BUNSEKI KAGAKU

Chemical Analysis of Beryllium. XV

TOMOYUKI AKIYAMA

1954 Volume 3 Issue 6 Pages 467-470
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.467

JOURNAL FREE ACCESS

Show abstractHide abstract

The beryllium in beryllium salt solution is precipitated as BeNH₄PO₄·4_1/2H₂O, this is dissolved in nitric acid, the phosphoric acid thus liberated is precipitated as ammonium phosphomolybdate, the precipitate is dissolved in a standard alkali solution and the excess alkali is titrated back with a standard sulfuric acid solution, and the amount of beryllium equivalent to the consumed alkali is calculated. Also, the sample precipitated as BeNH₄PO₄·4_1/2H₂O is taken up in hydrochloric acid, it is converted into oxine phosphomolybdate, it is dissolved in acid and the liberated oxine is estimated by bromatometry for indirect quantitative estimation of beryllium. The sample solution containing Ti, Al, Fe⁺⁺⁺ and Mn is treated with ammonium nitrate solution and methanol, and the hydroxides of Al, Fe⁺⁺⁺, Be and Ti are separated while hot, the precipitate is taken up in hydrochloric acid, adjusted to pH 4.2, boiled with potassium sulfate and potassium bromate for separation and deposition of titanium oxidehydrate, the iron in the filtrate is separated as sulfide, the filtrate from iron precipitate is utilized for estimation of aluminium by oxine method, then the filtrate is used for estimation of beryllium by usual method. There was some error in this method, but it was better than Moser's method (Monat. 43, 663, 1922). In case of using sodium sulfide method, the sample solution containing Fe, Al, Mn, Ca and Mg is heated with sodium carbonate, caustic soda and sodium sulfide, the precipitates of FeS, MnS, CaCO₃ and MgCO₃ are filtered off, the filtrate containing beryllate and aluminate are hydrolyzed with NH₄Cl for deposition of Be(OH)₂ and Al(OH)₃, these are taken up in hydrochloric acid, combined with the filtrate, the iron is removed by Rothe's method, the aluminum is separated by oxine method, then the beryllium is determined by usual method. However, this is not very promissing method.

View full abstract

Download PDF (308K)
Determination of Lead in Steel by the Dithizone Method

TAKAYOSHI YOSHIMORI, SHIZO HIRANO

1954 Volume 3 Issue 6 Pages 470-474
Published: December 15, 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.470

JOURNAL FREE ACCESS

Show abstractHide abstract

Simplified procedures for colorimetric and volumetric determination of lead in steel were investigated by use of dithizone method. The separation of lead in large amount of iron was effected by the following procedure: 0.10.3 g sample was decomposed with HCl-H₂O₂ or H₂SO₄-HNO₃ mixture, the oxidizing agent was boiled off, NH₄OH added until the solution remained slightly acid, reduced with NH₂OH-HCl, Rochelle salt added, made alkaline with NH₄OH, then treated with KCN to convert the iron as a complex salt, in which all the Fe⁺⁺⁺ was converted to Fe⁺⁺, the solution was heated on a water bath until it turned clear yellow, cooled to room temperature, the leadwas extracted with dithizone-CCl₄ solution and the lead in CCl₄ layer was estimated by colorimetric or extractive titrime tric method. The estimation of lead in steel by this method could be made in 20 to 40 minutes.

View full abstract

Download PDF (1328K)
Total Analysis of Cations by Paperchromatography (II)

ZENZO TAMURA, REIKO ASHIKAWA

1954 Volume 3 Issue 6 Pages 475-477
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.475

JOURNAL FREE ACCESS

Show abstractHide abstract

Following after the previous report¹⁾, we investigated the hindrance expected to occur in the process of the paperchromatographic total analysis of metalic ions by using the three developers (as indicated in Table 1).
At first, we investigated wether 100γ of the ions hindered or not the detection of 2γ of the other ones which had near R_f values to those of the formers, and found that by using selected color reactions (as showed in Table 1 and 2) such hindrance could scarcely occur.
Secondary we investigated hindrance caused by 100γ of the anions which disturbed the ordinary systematic analysis, and found that those anions moved with their own R_f values apart from the metalic ions, and hardly affected the R_f values and detective reactions of the cations (as showedl in Table 3).
Further more we found that Hg⁺², Sn⁺² and Fe⁺² were oxidized by air, MnO₄ was reduced by filter paper and Fe⁺³ partialy turned into Fe⁺² by light in the paperchromatographic processes.

View full abstract

Download PDF (440K)
Studies on the Second Derivertive Automatic Titration. I.

Automatic Titrator, Type AT-I, and Determir ation of a Main Factor Affecting Titation Errors

SEISHI TAKAGI, YOSHIHIRO MAEKAWA

1954 Volume 3 Issue 6 Pages 478-481
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.478

JOURNAL FREE ACCESS

Show abstractHide abstract

We designed a new automatic stop titration, using the second derivertive of the ordinary potentiometric titration curve, made by electrical second derivertive circuit, as a magnetic-cock-operatingsignal.
Namely, the second derivertive voltage stands zero before the end point, and then it increases (or decreases) as the titration approaches to the end point, and at the end point it suddenly decreases (or increases) beyond the zero line, returning to zero line smoothly after the end point.
So, if we use the second derivertive voltage as triggering signal, we can accomplish automatic stop titration, very easily.
In this report, we descrive the second derivertive automatic titrator and the stochastic experiment of determinating the main factor affecting the titration errors. The main factor has been proved to be titration speed, and the other factors, time constant of derivertive circuit, position of electrode and presence of input filter, have only less effect to titration errors.
The original paper of this report was presented before the meeting of the society of the Japan Society for Analytical Chemistry, Tokyo, October 24, 1953.

View full abstract

Download PDF (543K)
Studies on the Second Derivertive Automatic Titration.II.IV.

YOSHIHIRO MAEKAWA

1954 Volume 3 Issue 6 Pages 482-493
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.482

JOURNAL FREE ACCESS

Show abstractHide abstract

I designed two-speed-type, second-derivertive-automatic-titrator, as to decrease the titration errors and diminish the titration time.
This titrator acts as follows; the second derivertive voltage of ordinary potentiometric titration curve begins to increases (or decreases) near the end point, where the first relay circuit acts, closing first magnetic cock which has small leakage of liquid. And though, titration speed falls down near the end mint. the total titration time is short as yet.
With this titrator, I examined stochasticaly on the effect of titration speed to titration errors, and found that the faster the titration speed, the worse the precision and the accuracy.
The original paper of this report was presented before the meeting of the Society of the Japan Society for Analytical Chemistry, Tokyo, October 24, 1953.
The Heaviside's operational calculus of the character of some differential circuit are described.
In the calculus. I have taken the simple expression Eg= (1-ε^-hP)²/ h²P² as input voltage, the change of Eg shows similer jump with the potential jump in the ordinary potentiometric titration.
It has been proved that the best 2 nd derivertive voltage can be obtained when the time constant of the each differential circuit is the same, (on the assumption that the product of the time constants is constant), and the output voltage of the 2 nd derivertive circuits, designed by Prof. Seishi Takagi and author, have nearly exact 2 nd derivertive voltage of the input voltage.
This report inpart was presented before the meeting of the Japgn Society for Analytical Chemistry October 24 November 29 1953 and the Pharmaceutial Society of Japan. April 6, 1954.
The 2 nd derivertive automatic titrator type AT-III, which differs from AT-I or AT-II and has more excellent 2nd derivenive output voltage, was described.
With this titrator. many titrations were carried out and examined stochasticaly on the relation of the titration speed or the titration time to the titration error.
The titrations were carried out in the convinations of Na₂S₂O₃-I₂ and As₂O₂-I₂, and found that the automatic titrator type AT-III has good precision and acurracy.
This report impart was presented before the meeting of the Japan Society forAnalytical Chemistry, October 24. November 29. 1953. and the Pharmaceutical Society of Japan, April 6, 1954.

View full abstract

Download PDF (1103K)
A Semimicro Filter and Semimicro Quantitative Estimation of Aluminum and Magnesium by Oxine

GIICHI TAKEDA, KENJI MOTOJIMA

1954 Volume 3 Issue 6 Pages 493-497
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.493

JOURNAL FREE ACCESS

Show abstractHide abstract

The operation of filtering of a small amount of precipitate, washing of the precipitate, dissolving it in solvent and estimating it by volumetric or colorimetric method is very often used. However, the quantitative treatment of a small amount of precipitate is no easy problem and many difficulties are accompanied with this operation. The writer devised a simple filtering apparatus by application of a filter stick and a very rapid operation could be carried out. With the use of this apparatus, a semimicro quantitative estimation of aluminum and magnesium(10.05mg)by oxine is investigated and a suitable condition for formation of precipitate is determined.

View full abstract

Download PDF (706K)
Rapid Determination of Sulfuric Acid in Acid Mixtures by Use of Aniline

TETSURO MURAKAMI

1954 Volume 3 Issue 6 Pages 497-502
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.497

JOURNAL FREE ACCESS

Show abstractHide abstract

By application of difficult solubility of aniline sulfate in aniline, sulfuric acid in systems of H₂SO₄-CH₃COOH, H₂SO₄-CH₃COOH-(CH₃CO)₂O, and H₂SO₄-HNO₃ is estimated conveniently and rapidly within 2535 minutes, and the end point for titration of sulfuric acid liberated from hydrolysis of aniline sulfate is clear by use of standard alkali solution and phenolphthalein. The presence of water to the extent of 0.4cc gives no effect on the estimation of sulfuric acid in H₂SO₄-CH₃COOH system. Free sulfuric acid remained in the system of H₂SO₄-CH₃COOH-H₂O after treatment with sodium acetate (sulfuric acid equivalent to the added sodium acetate is consumed in this process) is estimated by this method.

View full abstract

Download PDF (998K)
Separation of Thiourea and Ammonium Thiocyanate

ISAMU TSUBAKI, MITSUO KIBOKU

1954 Volume 3 Issue 6 Pages 502-503
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.502

JOURNAL FREE ACCESS

Show abstractHide abstract

Ammonium thiocyanate and thiourea are interchangeable isomers. The authors found that treating a mixture of these two with mercuric chloride gives a precipitate of thiourea above pH 4, while the ammonium thiocyanate does not give precipitate below pH 6; thus, the thiourea is precipitated with mercuric chloride at pH 46 to separate from ammonium thiocyanate. The limit of detection of NH₄SCN in large amount of (NH₂)₂CS (1:10000) with mercuric chloride was 1γ. Also, the limit of detection of (NH₂)₂CS in large amount of NH₄SCN (1:10000) with selenious acid was 5γ.

View full abstract

Download PDF (328K)
[title in Japanese]

[in Japanese], [in Japanese]

1954 Volume 3 Issue 6 Pages 504
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.504

JOURNAL FREE ACCESS

Download PDF (69K)
[title in Japanese]

[in Japanese], [in Japanese]

1954 Volume 3 Issue 6 Pages 504a-505
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.504a

JOURNAL FREE ACCESS

Download PDF (287K)
[title in Japanese]

[in Japanese], [in Japanese], [in Japanese]

1954 Volume 3 Issue 6 Pages 505-506
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.505

JOURNAL FREE ACCESS

Download PDF (313K)
[title in Japanese]

[in Japanese]

1954 Volume 3 Issue 6 Pages 506
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.506

JOURNAL FREE ACCESS

Download PDF (241K)
[title in Japanese]

[in Japanese]

1954 Volume 3 Issue 6 Pages 506a-507
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.506a

JOURNAL FREE ACCESS

Download PDF (305K)
[title in Japanese]

[in Japanese]

1954 Volume 3 Issue 6 Pages 508-516
Published: December 15, 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.508

JOURNAL FREE ACCESS

Download PDF (1387K)
[title in Japanese]

[in Japanese]

1954 Volume 3 Issue 6 Pages 516-521
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.516

JOURNAL FREE ACCESS

Download PDF (1045K)
[title in Japanese]

[in Japanese]

1954 Volume 3 Issue 6 Pages 522-528
Published: December 15, 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.522

JOURNAL FREE ACCESS

Download PDF (1335K)
[title in Japanese]

[in Japanese]

1954 Volume 3 Issue 6 Pages 529-534
Published: December 15, 1954
Released on J-STAGE: April 28, 2009

DOIhttps://doi.org/10.2116/bunsekikagaku.3.529

JOURNAL FREE ACCESS

Download PDF (618K)
Erratum

1954 Volume 3 Issue 6 Pages e1a
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1a

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum to : Analytical Chemistry by Mesns of Oxalic Acid.IV.

1954 Volume 3 Issue 6 Pages e1b
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1b

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum to : Electrochromatography II.III.

1954 Volume 3 Issue 6 Pages e1c
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1c

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum

1954 Volume 3 Issue 6 Pages e1d
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1d

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum

1954 Volume 3 Issue 6 Pages e1e
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1e

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum to : Radiochemical Studies on "Bikini Ashes"(March1, 1954).PartI.

1954 Volume 3 Issue 6 Pages e1f
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1f

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum

1954 Volume 3 Issue 6 Pages e1g
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1g

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum to : Electrochromatography. (IV)

1954 Volume 3 Issue 6 Pages e1h
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1h

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum to : Improved Procedure for Microdetermination of N-Methyl Group

1954 Volume 3 Issue 6 Pages e1i
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1i

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum to : Chemical Analysis of Beryllium. XIV

1954 Volume 3 Issue 6 Pages e1j
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1j

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum

1954 Volume 3 Issue 6 Pages e1k
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1k

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum

1954 Volume 3 Issue 6 Pages e1l
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1l

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum

1954 Volume 3 Issue 6 Pages e1m
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1m

JOURNAL FREE ACCESS

Download PDF (213K)
Erratum

1954 Volume 3 Issue 6 Pages e1n
Published: 1954
Released on J-STAGE: January 14, 2010

DOIhttps://doi.org/10.2116/bunsekikagaku.3.6_e1n

JOURNAL FREE ACCESS

Download PDF (213K)

Register with J-STAGE for free!