in the NIST bovine liver and rice flour, even for the volatile elements, such as As, Se and Br. However, relatively poor accuracy was obtained for the analysis of pine needles.

Flow injection analysis of silicate rocks for titanium

A flow injection spectrophotometric method has been developed for the accurate, continuous determination of titanium in silicate rocks. A rock sample solution is prepared by fusion with a mixture of lithium carbonate and boric acid and subsequent dissolution of the melt with 1 M hydrochloric acid. The preparation technique is the same as that used for the determination of total iron and aluminium in silicate rocks by flow injection spectrophotometry. An aliquot of the sample solution is injected directly into the apparatus with no pre-treatment. The system consists of the reduction of iron(III) with ascorbic acid and measurement of the absorption of the titanium-diantipyrylmethane (DAM) complex at 388 nm. In spite of the slow reaction of titanium with DAM, satisfactory results are obtained with an appropriate optimised system. This system permits high throughput of 60 solutions per hour. The procedure has been applied to standard silicate rocks of the US Geological Survey and the Geological Survey of Japan. The precision ranges from 0.1 to 0.8% for titanium(IV) oxide contents of 0.2–2.2%.

Rapid Continuous Determination of Aluminium in Copper-Base Alloys by Flow-Injection Spectrophotometry

ZusammenfassungBei dem empfohlenen Verfahren werden Cu, Zn, Fe und andere Störelemente mit Hilfe von Thioharnstoff, Ascorbinsäure und EDTA maskiert und der Al-Xylenolorange-Komplex bei 506 nm gemessen. Mit Hilfe eines geeigneten Eichverfahrens werden trotz der trägen Reaktion von Al mit Xylenolorange zufriedenstellende Werte erhalten. 50 Bestimmungen können innerhalb von 1 h ohne jedes Verschleppen durchgeführt werden. Bei der Analyse von Messing und Al-Bronze (1,43–10,2% Al) wurde gute Übereinstimmung mit zertifizierten Werten erzielt. Die Standardabweichungen lagen im Bereich von 0,2–0,3%.SummaryA flow-injection spectrophotometric method has been developed for the rapid, continuous determination of aluminium in copper-base alloys. The system consists of the masking of copper, zinc, iron, etc. with a combined use of thiourea, ascorbic acid and EDTA and the measurement of light absorption of aluminium-Xylenol Orange complex at 506 nm. With appropriate standardization satisfactory results are obtained in spite of sluggish reaction of aluminium and Xylenol Orange. The system allows the analysis of solutions of copper-base alloys for aluminium to be conducted at a rate of 50 determinations per hour without any carryover. The results obtained for standard brasses and aluminium bronze (Al 1.43–10.2%) agreed well with the certified values. The precision (rsd) ranges are 0.2–0.3%.

Determination of beryllium in copper-beryllium alloys by flow-injection spectrophotometry

ZusammenfassungAls Reagens zur spektralphotometrischen Bestimmung von Berryllium in Cu-Be-Legierungen dient Xylenolorange. Cu, Co und Fe werden mit Hilfe von Thiosulfat und EDTA maskiert. Die Messung erfolgt im Absorptionsmaximum des Komplexes von 493 nm. Bei einer Durchflußgeschwindigkeit von 4 ml/min können 60 Proben je Stunde mit einer relativen Standardabweichung von etwa 1% analysiert werden.SummaryA method is described for the flow-injection spectrophotometric determination of beryllium in Cu-Be-alloys using xylenol orange as reagent. Cu, Co and Fe are masked by means of thiosulphate and EDTA. Absorbance is measured at the maximum of 493 nm. With a flow rate of 4 ml/min 60 samples can be analyzed per hour with a relative standard deviation of about 1%.

Correction method for X-ray fluorescent determination of chromium in high-alloy steels and nickel-base alloys

ZusammenfassungDie Eich-Gleichung für das neue Korrekturverfahren wurde vom JIS-Modell (Japanese Industrial Standards) abgeleitet und ist über einen weiten Bereich von Zusammensetzungen durch Herstellung von lediglich binären Fe-Cr-Standards einsetzbar. Das beschriebene Verfahren bietet eine bessere Genauigkeit als die Methode nach dem Korrekturmodell von Rasberry-Heinrich. Sie betrug 0,08% für hochlegierte Stähle und 0,14% für Nickellegierungen.SummaryA new interelement correction method has been developed for the X-ray fluorescent determination of chromium in high-alloy steels and nickel-base alloys. The calibration equation which was derived from the JIS (Japanese Industrial Standards) model is applicable over wide ranges of compositions by preparation of only Fe-Cr binary standards.The new approach gave better accuracy than that based on Rasberry-Heinrich correction model. The accuracies (σd) were 0.08% for high-alloy steels and 0.14% for nickel-base alloys.