p dng phng php sc k ct v sc k lp mng vo ging dy ho hc ph thng

Trn Mnh Cng

Trng i hc Khoa hc T nhin; Khoa ha hc Chuyn ngnh: Ha Phn tch; M s: 60.44.29 Ngi hng dn: PGS.TS. o Hu Vinh Nm bo v: 2011
Abstract. Trnh by tng quan: s lc v lch s pht trin sc k; nh ngha, nguyn tc ca sc k v phn loi cc phng php sc k; c s l thuyt v sc k; sc k lp mng (thin layer chromatography); sc k giy (paper chromatography); sc k hp ph lng (trn ct); khi qut v cht dip lc (chlorophyl) v carotenoit; khi qut v ion Co2+, Cu2+, Fe3+, Ni2+ v mui ca chng. Tin hnh thc nghim: cc ho cht v thit b cn thit; ch to bn mng t tinh bt sn dy; chit dch t l xanh; tin hnh sc k ct; tin hnh sc k lp mng (thin layer chromatography); tin hnh sc k giy (paper chromatography). Tm hiu cc kt qu thu c sau khi tin hnh thc nghim: tch cht mu trong l xanh, tch cc ion Fe3+, Cu2+, Co2+ ... Keywords. Ha phn tch; Phng php sc k ct; Phng php sc k lp mng; Sc k

Content: A. L do chn ti Sc k l mt phng php phn tch cht hin i c ng dng rng ri trong nhiu lnh vc ca cuc sng. Hc sinh ph thng nhiu nc trn th gii c hc v sc k, nhng nc cha dy sc k cho hc sinh ph thng. ti p dng phng php sc k ct v sc k lp mng vo ging dy ha hc ph thng l ti u tin Vit Nam nghin cu v kh nng a ni dung sc k vo dy trng THPT nc ta. B. Mc ch nghin cu Kho st la chn ra nhng th nghim sc k c th p dng dy cho hc sinh ph thng Vit Nam.

C. Tm tt lun vn

CHNG 1: TNG QUAN

1.1. S lc v lch s pht trin sc k [15, 18, 19] Nm 1903 nh thc vt hc ngi Nga Michael Tsvet dng ct nhm oxit (c ti liu ni ct canxi cacbonat) lm pha tnh v pha ng l ete du ho tch thnh cng chlorophyl t l cy. ng gii thch hin tng bng i lc hp ph khc nhau ca cc sc t v t tn phng php ny l phng php sc k (chromatography), sc k ngha l ghi mu v tch c nhng cht c mu. S pht trin phong ph ca sc k lm cho danh t sc k khng cn ng theo ngha ban u ca n. Tuy nhin tt c cc phng php sc k u c nhng nt chung nht: qu trnh tch da trn s chuyn dch ca hn hp cht phn tch qua lp cht bt ng (pha tnh) l cht rn hoc cht lng mang trn cht rn hoc giy v s chuyn dch c thc hin bng mt cht kh hoc cht lng (pha ng). 1.2. nh ngha, nguyn tc v phn loi cc phng php sc k [10, 15] 1.2.1. nh ngha Sc k l qu trnh tch lin tc tng vi phn hn hp cc cht do s phn b khng ng u ca chng gia pha tnh v pha ng i xuyn qua pha tnh. 1.2.2. Nguyn tc ca sc k Nguyn tc chung ca mi phng php sc k l da trn s phn b cc cht gia hai pha: mt pha thng c nh gi l pha tnh(stationary phase) v mt pha chuyn ng gi l pha ng (mobile phase). 1.2.3. Phn loi cc phng php sc k 1.2.3.1. Phn loi theo trng thi lin hp ca pha ng v pha tnh Gm sc k lng v sc k kh. 1.2.3.2. Phn loi theo c ch ca qu trnh tch Gm Sc k hp ph, sc k phn b, sc k trao i ion v Sc k ry phn t. 1.2.3.3. Phn loi theo cch hnh thnh sc . Gm phng php tin lu, phng php y,phng php ra gii. 1.2.3.4. Phn loi theo thit b hnh thnh sc . Gm sc k ct v sc k phng.

2 1.3. Sc k lp mng (thin layer chromatography) [15, 18] Sc k lp mng hay cn gi l sc k phng l k thut phn b rn lng. Trong pha ng l cht lng c i xuyn qua mt lp cht hp th tr nh silicagel hoc nhm oxit, cht hp th ny c trng thnh mt lp mng, u ph ln mt nn phng nh tm knh, tm nhm, hoc tm plastic. Sc k lp mng c dng trong c phn tch nh tnh v phn tch nh lng. H s di chuyn Rf l i lng c trng quan trng v mc tch. H s di chuyn Rf c tnh theo cng thc:
Rf l v hoc R f l0 v0

Trong l l khong cch t tuyn xut pht ti tm vt sc k, lo l khong cch t tuyn xut pht ti tuyn dung mi, v l tc di chuyn ca cht tan v vo l tc ca dung mi. Nh vy Rf ch c gi tr t 0 n 1. Khi Rf = 0 th cht tan hon ton khng di chuyn, cn khi Rf = 1 th cht tan di chuyn bng tc ca dung mi. C nhiu yu t nh hng n Rf nhng quan trng l: + Cht lng v hot tnh cht hp th + B dy ca lp mng + Cht lng v tinh khit ca pha ng 1.4. Sc k giy (paper chromatography) [15, 19] L mt phng php sc k dng giy hp th phn tch mt lng nh cht lng mang (cht ho tan) v ly ra khi vch cht ho tan tin gn n u kia ca mt bng giy. Trong qu trnh sc k cc cu t c tch dc theo lp mng ca t giy. c trng cho s chuyn ng ca cc cht trn giy l h s di chuy Rf nh sau:
Rf l ; hoc Rf = tc chuyn ng ca mt cu t/ tc chuyn l0

ng ca tuyn pha ng Trong l l on ng i ca cu t, lo l on ng i ca dung mi. Nu Rf ln qu th khng tch c cc cht, Rf b qu th tch chm. 1.5. Sc k hp ph lng trn ct (Adsorption liquid chromatography on columns) [15, 19] Phng php sc k hp ph lng da trn tnh cht hp ph khc nhau ca cc cu t trong hn hp cn tch. Gia nng cht trong dung dch v nng cht b hp ph trn b mt cht hp ph c mt cn bng ng, cn bng ph thuc vo nhit . S ph thuc ca lng cht b hp th vo nng ca n trong dung dch mt nhit khng i c c trng bi

3 ng ng nhit hp ph. Cn c vo ng ng nhit hp ph ta c th chn c iu kin sc k thch hp. Trong sc k hp ph lng trn ct th phng php ra gii c ng dng rng ri nht. Phi chn tc ti u i vi dung mi ra gii m bo thit lp cn bng hp ph, ng thi gim khuch tn dc. 1.6. Khi qut v cht dip lc (chlorophyl) v carotenoit (xanthophyl v caroten) [5, 9, 16] 1.6.1. Cht dip lc (dip lc t, chlorophyl) C 5 loi chlorophyl l chlorophyl a, b, c1, c2 v d (c ti liu chia thnh chlorophyl a,b,c,d v e), thc vt bc cao chlorophyl a v b rt ph bin. Cng thc ca chlorophyl a (C55H72O5N4Mg)

Cng thc ca chlorophyl b l (C55H70O6N4Mg), dip lc b ch khc dip lc a l nhm CH3 nhn pyron th hai c thay bng nhm CH=O. Chlorophyl khng tan trong nc, ch tan trong cc dung mi hu c. V vy khi mun tch chlorophyl ra khi l, bt buc phi dng mt dung mi hu c nh: ete, cn, benzen hay axeton, 1.6.2. Carotenoit Nhm carotenoit gm 2 nhm nh l Caroten v xanthophyl * Caroten - C40H56 l hirocacbon cha bo ho, khng tan trong nc m ch tan trong cc dung mi hu c. Caroten c mu vng da cam. Trong thc vt thng c 3 loi caroten: anpha, beta, gama caroten. Cng thc cu to ca alpha caroten(C40H56):

Cng thc cu to ca beta caroten(C40H56):

Cng thc cu to ca gama caroten(C40H56):

* Xanthophyl - C40H56On (n = 1- 6) l dn xut (dng oxi ho) ca caroten. Cc nguyn t oxi lin kt trong cc nhm: hidroxy, cacboxy, axetoxy, metoxy, epoxy,V oxi t 1 n 6 nn c nhiu loi xanthophyl v d: - Cripthoxanthin (C40H56O)

- Lutein (C40H56O2)

- Violaxanthin (C40H56O4)

- Neoxanthin (C40H56O4)

S phn cc ca dip lc a, dip lc b, caroten v xanthophyl

5 Mu sc v mc phn cc ca phn t cc cht tng dn theo th t t trn xung nh sau: Bng mu sc v th t phn cc ca cc loi dip lc, caroten v xanthophyl cht caroten pheophytin cht dip lc a cht dip lc b lutein violaxanthin neoxanthin mu sc vng mu xanh l cy liu mu xanh xanh mu vng xanh mu vng mu vng mu vng

1.6.3. Cc phng php sc k dng tch cc dip lc v carotenoit - Theo [15] c th tch cc cht mu thc vt trong l xanh bng sc k ct vi pha tnh l bt CaCO3 hoc bt ng, chit mu bng hn hp xng benzen (t l th tch 9:1), ra ct bng hn hp xng-benzen (t l th tch 10:1). Picmen s thnh 3 vng mu vng l carotenoit, mu xanh chlorophyl a v mu xanh vng l chlorophyl b. - Theo [16] dng sc k giy vi dung mi l ete du ho tch c: clorophin b, clorophin a, xanthophyl, caroten (theo th t t di ln). Trong thi gian 20-30 pht. - Theo [12] cho mu chit t l, hoa hoc qu cc thc vt bng n hexan chy HPLC vi h dung mi (gm axeton nitrin : metanol : clorofoc = 70 : 27 : 3) tch v xc nh c hm lng cc carotenoit: betacaroten, lutein, lycopen. - Theo [24] c th tch cc cht mu l xanh bng SKLM vi pha ng l hn hp 100 ml ete du ho, 11ml isopropanol v 5 git nc. - Theo [25] s dng SKLM silicagel vi pha ng l hn hp ca ete du ho, axeton, xyclohexan, etyl axetat v metanol tch c cc cht mu trong l cy rau bina (rau chn vt) trong 10 pht. - Theo [21] s dng SKLM silicagel vi pha ng l hn hp ca ete du ho v axeton t l 4:1 tch c cc cht mu trong l xanh t trn xung l Caroten (vng), Pheophytin (xanh -liu), dip lc a (mu xanh l cy), dip lc b (xanh-vng), Lutein (vng), violaxanthin (vng), neoxanthin (vng).

6 - Theo [26] s dng SKG vi pha ng l hn hp ca ete du ho v axeton t l 7:3 hoc 8:2 hoc 9:1 tch c cc cht mu trong l xanh. 1.7. Khi qut v ion Co2+, Cu2+, Fe3+, Ni2+ v mui ca chng [3, 7] 1.7.1. S lc v mui st(III) v ion Fe3+ [Fe(H2O)6]3+ mu tm nht. Khi kt tinh t dung dch, mui st(III) thng dng tinh th hirat v d FeCl3.6H2O mu nu vng, Mui st(III) thu phn mnh hn mui st(II) nn dung dch c mu vng nu v c phn ng axit mnh; tu theo nng , pH ca dung dch c th vo khong 2-3:
[FeOH(H2O)5]2+ + H3O+ [Fe(H2O)6]3+ + H2O
[Fe(OH)2(H2O)4]+ + H3O+ [FeOH(H2O)5]2+ + H2O Ch trong dung dch c phn ng axit mnh (pH < 1) s thu phn mi b y li. Ngc li khi thm kim hoc un nng dung dch, phn ng thu phn xy ra n cng to thnh kt ta (gel) hoc dung dch keo (sol) ca st(III) hiroxit bao gm nhng phc cht hiroxo nhiu nhn do hin tng ngng t to nn. Hay vit gn l: [Fe(H2O)6]3+ [(H2O)4Fe-(OH)2-Fe(H2O)4]4+ 4+ [(H2O)4Fe-O-Fe(H2O)4] V trn 700oC Fe2Cl6 b phn hu thnh monome FeCl3.

1.7.2. S lc v mui ng(II) v ion Cu2+ Trong nc khi c NH3 ion Cu2+ to phc cht vi NH3 bng cch thay th ln lt cc phn t H2O trong ion [Cu(H2O)6]2+ (mu xanh lam) bng cc phn t NH3 nhng vic thay th phn t NH3 th nm v th su l rt kh hn na hai phn t H2O cn li lin kt rt yu vi ion Cu2+ nn ion phc ca Cu2+ vi NH3 thng c biu din l [Cu(NH3)4]2+ (xanh chm). ihirat ng(II) clorua l nhng tinh th mu lc cng c kin trc lp phng lch nh ng(II) clorua khan nhng trong mi nguyn t ng c phi tr bi bn nguyn t Cl v hai phn t nc: Dung dch m c ca CuCl2.2H2O trong nc vn c mu lc nhng dung dch long c mu lam, mu c trng ca ion [Cu(H2O)6]2+. Khi un nng 150oC th CuCl2.2H2O mt nc thnh mui khan. ng(II) sunfat (CuSO4) l bt mu trng, ht mnh hi m ca khng kh to thnh hirat CuSO4.5H2O mu lam. Khi un nng, pentahirat mt dn nc v n 250oC bin thnh mui khan:
C C C CuSO4.3H2O 150 CuSO4.H2O 250 CuSO4 CuSO4.5H2O 100
o o o

7 ng(II) axetat l cht dng tinh th mu lc, d tan trong nc. N c cu to dng ime [Cu(CH3COO)2.H2O]2 trong nguyn t Cu trng thi lai ho d2sp3, nhng nhm CH3COO- l cu ni gia hai nguyn t Cu. 1.7.3. S lc v mui coban(II) v ion Co2+ CoCl2 mu xanh lam cn CoCl2.6H2O mu -hng. Khi tan trong nc ion Co2+ to ion bt din [Co(H2O)6]2+ c mu c trng l - hng, ion [Co(H2O)6]2+ tn ti trong mt s tinh th hirat nh CoCl2.6H2O mu hng, Co(NO3)2.6H2O mu - hng. Trong nc ion [Co(H2O)6]2+ thu phn mt phn lm cho dung dch c phn ng axit yu. CoCl2 mu xanh lam, nng chy 727oC v si 1049oC. Khi nhit phn tinh th hirat CoX2.6H2O cng nh mui hirat khc ca Co(II) xy ra hin tng mt nc dn km theo s i mu t - hng n xanh lam. V d:
C C C CoCl2.4H2O 58 CoCl2.H2O CoCl2.6H2O 49 CoCl2.2H2O 90 (-hng) (hng) (tm xanh) (xanh lam)
o

C 140 CoCl2
o

(xanh lam) Ion Co2+ to nn nhiu phc cht bt din vi s phi tr l 6 v d amoniacat coban(II) [Co(NH3)6]2+ c mu nu vng, [Co(H2O)6]2+ c mu c trng l - hng, Ion Co2+ cng to nn nhiu phc t din v d nh: [CoCl4]2-, [Co(OH)4]2-. Phc cht bt din ca Co(II) c mu -hng cn phc cht t din ca Co(II) c mu xanh lam. Trong dung dch nc, amoniacat coban(II) d dng tc dng vi oxi khng kh to thnh amoniacat coban(III): 4[Co(NH3)6]2+ + O2 + 2H2O 4[Co(NH3)6]3+ + 4OH1.7.4. S lc v mui Niken(II) v ion Ni2+ Trong nc ion Ni2+ hirat ha to ion bt din [Ni(H2O)6]2+ c mu lc v ion ny thy phn mt phn lm dung dch c phn ng axit yu. Trong tinh th hirat c trng hp khng c ion [Ni(H2O)6]2+ v d trong NiCl2.6H2O. NiCl2 mu vng. Ion Ni2+ to phc cht bt din v d [Ni(H2O)6]2+, [Ni(NH3)6]2+ u thun t. Mui Ni(II) khan kt hp vi kh NH3 to nn mui phc amoniacat cha ion bt din [Ni(NH3)6]2+ c mu tm vi Kb l 1,02.108 , [Ni(NH3)6]2+ c to nn c trong dung dch, s thay th nc trong [Ni(H2O)6]2+ bng NH3 lm mu bin i t lc sang tm.

8 1.7.5. Cc phng php sc k c dng tch ion Co2+, Cu2+, Fe3+, Ni2+ - Theo [15] c th dng ct anoinit tch hn hp 2 loi ion Fe3+-Zn2+, Cu2+Zn2+, Co2+-Zn2+ hoc Ni2+-Zn2+ ra khi nhau trong dung dch nc da vo kh nng to phc [ZnCl4]2- ca ion Zn2+ trong dung dch HCl 0,5 1,0M v b ct gi li. Ra ct bng dung dch HCl 1,0M cc ion Fe3+, Cu2+, Co2+ hoc Ni2+ s ra khi ct. - Theo [15] + SKLM kt ta trn lp silicagel cha 14% oxim tch v bn nh lng c Co2+,Cu2+, Fe3+, Ni2+. - Theo [26] SKG vi pha ng l hn hp HCl c, etanol v butanol trong khong 75 90 pht tch c cc ion Co2+, Fe3+, Cu2+, Hg2+, Ag+. - Theo [27] SKG vi pha ng l hn hp HCl c, etanol v butanol trong khong 75 pht tch c cc ion Co2+, Fe3+, Cu2+, Ag+. - Theo [28] SKG vi pha ng l hn hp 6ml HCl 8M v 19ml axeton tch c cc ion Co2+, Fe3+, Cu2+, Ni2+ ra khi dung dch mui nitrat trong nc - Theo [29] SKG vi pha ng l hn hp 10ml HCl 7,2M v 30ml butan-2-ol tch c cc ion Co2+, Fe3+, Cu2+, Ni2+ ra khi dung dch mui tan trong nc ca chng.

CHNG 2: THC NGHIM

2.1. Ch to bn mng t tinh bt sn dy Ly tinh bt sn dy, thch cao nung, keo dn dng nc v nc ct theo t l th tch tng ng 4 : 1 : 0,5 : 3,5 trn u trong cc thu tinh c va. Ly tha nha a va ln tm knh (khong 3,0 - 3,5 ml va cho 10 cm2 knh), dng tha gt v nh nhng nghing tm knh v cc pha cho va ph u ln tm knh ri ln gi phng cho kh t nhin nhit phng trong khong 10 gi. 2.2. Chit dch t l xanh Ly 10 gam l rau mung cn ti (khong 30 l) hoc l xanh khc ct nh cho vo ci s (b gn l), trn thm 2 gam bt CaCO3 trung ho dch axit ca t bo, c th cho mt t bt thu tinh cho d nghin. Nghin cc mu l n khi thnh mt th ng nht, cho 15 - 20 ml axeton 80% hoc cn etylic 90o vo ci s khuy u v 5 pht ri lc bng bng trn phu thu tinh, dung dch thu c trn vi 2,0 ml toluen ri chit bng phu chit ly phn trn (mu xanh m) c dch mu.

9 2.3. Tin hnh sc k ct S dng buret chun loi 25 ml lm ct sc k, pha tnh l silicagel kch thc ht 40 60 mesh, bt CaCO3, bt ng glucoz, tinh bt sn dy. Np silicagel vo buret t chiu cao ct khong 10 12 cm, bt ng glucoz 25 30 cm, cn bt canxi cacbonat np 15 20 cm l c. Dung mi s dng l cc h: ete du ha axeton; toluen axeton; toluen cn etylic tuyt i; axeton HCl c; NH4NO3 4M NH3 4M; CH3COOH 1,5M CH3COONH4 1,5M. Cho 3 - 5 git mu trc tip vo ct khng xo trn b mt lp silicagel (pha tnh) hoc mu dnh ln thnh thu tinh pha trn ca buret. Sau khi hon tt vic np mu ri th lt 1 ming bng hoc ph 0,3 cm ct sch bn trn mu khi np dung mi vo lp silicagel ( p) v mu khng b xo trn. tc chy ca dung mi khong 12 15 git/pht. 2.4. Tin hnh sc k lp mng (thin layer chromatography) Bnh khai trin l bnh thy tinh hnh tr cao 25 cm ng knh ming 10 cm, c np y kn. Bo ha hi dung mi trong bnh bng cch lt giy lc xung quanh thnh trong ca bnh, ri rt mt lng va dung mi vo bnh, lc ri giy lc thm u dung mi. Lng dung mi s dng sao cho sau khi thm u giy lc cn li mt lp dy khong 5 mm n 10 mm y bnh. y kn np bnh v yn 10 pht nhit phng. S dng bn mng TLC silicagel 60 F254 ca hng Merck c ct bng ko thnh bn hnh ch nht c kch thc 3,5 cm x 12 cm v bn t ch to t tinh bt sn dy kch thc 4 cm x 12 cm. S dng ng thu tinh mao qun hoc micropipet a mu ln bn mng. Th tch dung dch t 0,001ml n 0,005ml i vi trng hp a mu ln bn mng di dng im v t 0,l - 0,2ml khi a mu ln bn mng di dng vch. ng xut pht phi cch mp di ca bn mng 1,5cm - 2cm v cch b mt dung mi t 0,8 - 1 cm. Cc vt chm phi nh, c ng knh 2 6mm v cch nhau 15mm. Cc vt ba phi cch b bn ca bn mng t nht 1cm trnh hiu ng b. t bn mng gn nh thng ng vi bnh trin khai, cc vt chm phi trn b mt ca lp dung mi khai trin. y kn bnh v yn nhit khng i. Khi dung mi trin khai trn bn mng c mt on, ly bn mng ra khi bnh, nh du mc dung mi, lm bay hi dung mi cn ng li trn bn mng ri chp nh, o khong di chuyn ca dung mi v cc cht cn tch. Tnh h s Rf.

10 Vi tch cht mu thc vt trong l xanh lm vi cc h dung mi khc nhau, trong mi h dung mi kho st nhiu t l tm ra t l ti u. i vi tch cc ion kim loi cn kho st bng chm cc mu ring trc khi s dng mu hn hp. 2.5. Tin hnh sc k giy (paper chromatography) S dng giy sc k loi 3S v giy lc ng knh 12cm c ct thnh hnh ch nht kch thc 3,5 x 10cm. Cn dng kp nh gi mp trn ca giy sc k trnh b gp giy trong qu trnh chy sc k. Cc bc tin hnh c th tng t trin khai SKLM.

CHNG 3: KT QU V THO LUN 3.1. Sc k ct

3.1.1. Tch cht mu trong l xanh a) Pha tnh l silicagel.

dung mi ete du ho - axeton (9:1) thi gian15 pht

dung mi toluen axeton (9:1) thi gian18 pht

11 b) Pha tnh l bt canxi cacbonat.

dung mi ete du ho-axeton (9,5:0,5) thi gian 20 pht c) Pha tnh l glucoz.

dung mi toluen-axeton (9,5:0,5) thi gian 20 pht

dung mi: ete du ho - axeton (9,5:0,5), thi gian 20 pht.

12 3.1.2. Tch cc ion Fe , Cu , Co2+ a) Pha tnh l silicagel, pha ng l h dung mi: NH4NO3 4M NH3 4M (9:1), thi gian 15 pht, chiu di ct 15 cm.
3+ 2+

b) Pha tnh l silicagel, pha ng l h dung mi: CH3COONH4 1,5M - CH3COOH 1,5M (4:6), thi gian 15 - 20 pht, chiu di ct 15 cm.

13 3.1.3. Kt lun Vi sc k ct chng ti la chn c 7 th nghim n gin c th p dng vo dy trng trung hc ph thng gm: - 5 th nghim tch cht mu trong l xanh: - 2 th nghim tch hn hp cc ion Fe3+, Cu2+ v Co2+ trong dung dch nc dng mui nitrat hoc mui clorrua:

3.2. Sc k lp mng
3.2.1. Tch cht mu trong l xanh a) Bn mng silicagel ca hng Merck, h dung mi: ete du ho - axeton (5:5), thi gian 10 pht. Gi tr Rf ca cc cht mu trong l xanh, vi trng hp tch tt nht. V ete du ho : V axeton T.gian (pht) 5:5 10 Cc vt mu Vng Xanh ti Xanh vng Vng Vng Vng Rf 0,98 0,82 0,78 0,75 0,68 0,58

14 b) Bn mng t ch to t tinh bt sn dy, h dung mi ete du ho - axeton (8:2), thi gian 10 pht. Gi tr Rf ca cc cht mu trong l xanh, vi trng hp tch tt nht. V ete du ho : V axeton 8:2 T.gian (pht) 10 Cc vt mu Vng Xanh ti Xanh vng Vng Rf 0,90 0,51 0,41 0,30

3.2.2. Tch cc ion kim loi Fe3+, Cu2+, Co2+, Ni2+. a) Bn mng silicagel ca hng Merck, h dung mi: NH3 4M NH4NO3 4M (1:9), thi gian 10 pht. Gi tr Rf ca cc ion Fe3+, Cu2+, Co2+, Ni2+, vi trng hp tch tt nht. V NH3 : V NH4NO3 Rf 3+ 2+ Fe Cu Co2+ Ni2+ 1:9 0,0 0,26 0,12 0,42

15

b) Bn mng ch to t tinh bt sn dy, h dung mi: axeton HCl c (9:1), thi gian 10 13 pht. Gi tr Rf ca cc ion Fe3+, Cu2+, Co2+, vi trng hp tch tt nht. V axeton : V HCl c Rf 3+ Fe Cu2+ Co2+ 9:1 0,83 0,55 0,46

3.2.3. Kt lun Vi sc k lp mng chng ti la chn c 2 th nghim tch cht mu trong l xanh v 2 th nghim tch cc ion kim loi c th p dng vo dy trng THPT.

16

3.3. Sc k giy
3.3.1. Tch cht mu trong l xanh a) Giy sc k 3S, h dung mi ete du ho - axeton (9:1), thi gian 10 pht. Gi tr Rf ca cc cht mu trong l xanh, vi trng hp tch tt nht. V ete du ho : V axeton T.gian (pht) Cc vt mu Rf 9:1 10 Vng 0,86 Vng 0,64 Xanh 0,54 Xanh vng 0,45

b) Giy sc k l giy lc, h dung mi ete du ho - axeton (8:2), thi gian 3 10 pht. Gi tr Rf ca cc cht mu trong l, vi trng hp tch tt nht. V ete du ho : V axeton T.gian (pht) Cc vt mu Rf 8:2 10 Vng 0,95 Vng 0,76 Xanh ti 0,67 Xanh vng 0,54

17

thi gian 10 pht

thi gian 3 pht

c) Giy sc k 3S, dung mi toluen Gi tr Rf ca cc cht mu trong l xanh vi giy sc k 3S, dung mi toluen. toluen T.gian (pht) Cc vt mu Rf 10:0 8 Vng 0,97 Vng 0,92 Xanh ti 0,46 Xanh vng 0,35

18 d) Giy sc k l giy lc, dung mi toluen Gi tr Rf ca cc cht mu trong l xanh vi giy lc, dung mi toluen. V toluen :V cn etylic T.gian (pht) Cc vt mu Rf 10:0 8 Vng 0,98 Vng 0,93 Xanh ti 0,46 Xanh vng 0,36

3.3.2. Tch cc ion Fe3+, Cu2+ v Co2+ a) Giy sc k 3S, h dung mi: axeton - HCl c (9:1), thi gian 20 pht. Gi tr Rf ca cc ion Fe3+, Cu2+, Co2+, vi trng hp tch tt nht. V axeton : V HCl c Rf 3+ Fe Cu2+ Co2+ 9:1 0,92 0,72 0,66

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b) Giy sc k l giy lc, h dung mi: axeton - HCl c (9:1), thi gian 10 15 pht. V axeton : V HCl c Rf Fe3+ Cu2+ Co2+ 9:1 0,94 0,73 0,67

3.3.3. Kt lun Vi sc k giy chng ti la chn c 4 th nghim tch cht mu trong l xanh v 2 th nghim tch cc ion kim loi c th p dng vo dy trng THPT.

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KT LUN CHUNG
Qua qu trnh nghin cu chng ti la chn ra c 17 th nghim sc k gm sc k ct, sc k lp mng v sc k giy, c th tch cc cht mu trong l xanh hoc cc ion kim loi loi Fe3+, Cu2+, Co2+, Ni2+. Cc th nghim ny u d thc hin, thi gian ngn, khng cn s dng thuc th hin mu, ch s dng cc ha cht d tm kim hu ht t hoc khng c hi. Trong s 17 th nghim trn chng ti cng chn ra c 4 th nghim tt nht c th s dng dy trng THPT nc ta l: + Tch cht mu trong l xanh bng sc k ct, vi pha tnh l glucoz, pha ng l h dung mi: ete du ho-axeton (9,5:0,5). + Tch hn hp cc ion Fe3+-Cu2+-Co2+ bng sc k ct, vi pha tnh l silicagel, pha ng l h dung mi: NH4NO3 4M - NH3 4M (9:1). + Tch hn hp cc ion Fe3+-Cu2+-Co2+-Ni2+ bng sc k lp mng, vi bn mng silicagel ca hng Merck, h dung mi: NH4NO3 4M - NH3 4M (9:1). + Tch cht mu trong l xanh bng sc k giy, vi giy sc k l giy lc, h dung mi: ete du ho - axeton (8:2). Chng ti cng ci tin thay th bn mng silicagel trong sc k lp mng bng bn mng t ch to t tinh bt sn dy, thay th silicagel nhi ct trong sc k ct bng glucoz hoc bt canxi cacbonat, thay th giy sc k trong sc k giy bng giy lc. Cc s ci tin c u im l thay th cc ha cht, thit b t tin, bng nhng ha cht, thit b r tin, sn c Vit Nam hon ton khng c hi, m vn m bo hiu qu tch sc k v chuyn ti c cho hc sinh nhng kin thc c bn nht v bn cht, nguyn l v ng dng ca sc k. References : I. Ting vit 1. Nguyn B Hoi Anh (2003), i cng v sc k lng, NXB i hc quc gia Thnh ph H Ch Minh. 2. Nguyn B Hoi Anh (2003), cc qu trnh tch trong sc k lng, NXB i hc quc gia Thnh ph H Ch Minh.. 3. Nguyn Tinh Dung (2003), Ho Hc phn tch, phn III: cc phng php phn tch ho hc, NXBGD, H Ni. 4. L vn ng (2005), chuyn mt s hp cht thin nhin, NXB i hc quc gia Thnh ph H Ch Minh. 5. Trn ng K, Nguyn Nh Khanh (1995), Sinh l thc vt, NXB Gio dc.

21 6. Nguyn Thanh Khuyn (2000), Cc phng php sc k, Trung tm sc k thnh ph H Ch Minh. 7. Hong Nhm (2004), Ho hc v c tp ba, NXB Gio dc. 8. Nguyn Th Thu Nga (2005), gio trnh thc hnh ho hc phn tch, NXBGD, H Ni. 9. V Thanh Tm, Hong Minh Tn, V vn V (1993), Sinh l hc thc vt, NXB Gio dc. 10. Nguyn Vn Ri (2009), Cc phng php tch, khoa Ho, Trng HKHTN HQG H Ni. 11. Nguyn Vn Ri (2006), hng dn thc hnh b mn ho phn tch, khoa ho trng HKHTN HQG H Ni. 12. Tp ch Khoa hc HQGHN, Khoa hc T nhin v Cng ngh 23 (2007) 130-134 13. Phm Hng Vit (2001), sc k kh c s l thuyt v kh nng ng dng, NXB HQG H Ni. 14. Phm Hng Vit (2003), C s l thuyt ca phng php sc k, NXB Khoa hc K thut H Ni. 15. o Hu Vinh (ch bin), Nguyn Xun Dng, Trn Th M Linh, Phm Hng Vit (1985), Cc phng php sc k , NXB khoa hc v k thut H Ni. 16. Nguyn Duy Minh, Nguyn Nh Khanh (1982), Thc hnh sinh l thc vt, NXB Gio dc.

II. Ting Anh 17. Bowen, W. R. and Baxter, W. D (1980), Experimental Cell Biology, An Integrated Laboratory, Macmillan Publishing Co, Inc, New York. 18. D. Kealey, P. J. Haines (2002), Analytical Chemistry, printed in the united States of America. 19. Daniel C. Harris (2007), Quantitative Chemical Analysis, printed in the united States of America. 20. I.M. Hais, K. Macek (1963), Paper chromatography. Czechoslovak Academy of Sciences. Prague. 21. Verlag chemie Academic pess (1966), N.Y. Thin Layer Chromatography. 22. E. Hoftman (1967), Chromatography, Reynold. N.Y. 1967. 23. Jeff Altig (2009), Paper Chromatography of a Metal Cation Mixture, CHEM 121L ,volume 50, issue 5, pp. 134 139.

22 24. Peter Keusch (2003), Separation of Plant Pigments by Thin Layer Chromatography (TLC), Organic Chemistry Demonstration Experiments on VideoChemistry Visualized, University of Regensburg, vol. 40, issue 1, p. 36 40. 25. Anwar, M. H (1963), Separation of plant pigments by thin layer chromatography, Journal of Chemical Education, vol. 40, issue 1, p. 29. 26. Rollins, Charles (1963), Thin layer chromatographic separation of leaf pigments: A rapid demonstration Journal of Chemical Education, vol. 40, issue 1, p. 32 27. A. S. Ritchie (1961), A paper chromatographic scheme for the identification of metallic ionsJ. Chem. Educ, 38 (8), p 400. 28. S. Lincoln, R. A. Pohl and D. T. Haworth (1970), A thin-layer chromatography experiment for general chemistry, J. Chem. Educ, 47 (5), p 401. 29. David J. Rakestraw , Rebecca J. Whelan , Theresa E. Hannon and Richard N. Zare (2004), Application of Ion Chromatography to the Investigation of Real-World Samples, J. Chem. Educ, 81 (9), p 1299

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