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New specific reagent for palladium
‘1’11c t-ttoditied clectrotle lxwvd study of vxxicliutn it1 IJMI;.
gr:tpltic
most satisfactc,ry as a rafcrcnce in a polaroTJic Iialf-wave potcntids twt-c consistett and
;tgred ClOSCly With tflC Jxltenti:L!s given by &~ict%8_~tnx’tx AstJ Gt_x,\fx\xxa, WllO reported -2.03 V ‘us. S.C.E. Over a six-month pwiocl, tltc half-wave ;L ha1 f-wave potcntiaf of lwtcntial for tire sxmc reduction against tlte cadmium reference elec:trodc was - I .3r V witlt a stnndarcl deviation of 14 mV. Conversion to an S.C.E. refcrenw gave ;L ltalfwave potcntinl value of -2.og V.
New
specific
reagent
for
palladium
111 spite of tfte large numlxx of gcmcl rc;tgent_s for tlic iclcntifiontictn of lx&tbcwusc it rrl~pt-oacltcs vcr~ cl(>scly to an tlium 1, ;L ticiv rcnpx t clcst~rvcs description Tltis new rcagcnt is a colorless cott~pouncl wlticlt is cxsily ohtaincxl by icltxd rcapnt. tltc c~~itd~nsiitiott of cliucc~\~lntonosimc it,tt.(I 2-lt~clrnz;it~ol~~t~~otlti:~xolc : CHJ-C=N-OH CX3 --c=o
‘-42N -Nl-i--C
+
I
ttl
l-i20
+
CH3-c=hlOH I
f%
-_Cs=kJ-NH-CC Iii
wiclo range of l)HIt rcwts scnsitivcly with lx~lladiutn ovct ;i surprising1y front concentrated Iiyclroclrloric acid to conccntratccl itIlltTlOtli;t. solution-yiclcling a red-violet complcs c0tnlxx.tncl wlticlt ca.n lx extracted into clilorofortn. In analogy to nirkcl-ditncttt~lgl~osim~, it swtns likely iftat tttc inner coml~les salt pwcnts the formula: CU-,--C=N
/” \
/ I Ct-+-C=N-NH---C
Pd/2 tll
SHORT
=27
~:OMZtlI;FiICATIOSS
Solutions of the following ions were treated with an alcoholic aluminum, antimony, arsenic, reagent in alkaline and acid medium:
solution
of the
barium, beryllh.xm, bismuth, cadmium, calcium, cerium, cesium, c~~r~llliu~l(~II), cobalt, copper, gallium, germanium, gold, indium, iron, lead, lnntfwnum, lithium, magnesium, nickel, niobium, platinum, potassium, rlxodium, manganese, mercury, molybdenum, ruthenium, silver, sodium, strontium, tantalum, thallium, thorium, tin, titanium, tungsten, uranium, vanadium, zinc and zirconium. Disregarding the formation of hydroxide precipitates, only cobalt in alkaline meclium produces ;L reel compound (limit of identification 0.5 l4g) ; in nciclic solution none of tile ~~lx~veions interferes.
~‘?‘CJO?t~lWC
01 wicl solution is trcntcd in i1 micro test tube with 3-4 prwencc Of l>i~llZldiUIll a red-violet compouIld is formed \vllicll CLLII1x2estractcd wit11 5 drops of c:l~loroform. I_imit of idem!ificatio~i. 0.25 pg pllxlium. I.htz2 Of ciikrtio,a. I :200.000. In tlrc presence of cobalt the reaction must be made in acidic media. Fluoride, tartrate, citrate and osalate do not interfere; only cyanide prevents the reaction. It is pw,sihlc ta cletect p&ladium in alloys hy treating a ssnall amount of tlx s~tuiplc~witir z--3 drops of atpa ref.& and then \x+tlr a few clrcqxs of tltc reagent,
i\
drops
of
(Iicccivccl
tlrcq) of alkalirii!
tlie
I-cagcnt.
L;eIxu;iry
In
Iotli,
1970)
gr:tpltic
most satisfactc,ry as a rafcrcnce in a polaroTJic Iialf-wave potcntids twt-c consistett and
;tgred ClOSCly With tflC Jxltenti:L!s given by &~ict%8_~tnx’tx AstJ Gt_x,\fx\xxa, WllO reported -2.03 V ‘us. S.C.E. Over a six-month pwiocl, tltc half-wave ;L ha1 f-wave potcntiaf of lwtcntial for tire sxmc reduction against tlte cadmium reference elec:trodc was - I .3r V witlt a stnndarcl deviation of 14 mV. Conversion to an S.C.E. refcrenw gave ;L ltalfwave potcntinl value of -2.og V.
New
specific
reagent
for
palladium
111 spite of tfte large numlxx of gcmcl rc;tgent_s for tlic iclcntifiontictn of lx&tbcwusc it rrl~pt-oacltcs vcr~ cl(>scly to an tlium 1, ;L ticiv rcnpx t clcst~rvcs description Tltis new rcagcnt is a colorless cott~pouncl wlticlt is cxsily ohtaincxl by icltxd rcapnt. tltc c~~itd~nsiitiott of cliucc~\~lntonosimc it,tt.(I 2-lt~clrnz;it~ol~~t~~otlti:~xolc : CHJ-C=N-OH CX3 --c=o
‘-42N -Nl-i--C
+
I
ttl
l-i20
+
CH3-c=hlOH I
f%
-_Cs=kJ-NH-CC Iii
wiclo range of l)HIt rcwts scnsitivcly with lx~lladiutn ovct ;i surprising1y front concentrated Iiyclroclrloric acid to conccntratccl itIlltTlOtli;t. solution-yiclcling a red-violet complcs c0tnlxx.tncl wlticlt ca.n lx extracted into clilorofortn. In analogy to nirkcl-ditncttt~lgl~osim~, it swtns likely iftat tttc inner coml~les salt pwcnts the formula: CU-,--C=N
/” \
/ I Ct-+-C=N-NH---C
Pd/2 tll
SHORT
=27
~:OMZtlI;FiICATIOSS
Solutions of the following ions were treated with an alcoholic aluminum, antimony, arsenic, reagent in alkaline and acid medium:
solution
of the
barium, beryllh.xm, bismuth, cadmium, calcium, cerium, cesium, c~~r~llliu~l(~II), cobalt, copper, gallium, germanium, gold, indium, iron, lead, lnntfwnum, lithium, magnesium, nickel, niobium, platinum, potassium, rlxodium, manganese, mercury, molybdenum, ruthenium, silver, sodium, strontium, tantalum, thallium, thorium, tin, titanium, tungsten, uranium, vanadium, zinc and zirconium. Disregarding the formation of hydroxide precipitates, only cobalt in alkaline meclium produces ;L reel compound (limit of identification 0.5 l4g) ; in nciclic solution none of tile ~~lx~veions interferes.
~‘?‘CJO?t~lWC
01 wicl solution is trcntcd in i1 micro test tube with 3-4 prwencc Of l>i~llZldiUIll a red-violet compouIld is formed \vllicll CLLII1x2estractcd wit11 5 drops of c:l~loroform. I_imit of idem!ificatio~i. 0.25 pg pllxlium. I.htz2 Of ciikrtio,a. I :200.000. In tlrc presence of cobalt the reaction must be made in acidic media. Fluoride, tartrate, citrate and osalate do not interfere; only cyanide prevents the reaction. It is pw,sihlc ta cletect p&ladium in alloys hy treating a ssnall amount of tlx s~tuiplc~witir z--3 drops of atpa ref.& and then \x+tlr a few clrcqxs of tltc reagent,
i\
drops
of
(Iicccivccl
tlrcq) of alkalirii!
tlie
I-cagcnt.
L;eIxu;iry
In
Iotli,
1970)