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Polarographic determination of arsine in gaseous mixtures (in German).
A 52
Journal of Electroanalytical Chemistry
VOL. 1
avec une e r r e u r max. de 10% ~ p a r t i r de 3 ~ 10 ml de sang complet, le volume final 6rant de 0.5 m l. Le p o l a r o g r a p h e R rayons cathodiques p e r m e t de d o s e r 0.05 ~tg de plomb p a r ml. De. Mo. STUDY OF THE ANALYSIS OF LEAD IN CRUDE C O P P E R BY A. C. POLAROGRAPHY. K . I t s u k i , F. Suzuki and F. Sato. J a p ° A n a l ° , 8 (1959)92. Lead in crude c o p p e r was d e t e r m i n e d in an e l e c t r o l y t e of I M KCN, 1.5 M NaOH, 4% Na2SO a solution by using an a . c . polarograph. The ao c. and d. c. p o l a r o g r a p h i c m et h od s w e r e c o m p a r e d , and in e v e r y case the s . c , method was cons i d e r e d m o r e suitable f o r routine work. Ta. Fu. [165] POLAROGRAPHIC DETERMINATION OF ARSINE IN GASEOUS MIXTURES (in G e rm an . ) V. Va§~k. (Institute f o r Ind. Hygiene and Occupational D i s e a s e s , P r a g u e , C z e c h o s l o v a k i a . ) Collect° C z e c h o s l o v . Chem. C o m m u n s . , 24 (1959) 3500, In 0.1 M NH_4 NO 3 in 85% ethanolie solution a r s i n e shows an anodic p o l a r o g r a p h i e wave with a h a i f - w a v e potential +0.01 V (vs. sat. m e r c u r o s u l f a t e e l e c t r o d e ) . The h a l f - w a v e potential is a function of the pH. The l i m i t i n g - c u r r e n t c o r r e s p o n d s to an e i g h t - e l e c t r o n oxidation to a r s e n a t e and is pH-independent. The wave was o b s e r v ed with a P t - v i b r a t i n g e l e c t r o d e w h i e h p r o v e s that the wave is not caused by f o r mation of a s a l t o r c o m p l e x with m e r c u r y . F o r analytical p u r p o s e s waves produced in solutions of concentration l o w e r than 5 . 10-4 M As3H a r e suitable. PH 3 and SbH 3 i n t e r f e r e . The concentration of AsH 3 in the supporting e l e c t r o l y t e is 2.8 t i m e s h i g h e r than in the gaseous m i x t u r e . As the solubility is strongly dependent on the t er ~ p er at ur e , the analysis as well as the cal i b r at i o n is p e r f o r m e d while the gaseous m i x t u r e of n i t r o g e n and a r s i n e (or the analyzed sample) is being introduced into the supporting e l e c t r o l y t e in the p o l a r o g r a p h i c v e s s e l with the t e m p e r a ture of 25 ° c a r e f u l l y controlled, P. Zu. [166] POLAROGRAPHIC DETERMINATION OF ARSENIC IN IRON AND S T E E L . H. A s a oka. Jap, A n a l . , 8 (1959) 774. 1 g of the sample was d i s s o l v e d in 16 ml of (1+1) HNO3 with heating and diluted to 100 ml with water. A f t e r the addition of 5 ml of 5% Mn(NO3) 2 solution, the so lution was heated to boiling point and 3 ml of 2% KMnO 4 solution was added; it was then continuously boiled for 2 - 3 min. A f t e r f i l t e r i n g and washing, the p r e c i p i t a t e was d i s s o l v e d with 30 ml of (1+29) H2SO4 and a few drops of 30% H202 solution in a d i s t i l l i n g flask, and then the solution was e v a p o r a t e d to give SOs fumes. A f t er cooling 20 ml of concentrated HC1, 0.5 g of hydrazine sulfate and 2 ml of hypophosphorous acid w e r e added to the flask, and the d i s t i l l a t i o n was p e r f o r m e d in a s t r e a m of carbon dioxide. The d i s t i l l a t e was co l l ect ed in 50 ml of cold H20 in a s m a l l b e a k e r . The solution a f t e r being t r a n s f e r r e d to a 100 ml v o l u m e t r i c flask which contained 15 g of t a r t a r i c acid, was diluted to the m a r k with w a t e r and 2 m l of 0.2% gelatin solution was added. The p o l a r o g r a m of the solution was r e c o r d e d in the usual m a n n e r , and the f i r s t wave of a r s e n i c o c c u r r e d at -0.33V vs. S . C . E . Ta. Fu. [167] POLAROGRAPHIC DETERMINATION OF TRACES OF BISMUTH IN PURE SILVER BY THE USE OF A SODIUM C I T R A T E - E D T A MIXTURE AS THE SUPPORTING E L E C T R O L Y T E . M. Ishibashi, T. Nagai, T. Fujinaga and W. Funasaka. Jap. A n a l . , 8 (1959) 107. 40 g of the Ag sample was d i s s o l v e d in cone. HNO3 and 2 ml of 0.1 M AI solution, 40 ml of 4 M NH4NO3 and 60 ml of conc. NH4OH w e r e added. The AI(OH)a p r e c i p i t a t e which c a r r i e d down the Bi was dissolved, and the p r e c i p i t a t i o n r e peated again, 3 g of sodium c i t r a t e and 1 ml of 0.2 M EDTA w e r e added, the pH
Journal of Electroanalytical Chemistry
VOL. 1
avec une e r r e u r max. de 10% ~ p a r t i r de 3 ~ 10 ml de sang complet, le volume final 6rant de 0.5 m l. Le p o l a r o g r a p h e R rayons cathodiques p e r m e t de d o s e r 0.05 ~tg de plomb p a r ml. De. Mo. STUDY OF THE ANALYSIS OF LEAD IN CRUDE C O P P E R BY A. C. POLAROGRAPHY. K . I t s u k i , F. Suzuki and F. Sato. J a p ° A n a l ° , 8 (1959)92. Lead in crude c o p p e r was d e t e r m i n e d in an e l e c t r o l y t e of I M KCN, 1.5 M NaOH, 4% Na2SO a solution by using an a . c . polarograph. The ao c. and d. c. p o l a r o g r a p h i c m et h od s w e r e c o m p a r e d , and in e v e r y case the s . c , method was cons i d e r e d m o r e suitable f o r routine work. Ta. Fu. [165] POLAROGRAPHIC DETERMINATION OF ARSINE IN GASEOUS MIXTURES (in G e rm an . ) V. Va§~k. (Institute f o r Ind. Hygiene and Occupational D i s e a s e s , P r a g u e , C z e c h o s l o v a k i a . ) Collect° C z e c h o s l o v . Chem. C o m m u n s . , 24 (1959) 3500, In 0.1 M NH_4 NO 3 in 85% ethanolie solution a r s i n e shows an anodic p o l a r o g r a p h i e wave with a h a i f - w a v e potential +0.01 V (vs. sat. m e r c u r o s u l f a t e e l e c t r o d e ) . The h a l f - w a v e potential is a function of the pH. The l i m i t i n g - c u r r e n t c o r r e s p o n d s to an e i g h t - e l e c t r o n oxidation to a r s e n a t e and is pH-independent. The wave was o b s e r v ed with a P t - v i b r a t i n g e l e c t r o d e w h i e h p r o v e s that the wave is not caused by f o r mation of a s a l t o r c o m p l e x with m e r c u r y . F o r analytical p u r p o s e s waves produced in solutions of concentration l o w e r than 5 . 10-4 M As3H a r e suitable. PH 3 and SbH 3 i n t e r f e r e . The concentration of AsH 3 in the supporting e l e c t r o l y t e is 2.8 t i m e s h i g h e r than in the gaseous m i x t u r e . As the solubility is strongly dependent on the t er ~ p er at ur e , the analysis as well as the cal i b r at i o n is p e r f o r m e d while the gaseous m i x t u r e of n i t r o g e n and a r s i n e (or the analyzed sample) is being introduced into the supporting e l e c t r o l y t e in the p o l a r o g r a p h i c v e s s e l with the t e m p e r a ture of 25 ° c a r e f u l l y controlled, P. Zu. [166] POLAROGRAPHIC DETERMINATION OF ARSENIC IN IRON AND S T E E L . H. A s a oka. Jap, A n a l . , 8 (1959) 774. 1 g of the sample was d i s s o l v e d in 16 ml of (1+1) HNO3 with heating and diluted to 100 ml with water. A f t e r the addition of 5 ml of 5% Mn(NO3) 2 solution, the so lution was heated to boiling point and 3 ml of 2% KMnO 4 solution was added; it was then continuously boiled for 2 - 3 min. A f t e r f i l t e r i n g and washing, the p r e c i p i t a t e was d i s s o l v e d with 30 ml of (1+29) H2SO4 and a few drops of 30% H202 solution in a d i s t i l l i n g flask, and then the solution was e v a p o r a t e d to give SOs fumes. A f t er cooling 20 ml of concentrated HC1, 0.5 g of hydrazine sulfate and 2 ml of hypophosphorous acid w e r e added to the flask, and the d i s t i l l a t i o n was p e r f o r m e d in a s t r e a m of carbon dioxide. The d i s t i l l a t e was co l l ect ed in 50 ml of cold H20 in a s m a l l b e a k e r . The solution a f t e r being t r a n s f e r r e d to a 100 ml v o l u m e t r i c flask which contained 15 g of t a r t a r i c acid, was diluted to the m a r k with w a t e r and 2 m l of 0.2% gelatin solution was added. The p o l a r o g r a m of the solution was r e c o r d e d in the usual m a n n e r , and the f i r s t wave of a r s e n i c o c c u r r e d at -0.33V vs. S . C . E . Ta. Fu. [167] POLAROGRAPHIC DETERMINATION OF TRACES OF BISMUTH IN PURE SILVER BY THE USE OF A SODIUM C I T R A T E - E D T A MIXTURE AS THE SUPPORTING E L E C T R O L Y T E . M. Ishibashi, T. Nagai, T. Fujinaga and W. Funasaka. Jap. A n a l . , 8 (1959) 107. 40 g of the Ag sample was d i s s o l v e d in cone. HNO3 and 2 ml of 0.1 M AI solution, 40 ml of 4 M NH4NO3 and 60 ml of conc. NH4OH w e r e added. The AI(OH)a p r e c i p i t a t e which c a r r i e d down the Bi was dissolved, and the p r e c i p i t a t i o n r e peated again, 3 g of sodium c i t r a t e and 1 ml of 0.2 M EDTA w e r e added, the pH