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H CH MINH
B MN CNG NGH HO HC
-
BI BO CO NHM
MN: TH NGHIM HA L
GVHD: NGUYN BO VIT
LP DH08HH
Thng 1/2011
THY PHN ESTER BNG KIM
I. Yu cu
Sinh vin cn nm vng cc vn sau :
- Xc nh phn ng thy phn ester trong mi trng kim l phn ng bc 2.
- Nm vng ngha ca nng lng hot ha v nh hng ca nhit ln
hng s tc ca phn ng qua h thc Arrhenius.
- S dng phng php chun ngc xc nh nng NaOH
- Hiu l do phi un hon lu hn hp phn ng.
II. L thuyt
Phn ng gia ester acetat etyl v NaOH xy ra nh sau :
CH3COOC2H5 + NaOH CH3COONa + C2H5OH
t=0 a b 0 0
t ax bx x x
vi : a, b l nng u ca ester v NaOH
(a x) v (b x) l nng ca ester v NaOH thi im t
y l phn ng bc 2, biu thc hng s tc c dng :
k / t = [1 / (a b)] . ln {[b.(a x)] / [a .(b x)]}
(7.1)
Gi no , nt , n l th tch NaOH cn trong hn hp phn ng cc thi
im t = 0 , t , (phn ng han ton thi im t )
Nng NaOH cc thi im s t l vi cc th tch . Cn nng ester
thi im u v thi im t s t l tng ng vi (no - n) v (nt - n).
Do : CoNaOH = b = A . no
Coester = a = A . (no - n)
Ct NaOH = b x = A . nt
Ct ester = a x = A . [(no - n) no nt)] = A . (nt - n)
vi : A - l hng s t l.
Thay cc gi tr trn vo (7.1)
1 A.n0 . A.(nt n )
kt . ln
A.( n0 n ) A.n0 A.nt . A.(n0 n )
1 n .(n n )
kt . ln 0 t
An nt .( n0 n )
1 n .( n n )
kt . ln t 0 (7.2)
An n0 .( nt n )
no ?
Nng ng lng ca NaOH trong mu th s l :
CoNaOH = no x (1/100) x (1/1000) x (1000/25) = no / 2500
m CoNaOH = A . no.
Suy ra : A = 1/2500
* nh hng ca nhit n hng s tc
Phng trnh Arrhenius m t s ph thuc ca tc phn ng vo nhit :
k = ko . e-E / RT
(7.3)
vi : ko l tha s tn s hay tha s Arrhenius, khng ph thuc nhit
E - l nng lng hot ha ca phn ng.
Ly logarit 2 v : lnk = lnko - (E / RT)
Nh vy, ng biu din lnk = f(1/T) l ng thng c dc E/R
Gi k1, k2 l hng s tc cc nhit T1, T2 , khi :
Ln (k2 / k1 ) = - (E/R) . ( 1/T2 1/T1) (7.4)
Da vo (7.4) c th tm nng lng hot ha ca phn ng khi bit hng s
tc hai nhit khc nhau.
Nhit Thi im
5 10 20 30 40 50 x
T1 27.5 27.8 27.9 28 28.5 29 30
T2 30.1 30.5 30.6 30.8 31 31.1 45
2.Kt qu tnh:
Thi V NaOH chun V NaOH trong
Nhit (0C) im (ml) mu th (ml) K
27.5 0 4.8 7.7 0
27.5 5 5.2 7.3 4.545E-06
27.8 10 6 6.5 1.593E-05
27.9 20 6.6 5.9 2.737E-05
28 30 7 5.5 3.707E-05
28.5 40 8.5 4 1.074E-04
29 50 9 3.5 1.654E-04
T1=3 v
0 30 cng 9.7 2.8 2.776E-03
trung bnh 3.917E-04
30 0 4 8.5 0
30.1 5 4.6 7.9 7.161E-06
30.5 10 5 7.5 1.294E-05
30.6 20 6.1 6.4 3.560E-05
30.8 30 6.8 5.7 5.971E-05
31 40 7.4 5.1 9.471E-05
31.1 50 7.6 4.9 1.126E-04
v
T2=45 45 cng 8.4 4.1 1.655E-03
trung
bnh 4.610E-05
Tnh kT1 v kT2 theo phng php bnh phng cc tiu, ta c cc th sau
T bng s liu trn, p dng cng thc (*) ta tnh c nng lng hot ha E:
I. Yu cu :
Sinh vin cn nm vng cc vn :
- Nm c nguyn tc phng php phn tch nhit
- p dng quy tc pha gii thch dng cc ng cong ngui lnh
- Thit lp gin nhit - thnh phn khi lng ca h hai cu t kt tinh
khng to hp cht ha hc hay DD rn.
II. L thuyt :
Phng php phn tch nhit t trn c s nghin cu s thay i nhit ca
mt h ngui hoc nng dn theo thi gian.
p sut nht nh, nhit kt tinh ca mt nguyn cht c gi tr khng i
v gi nguyn trong sut qu trnh kt tinh. i vi DD, nhit bt u kt tinh
ph thuc thnh phn DD v trong qu trnh kt tinh mt cu t, nhit gim
dn cho ti khi xut hin cu t th hai cng kt tinh th nhit gi nguyn Te
(ng vi nhit eutecti ) cho ti khi qu trnh kt tinh kt thc. Sau nhit
tip tc gim.
Trn hnh 4.1, ng ngui (1) v (5) ng vi A v B nguyn cht. ng (2)
v (4) ng vi hn hp c gi tr %B tng dn. ng (3) ng vi hn hp c
thnh phn bng ng thnh phn eutecti.
Trn ng (1) v (5) cc on thng nm ngang ng vi qu trnh kt tinh A
v B nguyn cht.
Trn ng (2), (3), (4) on nm ngang b, c, e ng vi qu trnh kt tinh
eutecti, cn cc im b,c ng vi im bt u v kt tinh mt cu t no (cc
hn hp 2, 4). Nhng im ny xc nh d dng v dc ca ng biu
din thay i do tc gim nhit trc v trong khi kt tinh khng ging
nhau. Trong thc nghim vic xc nh im eutecti rt quan trng nhng li rt
kh. Thng dng phng php Tamman - nu iu kin ngui lnh han ton
nh nhau th di ca on nm ngang (thi gian kt tinh) trn ng cong
ngui lnh s t l vi lng eutecti. Nh vy nu t trn on ad thnh phn v
trn trc tung l di cc on nm ngang ca ng ngui lnh tng ng ni
cc u mt li., ta s c tam gic aId. nh I ca tam gic ng vi thnh phn
eutecti. Tam gic aId gi l tam gic Tamman.
Gin nhit - thi gian Gin nhit - thnh phn
* Ha cht :
- Hn hp Naptalen Diphenylamin pha sn theo cc thnh phn nh sau :
ng nghim 1 2 3 4 5 6 7 8
Naptalen (g) 10 8 6 4.5 3 2.5 1 0
Diphenylamin 0 2 4 5.5 7 7.5 9 10
(g)
3- Kt qu
a) Kt qu th : Ghi li nhit hn hp tng thi im ca 8 ng nghim.
b) Kt qu tnh:
- V th nhit - thi gian (ng cong ngui lnh) ca h. Xc nh nhit
bt u kt tinh ca tng hn hp. (nh du trn th)
- V th nhit - thnh phn ca h diphenylamin naptalen v xc nh
nhit eutecti, thnh phn eutecti ca h.
Bi lm:
nhit
thi nhit nhit nhit nhit nhit nhit nhit
gian(ph ng ng ng ng
t) ng 1 2 3 ng 4 ng 5 6 7 ng 8
1 80 76 68.5 72 55.4 64 56 62
2 78 71 63.8 66 52.5 62 52 58
3 78 70 62 60 48 56 49 54.5
4 77 68 62.5 53 44 50 46 53.5
5 77 67 62 49.5 41.3 47 45 53
6 77 66 62 47 36 44 46 53
7 76.5 64 61 45 30 42 45.8 53.5
8 75.5 63 59 44.5 28 38 45 52.7
9 74 61.5 57.5 44 30 44.5 52.7
10 73 60 57 44 33 44.5 52.7
11 71 59 55 42.8 32 44 52.7
12 70 58 53 40.5 28 43 52.7
13 68 55 51.5 40 42.8 52.7
14 67.5 53 49.8 38 42.5 52.7
15 65 50 48.8 35.5 42.5 52.2
16 48 48 33.5 44 52
17 46.5 32 43.5 51.2
18 45 42.5 50.2
19 43 42 49.1
20 41.5 41.7 47
21 40 40.8 42.5
22 38 40 40.5
23 35 38 38
24 33.5 36 34.5
25 30 34 30
26 32
27 31.8
28 30
29 29.8
30 29.8
Nhn vo th ta c ,thnh phn hn hp eutecti tng ng vi thnh phn hn
hp ca ng 6: 2.5 g naptalen, 7.5 g Diphenyl amin
Nhit ca eutecti l 30.
nbviet@hcmuaf.edu.vn
HP PH TRN RANH GII LNG - RN
I. Yu cu
Sinh vin cn nm vng cc vn sau :
- Nm vng nh ngha hp ph, ng ng nhit hp ph
- Kho st s hp ph acid acetic trong DD nc trn than hot tnh v thit
lp cc ng ng nhit hp ph tng ng.
II. L thuyt
Hp ph l hin tng c mt cht (dng phn t, nguyn t hay ion) tp
trung, cht cha trn b mt phn chia pha no (kh / rn, lng / rn, kh /
lng)
Trong trng hp cht hp ph rn, thng l cht c b mt ring (tng din
tch trn 1 gam cht rn) rt ln, c gi tr vo khong 10 1000 m2/g. Cc cht
hp ph cht rn thng dng l : than hot tnh, silicagel (SiO2), alumin (Al2O3),
zeolit
Trong s hp ph cc cht trn b mt ct hp ph rn, nguyn nhn ch yu
ca s hp ph l do nng lng d b mt trn ranh gii phn chia pha rn kh
hay rn - lng. Cc lc tng tc trong hp ph ny c th l cc lc Van der
Waals (hp ph vt l) hay cc lc gy nn do tng tc ha hc (hp ph ha
hc) hay so c hai loi tng tc trn cng tc dng.
Lng cht b hp ph trn b mt cht hp ph tu thuc vo nhiu yu t
nh :
- Bn cht ca cht hp ph v cht b hp ph
- Nng ca cht b hp ph
- Nhit , v.v
Thc hin TN nhit khng i, ta c th o c s mol cht b hp ph
trn 1 g cht hp ph rn ( hp ph ) cc nng cht b hp ph khc
nhau (C). ng biu din C gi l ng ng nhit hp ph.
Mt s phng trnh thc nghim v l thuyt c s dng biu th cc
ng ng nhit hp ph : Freundlich, Langmuir, BET, v.v
1- Phng trnh Freundlich
y l phng trnh thc nghim, p dng cho s hp ph cht kh hay cht
ha tan trong DD.
= k . C1/n (13.1)
Trong : k v 1/n l nhng hng s khng c ngha vt l
C - l nng DD khi hp ph t cn bng
no(mol)
Bnh Co (mol/l C (mol/l) Ln C (mol/c ln C/
m2)
1 0.01 0.2 0.1723 -1.758 0.0091 - 18.85
4.695
4 28 8
-
2 0.0073 4.918 18.82
0.008 0.16 0.1377 -1.983 1 28 8
-
3 0.0054 5.205 18.71
0.006 0.12 0.1027 -2.276 9 43 2
-
4 0.0033 5.702 19.82
0.004 0.08 0.066 -2.716 4 28 0
-
5 0.0017 6.380 17.99
0.002 0.04 0.031 -3.490 0 07 4
-
6 0.0007 7.197 16.81
0.001 0.02 0.013 -4.375 5 66 5
C1=nNaOH/V1=0.1*Vtb1/0.005=0.1*8.6167/0.005=0.1723
Tnh tng t cho nhng bnh khc
Dng phng php bnh phng cc tiu vit phng trnh cc ng
biu din :
- V th ln lnC suy ra hng s k, 1/n
T th trn ta suy ra :
1/n= 0.955
ln k= -3.035
k= 0.048075
- V th C / theo C suy ra k,
1/T = 10.86
T =0.09208
k =10.86*1/17.09=0.635459
So = . N . Ao ( m2/g)=0.09208*6.023*10^23*20.5=1.13694E+24(m2/g)
Vi : = 0.09208
Ao = 20.5
N s Avogadro = 6,023.10^23
Nhn xt: biu th ln theo lnC c chnh xc cao hn ( R2=0.9998) V th ng
ng nhit Freundlich ph hp hn. Vy phng trnh ph hp vi qu trnh hp ph
acid acetic bng than hot tnh l phng trnh ln T theo lnC.
BI S 3
TNH TAN HN CH CA CHT LNG
NHM: 3 Th 3, ngy 05, thng 04, nm 2016
Mao c Huy.
Nguyn Duy Khnh.
Tm tt:
I. Gii thiu.
Cht/ bnh. 1 2 3 4
Nc (ml) 9 7.5 6 4
Axit axetic (ml) 1 2.5 4 6
IV. KT LUN.