Guidelines When Using the RCS Setting Up a DSC Ramp Procedure Setting Up a DSC Isothermal Procedure Setting Up a DSC

DSC Heat/Cool/Heat Procedure Setting Up a DSC Cell/Cooler Conditioning Procedure Hng dn s dng h thng RCS (Guidelines When Using the RCS) Khi RCS c ci t, cc iu kin hot ng v hiu chnh h thng cn tun th cc hng dn sau.
Xc nh vic chuyn i RCS c thit lp,tc l RCS phi ch EVENT.

bt h thng RCS, chn Event/On t thanh iu khin Control. C th thy Adjusting the Event, Storage, Air, v Air Cool Selection.
Lm kh, RCS s dng ngun kh kh, khng nhim m nh l kh nn (base

purge). Kh Nit kh thng c s dng. Kh ny phi c duy tr lin tc, nu khng hi m khng kh s vo v lm nhim bn h thng.
Ti ng dn Tools/Instrument Preferences/Cooler Page ca phn mm iu

khin DSC. Kim tra ng kiu thit b lm lnh (RCS 40 hay RCS 90) cn cho hot ng ca my. Kim tra Leave RCS on.
Kim tra dng kh th cp khi np m (Activate secondary purge when lid is

opened) (ch RCS v LNCS), nu cn thit. Qu trnh lm sch RCS s t ng khi m bng AutoLid. Np thit b phi ng ch bt c lc no mu load hay unload.
Chn Tools/Instrument Preferences/DSC page ca phn mm v thit lp nhit

n nh (Standby Temperature).
Nu c b phn ly mu t ng, chn Tools/Instrument Preferences/Autosampler

page v b RCS Off trong hp thoi. iu ny cho php chc nng Event ca RCS hot ng.
Khi thit lp phi m bo kim tra cc iu kin sau. Ca s nhit phi c

kch hot v khong nhit phi trn nhit mi trng. KHNG m cc thit b DSC di nhit mi trng.

 Khi h thng DSC-RCS hot ng, khng tt RCS nu khng h thng s khng

c s dng trong mt thi gian di ( nhiu hn 2 hoc 3 ngy). Do , khng tt RCS khi my ang chy. CH : Khng c vt qu 100 C gia u lm mt RCS v ngun RCS. Thit hi nghim trng h thng c th xy ra. LU : Khng s dng RCS ng nhit trn 400C. Thit hi c th xy ra nu s dng nhit cao trong thi gian di. Thit lp tc gia nhit cho DSC (Setting Up a DSC Ramp Procedure) thit lp gia nhit cho DSC, c th chn mt trong hai k thut: DSC Wizard hoc Experimental View - Procedure Page. Xem hng dn pha di cho mi k thut. Khi thc hin gia nhit DSC, hiu chun, hoc hng s cell/hiu chun nhit th nghim cc thng s sau y nn chn:
Nhit bt u v kt thc (Start and Final Temperatures): nhit bt u

thc t v kt thc c chn cho qu trnh o c th phi nm trong gi hn nhit ca DSC v RCS. Nhit ny nn nm vng m s chuyn tip mu c th s xy ra v chng phi nm di hoc trn cc qu trnh chuyn i so vi ng nn n nh. C th chn bt u thit lp t mt trong cc la chn sau y:
a. Current Temperature - l nhit ca cc h thng DSC ti thi im hin ti

(30 n 35C). Trng hp ny, gia nhit bt u ngay lc tin hnh o.

b. Another Temperature - chn nhit c th (mc nh l 50C). Trng hp

ny, h thng cn bng nhit chn trc khi qu trnh gia nhit ramped heating bt u.
Ramp (Heating) Rate: gii hn chp nhn ca qu trnh gia nhit/lm mt

(heating/cooling) cho DSC thng thng l 0.01 n 100C/pht. Gii hn ny ph thuc vo gi tr thay i bao gm phm vi nhit gii hn v thit b lm mt. Tng ch s heating/cooling thng tng nhy, c bit cho qu trnh nhit nh chuyn tip thy tinh. N cng lm rt ngn thi gian phn tch. Gim heating/cooling s cho phn gii tt hn (d quan st cc peak). Tc gia nhit 10 n 20C/pht v tc lm mt 5 n 10C/pht l ti u cho hu ht cc vt liu.

 Phm vi nhit phn tch cho cc h thng DSC l -180 n 725C , nhng c

th gim ty thuc vo loi chn mu v thit b lm mt c s dng. (Ch : Ch c cc kh tr nh nit c th c s dng trn 600C). nh gi cc vt liu di nhit phng hoc chy lm mt my. Thng thng, s dng h thng lm mt bng lng nit, LNCS, (-150 n 550C) hoc RCS, (-90 n 550C). Ngoi ra cn c nhiu loi chn DSC khc. Tt c trong s chng c th c s dng n 725C, ngoi tr chn nhm ch nn s dng n 600C (do nhm nng chy 660C).
Additional Conditions: Cc iu kin th nghim khc c th c thay i

ti u ha cc trng hp c th. S dng Advanced Parameters and Post-Test Conditions. i vi hu ht cc qu trnh, gi tr mc nh ca h thng c xut. Using the DSC Wizard : Nhp cc thng s mong mun, sau chn Next tip tc Using the Experimental View Procedure Page:
1. Trong Procedure Page. Chn qu trnh cn chy t danh sch c sn c lp

trnh trc.
2. Nhp cc thng s mong mun. Khi hon tt thit lp, c th nhp thm thng

tin bng cch chn Notes Page and Summary Page.

3. Nhp vo nt Apply khi hon tt, lu cc thay i hoc nt Append lu cc

thay i chy trong qu trnh ny v thm trong qu trnh chy khc. Thit lp DSC ng nhit (Setting Up a DSC Isothermal Procedure) ng nhit DSC cung cp ch dn v tnh n nh ca vt liu nhit nh gi. Dng kh tr, bao quanh vt liu khng i hoc c chuyn sang nhit ang xt to ra mt s tng tc mu vi kh quyn (v d nh, tnh n nh oxy ha). Nu mun thit lp ng nhit DSC, c th chn mt trong hai k thut the DSC Wizard hoc Experimental View - Procedure Page.
Nhit ng nhit (Isothermal Temperature): l gii hn nhit cn bng

trong qu trnh chy ng nhit, ph thuc qu trnh lm mt. Nhit ng nhit trong phm vi hot ng ca thit b lm mt c chn (v d, -90 n 550C cho RCS). Tuy nhin, cc qu trnh ko di gn gii hn nhit ca thit b lm mt

c th nh hng n thi gian sng ca thit b. V vy, vic s dng h thng lm mt Finned Air Cooling (FACS) c khuyn khch cho qu trnh ng nhit trn 350C. Ngoi ra, khi chy ng nhit trn 600C nn c thc hin vi mt kh tr. Phng php tiu chun kim tra nhit cn bng c xc nh. V d, polyolefin n nh oxy ha c nghin cu phn tch ti 200C da trn Phng php ASTM D3895-80. CAUTION: khng s dng RCS khi chy th nghim ng nhit trn 400 C. Thit b c th h hi nu s dng nhit cao trong thi gian di.
Switch to Gas 2 (requires a Mass Flow Controller): Ty chn chuyn i kh

sau khi t c nhit cn bng gip o lng cc c tnh vt liu khng ch da vo nhit , m cn da trn khng kh xung quanh vt liu (v d, s n nh trong oxy [chng suy thoi oxy ha]).
Thi gian ng nhit (Isothermal Time): Thi gian ng nhit nn c thit lp

1 gi tr ln hn so vi yu cu o lng. Nu khng bit thi gian ng nhit th nn chon 1 gi tr ln.

End Experiment When: Thi gian phn tch s "kt thc qu trnh" ti gi tr

thit lp. Qu trnh ng nhit DSC thng dng li da trn s pht hin dng chy nhit (mW/pht) ln hn mt gi tr "ngng". Ngng ny phi ln m bo rng qu trnh xy ra. 0,5 mW/pht l ti u. Kim tra mc End Experiment When v chn cc thit lp mong mun trong ty chn.
Additional Conditions: Cc qu trnh khc c th c thay i ti u ha cc

qu trnh c th. S dng Advanced Parameters v Post-Test Conditions. i vi hu ht cc qu trnh, gi tr mc nh ca h thng c ngh. Ci t gia nhit/lm lnh DSC (Setting Up a DSC Heat/Cool/Heat Procedure) DSC Heat/Cool/Heat c thit k xa lch s nhit ca qu trnh trc bng cch gia nhit vt liu trn nhit chuyn tip (v d, chuyn ha thy tinh nng chy), s hi phc, sp xp li phn t c th xy ra, sau lm mt vi 1 tc c thit lp trc khi gia nhit ln na. ng nhit u tin cung cp thng tin "as received". Qu trnh lm mt nh l lch s nhit. V vy, bt k s quan st khc bit no gia cc vt liu ging nhau trong ng nhit th hai c lin quan n s khc bit bn trong vt liu (v d, trng lng phn t) hn l tc dng lch s nhit trc .

Nu mun thit lp mt DSC heat/cool/heat, c th chn mt trong hai k thut DSC Wizard hay Experimental View - Procedure Page Khi thc hin DSC heat/cool/heat, cc thng s sau y cn phi c chn:
Nhit bt u (Start Temperature): nhit bt u v tng ln c la

chn cho mt qu trnh c th v phi nm trong nhit ca DSC cell/cooling ang s dng. RCS v LNCS c th c s dng cho cc cc qu trnh heat/cool/heat. FACS c th c s dng cho heat/cool/heat t 50 n 500C. Quench Cooler khng c s dng cho heat/cool/heat. Nhit ny nn nm cc qu trnh chuyn i mu c d kin s xy ra v di hoc trn cc qu trnh chuyn i thit lp ng nn n nh. C th chn bt u qu trnh t mt trong cc la chn sau y:
a. Current Temp - nhit ca thit b DSC ti thi im hin ti (thng l nhit

mi trng xung quanh, 35C). Trong trng hp ny, tc gia nhit bt u khi tin hnh qu trnh. b. Another Temp - chn nhit c th mong mun (mc nh l 50 C). Trong trng hp ny, h thng cn bng nhit chn trc khi bt u bt u gia nhit.
Upper Temperature: c c nhng kt qu d nh t qu trnh

heat/cool/heat, nhit trn c chn phi cao hn so vi qu trnh chuyn i "xa" lch s nhit trc . Thng thng ln hn 10 n 15C trn chuyn tip thy tinh hoc im tan chy.Tuy nhin, nhit trn cng cn phi thp ngn chn s phn hy.
Lower Temperature: Nhit thp nht t c trong qu trnh lm mt phi

di bt k nhit chuyn tip.

Heating Rate & Cooling Rate: gii hn heating/cooling ca DSC thng thng

l 0,01 n 100C/pht. Khong ny ph thuc vo gi tr bao gm c gii hn nhit bao ph v s c mt ca thit b lm mt. Tc heating/cooling nhanh thng lm tng nhy, c bit cho cc qu trnh nhit nh chuyn tip thy tinh. Chng cng gim thi gian phn tch. Tc heating/cooling chm nhn chung cho phn gii tt. Ch s heating 10 n 20C/pht v tc lm mt 5 n 10 pht/C l ti u cho hu ht cc vt liu.

 Additional Conditions: Cc iu kin th nghim khc c th c thay i

ti u ha cc trng hp c th. S dng Advanced Parameters v Post-Test Conditions. i vi hu ht cc th nghim, gi tr mc nh ca h thng c ngh. Ci t chy mt my DSC (Setting Up a DSC Cell/Cooler Conditioning Procedure) Khi thit b hoc ph kin lm mt c ci t vo h thng, th phng php ny nn chy lm kh h thng DSC v lm mt trc khi m h thng lm lm lnh v bt u chy my. Trong sut qu trnh chy ny th nhit c nng ln. Thc hin theo cc hng dn di y thit t cho h thng: 1. Tt ph kin lm mt, nu n m.
2. Ly mu khi bung mu nu c. 3. Xc nh ng dn, vo Tools/Preferences Instrument/Cooler page. 4. trang Procedure Page. Chn "Cell/Cooler Conditioning" chy t danh sch

c sn c lp trnh trc.
5. Nhp cc thng s cn thit: Conditioning Temperature: thit b s c un nng n nhit ny v gi ng

nhit lm kh. Nhit c ngh l 75C. Hold Time: y l thi gian m thit b s c gi iu kin nhit quy nh trn. Thi gian c ngh l 120 pht.
Enable secondary purge: Khi s dng RCS LNCS, mt ngun kh nit kh c

kt ni vi cng kh lm mt nu thit b c s dng trong mi trng c m cao hoc mi trng nhim bn. Nu chn vo (Enable secondary purge) chn kch hot dng kh th cp, dng kh th cp (secondary purge) s c s dng, dng kh th cp s cung cp thm kh kh vo RCS v LNCS khi AutoLid c m hoc khi PCA c s dng. Ty chn ny nn c trng khi khng c kh th cp kt ni vi cng kh lm mt. Xem thm: Kt ni ng ng dn kh lm mt ( Connecting the Cooling Gas Line). iu kin B sung (Additional Conditions): Cc iu kin th nghim khc c th c thay i ti u ha cc trng hp c th. S dng Advanced Parameters

and Post-Test Conditions. i vi hu ht cc th nghim, gi tr mc nh ca h thng c ngh.

6. Khi hon tt thit lp, c th nhp thm thng tin bng cch chn trang Notes

Page v Summary Page. Nu thit b c iu khin lu lng, kim tra tc dng thch hp c quy nh c th trang Notes Page. Tc dng c ngh l 50ml/pht.
7. Nhp vo nt Apply khi hon tt lu cc thay i.

8. Bt u chy. Sau khi chy n nh, bt thit b lm mt v n trong 30 pht trc khi bt u chy mu. Ch : c th s dng bt k chn la no trong Cell ti trang Procedure Page lm c s cho qu trnh kim tra ty chnh bng thit lp tu chn mong mun t danh sch, sau nhp vo nt Apply v thay i th nghim ty chnh. Sau , c th vo Procedure Page v sau Editor thc hin cc thay i mong mun.