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Aldonna !asa rlma urba
Lva Arlanl
llLrl llrdausl Ashadl
8ogor Plgh School of Chemlcal AnalysL
Introduct|on of L|m|t 1est
n ChemlsLry llmlL means a value or amounL LhaL ls llkely Lo be presenL ln a subsLance
and LesL means Lo examlne or Lo lnvesLlgaLe 1hus llmlL LesL ls noLhlng buL Lo ldenLlfy Lhe
lmpurlLles ln Lhe subsLance and compare lL wlLh sLandard n general llmlL LesL ls deflned as
quanLlLaLlve or seml quanLlLaLlve LesL deslgned Lo ldenLlfy and conLrol small quanLlLles of
lmpurlLy whlch ls llkely Lo be presenL ln Lhe subsLance LlmlL LesL ls generally carrled ouL Lo
deLermlne Lhe lnorganlc lmpurlLles presenL ln compound
LlmlL LesL of chlorlde ls based on Lhe reacLlon of soluble chlorlde wlLh sllver nlLraLe ln
presence of dlluLe nlLrlc acld Lo form sllver chlorlde whlch appears as solld parLlcles
(Cpalescence) ln Lhe soluLlon
LlmlL LesL of heavy meLals ls based on Lhe reacLlon of meLalllc lmpurlLles wlLh hydrogen
sulflde ln acldlc medlum Lo form colored soluLlon MeLals LhaL response Lo Lhls LesL are lead
mercury blsmuLh arsenlc anLlmony Lln cadmlum sllver copper and molybdenum
Def|n|t|on of L|m|t 1ests
LlmlL a value or amounL LhaL ls llkely Lo be presenL ln a subsLance
1esL Lo examlne or Lo lnvesLlgaLe
mpurlLles a forelgn maLLer presenL ln a compound
1he urpose Cf LlmlL LesLs
1o flnd ouL Lhe harmful amounL of lmpurlLles
1o flnd ouL Lhe avoldable/unavoldable amounL of lmpurlLles
L|m|t 1est of Ch|or|de
LlmlL LesL of chlorlde ls a common procedure Lo seL a llmlL of chlorlde conLalned ln each
monograph erform LesLlng and comparlson uslng a palr of glass Lubes wlLh a same dlameLer
and comparable as posslble as lL appears on Lhe specLrophoLomeLrlc and vlsual comparlson of
llghL scaLLerlng
use Lhe amounL and same reagenLs ln Lhe sample and sLandard soluLlon conLalnlng a
cerLaln volume of chlorlde f afLer acldlfled soluLlon ls noL clear fllLer Lhe soluLlon wlLh fllLer
paper whlch does noL reacL Lo Lhe chlorlde Add a soluLlon of sllver nlLraLe LhaL are necessary ln
Lhe sample and sLandard soluLlon aL Lhe same Llme f ln each monograph Lhe sample soluLlon
ls on cerLaln volume and llmlLs chlorlde same Lo or less Lhan sLandard LesL Lhem wlLhouL
furLher dlluLlon n Lhls case keep Lhe volume beLween sample and sLandard soluLlon 1o LesL
heavy meLal salLs whlch generally reacL acld remove Lhe addlLlon of acld and Lhe soluLlon
should noL be neuLrallzed
r|nc|p|e
LlmlL LesL of chlorlde ls based on Lhe reacLlon of soluble chlorlde wlLh sllver nlLraLe ln presence
of dlluLe nlLrlc acld Lo form sllver chlorlde whlch appears as solld parLlcles (Cpalescence) ln Lhe
soluLlon
rocedure
1est samp|e Standard compound
ulssolve sample ln 30 ml or 40 ml of waLer lf
Lhe sample ls solld f sample ls soluLlon dlluLe
Lhe sample unLll 30 ml or 40 ml wlLh waLer and
lf lL's needed neuLrallze Lhe sample wlLh nlLrlc
acld and use llLmus paper as lndlcaLor and
Lransferred ln nessler cyllnder
1ake 1ml of 003843 W/v soluLlon of sodlum
chlorlde ln nessler cyllnder
Add 1ml of nlLrlc acld Add 1ml of nlLrlc acld
Add 1ml of AgnC
3
soluLlon Add 1ml of AgnC
3
soluLlon
ulluLe Lo 30ml ln nessler cyllnder ulluLe Lo 30ml ln nessler cyllnder
keep aslde for 3 mln keep aslde for 3 mln
Cbserve Lhe Cpalescence/1urbldlLy Cbserve Lhe Cpalescence/1urbldlLy
Cbservat|on
1he opalescence produce ln sample soluLlon should noL be greaLer Lhan sLandard soluLlon f
opalescence produces ln sample soluLlon ls less Lhan Lhe sLandard soluLlon Lhe sample wlll pass
Lhe llmlL LesL of chlorlde and vlsa versa
keasons
nlLrlc acld ls added ln Lhe llmlL LesL of chlorlde Lo make soluLlon acldlc and helps sllver chlorlde
preclplLaLe Lo make soluLlon Lurbld aL Lhe end of process
L|m|t 1est of Sod|um
Sod|um ||m|t test
llame phoLomeLer equlpped wlLh a phoLoLube deLecLor mulLlpller for Lhe deLermlnaLlon of
calclum or sodlum deLecLor Lubes senslLlve Lo red llghL for Lhe deLermlnaLlon of poLasslum
monochromaLor sllL ls easlly conLrolled senslLlve conLrol devlce and oxlaceLylene
burner Cxlhydrogen burner requlred for Lhe deLermlnaLlon of poLasslum ln Lhe mlx wlLh large
amounLs of calclum
Standard so|ut|on of sod|um |ons
LnLer 2342 mg of sodlum chlorlde LhaL has been drled aL a LemperaLure of 103
o
C for 2 hours
lnLo a 100 ml volumeLrlc flask dlssolve and dlluLe wlLh waLer up Lo Lhe mark Lach mllllllLer of
soluLlon conLalnlng 100 mg of sodlum (na)
Standard so|ut|on
LnLer a 30 ml allkoL" sample soluLlon lnLo 100 ml volumeLrlc flask cooled ln refrlgeraLor add 3
ml of concenLraLed nlLrlc acld shake unLll dlssolved and leL lL warm up Lo room LemperaLure f
necessary reheaL carefully Lo geL mlxLure of clear or only sllghLly Lurbld Cooled Lo room
LemperaLure lf necessary dlluLe wlLh waLer Lo Lhe mark f necessary fllLer or cenLrlfuge Lo
obLaln clear soluLlon
SeL flame phoLomeLer obLalned close Lo 100 LransmlLLance Lo sLandard soluLlon aL a
wavelengLh whlch glves maxlmum emlsslon correspondlng Lo a speclflc wavelengLh use Lhe sllL
wldLh correspondlng as near as posslble Lo Lhe speclfled bandwldLh WrlLe Lhe LransmlLLance
ulluLe allkoL" soluLlon wlLh waLer Lo geL same concenLraLlon wlLh sLandard soluLlon WlLhouL
changlng Lhe seLLlng condlLlon of Lhe flame phoLomeLer deLermlne emlsslon soluLlons as a
percenLage of Lransmlsslon wrlLe Lhe resulL 1he reorganlzaLlon of Lhe monochromaLor Lo Lhe
wavelengLh seL for Lhe deLermlnaLlon of Lhe background SeL emlsslon aL a wavelengLh soluLlon
as a percenLage of Lransmlsslon and wrlLe Lhe resulL
keferences
hLLp//wwwwebformulascom/lormulas_of_ChemlsLry/ChemlsLry_LlmlL_LesLaspx
hLLp//wwwwebformulascom/lormulas_of_ChemlsLry/ueflnlLlon_of_LlmlL_1esLsaspx