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Ch-1 , Impurities (PIC).pdf

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ManishKumar253026

L3 Chemical processes used in manufacturing can introduce impurities into the final product. Impurities may come from (1) reagents employed, which may contain impurities themselves or react with manufacturing equipment, (2) incomplete removal of intermediates, and (3) airborne particulate contamination during manufacturing. Proper quality control measures like purification processes and controlled storage conditions are needed to minimize impurities in pharmaceutical products.

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21 20 Dmmonia- kimit es os lson! 10 Ceale am allka lene media hepaoducedeoroplez i eoloualess In acidtc ond neutial meolta CoO Pe CH-8H e8 Eesous -Jhioglyollal comple Ctezie acid pAeveniS -lbe Daecipiation 6 Iion by ammonia Limit punciple thvotued n /he eSE 1 based on dhe &eaciion beluoe.en the Coloua infensily pacduced by -lhe Sample Sal eaLeus om0kencacis eotth ihho9l4 Colttc acid tn pzesence o6 ammoma and ciesuc acid do p&nduce hezRouslhioglyeollal Comple Sanne oz "less as eorppazed-Jo SddSol passe_ he limit dest fa I&on Colour Infensily psoduced by he Sarople Saf: smOze han heSiondaid selj 1E ads1he Aimif Hesk 1he produceod Complex 1s aeddish do puzple cotou DAoceduze: -lake a paia ofoml of The Coteus infensily depends pon the amcunt oh besous impusxires Messeas eylinelez amd label one a detE and ofhe as Slamdad Test Sid BcHe G6 Jeagent Tioglu coiti accd:- Specihced quanttly 06 ae am c6 Sid Scub dissotued ds calei ndd a Aps e6 ioglse1aEAend dd adps e /moycottteacid ia IRoDSel acts a zeducing agent tt edu eaaie hoam Dh 12en 6euous horm rio qy ee lLi'c aad ieact etdh feareus hoim 86 LAOD amd 6oem feascasdhrogtycotal Hedia t made atka line coeth ammonia. Nake cup heCOCuoe up fo 5om u/h Comple 6 Ala and altoco 6 Sland e t e min
23 22 ammoMuM CLi2o le, polasstum Cyande Aimt est Jos lead: kupola0ylammne hydtochloaide eogent e Liit es Jor lead 1s baned upon uhe Aeactibo between dead amd dtphenyldhiocarbazcne ldithozone) Pknown quoniil beSample Solution daonsfezxedlo a Sepazating upnel N=N 10 ce Gml 06 amrmonium cclzal, NHNHCsH > S N=N 3ml O pOHasstum cyamde +Pb N-N dm0hydkoxyl amine kydeochloatde d dps phenelAed and Batutton io made alkoltne by addinq m Dithizone in chloRohORm,is able xfaac Aead keom alkalne Setutton do sosm Lead dithizone complex ammona Batutton his hen exteocted uotih Sml poRttons oithogone Solution unti ie becomes 9ieen: he dithzone tchloeohoam geen m Celee cohile ead-dithizone Vvotet m A he Combined exteacisaae Shaken coiJh Chfeu Soml a IN HNo chloRafoeM layezs discasded The inensily e6 Iho Coteu of complex depends cupon he amount a6 Lead Im pAoceduset Kead paesent as an impculy i /he Subedante, geisBepaiafed by etzaoltng" 6 To-lhe auid Sotution Sml 0 Slamelasd dithozone 6otutioD i added along cwcth Am 06 ammonium Cyanide ama &otufton Shakenhor 30Seconds GD alkaline SoluHion Cetth a dhzone A Coni2ot/8iandasa tspAepaied evcth a et Oh detuted glandatd lead Sotutton equtuales lo-heamount 06 Lead peRmHed he gample Y. efeaciion 6otution he infesberence 96 Clkez con, meials efe are awotded by maiDlauningeplimum ph hor ke exiLacd in9 by emplogrng eoleUR Inlensiy CompeLed
Melhod:J-Os clealcalccLless Salufton unde Spectfce dondtccons Limit Hest o heauymefals mittest t Casted eut o 辿cnd Ocu est Sotufcan ConfenE e6 metalltc Impuzitie_ dbat axe cotccied by Audaogen Sulphide HS) Simolad selufton 1ake lhe speccfie gi O3m e Siandaud lead e Sample Solufton DAneple H+ HSs be pH be do4 ky addtnq d MS 2H Pdiust Jbe pH 3/a4 cecdh acettc acid 6a) he ammenia oi cecccacid Basedon dhe ieactcon betaveen meiai ion cocth Kyd tcgen Sulphide cetth dhe dosmaiton e meialtte Sulphide a beece0 coloualcon oa black pl OmmoDia dilule Ho 35ml cochb didt l谷lo 3Sm coch disteled ewale desClled coalcz TesE sotutton is Compared cocth he Standard Soluicon cohich io eemprepaled Hom SBandard lead setutcen taOetl ndd tonml C6 H S 6ndd lol GG C6aeshly piepaied) 6seshly psepared h The uscual limmt a pe p has been opp DiluleHo Sool coclh dittttled Ho (6 dilule do Saml wb Tp hao adepied haee meibods boa-be Limit dest 0a heauy mefals dtsfeted d0 Me-hod n ethod: - is ctsed feSubstance cohich 9tues a cleau Colesless Solufcon CundesSpeca ce Conditcop Medhod I ta cAsed 6or /hose Substances Slandad Can be piepated as diiected by Method2 Tast soluition Gan be pAepaed by Subsi ance cohich do no gcue clea ceteuLless SoluH cweighing a 8pecchee 9uaniilj 6 Subsi ance uDdes he est Canalttcorns or Mefhod Hefhod -s cLsed bas Subsfances /hal- aS pes moncgsaph p_ a Cicu cible. Mecsfen coh igSo4 onile cna lo6tomefil Complefed hazsed gcue a cleal coloutless Set n laat medtum
21 26 Limit fest hor ARsenic d d e dteps e6 HNO fill nomore umes ase keleased heat do so0 C Dlloco o coof 6 aodd Mocstened ch toml o6 del DASen損c (S a uell - knocon undesi20ble omd haumhcul impcaiy cohich tspaeser medicenal Substancy cohich ts pxesenk n m O6 Hc euapoeal谷 do.dlyness dtgestbo eoo minules Nctufka lde cocth ammonia Soludton Make ftust acidte cocth acebte accd lo Adjcus 8-4 hctter 6 necessay diustooume ef 6tcesale do aSl nNes Les's eytinder 13 dd tomle6 t3 detulecocfh cwaler Ihe appaialus is Inocon as GutzeiE appasalui 8 Dacnccple:- tslhe baSed on -lbe eactcon 0 aRsentous Slale ts ieduced PRsenie Ib lo aASine gas Compae he cetous coth SBamdasd Cel辿u Is 9as i passed Ovez mexcaic.cbloaide Dape lo pRoduce -lo bzocon a siain, 6Rom yellouo Jpiensily and lengih depencds cupon be Me fhod. amounk oG D&senic preseni SHd Sof coas piepaxed by cuscbg ml o6 Stamdad lead sel andS daule Nae Setufton Nakeup she Cotumea o Soml colh cwafez SBandaid Slao p2odcuced 6Rom a dehcile quantilj o6 aLsenic Reactcon' ALSenic_eu'st ID duo talency &iale Test sotuHcon- Take 2Sm 0 8o: piepatea bymon0g Ta'walent azsenic dtssolue oml tuatel, add 6m o ddl Naou Setulton Nake cp he votume o Som cedh cuatei o each add diops o6 Sodtam Sculphidee MtA,Keep astde 6oz Sminules: pentaualent aLsenie
28 29 he Sample sdissotued thacte cobic Slep:4 aRStDe gaspeaduces yettoco 8tadnon Jbe ezcuate chloacde paper Slp: ContueE_ Hhe aRsenie tmpuaol inlo5 asSemou_ aud 0R assenic_acid depeDdtho upon be tDJhe Sample Lead acefale cotton plug teaps he H9 fyokmed b Caleny Slale G asseie pesen Ot4 As-OH oR) P30g H aivalent RzSenioctS aee CHCoo Pb + H Pb$ +CHaCooH Ce tS =0Se o) ASO4 Iniensiq oh 8iatn is compaied coc促h Ibe Slamcl叩nel SBeth 8lEp DRsenic accd c l tS essenttal do mainfain he sal谷 ag Tn Resente o ledcuccneagentsLka pOtasscum lodide CKI), SlanDoud eblozcdle Cenel,) pentaualentaRsenic aca s ConueRded cnio acalenE a2senious acie evolutcon 0hydkogen cohich ib dukn ts dependentupon he )he amount and &uhace asea o6 Zenc ) Ihe Con 06 he acid and C) JheSalt io he eacicon medtum he lemperakueRe he dimension 0G she appaaleis >dgSOt3h d Slep: DAseious a Cxel_seacfs_cIEAh nascenh evotufon giues 2cse -lo a Long and Rapid hydkogen ama pAoduce asscne ga8 alth6use 8/atn Slocoeuotution giues Stie l6 a Sbozt Stain AStt40 O6Ihfense_cotouRadton
30 31 The oo Rubber bungs coniack by ustn9 Rubber bamd oa spain9 cep ppara lcis aRe kept ih ee elose Conscst 06 a coede moutbed 0m Capaciy ha mouth 06 3scm dtame le lass botte e6 Rote 0 hote_. Clower end) boGcte tsbeoced wh a subbe bung ROLgtobich passe_ a 9tassiube, 2oem long enteenal diamelei- 0 8em amo Intesa l diame le - Duacnq he Hest, been pass tng Ibe he lhe evotued 9ases haue haough /he Side hole, bung Jhat ocwer hole Seae as am ec Go havng COa ler cOhoch Condenseg t fhe ConsfzicBed 6Sem paF O6 he dube Ko cwes end MescuRie ehloxide papez Dce he ube is constieled at SS 1ower end extzemiy ge paper mus be paeserued i a Jo Imm diame lec Stoppex竪d botite t lhe dalk hete 86 amm deomele amd a sde fc pape cohich bas got ezposed Ho Sunlugh+ vapotsa 06 ammonia, 9cves nea he ConstReteo part OHo be Aise lQ a tgbter colouaed Statn ppe end: Hgcl papex tS a Smo0h cohi le Ao less /han 6ctte paper ne Cupper end 8G he glasstabe shecced coeh coo ubber bungs each Kavcng a hole boxed Conttolty an 6 Smm di'ome ter Smm th wcd4h cohsch Soa ked a SatuRoHed Sef e6 lgelh anol hen ptessed o semoce Supe.s6luous Sof ane 6tnalty dried at 60 e In he da One 06 he bung has been Gebed o he Kead aceta leCotton coeot 06 Ihe Jube, tohile he Cupper end Seconc bung has o be 6cbced upon be cs bung used (6 teap amy kl,$ comch may 6e evol ved along Cocth aRSCnee Such a c0ay Vhat Hlgel papea S Sand cocthed betcween he Censal hole.
33 SpeeialpLoceduses ModcGtcafion io kT Ikaline Substance$ AIkalDe Substances ha ve Ho be dissotced in accdSo hat e66ervescence CeaSe S and 6.cltexed and 6cttesol s Haken boR T 6Ox chlorcde s and Sulphales in8otwble SubStance$ inSotuble Substance_ ase 9enezallq extaacted cocih coalei and hen ~ctered, and hbe 6ettezala Lused 6ox be test becouse he paesenee o6 insa(uble Subsfance modihce_ -/be epalescence and Co (o Salts oG ORqanic acids:- eg- Seduim bengoale Sodtum Satreylale efc Libexae 6zee coalertsoluble oeqonie acd dusing accdihccofbn cohich tsGctezed eb6 omd -Ihe6eltexa le CailyOue lemit Hest 4 Coleuzed 8ubstonces egl- eestal uecetet, Nata chil辿 geeen ete aie eanbeised ama he ash so pLoduced etRacied oa ler Deepy eoteued Substances Kave Ls be decotouuts ed befcse dest L Redeucad by becttn9 cudh alcekei ond Jhe Altera le used
34 6Redueing Substamce_ eg ypophosphoLocus aud cohoch Reaekcotth Sccvertka le i he limit dest 6oA chtORide_ Shoutal be Oxiotsed cochnifece acid OR Some oxiclgcog agen$ befoe caayn9 Other Out he lims4 Yest.

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Ch-1 , Impurities (PIC).pdf

  • 1. L 3 Seueces 6 Impu&tGre$ Rao matestal$ employect t manuJacfute fmpuRcles pxesent O2 assocta lecl cwclh Ihese ehemials moy be coazted /hRough manu/actuainq peoce8s ma Conlorminal he snal proolucf eg Roelk Salt Ca Sg md agnescum ehloRide So Ih谷 6cnal Nacl peepared onhis Source cocll Confatin CaSog amd Mge as Impcutl Roelk 8att CaSO Contans Small amis @f > Ndct Ce &g eompds a topuut les eg2 CuSog pxepaied by be acfcon of Sutpburte acud n Copper luantngs euSoy t Hho +属So Cu + 2504 Cu Juanings Kaue on amd arsemC aS mpuuGies k: 3:- Zinc sulphale psepased by he actcon 0 Sutphusc acd on Xtnc metalo4 Cene 0xide Xn +HSO Knsog tW2 Znot H2So4 Xn804 + Heo n Too ale knocon to Aave mpuu'fies itke A), u, Mg,n, ur, As, 8 Pe
  • 2. Race Reaqenf$ useo be mant/aCTC 7 P* e lbodg O_pAOocess itLsechtot mantueelure eagent_ cused he nonufacitLet Diocess akenof domptefeay Kemoued by SomeInfcuzcEfesaReu bC0peealed tol v lhe ma teitals olurcnq /be lmanuaciueting cuashing, ben bese may Come aS pLoeeSS Impuily m 1he AiDal DAOducf: a) eagenisemploed Ih be pROcess'- eq CaCo3 tpreparec by lbe nteeacfion EgL Rmmoiaied Mes culy may be- pAepated by addng meicuie chloLiale 6dtuul谷ammonia. eq o Sotuble Cac omo Sodlium Carbobal Tbe Caco mauy ontemdeaceseCacda a Sotufcon O Ala,co辿tc lGDo cashedl DRepeelytudh Colducwale Cacl.f Ne,Co3 c+ AIH OH NHlgcl+ AIHct +Ho CaCo + Nacl he piectpita l Ommcnia l辿d me eusic Cwashed cwHh_cotd eoalei o semate- ommoium hyaltoocide t6 t6 not twashed Comp te fely cocth coafez,he tnatPLOducE may Contam ammonium ydLoaide as Impiuly b) Reagens addedloSemeue Ofber ipuRtfies potasstum beomiole contaInsll/Roces lo baztum as mpukiliy But paf:baOmiale adaled lo Remove @xcess OGSulphalecohichm luen geARLses eg: precipilalecd CoaCOg may be pLepareel y -Ihe'mdesacicn eCack cocdh Na,coa JoBa as Impuly V Cac +la,co > CoC t+ Alact cSolvents CLa ler Tap cualek al Sof amal C as mpatid叩s lap caler AiOduce and meit May confao Jhese tbns as tmpuRile$ Cheapes-Salcent awailble be peeipilalecl CaCo aoashed (6 Remve exceS3 Ala, Co and Cac,_ 6 piecup鱈lole -no coashecl pLOpeA y TDe Se maLappea as LLSe &eol o coashing lhe -6enal mpcLlly /he hina pd
  • 3. 6 4 ChemicalpRocesses usediio be mandldc.cleae Eoa Supdbesis eh deugs manu chemica3 AeoctiopSucb asi pitaaBton,ihalogenalian, 0idoton,Recdactton hycisatysisetc: ase So6 kened coalek i lap cua ler spassed hrocugh he Sodiu fokm a6 Xeolil cohih gemoues devalentCalcan CcaNg)fzom laptoole: exchange oSodtim- So-/he hinal poduch may Conlains la'&C as impukidte s IDUolvec T-hese ichemical:pRCce.sse.s cighesent Cbemcals oze used i eq- tapcualez Lcohich eonainsmaq many4 disscluied teDS apdl rocLyCome as mpusclies thheAtoalpAccduchr. n 2 eg:2 potasStumlodtae is mofactueed dRom Mooline cohich is oblatne aom eip,a Seacueadi cyonide$endsiV5 getn6oemed cohenmteogenous ogoiematleri is buanE ceedh alkalie_.in )Deminesalused cuales lap waler packed ciocdh ron exchamge Xesins The walekhus cbiaincd ti hee hrom aN Na, ci, scand c pasSed -bzougb Columns Bud/he finalPAtducE may eonlam 0Rgaic Impusitfes fmosphezte iConfaminatton cduzinqlhe m a n u f a c i u a i e p r o c a s S Tp nalustaiaazecs, admaspheke is u) Dis4illed ooater2 isbest and faee hom all 040nie and n0kgaC mpuites, he 6chl pAOduct does not confatn shese_impuaithe alConamibatea cothdustpazktcles tike alumimum oide, gilica qlasspastcclos poLCelatnoathicles, pla辿cc 6ragments ekc) andSome gases kehyceogeH Sulphoole Sulphuroliokide and black sthoke CSoot) DukinqmanuJadleia辿 s OR pIRi6icaiion o- pharmacecitcal prodcuets bese impeLRHIeS enlelHhe 辿tnalpioalucks astimpcaifies: eq-AlaoHlabsoxbs atmospbeaieiCo laotttCo Na NacoytH,0 el) Pction D6 Seluents and keagenfs on Reaciion vesselS Duaing he manudactcuing PO.cess Some e dhe Sotuents and seaqents aeact coilh 1bo me dals afa AdaettbD vessel and may diS6otue -/he mefal anol aPpeau a topuaiktes tin hhal DAodick eg Cug Kn ReacF OHhaudtc Subetorecs uOSsel 2 SlODG_acidsleachef out atikalifrom boxostltcale alass
  • 4. E9 8 D1eimedtalai pxodecls in he mantilaclem&g e . ZnoLIS prepased bsi heatcng meialic. Zinc l6 batqhE 2eclnessina 辿uaRent/at: Tbe uapotis 0f zioc busD l6 oam incoxide AOCeSS SOme timesIntermediales mey be CaAktedIbaougb /0/he hcnalpiodeick lbe heattnq is less OR Supply O atz S/eSS /beD Xhe melel isDo~ Complelely egl= p0fassicum lodtole psepaRed ucecn9 Odthe cocth palosstum hydkoiale Conueetecd iol zipcooeide SO Hbetnal pedalcucE mciiy 2onton Zo as impc&iky These Sulting Solutian is eapcueated -lo elayness and /hen heaied cocth chascoal kTo+3e kI 3Co o hispiocess 1 the/ptekme.dial谷 DACducE uTo t not Completelq kemaced ConveRted tnfo ukI, -lhen it may eome as 8 HanulacHu叩inG hegards- n Cuen ina coell- Aunmanulahustng house Cextain bzazds exisk comch canglueRseL l6 peoceuc贈_ CoDiainationn A Impuirly ti he6cnalpLocluet a paa fiecalaleConiaminaiton DefecfS he manLdacfeairng pRacessi= In lhe manu,/aciuainq praaesses lhesease defeci ke mpeefec mixme, incompleteness,NoD-adherence to DAape demDeRouaeplesSULe DH oL seacfion Conditons ete tOhich may qietd chermecal Cornpecinds Ke impuatfie Ibe peesence cundanteelDazticculale matte can azise ID a humbez eA coayike accidentfal iDelcisconoA dcah10r glass O DORCelain,mefallia and plasFe agmentS ARomSteves qRonulatingtablettingand cllcnemachoDeS, 0AlevenLo poduck ConfacneRS I s lupe of Contamialion imay aAdseson ecthea bulk material used b Ibe AoRmulafion OR ROm use 06 ImpRapeely eleanec equpmentoConlaines$ OR Ibro.cugb lbe coearame leas encquipment ea Cacl ispRepaLedbey addinqpure CaCOaoi /beSlighe eccess eh ddl. tJel hotlocwed bij Stiubga0d hildeaafion Caco t Hel Cacl t Llh0+Co A -he aboueIDgRedienis _aRe no b) DAOceSSes&oRSa A mixed petbecetyihen SomeuDReaCfed Nel may appeaa In_ihe nal pRDdo. ieoss e3302Sokknqfom n Complele Sotution /a Solul辿 1d_a liyud p.sepakafion:
  • 5. 11 10 eg u n e v e n alisfaibufion a ScSpeneled pastceles his Can be auotaec by )checlcinq/be l labelsoD issueion 6ctleno 06 labeitengmacbine u ()des{ucfton or aeluen Cj Stock oG Dusectabels eAee C COSS-Conaminationi Ihe handling e6pococdees-ganulej loble ts and ib lorge- butk: aegctently L7 Constdeidble amount OG- ata-boxDe q. <fo3age CoDadition: A alust cuhich, (6 not contaatled, Can lead Ha Caass - coDtamination 0PROclucts$ eg bandling 4 Steiotdal ond olbe. Sntbete hoxmen辿s Chem'eal Subetopces coben piepated haueilo be saaed tin debbekenk lupes o C o n d a e n e s s d e p e n a l 1 n q upon lhe haduLe_oG- maderalibachi Stze lanal quaniili Ua&tocuS tupes afm旦aBeatalSl ase cAsedio Stozage puzPOse 1hese may bellplastic Doelhene 1&onvessels Sainlesssfeel, A l u m i n i u m C o p p e e t c : Reacfron a 6 l h e s e S u b s i a n c e s eoith Jhbe matestala e/he SBoxage: uesseioecuRs and-be DRoducis akmeo, aeehound astmpuecftes Ath Jhe slokecl mateials loadeqeualei 87tosagelCondiktonsi mdt/hec efbechs ase d) ceobial ContammnaBion he phaama ceuttealL Reqcuaement _a SteacyHestS hox all pRoducis Irntencded Ao pienteral adminstsoftorn and eptbalmie Oiepatafton eq= ltqud Pieparation.s amd Czeam 6O topical applicafion l6 brokenSkim O Muca u_ membeLanes aRe liable Jo bacfescail mould and fungal Condamioation Romadmosphece' curing manudac leutnq pioceSS Sloe2o pRodeefS bmauybecome Condaminated eocdb dustelbe bodttes o 6Dsecis, omd e v e n animal amd InSec exc2eta un less adeguale peeautcODSaie valeb e)_paclktoq erozs producks of Stmla appDEaLaDee Such as dabletS oh be Some Sze , cetocur and Shape paclaed ib Can cnstitulea polenfial SocRce o6 dangea baougbmis labellinq 6elthez 0R bol6 Similaz Coniatness b)Chemealu tnSiabiltiyi. Impualy Can alaoaicseioluaenq loRage as a 2竪seiltAchemical toslabiletG amaa Du0he e6 phoamacedAieal
  • 6. 3 12 hieb ale Dof1alc0aysp&ecen dable may Lead 6masked changes 1 he PRoducA Substapce.sase kDo COn lo tuneeg CDemmcaldecompasidion cohen Sloed cundes non-ideat conetttcon be bakize ef sdbe decomposiHion adue la ight ata, 0xtdakion coa(eRvapeoUCoe Temperaluelebbecfgi obd daaces ehmelall'c ton Can be auvocaed by Aigbth Sepsitite mafetals Shoutd be SLEiedmolakened glass vessels ok metalticcontaneas Vdo inhibit phol chenm'aal decoropesition antioidaDts Hikke B:H--Bufylatesl hyclucnyase:le Somefcme chemmiealand phystcol ehangesi eccoigtn 1StoAed peoclucts due /o c h o m g e t l e o p e x a l d e e n&ii br pROdeefs os lopical Usel muskunbee PLepaed cnde fempezaluee conditionS Such bat J5at aleaCapable agegcihstaneinq lhe eh6ects ef_changes lo empeza(uee paskesand etntmeDS tnUshbe oRmutaded aso e-lain/heckConststepciiaf bighee dempezatuzes etueDe NJ Reactioncocth containeLmaferialsi C Daneeslbat-he i2eactiorto:DecompasittonO6beDiodlic eluaing St0Rage betcueen Containeesand Cantepts Jakes place ond eahieb _cannotbeicanozed CeaMSandeintments Liabte l zeacE codh me/al Sue6aces eq Salelic aco ecnen must_nof be socked medale, eopdaminalionet lbe6tnalpac Jubes unless s/beqlbeve been lacquerec a loteanatty do tnhobit seaelcbn SpmeSubsfornces decamposeulon keepin Ihe cecompasifion becomeSt GaeaBekihinlb辿 paesence e h i g h l i - a t A K O A g e n he&esult dhdecbropesidionbs baiDgsabou egTamres phenolS,potenf dugsbet c podleddue l6hdecomDOsHiai坦n ezposuRe Ado-/be taimosphesel egL Some diugs imauy padLbyii bydeotyss oiidation etdl Dhysical eharmges be occeharnee og Chomge n phygtcal form06 behduh duaing StaLage DotUdADomi dCbedges e2gJSialOAmagglomeRodion gmodYeven Calking 6 Suspe}ded palicles 2 I1 DcccdentalSubstiicufton iox delcberale adulteRaitonCwth SepSpuatesio CLseles.s_mafestal
  • 7. 15 14 i ) Impuaiiies may decease -be Shelf Lihe hiSCon be pkecepied by Sloalein all-Joctc SubsHoncesdagathe Sepakafely, Ox th a loced Cepboatd: lhe&e ale many pbarmacectdtealchemical COhich aLe aduttetated ceth cheape Substam ces h e ezpensioepodasscum beomiolel may e6 /beSuhstances Ui) Impurciiesm a y Cause ebangesih cdous bColou& laste etc 2 he npbaamacopoetas eG Jbe vaatouS Couoiees Bese paescaibe "Test boz purii or Substance JhecaiReasonable nnkreedom Rom adulteLaded _estib cheaDe Socituo bitmide be S o a S e n s u R e dbe undestaoble impuRiGres n b eJes6oa pusdly haueibeen inact be tests h e ence'0Impuitie.sand t he lims a tolerance o hese dlImpukttcesS K G6eciS e6 mpuuaitie$ 3 ImpuRi辿tes hautn9 be tnjuRtous cohen paesentaboue carfain Limits lmpuatfes, even paesepEn taaces, may eresta cuioilat'ce eb6ech a ale aCeLtaiopexotd: lotce66ecis Can eg 3 omd pb LIMITTEST to Limit dest aze quantadtve o Semi-quodiidafiue Hesks designed -o tdenkilhq_and eonteolSmal q u a n d i t i e s o 6 _ i m p u t i e s _cohich aie lkely Ha i) ImpuRciies aze Sametime.$ hasmlessi oeoeuveR 6 hese aie paesen In_lasge Such popoaftbn-/he acft'e Staengdh o lhe Substance ges LovERed,ASbeeapecthrc eGhectsget locvered u)inpuatite imayCausea chmge m physical ana Chemieal pA0pezliesaf he Substonces, fheaeby maktbg she Subsianee medicinalty usetess (u) Impuacdies can bathe about dechri9.ca dihhieuldtes he 6oamulation ) Impuaiiles earp Cacuse in CoopattbiliG Coisb_Odhea Subsiones d ) b epRegenf yn be 8ubstances Cg'na Kimit esh oz chiordes. Kimit tes doSalpbale ioit desuo laan
  • 8. 17 passes-/be limit Hest The opalseence peodueed io -Jhe Sompfe Kimit destdor chloaides 1he ltmit des o chlotde ts based Seluffon t0sLmoLe eemplhan ha/ c6 he Slondaud Satutorn, Jhe gccen Sample atls s/be limmi dest Daincple' O D _ h e i e a c i o n betcweeD S i l v e r M I i a l e Coidh Sotuble chlorides10pROduce Silveriahi0tde epalscente. ihDieseDee DROceadune- lalcedcoo Messlez31cyluneles of Same bepAoducedapalScence depends CupOD he ameunt e Setuble ablolideDAeSeD h e Size, becght et Celienston). ai Maalkdbe as Sample/BHest omd Odher aSSAmdad/a/ oheHest /Sampleodissotue he Specfced amounEef Sc1bsiomce m dsiEtled cualeb Ddd lml 0f dil:WntQ3 DituLElowS0ml eeLIbldsAlled eoale Sotcufcon Sample C+ DaNo dt a3 egel t N dil HNO3 SJandad - Macl+DqNo Agel t AlaNg Refe ek icagentsi Stlvez nitialE- A Ihenladd iml eG DqAtoa nd Sttaied Cwetl amd altoco lo Stamel hoR mnule3 E seacls_cotib SetubleChlorcele con amd pLoduce cpalscence est SHamdac Dissotue /be Speciteolpipe-lle ou Iml q 4 9 Sample m dsta: 0:Os84S cofu aDdalIml efedil HNo Addim) ef dil: HAlg Diluled lo 5oml cocth Diluted-Jo5omlcoh dstclled cwaler& Add Im06 AAlO3 Add im 06 BNO Mo /be S6tufton(5 x JheSe PIopez y caidha glass Sodand alloc0 do Soma ea mn: Dil: HN02 Li hef0lmead Agcl opalscence i_insotuble dil HINGG NeutLalses alkai mefal kydeoxides ilact )_e alestilled cwalet amd Caibenales (i)1 pAevenh_iotes 6eRence o6 Osbe adicalL alloco o Stamd Smn be apalscencep2odeiced tn he Sampte SeluHioo t Saroe 0 less as bat OG- SJandaiol epalsCence, he gcuen Somple
  • 9. 13 18 b) (E Deultalises_aikal medal ydickides and Catbonalei c) pseuenis -Jhe Inteadezence o Othez lons Limt dest or Sulphal辿S dt He Bas t kel: K8 Bacla Substance poses -lhe t i t e s t 16 /e duzbidily paoduced Ol Same as -ha e6 SHondaid Sol Tne p2cnuple)= he paiociple Inuotved 1 h e l m t des oz Sulphale isbased oD Jhe ieaciioD betcueen Bac and etuble Sulphales ip paesente at dti:Meldo paoduce Baso4 duabidr I he Sample ts less DRoced uke- Take a paik e4 NessleRS Cyuneler a n he othez as he pecdeced dcuubidlily depenols upon /he label One a Siamdard nd 8ianelaicl omounte sulphale Iopilg est Solufon SHamdauel &e Rele e6 Leagents Te Bod test_Sotufion inhe P bas been ieplaced by Bauum&ulphbale &eagent (i) Banium Bulphale zeagent Contatns I:Dissolue he Speci6ced quonfily O be Sub: b_distclled eoalet placet Io 9lc27 disiened wa le Ddd 3ml of dtl uo aBatum ehlode- Reachs cwth Sulphale toDand paoduces uubid Rdd Iml 9 dtlHci 3Makecap Je Uol: up lo S wtih dtstilled -a 3 HaRe cup-lbc vel up Jo Aiml g dSH led b_potasstum Sulphale 8 added do Incsease he Sen sittvrly e heseocfton Ddd 5ml GaSc4 4Dald Eml O Basa4 gen Aeagen Sulphale aee alcobel!- helps JoPrevenE O well allow do Supez saduaation and ex unmfoam euabidelq Piaduces a moe b Sord oa&mint' Standdoa iminf贈 ) dlt Hel 1he hosmed easCq ubid istbSoluble i坦 dt cI
  • 10. 21 20 Dmmonia- kimit es os lson! 10 Ceale am allka lene media hepaoducedeoroplez i eoloualess In acidtc ond neutial meolta CoO Pe CH-8H e8 Eesous -Jhioglyollal comple Ctezie acid pAeveniS -lbe Daecipiation 6 Iion by ammonia Limit punciple thvotued n /he eSE 1 based on dhe &eaciion beluoe.en the Coloua infensily pacduced by -lhe Sample Sal eaLeus om0kencacis eotth ihho9l4 Colttc acid tn pzesence o6 ammoma and ciesuc acid do p&nduce hezRouslhioglyeollal Comple Sanne oz "less as eorppazed-Jo SddSol passe_ he limit dest fa I&on Colour Infensily psoduced by he Sarople Saf: smOze han heSiondaid selj 1E ads1he Aimif Hesk 1he produceod Complex 1s aeddish do puzple cotou DAoceduze: -lake a paia ofoml of The Coteus infensily depends pon the amcunt oh besous impusxires Messeas eylinelez amd label one a detE and ofhe as Slamdad Test Sid BcHe G6 Jeagent Tioglu coiti accd:- Specihced quanttly 06 ae am c6 Sid Scub dissotued ds calei ndd a Aps e6 ioglse1aEAend dd adps e /moycottteacid ia IRoDSel acts a zeducing agent tt edu eaaie hoam Dh 12en 6euous horm rio qy ee lLi'c aad ieact etdh feareus hoim 86 LAOD amd 6oem feascasdhrogtycotal Hedia t made atka line coeth ammonia. Nake cup heCOCuoe up fo 5om u/h Comple 6 Ala and altoco 6 Sland e t e min
  • 11. 23 22 ammoMuM CLi2o le, polasstum Cyande Aimt est Jos lead: kupola0ylammne hydtochloaide eogent e Liit es Jor lead 1s baned upon uhe Aeactibo between dead amd dtphenyldhiocarbazcne ldithozone) Pknown quoniil beSample Solution daonsfezxedlo a Sepazating upnel N=N 10 ce Gml 06 amrmonium cclzal, NHNHCsH > S N=N 3ml O pOHasstum cyamde +Pb N-N dm0hydkoxyl amine kydeochloatde d dps phenelAed and Batutton io made alkoltne by addinq m Dithizone in chloRohORm,is able xfaac Aead keom alkalne Setutton do sosm Lead dithizone complex ammona Batutton his hen exteocted uotih Sml poRttons oithogone Solution unti ie becomes 9ieen: he dithzone tchloeohoam geen m Celee cohile ead-dithizone Vvotet m A he Combined exteacisaae Shaken coiJh Chfeu Soml a IN HNo chloRafoeM layezs discasded The inensily e6 Iho Coteu of complex depends cupon he amount a6 Lead Im pAoceduset Kead paesent as an impculy i /he Subedante, geisBepaiafed by etzaoltng" 6 To-lhe auid Sotution Sml 0 Slamelasd dithozone 6otutioD i added along cwcth Am 06 ammonium Cyanide ama &otufton Shakenhor 30Seconds GD alkaline SoluHion Cetth a dhzone A Coni2ot/8iandasa tspAepaied evcth a et Oh detuted glandatd lead Sotutton equtuales lo-heamount 06 Lead peRmHed he gample Y. efeaciion 6otution he infesberence 96 Clkez con, meials efe are awotded by maiDlauningeplimum ph hor ke exiLacd in9 by emplogrng eoleUR Inlensiy CompeLed
  • 12. Melhod:J-Os clealcalccLless Salufton unde Spectfce dondtccons Limit Hest o heauymefals mittest t Casted eut o 辿cnd Ocu est Sotufcan ConfenE e6 metalltc Impuzitie_ dbat axe cotccied by Audaogen Sulphide HS) Simolad selufton 1ake lhe speccfie gi O3m e Siandaud lead e Sample Solufton DAneple H+ HSs be pH be do4 ky addtnq d MS 2H Pdiust Jbe pH 3/a4 cecdh acettc acid 6a) he ammenia oi cecccacid Basedon dhe ieactcon betaveen meiai ion cocth Kyd tcgen Sulphide cetth dhe dosmaiton e meialtte Sulphide a beece0 coloualcon oa black pl OmmoDia dilule Ho 35ml cochb didt l谷lo 3Sm coch disteled ewale desClled coalcz TesE sotutton is Compared cocth he Standard Soluicon cohich io eemprepaled Hom SBandard lead setutcen taOetl ndd tonml C6 H S 6ndd lol GG C6aeshly piepaied) 6seshly psepared h The uscual limmt a pe p has been opp DiluleHo Sool coclh dittttled Ho (6 dilule do Saml wb Tp hao adepied haee meibods boa-be Limit dest 0a heauy mefals dtsfeted d0 Me-hod n ethod: - is ctsed feSubstance cohich 9tues a cleau Colesless Solufcon CundesSpeca ce Conditcop Medhod I ta cAsed 6or /hose Substances Slandad Can be piepated as diiected by Method2 Tast soluition Gan be pAepaed by Subsi ance cohich do no gcue clea ceteuLless SoluH cweighing a 8pecchee 9uaniilj 6 Subsi ance uDdes he est Canalttcorns or Mefhod Hefhod -s cLsed bas Subsfances /hal- aS pes moncgsaph p_ a Cicu cible. Mecsfen coh igSo4 onile cna lo6tomefil Complefed hazsed gcue a cleal coloutless Set n laat medtum
  • 13. 21 26 Limit fest hor ARsenic d d e dteps e6 HNO fill nomore umes ase keleased heat do so0 C Dlloco o coof 6 aodd Mocstened ch toml o6 del DASen損c (S a uell - knocon undesi20ble omd haumhcul impcaiy cohich tspaeser medicenal Substancy cohich ts pxesenk n m O6 Hc euapoeal谷 do.dlyness dtgestbo eoo minules Nctufka lde cocth ammonia Soludton Make ftust acidte cocth acebte accd lo Adjcus 8-4 hctter 6 necessay diustooume ef 6tcesale do aSl nNes Les's eytinder 13 dd tomle6 t3 detulecocfh cwaler Ihe appaialus is Inocon as GutzeiE appasalui 8 Dacnccple:- tslhe baSed on -lbe eactcon 0 aRsentous Slale ts ieduced PRsenie Ib lo aASine gas Compae he cetous coth SBamdasd Cel辿u Is 9as i passed Ovez mexcaic.cbloaide Dape lo pRoduce -lo bzocon a siain, 6Rom yellouo Jpiensily and lengih depencds cupon be Me fhod. amounk oG D&senic preseni SHd Sof coas piepaxed by cuscbg ml o6 Stamdad lead sel andS daule Nae Setufton Nakeup she Cotumea o Soml colh cwafez SBandaid Slao p2odcuced 6Rom a dehcile quantilj o6 aLsenic Reactcon' ALSenic_eu'st ID duo talency &iale Test sotuHcon- Take 2Sm 0 8o: piepatea bymon0g Ta'walent azsenic dtssolue oml tuatel, add 6m o ddl Naou Setulton Nake cp he votume o Som cedh cuatei o each add diops o6 Sodtam Sculphidee MtA,Keep astde 6oz Sminules: pentaualent aLsenie
  • 14. 28 29 he Sample sdissotued thacte cobic Slep:4 aRStDe gaspeaduces yettoco 8tadnon Jbe ezcuate chloacde paper Slp: ContueE_ Hhe aRsenie tmpuaol inlo5 asSemou_ aud 0R assenic_acid depeDdtho upon be tDJhe Sample Lead acefale cotton plug teaps he H9 fyokmed b Caleny Slale G asseie pesen Ot4 As-OH oR) P30g H aivalent RzSenioctS aee CHCoo Pb + H Pb$ +CHaCooH Ce tS =0Se o) ASO4 Iniensiq oh 8iatn is compaied coc促h Ibe Slamcl叩nel SBeth 8lEp DRsenic accd c l tS essenttal do mainfain he sal谷 ag Tn Resente o ledcuccneagentsLka pOtasscum lodide CKI), SlanDoud eblozcdle Cenel,) pentaualentaRsenic aca s ConueRded cnio acalenE a2senious acie evolutcon 0hydkogen cohich ib dukn ts dependentupon he )he amount and &uhace asea o6 Zenc ) Ihe Con 06 he acid and C) JheSalt io he eacicon medtum he lemperakueRe he dimension 0G she appaaleis >dgSOt3h d Slep: DAseious a Cxel_seacfs_cIEAh nascenh evotufon giues 2cse -lo a Long and Rapid hydkogen ama pAoduce asscne ga8 alth6use 8/atn Slocoeuotution giues Stie l6 a Sbozt Stain AStt40 O6Ihfense_cotouRadton
  • 15. 30 31 The oo Rubber bungs coniack by ustn9 Rubber bamd oa spain9 cep ppara lcis aRe kept ih ee elose Conscst 06 a coede moutbed 0m Capaciy ha mouth 06 3scm dtame le lass botte e6 Rote 0 hote_. Clower end) boGcte tsbeoced wh a subbe bung ROLgtobich passe_ a 9tassiube, 2oem long enteenal diamelei- 0 8em amo Intesa l diame le - Duacnq he Hest, been pass tng Ibe he lhe evotued 9ases haue haough /he Side hole, bung Jhat ocwer hole Seae as am ec Go havng COa ler cOhoch Condenseg t fhe ConsfzicBed 6Sem paF O6 he dube Ko cwes end MescuRie ehloxide papez Dce he ube is constieled at SS 1ower end extzemiy ge paper mus be paeserued i a Jo Imm diame lec Stoppex竪d botite t lhe dalk hete 86 amm deomele amd a sde fc pape cohich bas got ezposed Ho Sunlugh+ vapotsa 06 ammonia, 9cves nea he ConstReteo part OHo be Aise lQ a tgbter colouaed Statn ppe end: Hgcl papex tS a Smo0h cohi le Ao less /han 6ctte paper ne Cupper end 8G he glasstabe shecced coeh coo ubber bungs each Kavcng a hole boxed Conttolty an 6 Smm di'ome ter Smm th wcd4h cohsch Soa ked a SatuRoHed Sef e6 lgelh anol hen ptessed o semoce Supe.s6luous Sof ane 6tnalty dried at 60 e In he da One 06 he bung has been Gebed o he Kead aceta leCotton coeot 06 Ihe Jube, tohile he Cupper end Seconc bung has o be 6cbced upon be cs bung used (6 teap amy kl,$ comch may 6e evol ved along Cocth aRSCnee Such a c0ay Vhat Hlgel papea S Sand cocthed betcween he Censal hole.
  • 16. 33 SpeeialpLoceduses ModcGtcafion io kT Ikaline Substance$ AIkalDe Substances ha ve Ho be dissotced in accdSo hat e66ervescence CeaSe S and 6.cltexed and 6cttesol s Haken boR T 6Ox chlorcde s and Sulphales in8otwble SubStance$ inSotuble Substance_ ase 9enezallq extaacted cocih coalei and hen ~ctered, and hbe 6ettezala Lused 6ox be test becouse he paesenee o6 insa(uble Subsfance modihce_ -/be epalescence and Co (o Salts oG ORqanic acids:- eg- Seduim bengoale Sodtum Satreylale efc Libexae 6zee coalertsoluble oeqonie acd dusing accdihccofbn cohich tsGctezed eb6 omd -Ihe6eltexa le CailyOue lemit Hest 4 Coleuzed 8ubstonces egl- eestal uecetet, Nata chil辿 geeen ete aie eanbeised ama he ash so pLoduced etRacied oa ler Deepy eoteued Substances Kave Ls be decotouuts ed befcse dest L Redeucad by becttn9 cudh alcekei ond Jhe Altera le used
  • 17. 34 6Redueing Substamce_ eg ypophosphoLocus aud cohoch Reaekcotth Sccvertka le i he limit dest 6oA chtORide_ Shoutal be Oxiotsed cochnifece acid OR Some oxiclgcog agen$ befoe caayn9 Other Out he lims4 Yest.