1

M U
1.1. L do chn ti: St l mt nguyn t c vai tr quan trng trong cuc s ng ca chng ta, st c nhiu trong mu, hm lng st trong c th khong 7.10 -3% trng lng c th . Thiu st s nh hng n sc kho nh gy b nh thiu muDo vy chng ta cn phi tm cch b sung st cho c th thng xuyn v ung thuc l vic d lm nh t ngoi ch n hp l. Trn th trng c rt nhiu loi thu c cha st nhng ti ny chn thuc Ferrovit (Thi Lan). C nhiu phng php xc nh hm lng st trong thuc nhng phng php complexon v phng php oxi ho- kh c nhiu u im ring. Do vy, chng ti chn ti: Xc nh hm lng st c trong vin thuc Ferrovit b ng phng php complexon v phng php oxi ho- kh lm ti cho kha lu n ny. 1.2. Mc tiu ca ti: Bit c vai tr quan trng ca phng php oxi ho kh v ph ng php complexon. Nghin cu kh nng xc nh hm lng Fe2+ bng phng php oxi ho kh. Nghin cu kh nng xc nh hm lng Fe3+ bng phng php complexon. So snh gia hai ph ng php trn. 1.3. Nhim v ca ti: Nghin cu kh nng xc nh Fe2+, Fe3+ bng phng php complexon v phng php oxi ho kh. Xc nh hm lng st trong thu c Ferrovit. So snh hm lng st thu c vi hm lng st trn bao b. 1.4. Phng php nghin cu: C nhiu phng php xc nh hm lng cc nguyn t, nhng y s dng hai phng php: Phng php oxi ho - kh. Phng php complexon.

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CHNG 1: TNG QUAN

1.1. Gii thiu v nguyn t s t: St l nguyn t kim loi ph bin th hai (sau nhm) v l nguyn t ng th t v hm lng trong v tri t. Ngi ta cho rng nhn ca tri t ch yu gm st v niken. St chim 1,5% v khi lng ca v Tri t. Mt s hng s vt l quan tr ng: K hiu: Fe; S th t: 26 Khi lng nguyn t: 55,847 Cu hnh electron: [Ar] 3d64s2. Bn knh nguyn t ( Ao): 1,26 Th in cc tiu chun (V): E o Fe 1.2.1. Tnh ch t v t l : St l nguyn t n m phn nhm VIIIB trong chu k 4 ca bng h thng tun hon Mendeleev. St l kim loi c mu trng xm, d rn, d dt mng v gia cng c hc khc. St c bn dng th hnh ( d ng , , , ) bn nhng khong nhit nht nh: Fe-
700oC
911oC
1390oC
1 53 8 o C
3+

m in theo Pauling: 1,83 Nhit nng ch y (oC): 1538 Nhit si (oC): 2880 Kh i lng ring (g/cm3): 7,91
/ Fe 2 +

=+0,77; E o Fe

2+

/ Fe 0

=-0,44;E o Fe

3+

/ Fe 0

= -0,036.

1.2. Tnh cht vt l v ho hc ca s t:

Fe-

Fe-

Fe-

Fe lng.

St to nn rt nhiu h p kim quan trng c bit l vi Cacbon, tu lng cacbon c trong st m ngi ta chia ra thnh: St mm (< 0,2% C), thp (0,2 1,7% C) v gang (1,75% C). 1.2.2. Tnh ch t ho hc: St l m t kim loi c hot tnh ho hc trung bnh. iu kin thng khng c hi m, st khng tc dng vi nhng nguyn t phi kim in hnh nh oxy, lu hu nh, clo, brom v c mng mng oxit b o v. Khi un nng, c bit l trng thi b t nh, st tc dng vi hu ht phi kim. Khi un nng trong khng kh kh, st to thnh Fe3O4.

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St tinh khit bn trong khng kh v nc. Ngc li, st c cha tp cht b n mn di tc dng c a hi m v oxy trong khng kh to nn g st: 4Fe + 3O2
n H 2O

2Fe2O3.

Do lp g st xp v gin nn khng b o v c st khi b oxi ho tip. St to thnh hai dy h p cht Fe2+ v Fe3+. Mui Fe2+ c to thnh khi ho tan st trong dung d ch axit long tr axit nitric. Mui ca Fe2+ vi axit mnh nh: clorua, sunfat... d tan trong nc, cn mu i c a cc axit yu nh: sunfua, cacbonic... kh tan. Khi tan trong nc, mu i st dng [Fe(H2O)6]2+ mu lc nh t. Mu lc c a [Fe(H2O)6]2+ rt yu nn thc t dung dch ca mu i Fe2+ khng c mu. Quan trng vi thc t nht l (NH4)2Fe(SO4)2.6H2O, c gi l mu i Mohr. Tinh th mui Mohr c mu lc, d kt tinh, khng ht m v bn i vi oxy khng kh nn c dng pha dung d ch chun Fe2+ trong ho h c phn tch. Mui Fe3+ b thu phn mnh nn dung d ch c mu vng nu. Ch trong dung dch c phn ng axit mnh (pH < 1) s th y phn mi b y li. Cc mu i Fe3+ cng d b kh v mu i Fe2+ bng nhiu ch t kh khc nhau nh: N2H4, HI... 2Fe3+ + 3I2Fe2+ + I3Fe2O3 c mu nu, c iu ch bng cch nung kt ta Fe(OH)3. Fe2O3 khng tan trong nc, c th tan m t phn trong kim c hay cacbonat kim loi kim nng chy. Ion Fe3+ trong dung dch tc dng vi ion SCN- to nn m t s phc thioxianat. Ho phn tch thng s d ng phn ng ny nh tnh v nh lng Fe3+ ngay c trong dung dch long. 1.3. Gii thiu v vai tr ca nguyn t st: Hm lng st trong c th l rt t, chim kho ng 0,004% c phn b nhiu lo i t bo ca c th . St l nguyn t vi lng tham gia vo cu to

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thnh phn Hemoglobin ca hng cu, myoglobin ca c vn v cc sc t h h p m bo v trong cc enzim nh: catalaza, peroxidazaSt l thnh phn quan trng ca nhn t bo. C th thiu st s b thiu mu nht l ph n c thai v tr em. Trong c th st c hp thu ng tiu ho di dng v c nhng phn ln d i d ng hu c vi cc cht dinh dng c a th c n. Nhu cu h ng ngy ca m i ngi l t kho ng 10 - 30 mg. Ngun st c nhiu trong th t, rau, qu, lng trng, u a, mn 1.4. Phng php chu n complexon: 1.4.1. Cc cht ch th dng trong chun complexon: 1.4.1.1. Eriocrom en T (k hiu: ETOO, NET): Cng thc dng H3In c pK1 <0 (phn li hon ton); pK2 = 6,3; pK3 = 11,6. H3In pKi: Mu pH tn ti = <0 H2In = 6,3 Xanh pH = 7 11 Cc phc c a ion kim lo i vi ch th ETOO th ng c mu hng ( nho), v th cc php chu n complexon vi ch th ETOO u c tin hnh trong kho ng pH = 7 11 s chuyn mu c tnh tng ph n ( h ng xanh). 1.4.1.2. Murexit (k hiu: MUR): Cng thc dng H4In- (tn ti dng mu i amoni) c pK1 <0 (phn li hon ton); pK2 = 9,2; pK3 = 10,9; pK4, pK5 ln HIn2= 11,6 Vng da cam pH < 7 pH > 11 In3-

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H4InpKi: Mu pH tn ti Tm hng <9

= 9,2

H3In 2-

= 10,9

H2In 3-

Tm pH = 9 11

Tm xanh pH > 11

Cc phc ca ion kim lo i vi ch th Murexit thng c mu (CaH2In) hoc mu vng cam (CuH2In, NiH2In, Co2HIn ). Cc php chun complexon vi ch th Murexit u c tin hnh trong kho ng pH > 11 c hiu sut to phc tt nh t. 1.4.2. Cc phng php chu n complexon: C nhiu phng php chun complexon, nhng thng gp 3 phng php sau y: 1.4.2.1. Chun trc tip: Phng php chun complexon n gin nht l phng php chun trc tip. Trong ph ng php ny, ngi ta iu ch nh pH thch hp c a dung d ch chu n bng m t h m v sau thm dung dch chun t buret, thng l complexon III Na2H2Y, vo dung dich chun cho n khi i mu ca ch t ch th t mu c a phc kim lo i ch th sang mu c a cht ch th trng thi khng to phc. ngn nga s to hiroxit kim loi pH chun ngi ta thng thm cc cht to phc tng i yu, V d , dng hn hp m NH3 + NH4Cl duy tr pH = 10,0 khi chun Zn2+, Cu2+, Ni2+ gi cc ion ny trong dung dch dng ph c vi amoniac. 1.4.2.2. Chun ngc: Trong trng hp khng th chun trc tip c, V d khng th c cht ch th thch hp cho kim loi xc nh, hoc khi phn ng to phc gia ion kim lo i v EDTA xy ra qu chm, hoc pH chun kim loi b kt ta di dng hidroxit kim loi, th phi s dng phng php chun ngc. Trong trng hp ny ngi ta thm vo dung dch cn chun m t lng chnh xc EDTA l y d v thit lp iu kin (nhit , pH) ion kim loi M1 phn ng hon ton vi EDTA. Sau chun lng EDTA d bng m t dung d ch

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chu n ion kim loi M2 ly t buret cho n khi i mu cht ch th t mu ca d ng ch th khng to phc sang mu ca ph c ch th - kim loi M2. 1.4.2.3. Chun th: Khi khng th chun trc tip kim lo i M1 b ng EDTA th c th thay th M1 bng mt lng tng ng kim lo i M2 c th chun trc tip b ng EDTA. Mu n vy, ngi ta cho m t lng d dung dch complexonat M2 (M2Y) vo dung dch chun v sau khi phn ng trao i: M2Y + M1 M1Y + M2 xy ra th chu n M2 bng EDTA. 1.5. Phng php chu n oxi ho- kh: 1.5.1. Cc cht ch th dng trong chun : 1.5.1.1. Cc ch t ch th c bit: L nhng ch t ch th c phn ng chn lc vi m t dng no c a cp oxi ho - kh v gy ra s i mu. V d : Dng h tinh bt trong php chun o iot do h tinh bt to c vi iot phc mu xanh. H tinh b t + I2 mu xanh lam c trng. Dng ion thioxianat SCN l ch th trong php chun st do ion ny to c vi ion Fe3+ phc mu mu: iSCN- + Fe3+ [Fe( SCN)i] 1.5.1.2. Cht ch th l bn thn cht oxi ho kh: V mt d ng ca ch t oxi ho kh c a cht ch th c mu khc vi mu ca dng oxi ho hoc kh lin hp. Do trong php chun n cn c dng lm cht ch th. V d: Trong php chu n nhiu ch t kh vi kali pemanganat khng cn dng ch t ch th, v lng d rt t MnO4- lm cho dung dch c mu tm, nn bn thn ion ny cng l cht ch th . K= M Y / M Y 1 2 (7.51)

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1.5.1.3. Cht ch th oxi ho- kh: Cht ch th oxi ho kh l nhng cht ch th m mu sc ca chng thay i khi t n mt gi tr th oxi ho kh nht nh. V b n thn cht ch th c tnh cht oxi ho kh v mu dng oxi ho khc mu d ng kh. Loi cht ch th ny rt quan trng v s lng ca chng rt ln v ph m vi s d ng kh rng. Th oxi ho - kh ca ch t ch th oxi ho kh: Phn ng oxi ho kh c a cht ch th l ph n ng thu n nghch: In Ox + ne InKh In Ox l d ng oxi ho c a cht ch th , c mu khc vi mu ca d ng InKh. V d: iphenylamin l cht ch th oxi ho - kh: InOx tm + 2e In Kh khng mu Eo = 0,76V

Vi E < 0,76 th dung dch khng mu; E > 0,76 th dung dch c mu tm. Yu cu vi ch t ch th oxi ho - kh: Cht ch th oxi ho- kh c th c s dng cho kt qu ng trong trng hp, n u s thay i mu c a n trng vi im tng ng, tc l c khong tc dng trong vng bc nh y. C nhng yu cu sau vi ch t ch th oxi ho - kh: + Mu sc ca dng oxi ho - kh phi khc nhau. S thay i mu phi thay i r khi dng mt lng nh cht ch th; + Ch t ch th cn ph i c tc dng im tng ng vi mt lng d rt nh cht kh hay cht oxi ho; + Khong tc dng ca n phi nh; + Cht ch th phi bn i vi tc d ng c a mi trng xung quanh: oxi ca khng kh, kh cacbonic, nh sng, v.v Cc lo i cht ch th oxi ho - kh: + iphenylamin NH(C6H5) 2: Rt t tan trong nc, b oxi ho b i nhiu cht oxi ho. Dung dch gc c pha ch trong dung dch H2SO4.

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+ Axit iphenylamin sufonic: Mu i natri v bari c a axit ny tan trong nc. Th thc ca cht ch th pH = 0 l 0,88 V. C th dng cc cht ch th ny chun cc cht oxi ho bng FeSO4. + Feroin: Ion Fe2+ phn ng vi o-phenantrolin C12H8N2 to thnh ion phc Fe(C12H8N2)32+ c mu , khi b oxi ho th chuyn thnh Fe(C12H8N2)33+ c mu xanh nh t: Fe(C12H8N2)32+ Erioglauxin A v.v 1.5.2. Cc phng php chu n oxi ho kh: 1.5.2.1. Phng php pemanganat: C s ca phng php: Phn ng oxi ho bng ion pemanganat MnO4- l c s c a phng php pemanganat, c th thc hin trong mi trng axit, kim hoc trung tnh. Nhng th ng gp chu n trong mi trng axit. Pha ch dung dch chun KMnO4 theo cc bc sau: Ho tan lng cn KMnO4 trong nc ct, un si dung dch mt thi gian, lm lnh ri lc ht vt MnO2. Dung dch thu c cn chun ho li bng cht chun gc H2C2O4.2H2O nhit 80 90 oC. Cc phng php chun pemanganat: + Chun trc tip cht kh b ng pemanganat: C th dng ph ng php ny chun trc tip cc cht kh: oxalat, Fe(II), ioua, feroxianua Trong iu kin thc nghim thch h p, c th dng pemanganat chun cc cht khc. V d: Trong mi trng trung tnh c th chun Mn(II) thnh Mn(IV): mi trng c HCl, NH4F hoc pirophotphat c th chu n Mn(II) thnh Mn(III); chun NO2- thnh NO3-. + nh lng ch t kh qua phn ng vi Fe(III): C mt s kim loi khng th chun trc tip bng KMnO4. Ngi ta cho chng tc dng vi lng d Fe3+ to thnh Fe2+. Sau chun Fe2+ bng KMnO4. Fe(C12H8N2)33+ + e Ngoi ra, mt s cht ch th oxi ho kh khc: Inigo, monosunfonat,

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V d: Chun Cr(II) thnh Cr(III) + nh lng gin tip ch t kh dng pemanganat d: Nhiu cht kh phn ng qu chm vi pemanganat nn khng th chun trc tip c m cho chng tc dng vi lng d chnh xc KMnO4 d. Sau chu n lng d b ng natri fomiat ho c bng ph ng php iot. V d: Chun Ioua thnh Io at, xianua thnh xianat + nh lng gin tip ch t oxi ho dng cht kh d: Nhiu cht oxi ho phn ng ch m nn khng th chun trc tip vi cht kh . Ngi ta cho phn ng vi lng d cht kh . Sau chu n lng d ch t kh bng dung d ch KMnO4. V d : Dng Fe(II) d kh Cr(VI) thnh Cr(III). Sau chu n Fe(II) d b ng dung dch KMnO4. + nh lng gin tip cc kim lo i to c kt t a oxalat: Kim lo i c lm kt ta di dng oxalat kh tan, sau l c, ra kt ta, ho tan trong axit r i chun axit oxalic to thnh bng dung dch pemanganat. C th dng cch ny chu n canxi, caini, km, ch, coban, niken, thori, nguyn t t him. 1.5.2.2. Phng php icromat: C s c a phng php: Ph n ng oxi ho bng ion Cr2O72- (c th l K2Cr207) l c s ca phng php ny. Dung d ch chu n icromat rt bn, c th axit ho b ng axit sufuric, axit pecloric long, c th chu n bng icromat nhit thng khi c mt HCl n nng 3,5M. Cht ch th dng trong phng php icromat: C th dng cc cht ch th iphenylamin, iphenylbenzi in v tt nht l natri iphenyl sunfonat. ng dng : ng dng quan trng ca phng php icromat l chun Fe(II). C th chun trc tip hoc gin tip. + Chun cc ch t oxi ho: Cho cht oxi ho tc dng vi lng d Fe(II). Sau chu n ngc Fe(II) d b ng K2Cr2O7.

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10

+ Chun cc cht kh: Cho cc cht kh tc dng vi Fe(III) v chun Fe(II) to thnh, nu cht kh phn ng chm vi Fe(III) th c th thm d icromat ri chun ngc icromat bng Fe(II). u im: u im ca phng php ny l c th iu ch cht chun tinh khit mt cch d dng v r tin, d b o qun, dung d ch chun b n, c th chu n khi c HCl nng khng qu cao. V nhiu phng php khc nh: phng php Xeri (dng Ce4+ lm cht oxi ho); phng php Bromat (dng BrO3- lm ch t oxi ho); phng php Vanadat (dng VO2+ lm cht oxi ho); phng php It (dng I- lm cht kh hoc I2 lm ch t oxi ho). 1.6. Gii thiu v thuc Ferrovit: Thiu mu l do s mt cn bng gia s tiu hu qu mc vi s gim thiu qu trnh ti to mu . Mu c sinh ra t tu xng. ngi trng thnh, h ng ngy c th mt i 40- 50ml mu. Nu tu xng khng ti to li s lng mt gy ra hin tng thiu mu vi cc triu chng th hin bn ngoi nh: da xanh, nim mc nht nhc, mng tay mng chn mm d gy, nt mp, vim li kh nut, tc kh d gy,ng thi, thiu mu lm nh hng dng ch y v khng kh trong mu lm tim p nhanh, n u ko di s gy ra b nh l tim: suy tim xung huyt, vim c tim,C nhiu nguyn nhn d n n thiu mu. Trong , thiu mu do thiu st hay cn gi l thiu mu hng cu nh nhc sc l mt h i chng thiu mu thng hay gp. Hng ngy tu xng s dng khong 30mg st to hng cu, mt lng st c s dng li t qu trnh tan mu, lng cn li phi c cung cp t thc n. Cng dng ca thuc Ferrovit: Ferrovit phng nga bnh thiu mu do thiu st ph n c thai, cho con b, tr em tui dy th, ph n trong th i k kinh nguyt. Ferrovit b sung st, axit folic v vitamin B12 trong cc trng hp mt mu do ph u thu t, ch n thng, nhim giun, ngi hin mu, Cch dng: ung mi ngy mt vin sau ba n.

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11

Lo thuoc Xuat su vien thuoc Trong vin thuc Ferrovit st tn ti di dng st fumarat, c cng thc C4H2FeO4:

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12

CH NG 2: K THUT THC NGHIM

2.1. Dng c v thit b nghin cu: Cc dng c thu tinh o th tch nh: pipet, buret, bnh tam gic, bnh nh mc, phu chit. Cn phn tch, my khuy t, l nung, t sy 2.2. Chun b mu: Mu c mua t i ca hng thuc. 2.3. Ho cht: EDTA. K2Cr2O7 Cc ho ch t khc: HNO3, HCl, H2SO4, NH3, H3PO4... Ch th: iphenylamin, axit sunfosalixilic. 2.4. Cch pha dung d ch v cch tin hnh: 2.4.1. Cch pha dung dch: Ho tan vin thuc Ferrovit vi 20ml nc nng trong bnh tam gic 250ml + 5ml dung dch HCl m c. y cc bng mt knh ng h, un nh n tan hon ton (thm 10 20 git HNO3, nu mu kh tan). Thm kho ng 30ml nc, dung d ch c mu vng c a FeCl3. Dung dch chu n EDTA 0,0500M: Ha tan 4,6530g Na2H2Y.2H2O trong bnh nh mc 250 ml, nh mc bng nc ct n vch. Cc dung dch long h n c pha ch b ng cch pha long ho c ly nhng lng cn nh hn. Dung dch chun K2Cr2O7 0,0200M: Ho tan 1,4709g K2Cr2O7 trong bnh nh mc 250 ml, nh mc b ng nc ct n vch. iphenylamin: ha tan 1g cht ch th trong 100ml H2SO4 c. Axit sunfosalixilic: ha tan 5g cht ch th trong 95ml nc ta c dung d ch axit sunfosalixilic 5%. 2.4.2. Cch tin hnh th nghim: 2.4.2.1. Chun dung dch Fe(II) bng K2Cr2O7: Mun nh tng hm lng st trong dung dch, phi kh Fe3+ thnh Fe2+ (th ng dng NH2OH) nh sau:

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13

Dung d ch mu + 3ml NH2OH v un n khi mt mu vng. Sau cho thm 5ml HCl 1M (hoc H2SO4 1M)+ 2ml H3PO4 c + 4-5 git iphenylamin. Chun bng dung dch K2Cr2O7 n khi dung dch c mu tm. 2.4.2.2. Chun dung dch Fe (III) bng EDTA: Mun nh tng hm lng st trong dung dch, phi oxi ho Fe2+ thnh Fe3+ (th ng dng (NH4)2S2O8) nh sau: Dung d ch mu + thm mt t tinh th (NH4)2S2O8, un nh vi pht. ngui + vi git ch th axit sunfosalixilic, thm tng git NH3 cho n khi dung d ch c mu tm m (pH khong 2,5). Chun b ng EDTA n khi dung dch mt mu tm (dung dch c mu vng nh t ca FeY-).

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14

CHNG 3: KT QU V THO LUN

3.1. Chun bng phng php oxi ha kh:
Chun Fe2+ bng K2Cr2O7 Tin hnh chun bng K2Cr2O7 0,0200M ta thu c kt qu sau: Kt qu t 1: Bng 3.1: Th tch K2Cr2O7 0,0200M dng chun Fe2+ (t 1) S th t 1 2 3 Gi tr trung bnh Phn ng chu n Fe2+ b ng K2Cr2O7: 6 Fe2+ - e Fe3+ Cr2O72- + 14H+ + 6e 2Cr3+ + 7H2O Cr2O72- +14H+ + 6Fe2+ 6Fe3+ + 2 Cr3+ + 7H2O T ph n ng ta c: S mol Fe2+ = 6 x s mol Cr2O72= 6.7,83.0,0200/1000 = 9,40.10-4mol Kh i lng st fumarat c trong mu l: m =9,40.10 -4.169,9 = 0,1597g Kt qu t 2: Tin hnh tng t nh t 1, ta thu c kt qu nh sau:
VK 2Cr2O7

7,85ml 7,80ml 7,85ml 7,83ml

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Bng 3.2: Th tch K2Cr2O7 0,0200M dng chun Fe2+ (t 2) S ln chun 1 2 3 Gi tr trung bnh
VK 2Cr2O7

7,75ml 7,75ml 7,80ml 7,77ml

S mol Fe2+ = 6.7,77.0,0200/1000 = 9,32.10-4mol Kh i lng st fumarat c trong mu l: m = 9,32.10-4.169,9 = 0,1583g B ng 3.3: Khi lng st fumarat c trong vin thu c Ferrovit theo phng php chun Fe2+ bng K2Cr2O7 STT 1 2 Gi tr trung bnh
VK2Cr2O7

Kh i lng st fumarat 159,7mg 158,3mg 159,0mg

7,83ml 7,77ml

Khi lng ghi trn bao b: 162,00mg C4H2FeO4/vin Qua 2 t chun thu c khi lng st fumarat c trong mu phn tch l 158,3 159,7mg. Kt qu ny so vi khi lng ghi trn bao b chnh lch khng nhiu, t 2,3 3,7mg. Sai s tng i c tnh theo cng thc: q% =
Xa 159, 0 162, 00 .100% = 1,852% .100% = 162, 00 a

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Ta thy sai s ca php xc nh l khng qu ln nn c th dng phng php ny xc nh hm lng st trong vin thuc Ferrovit.

3.2. Chu n b ng ph ng php complexon: Chu n Fe(III) b ng

EDTA. Tin hnh chun bng EDTA 0,0500M ta thu c kt qu sau: Kt qu t 1. Bng 3.4: Th tch EDTA 0,0500M dng chu n Fe3+ (t 1) S ln chu n 1 2 3 Gi tr trung bnh Phn ng chu n Fe3+ b ng EDTA: Fe3+ + H2Y2- FeY- + 2H+ T ph n ng ta c: n Fe3+ = nEDTA = 18,83.0,0500/1000 = 9,42.10-4mol Kh i lng st fumarat c trong mu l: m =9,42.10-4.169,9 = 0,1600g Kt qu t 2: Bng 3.5: Th tch EDTA 0,0500M dng chu n Fe3+ (t 2) S ln chun 1 2 3 Gi tr trung bnh VEDTA 18,95ml 19,00ml 18,90ml 18,95ml VEDTA 18,80ml 18,85ml 18,85ml 18,83ml

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Phn ng chu n Fe3+ b ng EDTA: Fe3+ + H2Y2- FeY- + 2H+ T ph n ng ta c: n Fe3+ = nEDTA = 18,95.0,0500/1000 = 9,48.10-4mol Kh i lng st fumarat c trong mu l: m =9,48.10-4.169,9 = 0,1610g B ng 3.6: Khi lng st fumarat c trong vin thu c Ferrovit theo phng php chun Fe3+ bng EDTA STT VEDTA Kh i lng st fumarat

1 2 Gi tr trung bnh

18,83ml 18,95ml

160,0mg 161,0mg

160,5mg

Khi lng ghi trn bao b: 162,00mg C4H2FeO4/vin Qua 2 t chun thu c khi lng st fumarat c trong mu phn tch l 160,0 161,0mg. Kt qu ny so vi khi lng ghi trn bao b chnh lch khng nhiu, t 1,0 2,0mg. Sai s tng i c tnh theo cng thc: q% =
160,5 162, 00 Xa .100% = .100% = 0,926% a 162, 00

Ta thy sai s ca php xc nh l khng qu ln nn c th dng phng php ny xc nh hm lng st trong vin thuc Ferrovit.

3.3. So snh khi lng s t fumarat tnh theo 2 phng php chun trn:
T kt qu thu c trn, chng ti tin hnh so snh theo b ng sau:

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Bng 3.7. So snh kh i lng st fumarat tnh c theo hai phng php Khi lng STT Phng php 158,3 159,7mg oxi ho kh Phng php 160,0 161,0mg complexon Gi tr thc 162,00mg (Gi tr trn bao b) T bng 3.7 ta thy: Sai s tuyt i c a hai phng php so vi gi tr th c khng qu ln (nh h n 4,0mg). Sai s tng i c a hai phng php < 2%. Ph ng php chu n oxi ho kh c sai s ln h n phng php complexon, iu ny c th do qu trnh oxi ho Fe2+ Fe3+ (phng php complexon) l tt hn qu trnh kh Fe3+ Fe2+ (phng php oxi ho kh). V v y, trong thc t ngi ta thng tin hnh xc nh hm lng st theo phng php chun complexon. Tuy nhin phng php ny ch xc nh t t khi hm lng st kh ln. Nu hm lng st qu b th ngi ta thng dng phng php trc quang. (Xc nh st di dng Fe2+ vi thuc th o-phenantrolin; Xc nh st di dng Fe3+ vi thuc th SCN- ho c Axit sunfosalixilic) 1,0 2,0mg 0,926% 2,3 3,7mg 1,852% C4H2FeO4 Sai s tng i trung bnh

Sai s tuyt i

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KT LUN
T thc nghim xc nh hm lng st trong thuc Ferrovit ta thy: Phng php complexon v phng php oxi ha- kh c s dng c hiu qu trong php chun ny. + Phng php oxi ho kh c sai s 1,852%. + Phng php complexon c sai s 0,926%. C hai gi tr ny khng qu ln, c th chp nh n. S chnh lch hm lng st gia hai phng php ny l khng nhiu. Qua ta th y vai tr ca hai phng php trn trong qu trnh phn tch nh lng.

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TI LIU THAM KHO.

1. o Th Phng Dip Vn Hu (2007), Cc ph ng php nh lng ho hc, NXBHSP, H Ni. 2. Nguyn Tinh Dung (2003), Ho hc phn tch, phn III: Cc phng php phn tch ho hc, NXBGD, H N i. 3. H S Linh (2005), Nghin cu s to ph c gia Fe(III) vi thu c th PAR bng phng php tr c quang. ng dng xc nh hm lng s t trong vin nang Ferrovit Dc phm Thi Lan, Lun vn Thc s, H Vinh. 4. Nguyn Th Thu Nga (2005), Gio trnh Thc hnh ho h c phn tch, NXBGD, H N i. 5. Nguyn Ngc Phng (2006), Xc nh hm lng iot c trong mui iot bng phng php oxi ho kh, Kho lu n tt nghip, H ng Thp. 6. H Vit Qu (1999), Cc ph ng php phn tch ho h c hin i, NXBHQG, H Ni.

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