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2. M u 3. CC THNH PHN CA THIT B SC K KH 4. Qu trnh bt u khi mt lng nh mu c a vo bung tim dng kh hay lng Bng tin c nhim v ha hi mu v trn n vi dng kh u ct. Ct thng c cu to l ng trn di rng gia (rt hp) chiu di ct t 1 ti 100m, ty thuc loi ct v lng pha tnh. Mt ct c th dng vi ngn ln tim v t trong l iu chnh nhit . cui ct dng kh mang i qua mt b phn l detector trc khi ra ngoi CC THNH PHN CA THIT B SC K KH 5. CC THNH PHN CA THIT B SC K KH 6. KH MANG V YU CU CA DNG KH MANG Yu cu ca kh mang Tr Ph hp vi detector tinh kit cao D s dng R Khng c nguy c pht chy Cho hiu qu ct l tt nht. 7. Cc loi kh mang Hydrogen Kh nng dn nhit tt nht Nhc im: N phn ng vi cc hp cht khng no v d bt la Helium Kh nng dn nhit tt Gi thnh t Nitrogen nhy gim Gi thnh r KH MANG V YU CU CA DNG KH MANG 8. KH MANG V YU CU CA DNG KH MANG 9. KH MANG V YU CU CA DNG KH MANG Dng kh mang phi bo m l duy tr tc ti u trong sut qu trnh 10. TIM MU V BUNG TIM Phng php tim mu ph bin nht l s dng microsyringer Lng mu tim nh c th ti 0,5l Qu trnh xuyn qua vch ngn cao su a mu vo phn ha hi u ct 11. TIM MU V BUNG TIM 12. c c ti lp tt trong nhng ln tim ngi ta s dng k thut tim Autosamplers. Nhng Syringer t ng trong qu trnh ht, tim mu v ra TIM MU V BUNG TIM 13. Bung tim: c thit k da trn k thut tim mu: Tim ha hi trc tip Tim trn ct mao qun Tin trn ct lnh TIM MU V BUNG TIM 14. Bung ha hi trc tip K thut thut ny p dng cho ct nhi hay ct megabore. Tc dng t khong 10ml/pht. Bung tin l ng kim loi chn bn trong ng thy tinh. ng kim loi c gia nhit n nhit si ca cc cu t cn tch. Phn u ca bung tim l vch bng cao su. Phn cui ni vi ct TIM MU V BUNG TIM 15. TIM MU V BUNG TIM Bung tim split/ splitless 16. Bung tim split Ct capillary c th thc hin qu trnh phn tch trn mt th tch rt nh mu v d 0,1l Nhng bung tim c dng cho mc ch ny c th tin hnh theo hai kiu chi dong v khng chia dng (split and splitless) Mu tim sau khi ha hi c trng vi dng kh mang t l dng khong 50-100ml/pht. Ton bt kh chi lm 2 phn theo t l khong 1:20 hay 1:500. Trong ch c phn nh i vo ct. TIM MU V BUNG TIM 17. Bung tim splitless Thch hp cho phn tch lng vt nhng cu t c nng nh hn 0.01% mu v KT tim ny c khong 80 % mu c gii thiu vo ct. H thng tim mu tng t nh trng hp tim mu chia dng. Mt th tch ln (khong 2 l) ca dung dch c pha long trong dung mi c nhit si thp c tim chm (khong 2s) vo trong ng thy tinh ca bung tim mu. TIM MU V BUNG TIM 18. Tim trn ct lnh K thut ny khng ha hi trong . Mu c chuyn trc tip ln ct capillary. Mt microsyringer c mi kim ng knh khong 0,15mm, c th a mu ln ct. K thut ny ph hp vi nhng hp cht khng bn nhit, cng nh nhng cht c im si cao Nhit c tng t t to iu kin cc hp cht ln lt i qua ct. TIM MU V BUNG TIM 19. Bung tim ha hi theo lp trnh nhit Bung tim c cu trc nh bung tim split v splitless, nh y nhit c tng theo mt lp trnh t 20 n 3000C trong vi chc giy. C ba k thut tim trn bung ny TIM MU V BUNG TIM 20. Tim lnh chia dng (Split cold injection) Mu c np vo bung tim. Sau tin trnh gia nhit cho bung ha hi xy ra theo chng trnh c ci t. Dung mi v cc cht c im si thp i vo ct trc sau l cht c im si cao hn Van chia dng m sut qu trnh TIM MU V BUNG TIM 21. Tim lnh khng chia dng( splitless cold injection) K thut ng dng cho xc nh hm lng vt Trong tin trnh tim lnh chia dng van chia dng ng li trong sut qu trnh ha hi Tim vi loi b dung mi Sau khi np mu th van 2 m ra loi b dung mi. Sau tin trnh gia nhit bt u cc cht c nhit thp vo trc ri mi n nhng cht c nit si cao. Vi k thut ny mu tim c th t t 50 m 500l TIM MU V BUNG TIM 22. B PHN IU CHNH NHIT B phn iu nhit nhit l l gia nhit c th tch tng ng khong 2-3 ct sc k. L c th gia nhit rt nhanh khong 1000C/pht Mc iu nhit chnh xc ti 0.10C L c ci t thng vi bnh cha kh CO2 ,N2 nn c th thc hin nhit thp 23. Phn loi ct Ct nhi (packed column): ID: 2 - 4 mm, L: 2 - 3 m - Pha tnh - Cht hp ph c nhi vo ct - Phn tch kh (gas analysis - Np mu n gin - chnh xc cao- Ct mao qun (open-tubular or capillary column): - ID: 0,25 - 0,5 mm, L: 25 - 50 m - Np mu kh khn - Rt d b tr trong l - Pha tnh c ph vo mt trong ca ct (0,2 - 1m) - CT SC K KH 24. Ct sc k (Column) wall-coated open-tubular (WCOT) column CT SC K KH 25. Cu to ca ct nhi V ct: thp khng g hoc thy tinh Pyrex Cht hp ph (Adsorbents): hai loi cht c nhi vo ct : + Cht hp ph. + Cht mang (support) c ph pha tnh - Cc cht hp ph thng s dng: + Alumina (Al2O3): Hot ha 200 C - 1h: tch kh v cc hyrocacbon n C5, kch thc ht: 100/120 mesh, kch thc l xp:1 - 100 . + Silica (SiO2): tch cc kh c M nh v cc Hydrrocacbon nh B mt ring 750 m2/g, kch thc l xp trung bnh: 22 B mt ring 100m2/g kch thc l xp trung bnh: 300 . CT SC K KH -. 26. Cu to ca ct nhi Cc cht hp ph thng s dng: Zeolith: Tch cc kh c M nh bng phng php ry phn t (molecular sieves) -Cc zeolith k hiu: 5A v 13X: thng c s dng tch H2, O2, N2, CH4, CO, Ar, Ne Cacbon: - Cacbon hot tnh: b mt ring 1000 m2.g-1 - Graphit: b mt ring 5 - 100 m2.g-1 Cc hp cht cao phn t: - Co-polymer ca polystyrene v divinylbenzene - L xp: macropore v micropore - B mt ring ln v xp cao . CT SC K KH 27. Cu to ca ct nhi Cc cht mang s dng cho GLC: - Celite (mt dng c bit ca khong diatomic), Celite nung, Celite nung hot ha bi Ag hoc Au, cc ht vi cu thy tinh, polymer, teflon Bin tnh Celite: Nung 900 C vi Na2CO3 v tr nung: silica cristobalite, cc vt kim loi tc dng vi Silica gy mu (hng) cho vt liu. Chromosorb P, Chromosorb W, Chromosorb G v Chromosorb S Vi cu Polystyren CT SC K KH 28. Chuyn cht hp ph ln cht mang: S dung cc nhm Silanol ( Si-OH) Hexamethyldisilazane + Si-OH gc trimethylsilyl Phng php tm (slurry method of coating) CT SC K KH 29. Cu to ca ct mao qun (capillary or open-tubular column) CT SC K KH 30. Bin tnh b mt fused silica phn cc (polar) ca cc gc Silanol trn b mt - Khng phn cc: Hydrocacbon( dialkyl siloxan) - Phn cc yu: - CN, - CO, OH - Phn cc mnh: polyeste CT SC K KH 31. B. Sc k kh (Gas-Liquid Chromatography) So snh ct nhi v ct mao qun 32. PHN LOI CT C 3 loi ct: s khc nhau ca ba ct ny chnh l hiu qu tch ca chng Ct nhi ( parker column) Ct mao qun( capillary column) Ct Wide bore 33. Ct nhi (packed column) Ct ny hin nay t c s dng Ct c ng knh trong t 3.18 n 6.35 mm v di t 1- 3m Ct c lm bng thp hay thy tinh. Mt trong c x l khng tng tc vi cu t mu. Ct ny c th chu c t l dng kh t 10 40 ml/pht Cc ht cht mang hnh cu tr v mt ha hc c nhi vo ct. Pha tnh c tm ln b mt cht mang hay lin kt vi b mt cht mang (khong 30% din tch). CT 34. Cc cht mang xp c tnh b mt c bit c th t 8m2/g. Nhng ht cht mang c ng knh khong 0,2mm v c lm t diatomit hay tinh th silicat. Nhng cht mang ny sau khi tinh ch c t tn trn th trng l chromosorb .Mt cht mang khc c tng hp t nhng ht rt nh SiO2 c tn l Spherosil . C hai cht mang ny u c hot tnh ha hc ging silica gel v cng c cha nhm silanol CT 35. Ct nhi c hiu qu tch thp, nhng vn c dng thng xuyn cho nhng mu c thnh phn n gin, do chng d sn xut v khng chn la pha tnh ln. Ct nhi khng th phn tch hm lng vt. CT 36. CT Ct mao qun (capillary) 37. Ct mao qun thng c lm t nhng tinh th silicat c tinh khit cao. ng knh bn trong ct t 0,1 n 0,35mm v di t 15 ti 100m Lp phim mng ca pha tnh c chiu dy khong 0,05 ti 5 m . Sau khi x l b mt trong ca ct th pha tnh c phun ln hay c hnh thnh bng qu trnh trng hp bn trong ct. CT 38. Nhng ct ny do lm t nha nn c th qun v cun trn xung quanh mt vng trn c dnh bi khung kim loi B mt bn trong ca ct thng c x l c th to lin kt cho pha tnh.Qu trnh ny c th tin hnh bngdung dch HCl 3500 C, hoc ph mt lp mng oxyt nhm hoc silica gel ty thuc vo mc ch s dng lin kt vi pha tnh Nhng lin kt cng ha tr Si-O-Si-C cho php cc hp cht ha hc gi trn bn mt silica Ct thng c hot ha bng nhng dung mi ph hp m bo cht dng CT 39. Ct 530 m Bn cht ging ct capillary nhng ng knh trong l 530m v chiu di ct t 5 n 50m 40. C IM Loi ct ny c lm t nhng ng silica c ng knh trong l 530 m. Ct c quy c gi l Megabore , Macrobore hay Ultra.T l dng pha ng s dng cho nhng loi ct ny c th n 15ml/pht, thp hn so vi ct nhi Tnh phn gii ca nhng ct ny thp hn so vi ct capillary. u im ca ct 530 so vi ct nhi l khng c hin tng chy mu ct (pha tnh mt dn theo thi gian) 41. PHA TNH RN Cc polyme xp l pha tnh rn dng cho ct nhi ph bin nht c chn trong phn tch cc cht kh, cc cht hu c t carbon, cc acid, amin. Polyme xp thng dng nh : Chromosorb (101 - 108) Porapak (N, P, Q, R, S, T)... c cu trc l cc polyme ca divinylbenzen, styren, dimetylacrylat... Molecular sieve: l silicate nhm v mui kim loi kim, c kch thc rt nh. Hai loi thng dng cho sc k kh c kch thc l 5A v 13A 42. PHA TNH LNG Cc hydrocarbon: Cc ether, ester: Cc mui hu c dng lng Cc poly(siloxane) 43. Cc hydrocarbon: Octadecane ( C18H38) Hexadecane (C16H34) Squalane (C30H62) Apolane-87 (C87H176) 44. KHUNG SILOXAN 45. Ct capillary L loi ct ng m, c lm t nhng tinh th silicat tinh kit nht, thu t qu trnh nung SiCl4 trong oxy 46. PHA TNH 47. NGUYN L HOT NG CA CC DETECTOR TRONG SC K KH
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