AD-A221
COPY
135
AD
BY PRECIPITATION.FORMATION TITRATION
SAMUEL SOPOK
DTIC
,IARCH
'990
,ff0
05
o"
04lf
I
I
OISCIAIMER
Thc findings
DcPartncnt
docrrcnts.
DESTRUCTIGi NOTIG
I}oD
in
DoD s2oo.22-t1,
s2oo.l-R, Info:ration
stc
;=;
REFoRT
PERloo covEto
TN COPPER
DETERMINAION OF SODIIJM CYA{IDE
BY
SOLUTIONS
PIATING
AND CADMIIJ}'! CYA}IDE
PRECIP ITATION-FORMATION TTTRATION
iEIxrttox
U.S.
ErG
ArnY A3DEC
ffi^Ho^oonEss
Arff,Y
truraen
xaE
U.S.
,ffi.nEPonr
March l99O
ARDEC
Approved
@ocnGD")
Chenical AnalYsis
laa
Plating Solutions
Platinq Solutions
Titration
ion-Formation
PreciPitat
Cadnium CYanide
SodiLn CYanide
Copper Cyanide
ffirrtrDlocli'at
adequarelv
lacks an acceptable analvtical merhod ro
cadmirm-::::t:i*:tl:
d
detennine and monitor sodium cva'a-li coPper
::::ffiH i:"J:";;:i"n"ni""';;;:of this salt in these
*"it"ring-1"^:':il:':,T:'l:ui:
presented providing "."pi"r" .rr"ry=i" .r,a
cyanide are 58 g'l1
salun
plating nrocess.-.s.' *: ptin* o'.r"iir,i--t*g""-of
maxi.mum in copper .r.r,iu'n,;;i"; ="i:il;":I?1:-n1:-'.?:tTH
ranse of
in rhe :1"::T.,*
preclsiel:
.I;l:T.ff;
il"r..*"
ii'r'i",'"r:::
]}lH ;1.;::;':";il;:.'^il."l"lii.1ns
DO t
toL
,at rl
rm
or?o
o, t tloY
aS 13
o.lo|.Etc
. CONTID 1:"
ON RE:VERSE)
[,NCI.ASSIFIED
aCUtttV CLA3tFtCAftOX OF fXt3 ,AOClrr D... a..?.)
TAELE OF COIITEI{TS
Eese
ACKNOI{LEDGEMENTS
ITROOUCTION....
i
1
EXPERIHENTAL PROCEDURE
...
REF
EREI{cES
TABLES
:,
:I.
IN
COPPER
III.
IN
CAOMIUM
:V.
PRECISION
v.
PRECISION OF
VL
PRECISION OF
VII.
PRECISION OF
STANOARO SOLUTION
SOLUTION
NTIS
GFA&I
u
n
DTI,C IB
Uannouced
i JusttflraLl
I
in,t I
idi-_t_
I
ACTilOXLEDGE!,IET{TS
Specia) thariks are given to E'l]en Fogarty and Rose Neifeld of Benet
;aboratories for their rssDective word processing and technical editing work on
th'is nanuscriot.
11
^l
IT{TROOUCTIOtr
The chemical
method
to deternine
and monitor sodium cyanide in copper and cadmium cyan'ide plat'ing solutions in
causes
serious problems for the me'ral finishing industry sueh as poor quality products
and wasted resources.
only
The
common
these solutions
is a co] or
to determine
test kit
comparison
cyanide in
sod'ium
specific
The
and
mon'i
method described
acceptab'le analysis
PROCEOURE
orocedure
sect.ion.
is by Fritz
An
and Schenk
(ref 3).
a 50 + 0.S-gt
tion),
'1 sodium
cyanide solution
is a
1? 1
(l g/1
sodium hydroxide
t,i
trant
rs
ution.
These
indicator
powder and
The procedure
ammoni,m hydrox.ide
solution.
same
for
the
beaker.
and a
Then
the beaker is fil]ed to about the 100-ml mark with deionized v{ater
iodtde'indicator
The
anc!
added
gram
of
potassium
amount
ye11ow
All standard
cyan'ide concentrations
in triplicate.
Sod'ium
chemical
stoiciliometry.
RESULTS ANO OISCUSSIOI{
Exoerimenta'l standard
solutions.
Experimenta'l sample
copper cyanide sample so] ut'i ons one and two and
sample
these
cadmium cyanide
solutions three and four. The titration can be summarized using the
fo!lowing equations. The f irst tvro involve the cyanide-si'l ver ion relationsh'io
ano the th'i
Sriver
cyan'icle
ammonium
ationship:
(1)
\)
2A9CN
(3)
AgI
The calcu'lat'ion
original
* I- <-->
re'l
sample so'l
sodium cyanide
in
the
utions is
g/'l
NaCN
= (50)(All(B)
()
where
where
(
refs
the constant
Eq.
(4
standard
many constants
2,3 ) .
Using Eq.
samo'le
ihe
va'l ue i n
titrant for
= m] of
samole
solutions one and two in Table II are 35.1 and 49.9 g/1. Lirewise,
same
samo]e
rrsno
solutions three and foulin fable III are 84.9 and 140.1
gz1.
efficient use of
resources. fhe opt'imum operating ranges of sodium cyan'ide are 58 q,l max:rnrm :n
the coooer cyanide platrng solrtions and 149 gr'1
maximum
in the caomium.:yan.:r)
oirting onl*.iions. he nesu'l t'ing precisions are in the range of 0.5 rc t.0 :.
orovioing adequate monitoring of these metal finishing solutions suoporteo bv
srx years of testing.
,a
REFEREIICES
t.
"EM Quant
Corooration, Cherry
2.
0. Peters, J.
H'i
Elt
Science Civision
of
Herck
l, NJ, 1980.
of Analytical
Chemistrv, W.
B.
Saunders
Company
i. Fritz and G.
A1
Schenk,
q@cal
Chen.istrv, Fif
198?
_^
th
Ectitron.
TAELE
Rep I
I.
Titrant
icates
Used (ml)
10. 2s
10. 20
10.20
((avgl
t0.22
r
_t
TABLE
II.
i
Sample One
I - i '-nt Jsed
-----t---
Sample
(ml
Two
:<
10. 20
?. i5
10. 20
.20
10. 20
?.1?
10.20
TAELE
III.
----f
I
?eO; rCareS
I
Samg
le 'hree
--T-I
' _ :::_:':11.''''
Samole Forr
__L__""1: :'"0
i?.35
28. 60
1?.35
28,65
1?.35
28. 65
1?.35
28. 63
x(avg)
'*''
AELE
Rep l
IV.
PRECISIOT OF
A 2-MI CLASS.A
PIPET
2-ml Pipet
volume (ml)*
icate
2.01
i .99
.99
.99
.01
.00
x(avg)
Sn
.00
0.01
V.
PRECISIO}I OF
A 5O.g/.I soolut
Reo l i
cate
49. 9?
49. 99
9.99
50.01
50.00
50.02
X(avg)
Sn
50.00
a,o2
are :alculated.by
methods
TABLE
/I.
PRECISIOT{ C2
Repl
icate
Si'lver
TTRANT SOLUTIOT{
trat
N'i
1?.1
1?
t7 .2
16.8
16. 9
16.8
(avg)
17.0
.0
o.2
Sn
__J
VII.
Rep I : cate
A sO.mI CLASS.A
24.9A
25.02
25.05
24.98
25. 05
Sn
BURET
Volume 11 *
'I
x(avg)
*Volumes are
PRECISION OF
.98
25.00
0.0
calculated from the Height-volume relationship of a contained deionized ,rater solution corrected
or temperature at a point one-half ful'l --25 rnt.
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