Dai Cuong Ve GC - Diendandaihoc.vn

AI CNG VE
SAC KY KH
TS. NGUYEN BA HOAI ANH
SAC KY KH
(GAS CHROMATOGRAPHY)
) LA PHNG PHAP TACH
) DA TREN 2 QUA TRNH
* HAP PHU
* GIAI HAP PHU
) XAY RA LIEN TUC GIA 2 PHA:
* PHA TNH : THNG LA RAN HOAC LONG
* PHA ONG : LA KH
) NH TNH : DA VAO THI
GIAN LU
) NH LNG : DA VAO
CHIEU CAO HOAC DIEN TCH
PEAK
KHI NOI VI CAC AU DO (DETECTOR)
PHNG PHAP CHO PHEP
Start
tM
tR1
tR2 tR3 tR4
INJECTOR
DETECTOR
CHROMATOGRAPHY
M
O
B
I
L
E
P
H
A
S
E
S
T
A
T
I
O
N
A
R
Y

P
H
A
S
E
S O KHOI CUA MOT MAY SAC KY KH
S O MOT HE SAC KY VI AU DO FID
Bo Loc/ Bay hydrocacbon
A
i
r
H
y
d
r
o
g
e
n
G
a
s

C
a
r
r
i
e
r

Column
He thong lay va
x ly so lieu
Syringe/Sampler
Injector
FID
ong ho ieu ap
H
RESET
Lo cot
S O KHOI CUA MOT MAY SAC KY KH (tt)
CAC BO PHAN C BAN BAO GOM :
3 NGUON CUNG CAP KH MANG : THNG LA BNH KH HOAC
MAY SINH KH (1)
3 HE THONG IEU KHIEN AP SUAT HOAC TOC O DONG KH
MANG (2+3): IEU KHIEN C HOAC IEN T
3 BUONG BM MAU (4): CO NHIEU LOAI KHAC NHAU VI MUC
CH PHAN TCH KHAC NHAU : PACKED, WBI, SPL/SPLESS/OCI-
PTV, GAS INJECTOR SYSTEM
S O KHOI CUA MOT MAY SAC KY KH (tt)
3 LO COT (COLUMN OVEN) (5): DUNG E IEU KHIEN NHIET O
COT TACH
3 COT TACH (6): LA NI XAY RA CAC QUA TRNH TACH CHAT.
CAC LOAI COT GOM COT NHOI, COT MAO QUAN
3 AU DO (DETECTOR) (7): CO NHIEU LOAI KHAC NHAU TUY THEO
MUC CH PHAN TCH. DUNG E PHAT HIEN CHAT VA NH
LNG : FID, ECD, NPD, TCD, MS
3 HE THONG GHI NHAN VA X LY TN HIEU : DUNG E THU THAP
VA TNH TOAN CAC KET QUA.
Start
tM
tR1
tR2 tR3 tR4
Injector
Detector
Column
Carrier gas
OVEN
COLUMN
AIR
H2
N2(He)
INJECTOR DETECTOR
COMPUTER
PRINTER
AUTOSAMPLER
SPLIT
SEPTUM PURGE
MAKE UP
LOC AM moisture filter
LOC HYDROCARBON hydrocarbon filter
LOC OXYGEN oxygen filter
MAY SAC KY VI BO TIEM MAU T ONG
BO TIEM MAU T ONG
MAY SAC KY NHN T PHA TRC
COT NHOI LAM
BANG THUY TINH
COT MAO QUAN
LO COT
CONG TIEM MAU CHO COT NHOI VA MAO QUAN
INJECTOR CHO COT NHOI
Split/Splitless INJECTOR CHO
COT MAO QUAN
AU DO (DETECTOR)
DETECTOR FID
DETECTOR TCD
AU DO (DETECTOR)
DETECTOR FPD
AU DO (DETECTOR)
DETECTOR ECD
AU DO (DETECTOR)
DETECTOR FTD CHO
COT CAPILLARY
DETECTOR FTD CHO
COT NHOI
MAY GC VI AU DO MS VA HE THONG TIEM MAU T
ONG (BAO GOM CA HEAD SPACE)
HE THONG TIEM MAU T
ONG VI HEAD SPACE
DETECTOR MS
CAC PHNG TRNH VA AI LNG C BAN
TRONG SAC KY KH
THI GIAN LU :
Start
t
M
t
R
TRONG SAC KY KH (TT)
B THI GIAN LU
) THI GIAN LU (GI) TUYET OI t
R
: THI GIAN TNH T LUC BM MAU
EN KHI CHAT I RA NGOAI (XUAT HIEN NH PEAK CUA CHAT).
THNG C DUNG TRONG NH DANH.
) THI GIAN CHET t
M
: THI GIAN MOT CHAT HOAN TOAN KHONG TNG
TAC VI COT TACH (KHONG B LU GI) I QUA COT (CAC CHAT NH
METHAN, ARGON THNG C S DUNG TUY AU DO). CON GOI LA
THI GIAN CHAT C LU GI TRONG PHA ONG .
) THI GIAN LU THC t
R
: THI GIAN CHAT B LU GI TRONG PHA TNH.
C TNH THEO CONG THC:
t
R
= t
R
t
M
start
tM
tR1 tR2
B HE SO PHAN BO: KY HIEU Kd
) LA AI LNG AI DIEN CHO CAN BANG ONG CUA CHAT
TRONG HAI PHA : PHA TNH VA PHA ONG
) C TNH THEO CONG THC:
Kd = Ci,s/Ci,m
TRONG O : Ci,s : NONG O CHAT i TRONG PHA TNH
Ci,m: NONG O CHAT i TRONG PHA ONG
) HE SO Kd CANG LN CHAT CANG B GI LAI LAU TRONG COT
B T SO PHAN BO k
3 ANH GIA KHA NANG LU GI CUA PHA TNH OI VI CHAT PHAN
TCH. CAU T KHONG B LU GI CO k = 0
3 C TNH THEO CONG THC:
k = n
i,s
/n
i,m
= t
R
/t
M
n
i,s
: so mol chat i trong pha tnh; n
i,m
: so mol chat i trong pha ong
3 HE SO PHAN BO VA T SO PHAN BO LIEN HE QUA BIEU THC
Kd = .k
3 GOI LA TY LE PHA. = Vm/Vs
Vm : the tch cot b chiem bi pha kh; Vs: the tch cot b chiem bi pha tnh
Vi cot nhoi trong khoang 10 50, vi cot mao quan trong khoang 100 - 500
B SO A LY THUYET n
) C TNH BANG CONG THC
n = 16(t
R
/w
b
)
2
= 5.545(t
R
/w
h
)
2
Trong o : t
R
la thi gian lu tuyet oi con w
b
va w
h
la o rong peak o tai
chan ng nen va tai na chieu cao peak.
) SO A LY THUYET HIEU DUNG N C TNH TNG T
N = 16(t
R
/w
b
)
2
= 5.545(t
R
/w
h
)
2
W
b
W
h
W
h
=W
0.5
= 2.354 V
Wb = 4 V
B HIEU QUA TACH :
) C BIEU DIEN THEO SO A LY THUYET/1MET CHIEU DAI
COT (n/L HOAC N/L)
) HOAC C BIEU DIEN QUA CHIEU CAO A LY THUYET h
h = L/n
) HOAC CHIEU CAO A LY THUYET HIEU DUNG H (HETP)
H = L/N
) N V CUA h VA H LA milimet
B CHIEU CAO A LY THUYET CO THE XAC NH THEO PHNG
TRNH VAN-DEEMTER
h = A + (B/u) + Cu
Vi u la toc o thang cua kh mang (cm/s)
A la he so khuech tan xoay dien ta cac ng i cua kh mang do
khuech tan xoay trong cot gay ra
B la he so khuech tan doc theo chieu dai cot
C la he so tr khang chuyen khoi
B TOC O THANG u (linear velocity) THNG C CHON SAO CHO THU
C H NHO NHAT (SO A LY THUYET LN NHAT)
B GIA TR TOI U CUA u TUY THUOC VAO LOAI KH MANG
Carrier gas linear velocity
B O CHON LOC D : GIA 2 CHAT i VA j C TNH BANG
D = t
Ri
/t
Rj
Vi t
Ri
> t
Rj
hay D > 1.
) NEU D CANG LN HN 1 TH HAI CHAT CANG DE TACH RA KHOI
NHAU.
B O PHAN GIAI R : LA AI LNG CHO PHEP ANH GIA HAI CHAT
CO THE TACH RA KHOI NHAU KHONG.
R = 2(t
Ri
t
Rj
)/(w
bi
+ w
bj
)
) GIA TR R LIEN QUA EN KHA NANG TACH C MO TA
TRONG BANG DI
KHA NANG TACH THEO R
R KHA NANG TACH GHI CHU
t0.5 BAT AU NHAN RA PEAK
TH 2
< 1 < 94% KEM, KHONG TACH C
t1 - 1.5 94% - 100% THNG CHAP NHAN LA
TACH C
t1.5 100% TACH HOAN TOAN
MOT SO DANG PEAK TRONG SAC KY KH
B DANG OI XNG (SYMETRICAL ) :
) AY LA DANG LY TNG, PEAK OI XNG THEO HAM PHAN BO
GAUS. THNG THU C KHI QUA TRNH PHAN BO CHAT GIA
HAI PHA ONG VA TNH XAY RA NHANH, T HOAC KHONG PHU
THUOC VAO NHIET O.
) NEU LNG MAU TIEM VAO KHONG VT QUA DUNG LNG
CHO PHEP CUA COT TH THI GIAN LU KHONG PHU THUOC
VAO LNG MAU TIEM VAO
) O OI XNG THNG C BIEU DIEN QUA HE SO OI XNG
ASYMMETRY FACTOR (5%, 10%...)
B DANG KHONG OI XNG : GOM HAI DANG
) TAILING (KEO UOI)
) LEADING (HAY FRONTING NGC LAI VI TAILING)
) HIEN TNG NAY XAY RA KHI :
NONG O CHAT PHAN TCH QUA LN (THNG XAY RA
TAILING)
CO S HAP PHU CHAT PHAN TCH QUA MANH CHAT PHAN TCH
TREN PHA TNH (CA HAI DANG)
THI GIA LU SE THAY OI TUY LNG MAU BM
CAC LOAI COT DUNG TRONG SAC KY KH
B PHNG PHAP SAC KY KH S DUNG HAI LOAI COT :
) COT NHOI
) COT MAO QUAN
) TUY THEO LOAI MAU, O PHC TAP CUA MAU, LOAI MAY SAC
KY MA CHON COT NHOI HAY COT MAO QUAN
) INJECTOR (VAN TIEM MAU), DETECTOR (AU DO) CHO COT MAO
QUAN VA COT NHOI CO CAU TAO KHONG HOAN TOAN GIONG
NHAU.
CAC LOAI COT DUNG TRONG SAC KY KH (TT)
B COT NHOI :
) THNG C DUNG VI CAC MAY SAC KY THE HE CU HOAC
CAC MAY DANH CHO MUC CH AC BIET.
) THNG LAM BANG THEP KHONG G, THUY TINH
) CHIEU DAI KHOANG T 1 3 M
) NG KNH COT KHOANG 1/8 1/4 INCH
) THNG C NHOI BI CAC HAT CO NG KNH 100 120
mesh (150 125um)
B COT NHOI :
) HIEU QUA THAP DO SO A LY THUYET THNG NHO HN 8000.
) NEU COT QUA DAI SE GAY AP SUAT AU COT QUA LN, V VAY
COT KHONG THE DAI QUA, DAN EN SO A LY THUYET THAP
) HIEN NAY CO MOT SO LOAI COT NHOI MI CO NG KNH
NHO (NHO HN 1mm) CHO PHEP NANG CHIEU DAI COT LEN VAI
CHUC MET. THNG DUNG CHO MOT SO NG DUNG AC BIET
MA COT MAO QUAN KHONG AP NG C.
B COT NHOI :
) CO HE SO LU GI CAO GIUP PEAK OI XNG NGAY CA
NONG O LN VA SO A LY THUYET HIEU DUNG CAO.
) NG KNH COT LN NEN T CHUANH HNG CUA TAP
CHAT.
) MAU KHONG OI HOI PHAI TINH CHE KY .
) MAU THNG BM VI THE TCH LN NEN SAI SO GIA CAC
LAN BM NHO (TRNG HP BM MAU BANG TAY)
B COT NHOI :
) CAC COT NHOI CO NG KNH NHO (<1mm) C DUNG
TRONG :
+ CAC PHEP PHAN TCH CAN O PHAN GIAI CAO
+ HOAC C CHE HAP PHU AC BIET
+ HOAC DUNG PHAN TCH VI NHIET O RAT CAO
+ HOAC TOC O TANG GIAM NHIET O RAT NHANH
CAU TAO CUA MOT SO LOAI COT SAC KY
B COT MAO QUAN :
) THNG C LAM BANG VAT LIEU FUSED SILICA CO TNH
BEN VA MAT VAT LY RAT CAO VA TR VE MAT HOA HOC.
) CO CHIEU DAI THONG THNG T 10 30 M. TRONG NHNG
TRNG HP CAN TANG HIEU QUA TACH NGI TA CO THE
CHE TAO CAC COT CO CHIEU DAI 100 150 M.
) NG KNH COT THNG TRONG KHOANG 0.53mm 0.1mm
) COT MAO QUAN C CHIA LAM HAI LOAI CHNH LA :
- WCOT (WALL COATED OPEN TUBULAR)
- PLOT (POROUS LAYER OPEN TUBULAR)
B COT PLOT :
) TAI THANH ONG MAO QUAN FUSED SILICA C PHU MOT
LP HAT XOP, ONG THI LA PHA TNH.
) BE DAY LP XOP VA PHA TNH TRONG KHOANG 5 50 m
) AY LA LOAI COT TRUNG GIAN GIA COT MAO QUAN VA COT
NHOI
) THNG C DUNG THAY THE COT NHOI DO PHA TNH
GIONG HET COT NHOI.
B COT WCOT :
) TAI THANH ONG MAO QUAN FUSED SILICA C PHU TRC
TIEP MOT LP PHA TNH.
) LP PHA TNH THNG DANG SET GAN NH AC NEN AY
CHNH LA DANG SAC KY LONG KH.
) NEU LP PHA TNH KHONG GAN TRC TIEP LEN THANH COT
MA QUA MOT LP TRUNG GIAN TH GOI LA COT SCOT
(SUPPORT COATED OPEN TUBULAR)
) BE DAY CUA LP PHA TNH NAY QUYET NH HE SO LU GI
VA DUNG LNG MAU CUA COT.
B COT WCOT (TT) :
) THNG CHIA LAM 3 LOAI :
9 COT ONG HEP (narrow bore) : CO NG KNH TRONG T
0.05 0.1 mm. THNG DUNG TRONG FAST GC.
9 COT THONG THNG (conventional) : CO NG KNH TRONG
T 0.18 0.32 mm. THNG C S DUNG TRONG CAC PHEP
PHAN TCH THONG THNG HIEN NAY.
9 COT ONG RONG (mega bore hoac wide bore) : THNG C
DUNG VI CAC MAY GC ANG S DUNG COT NHOI, DO
LNG MAU VA TOC O DONG KH MANG KHA LN
PHA TNH DUNG CHO COT SAC KY
B YEU CAU CHUNG CHO PHA TNH :
) T BAY HI
) BEN NHIET
) TR VE MAT HOA HOC
) THNG PHA TNH C CHON TRONG PHAN TCH DA TREN
O PHAN CC
) PHA TNH CUA COT VA CAC CHAT PHAN TCH CAN CO O
PHAN CC TNG T TH MI TACH TOT (CAC CHAT GIONG
NHAU HOA TAN TOT VAO NHAU)
PHA TNH DUNG CHO COT SAC KY(TT)
B PHA TNH RAN CHO COT NHOI :
) CAC PHA TNH RAN CO U IEM HN PHA TNH LONG NH :
9 CHAT HAP PHU RAN BEN VA ON NH TRONG MOT KHOANG
NHIET O LN
9 HIEN TNG CHAY MAU COT (BLEEDING) HAU NH KHONG
XAY RA (AC BIET VI CAC CHAT HAP PHU VO C VA RAY
PHAN T MOLECULAR SIEVE)
9 DUNG TACH RAT TOT CAC HYDROCACBON NHE, KH HIEM, KH
TR, CAC ALCOL
9 MOT SO PHA TNH THNG DUNG LA DIATOMIC, MOLECULAR
SIEVE, PRORAPAK, CHROMOSORB, TENAX
PHA TNH DUNG CHO COT SAC KY (TT)
B PHA TNH RAN CHO COT PLOT:
) CAC PHA TNH VE CAN BAN GIONG NH TRONG COT NHOI
) TUY NHIEN KCH THC HAT NHO HN (THNG 1m HOAC
NHO HN) VA CO O ONG NHAT CAO HN E DE PHU LEN
BE MAT COT MAO QUAN FUSED SILLICA
) CO DIEN TCH BE MAT VA HE SO TAI LN NH COT NHOI
NHNG COT DAI HN NEN HIEU QUA TACH, O ON NH VA
O LAP LAI CAO HN COT NHOI.
) CHO PHEP PHAN TCH NHNG HP CHAT RAT PHAN CC MA
COT WCOT KHONG PHAN TCH C HOAC RAT KHO PHAN
TCH.
B CAC PHA TNH LONG :
) CHU YEU S DUNG CHO COT WCOT
) CAC PHA TNH THNG C PHAN LOAI THEO O PHAN CC
) TRONG NHOM CAC PHA TNH C BAN NHOM
METHYLSILICONE (hay Polydimethyl siloxane ) LA QUAN TRONG
NHAT VA HAY C S DUNG NHAT.
) QUA TRNH TACH DA CHU YEU TREN NHIET O SOI CUA CHAT
VA TNG TAC GIA CHAT VI PHA TNH.
B MOT SO PHA TNH THNG S DUNG (O PHAN CC TANG DAN)
1,2,3-TRIS(2-CYANOETHOXY)PROPANE
ETHYLENE GLYCOL SUCCINATE
CYANOPROPYL(100%) SILICONE
DIETHYLENE GLYCOL SUCCINATE
POLY(ETHYLENE GLYCOL) ESTER HOA VI AXIT 2-
NITROTEREPHTHALIC
CYANOPROPYL(50%)PHENYL SILICONE
POLY(ETHYLENE GLYCOL), m > 40000
METHYLPHENYL(25%)CYANOPROPYL(25%) SILICONE
METHYLTRIFLUOROPROPYL(50%) SILICONE
METHYLPHENYL(50%) SILICONE
METHYLPHENYL(5%)SILICONE
METHYLSILICONE
QUA TRNH SILAN HOA CUA CHAT MANG PHA TNH
Si O C Cl
CH
3
CH
3
Si O C OCH
3
CH
3
CH
3
+ CH
3
OH
Si OH
Si O C Cl
CH
3
CH
3
Cl Si Cl
CH
3
CH
3
+
+ HCl
Chat mang
(thanh cot)
Dimethylchlorosilane (DMCS)
Phan ng
Silan hoa
Ra vi
Methanol
V tr hoat hoa
Chat mang a c
silan hoa
MOT SO PHA TNH TEN THNG MAI VA NG DUNG
Cac Hydrocarbon Khong phan
cc
Squalane Cycloparaffin
Axit beo a ester hoa ; alkaloid; dc
pham; cac hp chat halogen hoa
Hi phan cc OV-3,
SE-52
Poly(phenylmethyl
dimethyl) siloxane
(10% phenyl)
Phan cc cao
Phan cc
trung bnh
Phan cc
Khong phan
cc
Tnh phan
cc
Axit beo cha no nhieu noi oi; axit
t do; alcol
OV-275 Poly(dicyanoalkyldi
methyl) siloxane
Dc pham ; steriod; thuoc bao ve
thc vat; glycol
OV-17 Poly(phenylmethyl
dimethyl) siloxane
(50% phenyl)
Axit t do; alcol; ether; tinh dau;
glycol
Carbowax Polyethylene glycol
Cac ng dung thong thng cua cot
khong phan cc; hydrocarbon; nhan
thm; dc pham ; steroid; PCBs
OV-1,
SE-30
Polydimethyl
siloxane
ng dung Ten thng
dung
Pha Tnh
CAU TRUC CUA PHA TNH
B Polydimethyl siloxane (R = CH4) la khung
c ban cho viec tao thanh cac pha tnh khac
B Khi thay the nhom methyl bang cac nhom
khac se dan en s thay oi o phan cc va
kha nang tach
Phenyl C
6
H
5
Cyanopropyl C
3
H
3
CN
Trifluropropyl - C
3
H
6
CF
3
Polydimethyl siloxane
R Si O Si O Si R
R
R R
R R
R
n
CAU TRUC VA KHOANG NHIET O LAM VIEC CUA MOT SO
PHA TNH TRONG COT MAO QUAN
Sac ky o cua mot so cot mao quan vi cac pha tnh : (a) Polydimethyl siloxane ;
(b) 5(phenylmethyldimethyl) siloxane ; (c) 50(phenylmethyldimethyl) siloxane ;
(d) 50%poly(trifluoropropyl-dimethyl siloxane) ; (e) polyethylene glycol ; (f)
50%poly(cyanopropyl-dimethyl) siloxane
Kha nang tach tren 3 cot : (i) cot nhoi 2m x 1/4 inch; (ii) cot wide
bore 10m x 0.53mm x 2.5um HP 50; (iii) cot narrow bore 25m x
0.25mm x 0.25um Cabowax -20M
SO SANH GIA COT NHOI VA COT WCOT
ANH HNG CUA NG KNH COT VA BE DAY LP PHIM
Anh hng cua ng knh Anh hng cua be day lp phim
SO SANH SO A LY THUYET TREN NG KNH COT. CHIEU
DAI COT NHOI LA 2 m, COT MAO QUAN LA 30 m
B E NANG CAO HIEU SUAT TACH CO THE:
) LA CHON PHA TNH, CHIEU DAI COT, NG KNH COT
PHU HP VI LNG MAU, LOAI MAU. LA CHON CHNG
TRNH NHIET O PHU HP
) GHEP NOI HAI HAY NHIEU COT CO PHA TNH KHAC NHAU
) VI NHNG MAU CO THANH PHAN PHC TAP VIEC GHEP
NOI COT THNG C S DUNG.
) NHNG COT CO NG KNH KHONG KHAC NHAU NHIEU
CO THE GHEP NOI VI NHAU.
) NEU KET HP VI VAN CHUYEN COT T ONG CHO PHEP
T ONG CHUYEN COT TRONG QUA TRNH PHAN TCH.

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