BI GING

CC PHNG PHP PHN TCH SC K

Sample Mobile phase

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Detector signals
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Khoa Cng Ngh Ha Hc B mn Ha Phn Tch

H Cng Nghip TP.HCM

TS. Nguyen Ngoc Vinh

Phn 3:

ng dng GC trong phn tch LPG

S dng LPG Ha lng kh du m l qu trnh tch n gin. Ngi ta tch ring metan lm nguyn liu sn xut methanol, hn hp metan, etan c dng lm kh t cng nghip, gia dng, pht in hoc xut khu theo ng ng dn kh LPG thng phm thng c chia thnh 4 loi chnh da trn thnh phn hydrocarbon chnh ca n: Propan thng phm: s dng lm nhin liu cho cc ng c hot ng trong iu kin to thp, p sut cao Butan thng phm: s dng lm nhin liu cho ng c i hi bay hi thp hn Hn hp propane-butane: s dng lm nhin liu cho ng c i hi bay hi trung bnh

Propane chuyn dng: l sn phm c cht lng cao, s dng cho cc ng c yu cu nhin liu c kh nng chng kch n cao

 Trong cc loi trn ch c hh propan butane l thch hp ch bin kh t gia dng v chng c p sut bo ha v nhit bay hi thch hp vi nhng iu kin sinh hot c th. Do , LPG thng phm ch yu l hn hp ca propane - butane v mt lng nh propylene + butylene. LPG c s dng lm nhin liu gia dng v nhin liu cho t hoc xut khu

 LPG chy hon ton, khng c khi v tro, khng n mn, khng c hi vi con ngi v mi trng, l nhin liu sch s dng trong gia nh, giao thng v cng nghip. LPG cng l nguyn liu quan trng trong ngnh cng nghip ha du ca cc nc pht trin nh Nht, M. T LPG sn xut methanol, amoniac, ure, melamine, anhydric maleic ngha ca vic xc nh thnh phn hydrocarbon trong LPG Trong LPG, thnh phn hydrocarbon l mt ch tiu quan trng nh gi cht lng sn phm. T ch tiu ny chng ta c th xc nh cc thng s khc ca LPG nh t trng, p sut hi ring phn, ch s octane Ngoi ra khi s dng LPG lm nguyn liu cho cng nghip ha du th phi phn tch thnh phn n mt cch ton din, tt nht l bng sc k kh theo tiu chun ASTMD.2888

K thut phn tch sc k kh

u d trong phn tch LPG: phn tch thnh phn hydrocarbon ca LPG, sc k kh vi u d TCD v FID l k thut ch yu. Mi loi u d c u v nhc im khc nhau nhng TCD c s dng nhiu trong phn tch kh do kh nng nhn bit cht phn tch phi hydrocarbon.

 FID l mt trong nhng detector thch hp nht trong phn tch hydrocarbon do kh nng nhn bit cc hp cht hydrocarbon ca n. Tuy nhin, FID li khng nhy hoc rt km nhy vi khng kh, cc loi kh tr, cc oxyt lu hunh v carbon, H2S, NH3, CS2, hi nc v mt s cht kh v c khc.

 S p ng km hoc khng c i vi cc kh phi hydrocarbon s lm sai s % trong thnh phn hn hp rt ln Khc vi FID, u d TCD rt nhy vi cc loi kh v c khc bn cnh cc hp cht hu c. Cc cht kh ny u p ng v xut hin pic trn sc k khi qua u d TCD nn TCD lun l u tin hng u trong vic phn tch LPG v kh t nhin bng k thut sc k kh.

 nhy ca u d TCD ph thuc rt nhiu yu t: nhit detector, tc kh mang, dn nhit ca kh mang (H2, He), trong nhit khi u d c tc ng rt ln.
in tr trong t bo u d thng dng l Ni, Pt, Pt-Ir, W hay W-Rh. Vi phn tch nhit > 250oC th dng hon ton kim loi W, nu nhit 300 400oC th dng W Rh. in tr ca dy xo trong t bo thng l 20 - 40 T bo u d TCD thay i vi bt k s dao ng nhit trong qu trnh phn tch. iu ny dn n gi tr n (noise) cao hay ng nn b tri. Nhit khi u d phi c gi ti gi tr khng i vi chnh xc 0,5oC. nhy ca TCD ph thuc nhit p vo. Nhit u d cng cao th to dy xo cao in tr dy xo tng s thay i in tr dy xo khi dng kh mang cha mu i qua rt km nhy ca TCD gim. Nhit TCD nn nm trong khong 200 300oC trong phn tch LPG

Kh mang s dng trong phn tch LPG:

Vic chn kh mang da vi hai yu t quan trng l hiu nng tch ca ct v nhy cng nh nguyn l hot ng ca detector. Cc c tnh ca kh mang nh h s khuch tn, nht, tnh tr ha hc v tnh hp ph s quyt nh kh nng s dng loi kh mang . Cc loi kh mang thng s dng trong sc k kh gm c argon, He, nit, hydro. Nhng kh ny c tnh tr v khng phn ng vi cht phn tch.. c tnh ca cc cht kh v tc kh mang nh hng n chiu cao a l thuyt tc kh nng tch cc cht ca ct. Gin so snh u im cc loi kh mang nh sau:

Ct tch trong trong phn tch LPG: S ra i ca ct mao qun a phng php sc k t c nhng thnh tu quan trng. Cng ngh ch to ct mao qun hin nay ch to c nhng ct mao qun c nhiu loi pha tnh c phn cc khc nhau, c s a l thuyt rt cao.

Ct mao qun vi pha tnh va c tnh cht hp ph va c tnh phn b nng cao kh nng phn tch cc nhm cht c cu trc phc tp ln rt nhiu

Trong phn tch LPG bng phng php GC, ct mao qun tm pha tnh ch yu l SiO2, Al2O3. Vic phn tch kh i hi pha tnh phi c xp cao mi c kh nng tch cc cht kh (do LPG p sut thng bay hi nn pha tnh phi c xp cao mi hp ph c cc cht kh). Do pha tnh Al2O3 c kh nng to nhng l xp nh dc theo thnh ct mao qun nn c s dng nhiu trong sc k hp ph phn tch LPG Nhng loi ct thng mi thng s dng trong sc k hp ph l Kontakt-5781 (c), 13% ODPN/Al2O3 ca GreizDolan, 75% Se/Chomesor W-AW-DMCS PTN CASE s dng ct tch HP, 50 x 0,53 x 15, vi pha tnh l Al2O3, kh mang l He

K thut ly mu: S cn bng pha lng kh: trong phn tch mu LPG th k thut ly mu ng vai tr rt quan trng nhm hn ch sai s phn tch. T gin pha ph thuc p sut th tch nhit ta nhn thy c s thay i gia th rn lng, rn hi, lng kh. T c s thay i gia cc cu t trong hn hp

 Trong LPG cn c nhng kh khc nh CO2, N2, H2S, etanol, diethylsulfit, diethyldisulfit nhng ch yu l H2S v hi nc. Chng gy c cho mi trng khi s dng v lm hao mn thit b nhanh chng do tnh acid. Bnh ly mu lm bng kim loi chu p cao, chiu dy > 1cm, c van kha 2 u. Bnh c c nh trn gi d dng iu chnh van khi thc hin chy mu.

 Dng bnh kim loi chu p sut cao ( trnh gy n), c trng lp cht tr vi mu kh. ng dn lm bng nhm hoc thy tinh c van iu chnh p sut. Ni u ng vo st y bnh cha mu LPG. Cho kh t bnh mu i qua bnh nh ly mu, m van cho kh thot ra mt lc lm sch bnh chu p cha mu. Trong qu trnh ly mu th bnh ly mu phi c ui ht khng kh cng nh nhng kh khc cn st li trong bnh. ng van thot ra ca bnh chu p cha mu, kh ha lng trong bnh kh c chuyn t bnh mu sang bnh nh chu p do s cn bng v p sut Nu bnh mu LPG khng c ng dn xung y bnh th phi lt p bnh ly phn cht lng i din cho mu LPG. S dng kh LPG trong bnh ly mu phn tch. Nu bnh cha LPG c van gim p th khng cn chit LPG sang bnh nh m ni trc tip vo my GC phn tch.

B phn np mu (van chia 6 cng):

Qu trnh np mu LPG vo my GC l qu trnh t ng. a mu vo ct, ngi ta s dng van 6 cng. Cu trc ca van cho php ly c mt th tch nht nh ng thi thay c th tch kh cn thit nh vo h thng kh nh lng d dng lp t . H thng van 6 cng c trnh by nh bn di:
Mu Van x 2 6 5 Ct 4 3 Ct Mu Van x

Vng cha mu Kh mang/pha ng V tr A

Vng cha mu Kh mang/pha ng V tr B

Nguyn tc hot ng ca van 6 cng: Khi van v tr A th mu khng i qua ct, mu i qua cc cng 1-6-3-2 v i ra ngoi. di ca ng i qua vng cha mu cho php ly th tch kh vi n nh. Kh mang i qua cng 4-5 i vo ct khng mang mu. Khi van chuyn sang v tr B, lp tc mt th tch mu kh nht nh c a vo ct qua cng 6-5 v tin trnh tch cc cht
Mu Van x 2 Mu Van x

6
5 Ct 4 3 Ct

Vng cha mu Kh mang/pha ng V tr A

Vng cha mu Kh mang/pha ng V tr B

Nguyn tc hot ng ca van 6 cng:

Vn sai s din ra khi van chuyn t v tr A sang B. gim thiu sai s, p lc ca cc ln chy my phi n nh, lu lng kh thot ra phi bng vi kh np vo vng cha mu v p lc gia cc ln chy phi ging nhau. iu ny c kim tra bng cch m s bt kh thot ra.
Nhng nh hng trong qu trnh phn tch LPG Do vic phn tch LPG bng GC/ct mao qun nn ch s dng lng nh mu vo ct. H thng tim mu chia dng c s dng nhm trnh tnh trng qu ti cho ct tch. Vic ny dn n nh hng nhit injector trong qu trnh phn tch LPG Yu cu nhit injector phi tt c mu bay hi hon ton nhng khng phn hy. nhng cht c nhit ha hi cao l nguyn nhn gy nn sai s

Nhng nh hng trong qu trnh phn tch LPG Trong sc k kh, tch t mu ti u ct cng cao th vn phn gii cng d thc hin. Cn p t nhit thch hp thi im u lng mu tch t ti u ct ln. Thng thng nhit injector t 50 - 200 ty loi mu. Vi phn tch LPG, to injector thch hp khong 200oC C nhiu nguyn nhn gy sai s trong qu trnh phn tch LPG bng GC-ct mao qun vi u d FID hoc TCD. Khi xy dng phng php phn tch LPG cn phi kho st y cc yu t nh hng n qu trnh phn tch nh: Qu trnh np mu

Cc phng php ly mu t bnh ng mu kh LPG

Kho st cc yu t nh hng nhit injector, detector, l cha ct tch

Thank you For your attention