208 Z. Anal. Chem.

, Band 268, Heft 3 (1974)

Volumetric Determination
of Gold using Oxalic Acid
Volumetrische Goldbestimmung mi t Hilfe yon Oxals~ure
Best. yon Gold mi t Oxals~ure; Volumetrie
S. C. S. Raj an and N. Appal a Raj u
Depar t ment of Chemistry, S. V. Uni ver si t y
Ti rupat i , A. P. , I ndi a
Recei ved J ul y 10, 1973; revised October 1, 1973
I t ha s b e e n f o u n d t h a t oxa l i c a c i d c a n e a s i l y r e d u c e
gol d i ons t o me t a l q u a n t i t a t i v e l y e ve n i n a c i d me d i u m
p r o v i d e d t h e c hl or i de c o n c e n t r a t i o n i s k e p t t o a
mi n i mu m, t h e p H a d j u s t e d t o 1 . 5 - - 1 . 8 a n d t h e
r e a c t i o n c a r r i e d o u t a t a h i g h e r t e mp e r a t u r e . Sul -
p h a t e i ons e x e r t a f a v o u r a b l e ef f ect on t h e r e a c t i o n
r a t e . Pr o c e d u r e s h a v e b e e n wo r k e d o u t f or t h e
d e t e r mi n a t i o n o f g o l d i n pr e s e nc e o f i r on, c o p p e r a n d
zi nc a n d al s o o f p l a t i n u m a n d p a l l a d i u m a s f ol l ows :
Gold Determination in the Presence o/Pt and Pd. The sample
solution is evapor at ed over hot wat er bat h [1]. The residue
is dissolved in water, 5- - 10 ml of sat ur at ed K2SO ~ sol ut i on
are added, t he solution di l ut ed t o 100 ml and t he pH ad-
j ust ed t o 1. 5--1. 8 wi t h 5 N H2SO 4. The solution is heat ed
to 78--80~ 25 t o 30 ml of 0.1 N oxalic aci d solution are
t hen added wi t h st i rri ng at a r at e of 2- - 3 ml per minute,
mai nt ai ni ng t hi s t emperat ure. The heat i ng is cont i nued for
anot her 3 rain and t he contents are allowed t o cool. 50 ml
of 8 N sulphurie aci d followed by 25 ml of Zimmermann-
Rei nhar dt ' s reagent are t hen added and t he solution is
t i t r at ed wi t h 0.05 N permanganat e. A drop of t he redox
i ndi cat or, ferroin (0.025 M) is added near t he end poi nt ;
t he colour changes from r ed t o yellowish green. A slight
t ur bi di t y in case of Pd does not interfere.
Gold Determination in the Presence el Fe, Cu and Zn. The
solution is evapor at ed over hot wat er bat h in t he presence
of 5 t o 10 drops of cone. sulphuric acid, t aki ng care t hat t he
solution does not become compl et el y dry. The mass is
t r eat ed wi t h dist. water, t he pH adj ust ed t o 1.5 t o 1.8 wi t h
5 N NaOH solution while diluting i t t o 100 ml and t he anal ysi s
continued as described above. The colour change is from
deep red t o blue.
I n t h e f i r s t cas e 3 1 - - 4 9 mg of gol d h a v e be e n
d e t e r mi n e d i n pr e s e nc e o f a ma x i mu m a mo u n t of
80 mg o f p l a t i n u m a n d 60 mg o f p a l l a d i u m wi t h
e r r or s i n t h e r a n g e of 0. 00 t o - - 0. 780/ 0. I n t h e s e c ond
case, 2 4 - - 3 1 mg of gol d g a v e e r r or s o f - - 0. 850/ 0 t o
--}- 0. 65 ~ i n pr e s e nc e of f i ve- f ol d exces s o f ba s e me t a l .
Reference
1. Beamish, F. E. : Anal yt . chemi st r y of noble metals, p. 312.
Pergamon Press 1966
Prof. Dr. N. Appal a Raj u
Depar t ment of Chemi st ry
Sri Venkat eswara Uni ver si t y
Tirupati-517502, I ndi a
Specific Spot Test for Nitrite
with Sulphaguanidine
Spezifischer Tiipfe]nachweis yon Ni t r i t mi t Sulfaguanidin
Nachw. yon Iqi t ri t mi t Sulfaguanidin; Tiipfelprobe
G. S. Johar
Depar t ment of Chemistry, V. S. S. D. College
Kanpur , I ndi a
Received July- 6, 1973
A n e w c ol our t e s t i s r e p o r t e d f or t h e s i mp l e s p o t t e s t
d e t e c t i o n of NO2- i on us i ng t h e c o mmo n s ul phon-
a mi d e , s u l p h a g u a n i d i n e . Th e t e s t i s so h i g h l y speci f i c
t h a t t h e r e i s p r a c t i c a l l y no i n t e r f e r e n c e b y a n y of t h e
c o mmo n or l ess c o mmo n c a t i o n s or a n i o n s (i n-
e l u d i n g I % N3- , 103- , a n d 1 0 4 - ; p r o v i d e d me d i u m
of t h e t e s t s o l u t i o n i s n e u t r a l ) .
Procedure. A drop of neut r al or sl i ght l y acidic t est solu-
t i on is pl aced on filter paper and t r eat ed wi t h a drop of 1.5~
sulphaguanidine solution in di l ut ed hydrochloric acid. The
spot t ed par t of t he paper is t hen exposed over t he mout h
of a bot t l e containing cone. ammonia solution. A deep
orange-yellow or yellow fleck appears i f ni t ri t e is present.
Li mi t of det ect i on: 5 ~g NO 2-; l i mi t of di l ut i on: 1 : 10,000.
The reagent solution was prepared by dissolving 1.5 g of
powdered medical grade (t abl et form) sulphaguanidine in
100 ml di l ut ed HC1 (95 ml wat er + 5 ml cone. acid).
Dr. G. S. J ohar
Depar t ment of Chemistry
Vi kr amaj i t Singh Sanat an Dhar ma College
Kanpur , U. P. 208 002, I ndi a