Yachiyo Kakita

Extraction of reduced molybdosilicic acid and its application to the determination of traces of silicon

It is difficult to find satisfactory organic solvents for the extraction of reduced molybdosilicic acid, but extraction is possible with isoamyl or isobutyl alcohol if the acid concentration of the aqueous solution is increased before the extraction, the best results being obtained by extraction with isoamyl alcohol from 3.5-4.5N sulphuric acid medium. This makes the reduced molybdosilicic acid method much more sensitive and permits the determination of microgram amounts of silicon in various kinds of high-purity metals.

Spectrophotometric determination of micro amounts of nitrogen with organic solvent extraction: Application to metallurgical analysis

Abstract Spectrophotometric determination of nitrogen, as ammonia, with organic solvent extraction has been studied. The blue coloured compound formed from ammonia, phenol and hypochlorite (chloramine-T) is completely extracted with isobutyl alcohol or isoamyl alcohol only by using a salting-out reagent, and the optimum conditions have been established. This procedure has been applied to the determination of nitrogen in iron, steel and aluminium.

Determination of Microquantities of Manganese in Iron, Steel and Some Non-Ferrous Metals by Extraction and Absorption Photometry

ZusammenfassungBei dieser Bestimmung wird das Mangan mit Persulfat zu Permanganat oxydiert, dieses mit Tetraphenylarsoniumchlorid umgesetzt, der Komplex mit Dichloräthan aus 0.7 N schwefelsaurer Lösung extrahiert und die Absorption des Extraktes bei 528 nm gemessen. ppm-Mengen Mangan können in Eisen und Stahl sowie in Nickel, Kupfer, Aluminium und Magnesium bestimmt werden. Chrom stört in größeren Konzentrationen.SummaryThe photometric determination of manganese described is based on the oxidation of the Mn to permanganate by means of persulphate, reaction with tetraphenylarsonium chloride, extraction of the complex with dichloroethane from 0.7 N sulphuric acid solution and measurement of the absorption of the extract at 528 nm. Manganese can be determined in the ppm-range in iron, steel, nickel, copper, aluminium and magnesium. Interferences are caused by larger concentrations of chromium.

Determination of microquantities of manganese in iron, steel and some non-ferrous metals by extraction and absorption photometry

ZusammenfassungBei dieser Bestimmung wird das Mangan mit Persulfat zu Permanganat oxydiert, dieses mit Tetraphenylarsoniumchlorid umgesetzt, der Komplex mit Dichloräthan aus 0.7 N schwefelsaurer Lösung extrahiert und die Absorption des Extraktes bei 528 nm gemessen. ppm-Mengen Mangan können in Eisen und Stahl sowie in Nickel, Kupfer, Aluminium und Magnesium bestimmt werden. Chrom stört in größeren Konzentrationen.SummaryThe photometric determination of manganese described is based on the oxidation of the Mn to permanganate by means of persulphate, reaction with tetraphenylarsonium chloride, extraction of the complex with dichloroethane from 0.7 N sulphuric acid solution and measurement of the absorption of the extract at 528 nm. Manganese can be determined in the ppm-range in iron, steel, nickel, copper, aluminium and magnesium. Interferences are caused by larger concentrations of chromium.

New method for the spectrophotometric determination of ultramicro amounts of copper.

A deep yellow colour is formed by the reaction with phenol and chloramine-T in the presence of copper, and this reaction is used for the photometric determination of copper. An aqueous solution of copper and the reagents at pH 11.5-11.6 is heated. The molar absorptivity at 410 mmu, is 2.32 x 10(6). The method has been used satisfactorily to determine ultram amounts of copper in high-purity silicon.

The Extraction of Thallium with Methyl Isobutylketone.

タリウムについて,各種濃度の塩酸溶液ならびにその他の酸との混酸溶液からメチルイソブチルケトンによる金属塩抽出の基礎実験を行なった。タリウム(III)の10mgを含む塩酸溶液または他の酸を添加した混酸溶液にメチルイソブチルケトンを加えて抽出し,水溶液層中に残ったタリウムをオキシン法で光度定量して抽出率を求めた。抽出は20℃の液温で行なった。塩酸の濃度がL5～8Nで抽出を行なえば,99.8%以上の抽出率を示す。また塩酸に硝酸,硫酸または過塩素酸をおのおの適当な割合で添加した混酸を用いると,0.5Nの低い塩酸溶液でもいずれも99%程度の抽出率が得られ,これら他の酸の添加は抽出率を高める。硫酸溶液からの抽出は,8N付近で約21%の抽出率を示すにすぎない。

Studies on the Determination of Metals with Hexamine. I

1. 蒼鉛がヘキザミンと沃化加里とにより生ずる黄色及び橙色沈澱は二種の化合物であることを熱天秤により示した.2. 黄色沈澱は蒼鉛の定量に適さないのに反し,橙色沈澱は120～200°の範圍にて乾燥することによりBiOIの一定組成の沈澱として正確に定量することが出來ることを示した.3. 沈澱が完全なる酸の濃度が硝酸0.1N以下で,酸が多ければヘキザミンを多くしてpHを4以上にすることが必要である. SO4″, NO3′は多量共存しても影響はないがCl′及び有機酸鹽の存在に於いては定量不可能である.4. 沃素酸加里滴定法にて液状アマルガム還元器を使用することによりシアン化水素の危險がなく滴定を行ふことが出來,之を用ひてBiOIを鹽酸に溶解し沃素酸加里標準液にて滴定した.

On the Determination of Tungusten in Iron and Steel

The conditions for the determination of tungsten in iron and steel have been studied by the use of perchloric acid. Tungsten can be precipitated quantitatively with a single fuming of perchloric acid by the following treatment: the sample is dissolved in aqua regia and evaporated to white fume after addition of 50 c. c. of perchloric acid; after cooling, dilute hydrochloric acid is added and its total volume is made up to 150c. c. so as to adjust the concentration of hydrochlioric acid between 1_??_1.5 N. The solution issued is Warmed at 70_??_80° for an hour and then filtered. Applying this method also to the rapid determination, we have found that tungsten would be determined in about 20 minutes.

Determination of Metals in Alkaline Solution with Oxine

1. 酒石酸ソーダ含有のNaOHのアルカリ性溶液に於てCa, Mg, Cd, Zn及Cuをオキシンに依り定量を行ふ時,完全に沈澱するNaOHの濃度及び沈澱全く生成せざるに至るNaOHの濃度範圍を求めた.2. 上記5金属の完全に沈澱するNaOHの最大濃度及び沈澱全く生成せざる最小濃度は第1表に示す.3. 完全に沈澱するアルカリの濃度範圍に於てCdは沈澱量多くなりて定量は不可能である. Znは少しく多くなり正確なる定量法と云ふことは出來ない.又Caは稍少くなる傾向あり. Mg及びCuは正確なる定量法なることを明かにした.