Vận hành thiết bị TGA Q500

8/13/2019 Vn hnh thit b TGA Q500

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Vn hnh thit bTGA Q500

I. C sl thuytPhn tch nhit trng lng (TGA) l mt cng cphn tch nhit da trn sthay i khi lng

ca mu. N c kt hp vi mt thit biu khin php phn tch nhit v kt ni mt phn mmthng qua my tnh to nn mt hthng phn tch nhit.

Php phn tch nhit trng lng dng o lng v tc thay i khi lng ca vt liu,c xc nh thng qua hm tng nhit hoc ng nhit theo hm thi gian, trong siu khinca p sut. Kthut ny c thdng nh tnh1 bt kvt liu no m c gii hn trong sthayi khi lng v loi bschuyn pha do cc qu trnh phn hy, oxy ha hoc dehydrate ha.Thng tin ny gip nhn bit c hnh thnh phn trm m khi lng thay i v c thpht trinc cu trc trong cc qu trnh tng hp vt liu.

Cng ciu khin l mt my tnh c phn mm kt ni vi thit b. N c ththc hin ccc chc nng sau:

- Cung cp phn mm kt ni gia my tnh v thit bphn tch.- Phn mm cho php t cc thng scho qu trnh chy mu.- Lu trhoc phc hi cc dliu ca cc th nghim.- Chy chng trnh phn tch dliu (phn tch kt qu).Cu to TGA Q500 c 6 bphn chnh:

- Cn: l thit bcung cp php o chnh xc thng qua khi lng mu phn tch.- mu: l thit bdng chuyn mu n hthng cn v ngc lai.- L: tc dng ca l l iu khin p sut v nhit ca mu. TGA Q500 vi mt hthng

l chun. y sdng hthng l EGA, chng ph hp cho thit bTGA.

- Vmy: l mt hthng in v lp t hthng (phkin kt ni; heat axchange, nitrogentube,).

- Hthng trao i nhit, c tc dng gii nhit cho l khi phn tch.- TGA c 2 dng kh i vo, mt dng vo cn, dng cn li vo l.

II. Dng cv ha chtChn Platin: 2 Thit bTGA Q500:1

Kh Nit: 100ml/pht

III. Thc nghim1.

Khi ng hthng my TGA:- Mkh nit- Mmy TGA: Mcng tc pha sau my TGA- Mcomputer. Click chut vo biu tng TA Istrument Explore trn mn hnh destop- R chut vo biu tng my TGA, nhn chut phi 2 ln kt ni computer v chuog7

trnh iu khin TGA. Xut hin mn hnh giao din lm vic ca TGA2. Thc hin TARE chn


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Lu : Khi kt thc mt run, lun lun phi chbung t trvnhit phng trc khi chyRun mi hoc tt my.

6. Tt my:- ng bung t ( Furnace Up)- Vo ControlShutdown instrument- i my TGA shut down xong th turn off my vi tnh- Tt cng tc my TGA (pha sau my)- Kha kh Nit


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ng dng TGA trong phn tch vt liu

I. C sl thuytPhng php phn tch nhit lng (TGA) l th nghim kho st shay i khi lng camu theo nhit hoc theo thi gian.Khi nung nng vt liu, c nhng qu trnh bin i vtnh cht vt l, ha hc c trng chotng cht ring bit. Trong cng mt khong nhit , cc qu trnh bin i vcht c thxy ra ng thi. ng cong nhit m tqu trnh bin i ca vt liu.Ty thuc vo thng tin cn thu c tmu nghin cu, mu c kho st cc chnhit khc nhau: Gia nhit tc khng i (2, 5, 10, 200C min-1), hoc lu mu nhitkhng i.Kt quca phn tch TGA l sthay i khi lng hoc % khi lng theo thi gian hoctheo nhit .Sthay i khi lng xy ra khi mu mt khi lng hoc cc phn ng vi mi trngxung quanh (v d: phn ng gia mu vi O2, H2). Kt qul ng cong TGA xut hincc bc gim (hoc tng) khi lng.

Cc qu trnh lm thay i khi lng ca mu kho st:- Qu trnh bay hi, tch m, gii hp, mt nc kt tinh.- Qu trnh oxy ha ca kim loi trong khng kh hoc oxy.- Qu trnh phn hy cht hu c trong kh tr vi sto thnh sn phm kh.ng cong TGA cho bit sthay i khi lng ca mu. Phn tch TGA nh lng: Phn trmkhi lng, G%, c tnh trn gim khi lng m v khi lng u ca mu m0, theo cngthc sau:

[]

II. Ha cht v dng c:Calcium Oxalate CaC2O4.H2O Kh Nit : 100ml/pht

Calcium Carbonate CaCO3 Thit bTGA: 1

Monosodium Phosphate NaH2PO4.2H2O

III. Thc nghim;1. Khi ng hthng my TGA2. Thc hin TARE chn3. Phn tch gim khi lng cho mu CaC2O4.H2Oa. Ci t chng trnh

Click APPEND to 1 run mi

- Vo thSUMMARY khai bo: Test: chn chtest CUSTOM Sample name: khai bo tn mu Data sample: ng dn lu kt qu


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- Nhn nt Furnace trn mn hnh iu khin hoc tbn phm di chuyn l ln vtr baoquanh mu.

Trc khi bt u th nghim, cn m bo my TGA c kt ni vi phn mm iu khin vcn phi in y thng tin cn thit trn phn mm iu khin.

Nhn nt Start tin hnh phn tch mu

Sau khi mu c phn tch xog, chnhit thc ca l tr vgi trnhit phng mi tinhnh o cc mu ktip.

5. Kho st tc qut nh hng n kt quphn tch mu NaH2PO4.2H2Oa. Ci t chng trnhClick APPEND to 1 run mi

- Vo thSUMMARY khai bo: Test: chn chtest CUSTOM Sample name; khai bo tn mu Data sample: ng dn lu kt qu Pan type; loi chn Pt

- Vo thPROCEDURE ci t phng phpRamp 50C/min to 5000C

- Vo NOTES: ghi ch thm nu cn thit- Sau khi ci t xong cc thng scn thit, click APPLYb. Load muSau khi tare chn mu, tin hnh thao tc load mu NaH2PO4.2H2Ovo l nh sau:

- Cho mu NaH2PO

4.2H

2O phu 1 lp mng ln bmt chn ri t chn cha mu ln

Sample platform.Ch : Phi sdng nhp bng ng cm chn mu

- Nhn nt Load trn mn hnh iu khin chnh hoc tbn phm. Kh my stng loadchn mu vo cn.

- Nhn nt Furnace trn mn hnh iu khin hoc tbn phm di chuyn l ln vtr baoquanh mu.

Trc khi bt u th nghim, cn m bo my TGA c kt ni vi phn mm iu khin vcn phi in y thng tin cn thit trn phn mm iu khin.

Nhn nt Start tin hnh phn tch mu

Sau khi mu c phn tch xong, chnhit thc ca l tr vgi trnhit phng mi tinhnh o cc mu NaH2PO4.2H2O ktip cc tc qut 10

0C, 200C.

Tin hnh tng tcc bc trn thay i phng php:

NaH2PO4.2H2O tc qut 100C: Ramp 100C/min to 5000C

NaH2PO4.2H2O tc qut 200C: Ramp 200C/min to 5000C


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6. Phn tch kt qu:Vo Desktop chn biu tng TA Universal Analysis

Vo Open/Chn a lu tr/ Chn file kt qucn phn tch/OK

Vo GRAPH SIGNAL: chn Y2 l ng vi phn khi lng theo nhit xc nh im thay

i nhit c ddng

Vo Analyze weight change phn tch khong thay i khi lng theo nhit

Nu mun thay i kt quva chn/ Click chut phi chn Delete results

Lu kt qu: Sauk hi xl kt quvo File/Save analysis/Analysis Data/Ok

Lu file Excel

a. Xl kt quphn tch mu CaC2O4.H2O. Don thnh phn tng ng vi gim khilng.

b. Xl kt quphn tch mu CaCO3trn thtrng. Tnh hm lng CaCO3c trong mu.p dng cng thc: []

Khi lng mu m0; MCaCO3= 100; Mgas= 44

gim khi lng m

c. Xl kt quphn tch mu NaH2PO4.2H2O vi cc tc qut. Ghp cc phtrn cng gin. So snh v kt lun.Lu : Khi kt thc 1run, lun lun phi chbung t trvnhit phng trc khi chy run

mi hoc tt my.7. Tt my:

- ng bung t ( Furnace Up)- Vo ControlShutdown instrument- i my TGA shut down xong th turn off my vi tnh- Tt cng tc my TGA (pha sau my)- Kha khNit


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Vận hành thiết bị TGA Q500