TRNG H CNG NGHIP TP H CH MINH VIN CNG NGH SINH HC & THC PHM B MN: PHN TCH THC PHM

TIU LUN

Ging vin hng dn: Lp:

NGUYN C VNG HTP 4 TLT

Tp. HCM, thng 11 nm 2011

2

VIN CNG NGH SINH HC V THC PHM GVHD: NGUYN C VNG B MN: PHN TCH NH LNG TIU LUN:

DANH SCH NHM STT 1 2 3 4 5 6 7 8 9 10 11 12 13 THNH VIN MSSV 10320561 10378431 10347691 10369471 10318501 10321621 10347681 10323171 10312591 10353351 10345141 10323591 10319101 NHIM V Tm kim ni dung Tm kim ni dung Tm kim ni dung Tm kim ni dung Tm kim ni dung Tm kim ni dung Tng hp ni dung, chnh sa ni dung Tm kim ni dung Tm kim ni dung Tm kim ni dung Tm kim ni dung Tm kim ni dung Tm kim ni dung

Nguyn L Tho Hong Cp Th Thanh Huyn Phm Th Lang Mai Th Cm Nhung Nguyn Th Hng Nhung Nguyn Phc Quang inh Quang Thnh Tn Thnh H Hunh Phc Thng Trn Quc Thng Bi Th Kim Thoa H Thanh T Nguyn Th Thy Vn

3

Tp. HCM, thng 11 nm 2011 LI CM N

Qua thi gian thc hin bi tiu lun vi ch TM HIU V PHNG PHP SC K TRAO I ION gip chng em hiu su hn v phng php Sc k trao i ion trong Phn tch nh lng ca ngnh Ha hc cng nh trong ngnh cng ngh thc phm, v phng php phn tch thc phm bng sc k trao i ion; ng thi gip nng cao cc k nng cn thit khi lm bi tiu lun. c c nhng iu l nh s gip ca mi ngi. Chng em xin chn thnh cm n: Trng H Cng Nghip HCM to iu kin cho chng em tt nghip c tip tc hc lin thng ln i hc ti y. Vin CN Sinh Hc V Thc Phm cung cp cc ti liu hc tp mn Phn tch thc phm n chng em dng lm c s thc hin bi tiu lun ny. Thy: Nguyn c Vng tn tnh hng dn cho c lp ni chung v nhm chng em ni ring c th hon thnh trn vn bi tiu lun ny. Gia nh, bn b ng vin v gip .

Tp. HCM, thng 11 nm 2011 Nhm: Sc k trao i ion

4

MC LC. LI CM N...................................................................................................2 MC LC........................................................................................................3 PHN A. M U..........................................................................................6 1. T VN ....................................................................................................6 2. MC CH, YU CU.....................................................................................6 3. I TNG NGHIN CU............................................................................6 4. PHNG PHP NGHIN CU......................................................................7 5. PHM VI NGHIN CU..................................................................................7 6. KT QU NGHIN CU.................................................................................7 PHN B. NI DUNG.......................................................................................8 Chng 1. GII THIU V SC K..............................................................8 1.1. TNG QUAN V SC K............................................................................8 1.1.1. Vi nt lch s...............................................................................................8 1.1.2. Dnh ngha....................................................................................................9 1.2. PHN LOI V CC PHNG PHP TCH SC K............................9 1.2.1. Phn loi theo h pha....................................................................................9 1.2.2. phn loi theo c ch tch.............................................................................10 1.2.2.1. Sc k hp th............................................................................................10 1.2.2.2. Sc k phn b lng - lng........................................................................10 1.2.2.3. Sc k ion ( trao i ion)............................................................................10 1.2.2.4. Sc k ry phn t (sc k loi c)............................................................10 1.2.3. phn loi theo cch hnh thnh sc ...........................................................11 1.2.3.1. phn tch tin lu.......................................................................................11 1.2.3.2. phn tch th y........................................................................................11 1.2.3.3. Phn tch ra gii.......................................................................................12 1.3. CC LC LIN KT TRONG SC K.......................................................13 1.3.1. Lc lin kt ion.............................................................................................13 1.3.2. Lc phn cc................................................................................................13 1.3.3. Lc Van - de - Van (lc phn tn)................................................................145

1.3.4. Lc tng tc c bit..................................................................................14 1.4. S TNG TC GIA BA THNH PHN TRONG H SC K............14 1.5. MT S I LNG DNG TRONG SC K.........................................16 1.5.1. H s phn b KD v cch xc nh..............................................................16 1.5.2. S lin h gia tc di chuyn ca cht phn tch v KD ..........................17 1.5.3. Thi gian lu tR, thi gian lu hiu chnh tR ................................................17 1.5.4. Th tch lu Vm, th tch lu hiu chnh........................................................18 1.5.5. H s tch (cn gi l h s lu gi tng i).........................................18 1.5.6. Sc ...........................................................................................................18 1.5.7. a l thuyt.................................................................................................19 1.5.7.1. Khi nim a l thuyt..............................................................................19 1.5.7.2. a l thuyt c tnh thi gian khng lu gi, nef .....................................20 1.5.8. phn gii v cch lm tng phn gii..................................................20 1.5.8.1. phn gii...............................................................................................20 1.5.8.2. Cch lm tng phn gii........................................................................21 Chng 2. SC K TRAO I ION...............................................................24 2.1. KHI QUT V SC K TRAO I ION..................................................24 2.2. BN CHT CA QU TRNH SC K TRAO I ION..........................25 2.2.1. Ionit..............................................................................................................26 2.2.1.1. Nha trao i ion.......................................................................................26 2.2.1.2. Cationit......................................................................................................27 2.2.1.3. Anionit.......................................................................................................28 2.2.1.4. Ionit lng tnh..........................................................................................29 2.2.2. C ch trao i ion........................................................................................29 2.3. CC YU T NH HNG........................................................................31 2.4. THIT B NG DNG..................................................................................31 2.4.1. Mt s thit b sc k trao di ion dng trong phng th nghim..................31 2.4.2. ng dng ca sc k trao di ion trong phn tch nh lng......................33 2.5. SO SNH VI CC PHNG PHP KHC V TI U HA SC K TRAO I ION..........................................................................................................34 2.5.1. im ging nhau...........................................................................................346

2.5.2. im khc nhau............................................................................................34 2.5.3. Ti u ha sc k trao i ion.......................................................................35 PHN C. TI LIU THAM KHO................................................................37

7

PHN A. 1. T VN :

M U

Ngy nay vi s php trin nhanh ca khoa hc cng ngh thc phm, to ra nhiu to ra nhiu sn phm thc phm vi nhiu chng loi khc nhau p ng nhu cu ngy cng cao ca con ngi. C nhiu loi thc phm d b h hng hoc ko di thi gian bo qun, t dc ngun nguyn liu hay sn phm nh mong mun cn s dng cht bo qun hay thuc bo v thc vt, nhng c nhiu khi ngi ta s dng vt qu nng cho php gy nh hng xu n ngi tiu dng, thit hi ln n doanh nghip, tn tht nn kinh t Quc gia. S ra i v pht trin ca ngnh phn tch thc phm d to ra nhiu thit b phn tich nhanh v chnh xc cung gii quyt mt phn no v cc vn ny. V th, nhm chng em quyt nh chn mng phn tch thc phm bng phng php sc k, kt hp vi phng php trao i ion thc hin nghin cu mt ti hon chnh, l: Tm hiu v phng php sc k trao i ion 2. MC CH, YU CU: Mc ch: - tm hiu chung v phn tch thc phm bng phng php sc k. - tm hiu v bn cht, cc yu t nh hng, thit b ng dng v so snh vi cc phng php khc t nhm khc phc nhng nhc im nhng hn ch ca phng php sc k trao i ion nng cao tnh kh dng ca phng php ny. Yu cu: - Vn dng side bi ging ca thy Nguyn c Vng, cc cun sch v cc ti liu t nhiu ngun chuyn v phn tch thc phm bng sc k trao i ion nghin cu v phng php ny. 3. I TNG NGHIN CU: - Bn cht ca qu trnh sc k trao i ion - Cc yu t nh hng - Thit b v ng dng ca phng php ny8

- So snh vi cc phng php phn tch thc phm khc 4. PHNG PHP NGHIN CU: - Tm kim ni dung t nhiu ngun - Tp hp ni dung - Bin tp li thnh bi hon chnh - 5. PHM VI NGHIN CU: - Bi tiu lun c nghin cu v thc hin trong khong 2 tun, c thc hin ti trng H Cng Nghip HCM - Thng tin trong bi tiu lun c su tm t nhiu ngun. 6. KT QU NGHIN CU: - Lm r c bn cht, c ch ca qu trnh - Tm hiu su hn v sc kh trao i ion - Tm ra c nhng yu t nh hng n qu trnh - Nu c nhng ng dng v thit b trong chuyn ngnh phn tch thc phm. - So snh u v nhc im vi cc phng php khc - ra c nhng bin php cho s ti u ha ca sc k trao i ion.

9

PHN B.

NI DUNG.

Chng 1. GII THIU V SC K. 1.1. TNG QUAN V SC K. 1.1.1. Vi nt lch s. Phng php sc k c pht trin vo nm 1903 do nh thc vt hoc ngi Nga Michael C.Txvet.ng thc s l ngi u tin c cng tm ra phng php, gii quyt vn tch cc cht c tnh cht ging nhau theo mt c ch c o, hon ton khc vi phng php tch tng c trc y, tuy nhin pht hin ny b lng qun nhiu nm. Nm 1941, Martin v Synge pht trin sc k phn b trn giy v a ra l thuyt a gii thch cc qu trnh sc k, cc tc gi ng dng tch cc ancaloit t cc cy thuc phc v cho ch to dc phm. Do c cng trong vic pht trin l thuyt ca phng php cho nn nm 1952 hai ng c nhn gii thng Nobel v ho hc. Cng t nm 1952 nhng my sc k mi ra i t ra c u th do c hiu qu tch rt cao. Ct mao qun v cc detect sau ny c ci tin tng phn gii v nhy ca phng php ngi ta c th phn tch c cc cht c hm lng nh c ppm v ppb. T y phng php c pht trin nhanh, ng dng c nhiu trong thc t.10

V sc k lng mt k thut mi c pht hin t nm 1970 lm tng hiu qu tch l sc k lng hiu nng cao (high performance lipuid chromatography- HPLC): Cht nhi ct c ci tin, my tnh v thit b vo b tr c a vo, tng cng kh nng ca phng php. Ngy nay k thut ghp ni gia sc k v cc phng php khc c p dng. l k thut ghp ni gia sc k v khi ph ( GC-MS, GC-MS) sc k v cng hng ht nhn, sc k a chiu, sc k in mao qun (CEC)... Phng php c chnh xc v nhy rt cao, phn tch c nhiu i tng phc tp hn. 1.1.2. Dnh ngha. Sc k l qu trnh tch da trn s phn b lin tc cc cu t cht phn tch trn hai pha: mt pha thng ng yn c kh nng hp th cht phn tch gi l pha tnh, mt pha di chuyn qua pha tnh gi l pha ng; do cc cu t cht phn tch c i lc khc nhau vi pha tnh, chng di chuyn vi tc khc nhau v tch ra khi nhau. 1.2. PHN LOI V CC PHNG PHP TCH SC K. 1.2.1. Phn loi theo h pha. Phng php u tin c nhiu ngi quan tm, y l phng php phn loi n gin theo h pha tc l cht phn tch phn b gia hai pha l g? S phn loi cc phng php sc k:

h pha

C ch 11

1.2.2. phn loi theo c ch tch. 1.2.2.1. Sc k hp th. sc kh hp th l phng php da trn c s phn b cht phn tch gia pha tnh v pha ng nh tng tc phn t thng qua cc trung tm hp th. Pha tnh l cc cht rn hoc lng c din tch b mt ln, bn vng v mt ho hc. Chng hp th cht phn tch trn b mt ca chng cc mc khc nhau khi cho pha ng cha cht phn tch tip xa vi chng. Tu thuc lc lin kt gia pha tnh v tng cu t cht phn tch c trong pha ng, khi cho pha ng i qua pha tnh chng s di chuyn vi tc khc nhau. 1.2.2.2. Sc k phn b lng - lng. s phn bit gia sc k phn b lng-lng v s phn b thng thng l ch sc k phn b lng - lng cn c gi l sc k chit, pha tnh l cht lng pha ng cng l cht lng, s phn b cht phn tch gia hai pha lng ging nh qu trnh chit, cn s phn b ni chung l s phn chia cht phn tch vo hai pha khng cn xt ti lng hay rn. im khc nhau c bn gia sc k phn b lng - lng v sc k hp ph l ch: sc k phn b lng- lng c ng ng nhit tuyn tnh khong nhit ln, phng php c nhy cao nhng c nhc im l pha tnh khng c bn vng, hin tng tri mt pha tnh lm cho lp li b gim. 1.2.2.3. Sc k ion ( trao i ion). pha tnh thng l pha rn c kh nng trao i ion ca n vi cc cht phn tch trong pha ng.Cht c kh nng trao i cation gi l cationit, cn cht c kh nng trao i anion gi l anionit. Lc lin kt ch yu gia cht phn tch v pha tnh ch yu l lin kt tnh in , ph thuc nhiu vo in tch ca ion cht phn tch, pH ca dung dch v bn knh hidrat ho ca cc ion cht phn tch. V d: phn ng trao i ion gia cationit acid mnh v Ca2+ c th vit nh sau: 2R-SO3H + Ca2+ = (R-SO3)Ca + 2H+ Phn ng ca anionit baz mnh vi Cl- : R-N(CH3)3OH + Cl- = R-N(CH3)3Cl + OH1.2.2.4. Sc k ry phn t (sc k loi c).12

Pha tnh l cc cht rn c din tch b mt ln, xp, c nhng ng i trong lng cht rn, cn gi l mao qun c kch thc c phn t. Cc phn t cht phn tch c th thm vo cht mc khc nhau tu theo kch thc ca chng. Cc cht phn tch c kch thc ln khng th i vo su vo pha tnh c, s b ra gii nhanh cn cc phn t cht phn tch c kch thc nh phn b su vo pha tnh s b ra gii chm. Th t ra gii l cc cht c kich thc nh i ra sau v ngc li. Thi gian lu ca cc cht t l nghch vi kch thc phn t ca chng. Tuy nhin cht phn tch c th c tng tc khc vi pha tnh. Nh vy mt php sc k c th tch theo mt hay nhiu c ch khc nhau m chng ta khng xt y. 1.2.3. phn loi theo cch hnh thnh sc . 1.2.3.1. phn tch tin lu. cc cu t A, B, C c i lc vi pha tnh l A < B< C. Cho hn hp cht phn tch lin tc i qua ct, cht phn tch c i lc vi pha tnh thp nht i trc, tip theo l cht c i lc yu hn. Tuy nhin do chng ta cho lin tc cht phn tch vo nn i sau A l A + B v A+B+C. ch c mt phn cht tinh khit A i trcnng

B

C B A t. V

A A

Sc phn tch tin lu 1.2.3.2. phn tch th y. trong sc k ny, chng ta cng np lng nh hn hp cht phn tch A, B, C vo ct sau cho cht D l cht y lin tc i qua ct. i lc hp th l A