SKALARMETHODS

APPENDIX


SAN++
Issue110113/MH/99283511

ForTotalCyanide

Sulfideandsulfidecontainingcompoundsarepositiveinterferentsinthismethod.Whenacidified,sulfide
formshydrogensulfide,whichpassesthroughthegasdiffusionmembraneandproducesasignalatthe
silverelectrode.Inaddition,sulfideionreactswithcyanideioninsolutiontoreduceitsconcentrationover
time.TreatsamplescontainingsulfideaccordingtonextSection.DuringUVdigestion,somesulfur
compoundsmayproducesulfide.TA2reagentcontainsasulfidescrubberthatcanremoveupto50
mg/literS2fromthesystempriortoamperometricdetection.SulfideTestforthepresenceofsulfideby
placingadropofsampleonaleadacetateteststripthathasbeenpreviouslymoistenedwithacetate
buffer.Iftheteststripturnsblack,sulfideispresent(above50mg/literS2)andtreatmentisnecessary.If
thetestisnegativeandtherearenofurtherinterferencessuspected,adjustthepHto1213,refrigerate,
andshiportransporttothelaboratory.Ifthesamplecontainssulfideasindicatedwithaleadacetatetest
striporisknowntocontainsulfidesthatwillinterferewiththetestmethod,dilutethesamplewithreagent
wateruntiltheleadacetateteststripnolongerindicatesthepresenceofsulfide(<50mg/literS2).For
example,add200mloffreshlycollectedsampleintoabottlecontaining800mlofreagentwater,thentest
forsulfideagainasindicated.Ifthetestforsulfideisnegative,adjustthepHto1213,refrigerate,andship
ortransporttothelaboratory.Ifthetestforsulfideisstillpositive,furtherdilutionisrequired;however,be
carefulnottooverdilutethesampleasthedetectionlimitwillbeelevatedbythisfactor.Inthe
aforementionedexample,thedilutionfactorwouldbeequalto5(totalvolume/samplevolume).Clearly
indicatethedilutionvolumesonthesampleandchainofcustodyformsothatthelaboratorycan
mathematicallycorrecttheresult.

NOTESomeanalyticalmethodsprescribetheuseofleadcarbonateorleadacetatetoprecipitatesulfide;
however,sulfideandcyanidecanformthiocyanateinthepresenceofleadcausingdecreasedcyanide
recoveries;therefore,leadcarbonateandleadacetateshouldbeavoided.Methodsthatspecifythe
additionofbismuthnitratetotreatsulfideduringtotalcyanidedistillationshavebeendemonstratedby
ASTMD19.06tobeineffective.

NOTECaution:CyanidecanbeconvertedintothiocyanateinthepresenceofsulfideatahighpH,causing
highresults.

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