EXP#2 - Aspirin lab report PDF

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Aspirin lab report...

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Exp e r i me n t2Ana l y s i so fAs p i r i n

Ab s t r a c t : I nt hi se xpe r i me n t ,t heq ua nt i t yo fa c e t y l s a l i c y l i ca c i d( ASA)i nAs pi r i nt a bl e ta ndp o wde r we r ede t e r mi ne du s i n gt h eme t h odo fba c kt i t r a t i o n, a ndt h ec o nc e nt r a t i onofASAwa sc a l c ul a t e d i nt h ef or mofwe i g htpe r c e n t a g e . Th er e s u l t ss ho we dt h a ta s p i r i nt a bl e t sc o nt a i n e d3 19. 3mg , 3 10. 7 mg , 316. 3mg , r e s pe c t i v e l y ;a ndt h ea s p i r i np o wd e rc on t a i n e d7 8. 8% ofASA.De t e r mi n i n g t h ema s sorc o nc e nt r a t i o ni nAs pi r i nwa si mp or t a ntno tonl yi nt h efie l dofc h e mi s t r ya nd p ha r ma c o l o g y , buta l s oi nt h i swa ywec ou l da s s e s si ft h edr u gwe r ema d eu nde rp ha r ma c e u t i c a l ma nuf a c t ur e s ’s t i pu l a t i o n.

I n t r od uc t i on: As pi r i ni swi d e l ykno wnt or e d uc epa i n , i n fla mma t i on ,a ndpr e v e n ts t r o k e sa ndh e a r t a t t a c ks . Di ffe r e n tdos a g e sofAs pi r i nc o ul dpr o duc ed i ffe r e nte ffe c t sa ndt a r g e ti ndi ffe r e n t me di c a lt h e r a pi e s .Asoneo ft hec ommon l yu s e ddr u g si nt hegl o ba lma r k e t , i ti si mp or t a ntt h a t t h edr u gha st h es a mea mo untofdos a g eo rc o nc e nt r a t i ona si t sma nu f a c t ur e rde s c r i be d . Ot h e r wi s e , i ft h ed os a g eoft h edr u gwe r ee i t he rl o we ro rhi ghe rt h a ni ts h oul db e ,i twi l lputa h u g eh e a l t ht h r e a tont hep e opl ewhoa r et a ki n gi t .He n c e , i ti se s s e nt i a lt oa s s e s st he c o nc e nt r a t i o noft hed r u gn oton l yf o rt h ep ubl i ch e a l t hbu ta l s of ort hef ut u r er e s e a r c ha n d me di c a lpu r pos e . I nt hi se xpe r i me n t , t hema s sa ndc onc e n t r a t i ono fASAi na nAs p i r i nhe a da c h et a bl e twe r e d e t e r mi n e db yt heme t h odofba c kt i t r a t i on. TheAs pi r i nt a bl e t s( o rpo wde r )we r edi s s o l v e di n e x c e s ss t a n da r di z e dNa OH, i nwh i c h1uni to fASAr e a c t e dwi t h2uni t sofNa OH. Thea mountof e x c e s sNa OHwa st h e nde t e r mi ne db yt i t r a t i n gwi t hs t a n da r d i z e dHCli nas t a nda r ds t r o n ga c i d a n ds t r o n gb a s er e a c t i onb ya1: 1r a t i o . Th eme t h odbe hi ndt h i se xpe r i me ntwa se a s yt ou nde r s t a n d, a ndf ora na l yt el i k eAs pi r i n wh i c hha dl i t t l es ol u bi l i t yi nwa t e r , ba c kt i t r a t i o nwa si d e a l . Ho we v e r , t h eme t h odwa st i me c o ns umi n g , a ndl a r g es a mpl es i z ema yr e q u i r et ode c r e a s et h es y s t e ma t i ce r r ora ndt oma k e r e s u l t smo r ea c c u r a t ea ndc on v i n c i n g .

Expe r i me nt a l :

1 ) .Pr o c e du r e Re f e rt oLa bMa n ua lp3234 ;e x c e p tt heb l a nkt i t r a t i ono fNa OHwa ss ki p pe ds i nc e r u nni n goutoft i me . 2 ) .Me a s ur e me nt sf o rSa mp l ePr e pa r a t i o n # m( KHpht h a l a t e )( g ) 1 0 . 85 2 0 . 79 83±0. 00 01 3 0 . 77 01±0. 00 01 Ta bl e1. Ma s sofpo t a s s i u mh y dr o g e np ht h a l a t eus e di nsNa OHs t a n da r di z a t i o n.

# m( t a bl e t )( mg ) 1 4 33. 8 ±0. 1 2 4 35. 9 ±0. 1 3 4 27. 3 ±0. 1 Ta bl e2. Ma s sof3As pi r i nt a bl e ta ndAs pi r i npo wde r .

m( p o wd e r )( mg ) 4 40. 7 ±0 . 1 / /

Re s ul t sa ndDi s c us s i on: 1 ) .Da t a # m( KHpht h a l a t e )( g ) V( Na OH)( mL) 1 0 . 85 3 4. 3 8±0. 01 2 0 . 79 83±0. 00 01 3 1. 3 ±0. 01 3 0 . 77 01±0. 00 01 3 1. 9 2±0. 01 Ta bl e3. To t a lv o l u meofNa OHus e di ns t a n da r d i z a t i on.

# V( HCl )( mL) V( Na OH)( mL) 1 2 5±0. 03 1 9. 5 0±0 . 01 2 2 5±0. 03 1 9. 5 5±0 . 01 3 2 5±0. 03 1 9. 6 0±0 . 01 Ta bl e4. To t a lv o l u meofs t a nda r d i z e dNa OHus e di nHCls t a n da r d i z a t i on .

#

V1( HCl )f o rt a bl e t1

V2( HCl )f o rt a bl e t2

V3( HCl )f ort a b l e t3

V( HCl )f or

( m1=433 . 8±0. 1mg ) ( m2=4 35. 9 ±0. 1mg ) ( m3=427. 3±0. 1mg ) p o wd e r ( mL) 1

2 3. 0 0±0. 01

( mL) 2 3. 8 ±0. 01

( mL)

( m=440. 7±

2 3. 0 4±0 . 01

0 . 1mg )( mL) 2 1. 9 5±0. 01

2 2 1. 5 5±0. 01 2 2. 8 ±0. 01 2 2. 7 1±0 . 01 2 2. 2 1±0. 01 3 2 3. 5 ±0. 01 22. 46±0 . 01 2 2. 4 ±0. 01 2 1. 9 6±0. 01 Ta bl e5. To t a lv o l u meofHClus e di nba c kt i t r a t i onf o r3As pi r i nt a bl e t sa n dp o wde r .

2 ) .Re s ul t s # c ( Na OH)±s d( M) c ( HCl )±s d( M) 1 0 . 12 1±0. 003 0 . 09 47±0. 00 02 2 0 . 12 5±0. 003 0 . 09 49±0. 00 02 3 0 . 11 8±0. 003 0 . 09 52±0. 00 02 Ta bl e6. Co nc e nt r a t i onofNa OHa ndHClwi t hs t a n da r dde vi a t i on( s d )a f t e rs t a nda r d i z a t i o n.

Ta bl e t I n di vi d ua l Gr ou p # m( ASA)±s d( g ) %wt±s d m( ASA)±s d( g ) %wt±s d 1 0 . 32±0 . 03 7 3. 9±7 . 7 0 . 31 7±0. 0 09 7 3. 8±2 . 3 2 0 . 31±0 . 02 7 1. 0±5 . 0 0 . 31 7±0. 0 08 7 4. 0±2 . 7 3 0 . 32±0 . 01 7 4. 1±2 . 5 0 . 32±0 . 01 7 4. 0±2 . 3 Me a n 0 . 32±0 . 05 7 3. 2±1 . 8 0 . 32±0 . 00 9 7 3. 9±2 . 3 Ta bl e7. Thema s sa ndc on c e n t r a t i ono f3As pi r i nt a bl e t sf r o mi n di v i d ua lda t aa n dgr ou pd a t a . Me a nofi ndi vi d ua lda t aa ndgr o upd a t awe r ea l s oc a l c ul a t e d .St a nda r dd e vi a t i on swe r edi s p l a y e d ( s d ) .

Po wd e r

I ndi v i d ua l

Gr ou p

%wt±s d %wt±s d 1 7 8. 8±2. 0 7 6. 2±2 . 1 Ta bl e8. Thec o nc e nt r a t i o nofAs pi r i npo wde rf r omi n di vi d ua lda t aa ndgr o upda t a . St a nda r d d e vi a t i o ns( s d )we r edi s pl a y e d .

Tt e s t Ta bl e t :i ndi v i d ua lme a n( N=3) a nd

Tv a l u e * Tv a l u ea t95% 3 . 07 7 4. 30 3

ma nuf a c t ur eme a n Ta bl e t :gr o upme a n( N=18) a nd

3 . 62

ma nuf a c t ur eme a n Ta bl e tme a n( N=18) a n dpo wde rme a n 1 . 72 ( N=6 )

2 . 11 2 . 073 87

Ta bl e9. Tt e s twi t hc o r r e s po ndi n gtv a l uea t95% s i gni fic a ntl e v e la ndc a l c ul a t etv a l u e * .

335

330

325 tablet mean warning line WL upper

320

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305

300 1

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Fi gu r e1. She wha r tc h a r tofgr o ups a mpl e swi t ht h ema n uf a c t ur eme a na st h et a r g e tl i ne .

3 ) .Di s c us s i o n: Th er e s ul t sob t a i n e ds ho we dt ha ti na v e r a g eASAc onc e n t r a t i onwa s316 . 33mg / t a bl e t , 7 3. 2 %i nt a b l e twe i ghtpe r c e n t a g e , a nd78. 8% i np o wde rpe r c e nt a g e . Fr o mt h egr o upr e s u l t s , t h e a v e r a g eo fASAc onc e nt r a t i o ni nAs pi r i nt a bl e t swa s317. 57mg / t a bl e t , 73. 97% i nt a bl e twe i ght p e r c e nt a g e ,a n d7 6. 2% i npo wde rwe i g htpe r c e n t a g e . Wec ou l ds e et ha tt h e r ewe r eno tmu c h d i ffe r e n c eb e t we e ni n di vi d ua lr e s ul t sa ndgr ou pd a t ai nt heASAc on c e nt r a t i o na ndwe i g ht p e r c e nt a g ei nAs pi r i nt a bl e t ;wh i l et h e r ewa sa4 . 83 % di ffe r e n c eoft h ewe i ghtpe r c e n t a g ei nt h e As pi r i npo wde rbe t we e ni n di vi d ua la ndgr o upr e s ul t s . Ther a nd ome r r orma yc a mef r om e x pe r i me nt a la ppa r a t u sa ndgl a s s wa r e , a ndt hes y s t e ma t i ce r r o r swe r emos tpo s s i b l ec a u s e d d ur i n gt hep r oc e d ur eoft i t r a t i o n. Thee q u i v a l e nc epoi n twa sf ou ndb yob s e r vi n gt h ec ol or c ha n g e, a ndt h i swa sno ta c c u r a t ee nou gh .Th epoi ntwhe nt h ec o l o rc h a n g e d, i twa sa l wa y s s l i gh t l yo v e rt i t r a t e d. Toma k et her e s u l t sa sa c c u r a t ea spos s i b l e , wema yi n c r e a s et h es a mpl es i z e a n dt h enumbe roft i t r a t i ons .

Th es t a n da r dd e vi a t i oni nt h ei n di vi d ua lr e s ul t swe r es l i ght l yl a r g e ,a n dt h i si ndi c a t e dt h a t t h ev a l ue sob t a i ne dwe r es l i gh t l y“ s p r e a d”a r o undt heme a nv a l u e . Byi n c r e a s i n gt henumbe rof e x pe r i me nt sa nds a mp l es i z e , t h i sma yber e d uc e dt oar e l a t i v es ma l l e rv a l u e . Fr omt h ett e s tc ond uc t e d( r e f e rt ot a bl e9) , t h ec a l c ul a t e dtv a l u eofASAc onc e nt r a t i o n b e t we e ni n di vi d ua lme a na ndma nu f a c t ur eme a nwa s3. 07 7whi c hwa ss ma l l e rt h a nt h ec r i t i c a lt v a l u e( 4. 303) , s owec o ul dc on c l ud et h a tt h er e s u l t swe r eno ts i gni fic a nt l yd i ffe r e n t , a ndt he r e f o r e , t h eme a nswe r ec ons i d e r e dt obet h es a me . Fo rt h ec a l c u l a t e dtv a l ueofASAc on c e nt r a t i o n b e t we e ngr o upme a na n dma nuf a c t ur eme a nwa s3. 62whi c hwa sl a r g e rt h a nt h ec r i t i c a ltv a l u e ( 2 . 11 ) ,wh i c hwewe r ea bl et oc onc l u det h a tt h egr o upme a nwa sd i ffe r e n tf r o mt h ema nu f a c t ur e me a n.Byc ompa r i n gwi t ht h eASAc onc e nt r a t i o nofAs p i r i npo wde ra ndt a b l e t ,t h ec a l c ul a t e dt v a l u ewa s1 . 72wh i c hwa ss ma l l e rt h a nt hec r i t i c a lv a l ueof2 . 07 387. Thi si n di c a t e dt h a tt h e c o nc e nt r a t i o nbe t we e nAs pi r i npo wde ra n dt a bl e twe r eno ts i gni fic a nt l yd i ffe r e n t . Ac c o r di n gt ot h eShe wha r tc h a r t , t h e r ewe r es o meno ns uc c e s s i v epoi n t sf oundont he s a mes i d eoft hel o we rbo undoft h ea c t i onl i ne , whi c hi ndi c a t e dt hee x i t a n c eoft h es y s t e ma t i c e r r o r . Thev a l u e swe r epr o duc e db yd i ffe r e ntpe r s oni nt h egr o up, a ndwi t he a c hp e r s ononl yh a d as a mp l es i z eof3 ,whi c hc o ul dl a r g e l yc o nt r i b ut e dt ot h ee r r o rt e r m. Be s i d e s ,t h eAs pi r i npo wde r a n dt a b l e twe r eno tc ompl e t e l ydi s s o l v e di nNa OHwhi c hc o ul da l s oc a u s eas ma l l e r c o nc e nt r a t i o nc ompa r i n gt ot h er e a lv a l u e .Byi n c r e a s i n gt h es a mp l es i z ea ndt henu mb e rof t i t r a t i onf r omt h es a mepe r s on, t h es y s t e ma t i ce r r o rma yber e du c e d .

Co nc l u s i o n Th ei n di vi dua lAs p i r i nt a bl e td a t as ho we dn odi ffe r e nc ei nt h eASAc onc e nt r a t i on c o mpa r i n gwi t ht h er e a lv a l u epr o vi d e db yma nuf a c t ur e r , a ndt heASAwe i ghtpe r c e n t a g ewa s a l s onots i g ni fic a nt l yd i ffe r e ntbe t we e nt h ef or mo fAs p i r i nt a bl e ta ndp o wd e r . Ho we v e r ,t h e s a mp l ewa sr e l a t i v es ma l l a n df oramo r ea c c u r a t er e s u l t , mor es a mpl e sma ya s s e s s e d .

Ca l c u l a t i on : A.Ca l c ul a t i o nsf r o mi n di vi dua lda t a 1 ) .Conc e nt r a t i onofp o t a s s i u mh ydr o g e np h t h a l a t e Ta k et a b l e 1# 1a sa ne x a mp l e :

m =0 . 8 5g ,MM =2 04. 2 3g/ mol ,V=0. 0 5L c=( m/ MM) / V=( 0. 8 5g / 2 04 . 2 3g/ mol ) / 0. 05L=0 . 0 832 4M 2 ) . Con c e nt r a t i o nofNa OH Ta k et a b l e6# 1a se x a mp l e : n ( Na OH)=n( KHp ht h a l a t e )=m/ MM =0 . 8 5/ 204. 2 3 g/ mol=0 . 00 416 mol c( Na OH)=n/ V=0 . 0 041 6/ 0 . 03 433=0. 121 2M 3 ) . Con c e nt r a t i o nofHCl Ta k et a b l e6# 1a sa ne xa mpl e : St a nda r di z e dc( Na OH)=0. 1 21 4M, V( Na OH)=0 . 0 195 L,V( HCl )=0. 025 L n ( HCl )=n( Na OH)=c( Na OH)V( Na OH)=0 . 12 14M *0 . 0 19 5L=0 . 00 23 67mo l c ( HCl )=n( HCl ) /V( HCl )=0. 002 367 mol / 0 . 0 2 5L=0 . 0 94 69 2M 4 ) . Con c e nt r a t i o nofASAi nt a bl e t s Ta k et a b l e t # 1( t a bl e7#1i n di v i d u a l )a sa ne x a mpl e : V( HCl )=0. 0 23 L,c ( HCl )=0 . 0 949 34 8M,V( Na OH)=0 . 0 25 L,m( t a bl e t1)=0 . 4 338 g n ( Na OH) e x c e s s=n( HCl )=c ( HCl ) *V( HCl )=0. 0 94 93M* 0. 0 2 3L=0. 0 0 218 3mo l n ( Na OH)=n( Na OH) t o t a l-n ( Na OH) e x c e s s=c( Na OH) *V( Na OH)n( Na OH) e x c e s s

=0. 1 21 2M*0 . 0 25L-0 . 0 02 18 3mol=0. 000 851 5mo l n ( ASA)=n( Na OH) / 2=0 . 0 00 85 15mo l / 2=0 . 0 00 425 75mol m( ASA)=n( ASA) *MM( ASA) * 4=0. 0 0 042 57 5mol *1 80. 1 5 g/ mol *4=0 . 3 06 81g %wt=m( ASA) / m( t a bl e t1)=( 0. 3 06 81 g/ 0 . 4 3 38g ) *1 00 % =7 0. 626% 5 ) . Me a nc on c e nt r a t i ono fASA Ta k et a b l e7 # 1a se x a mpl e : Li k ea bo v e4 )c a l c u l a t e d, s i mi l a r l y ,wec ou l dg e ta l lm1, m2a ndm3o fASAi n1 t a bl e t . m1=0. 3 06 81g ,m2=0. 3 56 3g , m3=0. 2 94 66 7g m=( m1 +m2+m3) / 3=( 0. 3 06 81g+ 0 . 3 563 g+0 . 2 946 67 g ) / 3=0 . 3 192 g 6 ) . St a nda r dDe vi a t i o n( s d )ofASA Ta k et a b l e1# 1a se x a mp l e : m=0 . 31 92g ,m1=0. 3 0 681 g , m2=0. 3 56 3g , m3=0 . 2 94 66 7g Sd=

√

(m−m 1)2 +( m−m 2 )2+(m−m3 )2 2

=0 . 0 32 6

B.Ca l c u l a t i on sf r omgr o upd a t a 1 ) .Gr o upme a nofmgASA/ t a bl e t E8=AVERAGE( B8: B2 5)=317. 5 6 89 44 4 2 ) .Gr o upme a nof%wt ASAi nt a bl e t F8=AVERAGE( C8: C2 5)=73. 96 9 61 1 11 3 ) .Gr o upme a nof%wt ASAi npo wde r G8=AVERAGE( D8 : D1 3)=76. 19 0 33 3 33 4 ) .St a nd a r dd e vi a t i o n Gr o upASAmg / t a bl e t :E1 1=STDEV( B8 : B2 5)=8. 72 3 52 6 88 Gr o upASA%wti nt a b l e t :F11=STDEV( C8: C2 4)=2. 2 98 2 13 0 95 Gr o upASA%wti np o wde r :G11=STDEV( D8: D13)=2. 0 60 3 75 1 76 5 ) .Tt e s tbe t we e ni ndi v i d ua lme a na ndma nu f a c t ur eme a n

Wh e r e ´x

=32 5mg , xt=316. 3 3 mg ,s=4 . 8 8,N=3

t=3 . 077

6 ) .Tt e s tbe t we e ngr o upme a na n dma nuf a c t u r eme a n

Wh e r e ´x

=32 5mg , xt=3167. 5 7mg ,s=8. 72 ,N=18

t=3 . 62 7 ) .Tt e s tb e t we e ngr o up%wti nt a b l e ta nd%wti np o wde r

Wh e r e x´1 s=8 . 4 0

=7 3 . 9 7 %, x´2

=7 6 . 1 9%,N1=18 ,N2=6

Wh e r e x´1 t=1 . 7 2

=7 3 . 9 7 %, x´2

=7 6 . 1 9%,N1=18 ,N2=6 ,s=8 . 4 0...