TRNG I HC K THUT CNG NGH TP H CH MINH

Khoa Mi trng v Cng ngh sinh hc

BI GING
HNG DN TH NGHIM
ThS. V Hng Thi
Dng cho sinh vin ngnh Mi trng v Cng ngh sinh hc
Nm xut bn: 2009
GV: V Hng Thi 2
MC LC
Trang
LI NI U 5
BUI TH NGHIM 1 6
BI M U 6
A. Vn ly mu v chun b mu trc khi nh lng 7
B. Vn biu din s liu trong Ha phn tch 8
BI CHUN B 11
I. Mc ch 11
II. Ni dung 11
II.1. Mt s iu cn lu khi tin hnh phn tch nh lng 11
II.1.1. Chun b th nghim 11
II.1.2. Tin hnh th nghim 11
II.2. Ch khi thao tc vi cc dng c o chnh xc trong
Ha phn tch nh lng 11
II.2.1. Cn phn tch 12
II.2.2. Dng c o th tch 13
II.3. Cch x l s liu v biu din kt qu phn tch 15
II.3.1. Khi nim v sai s ca php o 16
II.3.2. Trnh t nh gi sai s 17
II.3.3. Ch s c ngha v cch ghi kt qu phn tch 18
II.4. Cch pha cc dung dch chun 19
II.4.1. Cht gc 19
II.4.2. Pha dung dch long t dung dch c 20
Cu hi cui bui 20
BUI TH NGHIM 2 22
PHNG PHP PHN TCH HA HC
(PHNG PHP PHN TCH KHI LNG) 22
I. Mc ch 22
II. Ni dung 22
GV: V Hng Thi 3
III. Thc hnh: Xc nh hm lng nc kt tinh trong BaCl
2
.2H
2
O 22
PHNG PHP PHN TCH HA HC
(PHNG PHP PHN TCH TH TCH) 23
I. Mc ch 23
II. Ni dung 23
III. Mt s thao tc cn ch khi tin hnh phn ng chun 24
IV. Thc hnh: Chun dung dch NaOH bng dung dch HCl 25
V. Cu hi ca bi thc hnh 26
BUI TH NGHIM 3 27
PHNG PHP PHN TCH HA HC
(PHNG PHP PHN TCH TH TCH tip theo) 27
I. Thc hnh: Chun oxy ha kh dng KMnO
4
27
II. Thc hnh: Chun to phc vi Complexon 28
III. Thc hnh: Chun to ta theo phng php Volhard 29
IV. Cu hi ca bi thc hnh 31
BUI TH NGHIM 4
PHNG PHP PHN TCH CNG C
(PHNG PHP PHN TCH IN)
Phng php phn tch o in th - Chun in th 32
I. Mc ch 32
II. Ni dung 32
III. Thc hnh: Chun dung dch Na
2
CO
3
bng dung dch HCl 33
theo phng php in th
IV. Cu hi ca bi thc hnh 34
BUI TH NGHIM 5
PHNG PHP PHN TCH CNG C
(PHNG PHP PHN TCH QUANG
Phng php ph hp thu phn t vng sng UV-VIS) 35
I. Mc ch 35
GV: V Hng Thi 4
II. Ni dung 35
III. Thc hnh: Xc nh nng ca SiO
3
2-
ha tan trong
mu nc bng phng php ng chun 37
IV. Cu hi ca bi thc hnh 38
PH LC 39
I. Phng php bnh phng cc tiu trong xc nh cc
h s ca ng hi quy 39
II. Phng php ni suy s liu t kt qu chun in th 41
TI LIU THAM KHO 43
GV: V Hng Thi 5
LI NI U
Trong h thng cc mn hc ca sinh vin Khoa Mi trng v Cng ngh sinh
hc ni chung, Ha phn tch l mt mn hc bt buc trong cc nm u tin. i
vi sinh vin ca c hai ngnh Mi trng cng nh Cng ngh sinh hc, Ha
Phn tch l mn hc c s quan trng, lm tin cho cc mn chuyn ngnh
nh Ha k thut Mi trng (i vi ngnh Mi trng), Phn tch v nh gi
cht lng thc phm (i vi ngnh Cng ngh sinh hc) v mt s mn hc
khc sau ny.
Ha hc phn tch vn c xem l mn khoa hc thc nghim, v th c th
nm vng v pht trin cc kin thc ha hc ng dng trong phn tch xc nh
thnh phn cc mu cht th cn phi tin hnh cc th nghim vi cc k nng
thc hnh cn bn cn thit c rn luyn tng bc trong phng th nghim.
Vi mc tiu trn, gio trnh Hng dn th nghim Ha Phn tch c son
ra nhm gip cc sinh vin khoa Mi trng v Cng ngh sinh hc i hc k
thut cng ngh TpHCM - hiu v nm chc cc kin thc l thuyt cng nh thc
hnh ca mn Ha Phn tch. Bi u tin ca gio trnh cng c li mt s kin
thc s dng thng xuyn trong Ha phn tch, c bit l khi nim v Nng
ng lng v trnh t nh gi sai s ca dy kt qu th nghim l nhng vn
sinh vin hay nhm ln. Bn bi tip theo ln lt gii thiu cho sinh vin cc v
d tiu biu v ng dng c th ca phng php phn tch ha hc (bao gm
phng php khi lng v phng php th tch) cng nh phng php phn
tch cng c (bao gm phng php o in th v phng php ph hp thu
phn t vng sng UV-VIS). l cc phng php phn tch c bn m sinh vin
ca Khoa Mi trng v Cng ngh sinh hc c hc trong mn Ha phn
tch trn ging ng. Cc bi th nghim c sp xp vi mc phc tp tng
dn nhm rn luyn k nng thao tc th nghim, ng thi chng li c thit k
mt cch tng i c lp cho php linh hot nht nh khi dy v hc cc bi
trn.
Xin chn thnh cm n cc ng nghip trong Khoa gp v hiu nh cc sai
st cho gio trnh. Tc gi mong rng s tip tc nhn c kin ng gp
gio trnh c hon chnh v ph hp hn. Mi kin ng gp xin vui lng gi
cho tc gi theo a ch vohongthi@yahoo.com.
Tc gi
GV: V Hng Thi 6
BUI TH NGHIM 1
BI M U
Nhim v c bn ca Ha hc phn tch ngy nay l phn tch nh tnh, nh lng, xc
nh cu trc, tch, phn chia lm sch i vi phn ng dng ca Ha phn tch trong
ngnh Mi trng cng nh ngnh Cng ngh sinh hc ni ring, phn tch nh lng
ng vai tr ch yu. Phn tch nh lng c nhim v xc nh hm lng mt cht,
thng l trong mt hn hp v th rn hay th ha tan trong cc dung dch.
Trc khi tin hnh phn tch nh lng, phi bit thnh phn nh tnh ca i tng
phn tch. Ni chung, i vi cc mu cn phn tch trong ngnh mi trng hay trong
ngnh cng ngh sinh hc, mc tiu t ra l phi xc nh c c th mt cht hay mt
cu t no cn c bit vi hm lng hin din trong mu l bao nhiu. Cng tc
phn tch nh tnh thng c kt hp vi cng tc phn tch nh lng, cng vi cc
thng tin thu thp c c lin quan d on s hin din ca cc cu t trong mu.
V vy trong gii hn ca gio trnh ny, thut ng Ha phn tch c hiu ng nht
vi thut ng Ha phn tch nh lng.
C th phn chia cc phng php phn tch nh lng thnh 2 loi: cc phng php
ha hc v cc phng php ha l v vt l (hay cng c hoc dng c).
- Cc phng php ha hc: ch yu da trn vic p dng cc phn ng ha hc c
lin quan n cu t phn tch. Phng php ny c t lu, n gin v d ng
dng mi ni m s chnh xc ch t ti mc nht nh ph thuc vo phn ng
ha hc. Cc phng php ha hc gm:
+ Phng php phn tch khi lng: tch cu t cn xc nh ra khi hn hp vi
cc cu t khc trong mu mt cch gin tip hay trc tip. Da vo khi lng
ca hp cht mi (to thnh sau) v khi lng ca mu ban u m tnh ra hm
lng cu t cn phn tch.
+ Phng php phn tch th tch: cn c vo th tch thuc th tc dng va
ht vi cht cn xc nh m tnh ra hm lng cht cn nh lng.
Hin nay, cc phng php ha hc vn c s dng rt rng ri v ph bin. Cc
phng php ny cn c tn gi l cc phng php kinh in.
- Cc phng php vt l v ha l (phng php cng c, phng php dng
c): da trn vic o mt tnh cht vt l no ( hp thu nh sng, dn in,
kh nng dn nhit) ca i tng cn phn tch trong mu. Tnh cht ny l mt
hm s ca nng cu t cn xc nh, t cn c vo kt qu o suy ra
hm lng cht cn nh lng. Hu ht cc phng php vt l v ha l u l
cc phng php i hi dng my o ngoi cc dng c thng thng nn n cn
c gi di tn khc rt thng gp trong cc gio trnh v Ha hc phn tch l
cc phng php dng c hay cng c. Trong thi gian gn y, cc phng php
vt l v ha l pht trin mnh nh cc u im nh nhy cao, tc phn
GV: V Hng Thi 7
tch nhanh, c th phn tch vi lng mu rt nh (dng vt). Tuy vy, n cng c
mt s nhc im nh phi dng mu chun, cng tc tin x l trc khi o c i
khi kh phc tp... V vy, cc phng php ha hc vn ng vai tr quan trng v
cn thit trong phn tch hin i, v ty theo tng trng hp c th la chn
phng php phn tch ph hp.
Cc bc ca qu trnh phn tch mu bt k bao gm:
- Chn mu i din, lm sao ch vi mt phn nh mu m c th i din cho ton
b i tng phn tch.
- Chuyn cht cn phn tch vo dung dch: khi tin hnh phn tch bng phng
php ha hc cn ha tan hon ton mu trong dung mi thch hp v tin hnh phn
tch trong dung dch. Khi s dng phng php vt l c th khng cn ha tan mu
nhng phi c mt s ng tc x l ha hc trc.
- Tin hnh phn tch bng phng php ha hc hay ha l. Vic che hay loi b cc
cu t cn tr khi phn tch cu t chnh (nu cn) bng cc phng php ha hc,
ha l v vt l c th c thc hin trc hay ng thi vi qu trnh phn tch.
- Ghi nhn kt qu ca php phn tch: o th tch thuc th dng khi phn ng
hoc ghi nhn kt qu tn hiu trn my o.
- Tnh ton kt qu phn tch bao gm nh gi kt qu v chnh xc ca kt qu
phn tch.
A. VN LY MU V CHUN B MU TRC KHI NH LNG
Cc bc ly mu v chun b mu thng hay b xem nh hn tm quan trng ca n.
Thc t th kt qu phn tch ch c ngha khi mu th nghim mang tnh i din cho
qun th v trc khi phn tch, mu phi c x l v dng thch hp. Theo kho st,
c n 70% cc trng hp b sai lch trong kt qu phn tch bt ngun t khu ly mu
v chun b mu.
1. Khi nim mt s loi mu thng dng:
- Mu ring: c chn ngu nhin, thng t cc v tr khc nhau hoc t cc bao gi
ring l khc nhau.
- Mu chung hay mu t hp: cc mu ring c nhp chung li vi nhau to thnh
mu t hp.
- Mu trung bnh th nghim: mu chung c nghin nh n mn thch hp hay
ha trn tht u, sau ly ra mt phn lm mu th nghim. Mu trung bnh th
nghim c chia thnh 2 phn bng nhau: phn em phn tch ( thc hin 3 th
nghim), v phn lu li ti PTN c th kim tra li khi cn.
2. Mt s ch khi chun b mu:
a s cc trng hp i hi phi ha tan chuyn mu dng rn thnh dng dung
dch c nng xc nh trc khi phn tch. Cng c trng hp d mu trng
GV: V Hng Thi 8
thi lng nhng vn cn phi x l mu trc khi tin hnh phn tch, v d phn tch
mt s kim loi bng phng php ph hp th nguyn t AAS, phn tch ch tiu nhu
cu oxy ha hc (COD) trong nc thi
- Khi ha tan x l mu, khng c lm mt mu v khng a thm qu nhiu
cu t vo mu s gy nh hng n kt qu phn tch.
- Dung mi v ha cht c la chn ha tan mu thng theo th t: nc
ct axit mnh baz mnh cht oxy ha mnh. Vi mi cu t cn xc nh
trong i tng mu nht nh c th i hi cch thc chun b mu ring, do
cn tra cu ti liu tm c th tc chun b mu ph hp.
- Cc phng thc chun b mu thng c p dng hin nay gm:
+ V c ha mu: ha tan mu trong mt axit hay hn hp nhiu axit (nh HCl,
HNO
3
+ HCl, HNO
3
+ HClO
4
+ HF..)
+ Tro ha mu: nung mu 550
o
C ri ha tan tro thu c trong axit.
+ Phn hy mu bng vi sng trong thit b vi sng: nhanh, an ton v ph hp
vi cc cu t d bay hi.
B. VN BIU DIN S LIU TRONG HA PHN TCH
1. Biu din ha hc:
Ngi ta thng biu din cu t phn tch theo dng tn ti ca n trong cht phn tch.
V d, Nit thng c biu din di cc dng NO
3
-
, NO
2
-
, NH
3
, NH
4
+
, cc mui
thng c biu din di dng ion nh K
+
, SO
4
2-
, cc ion kim loi trong cc hp
cht khc nhau thng c biu din di dng tng nh tng Fe, tng Mn
2. Biu din s hc:
Hm lng cu t c trong mu thng c biu din di dng hm lng %, hm
lng phn triu (mg/l hay ppm), hm lng phn t (g/l hay ppb).
3. Biu din nng trong phn tch nh lng:
a) Nng % (C%): khi lng cht tan c trong 100g dung dch.
b) Nng khi lng trn th tch (C g/l): khi lng cht tan trong 1 n v th tch
dung dch (g/l, mg/l).
c) Nng mol (C
M
hay mol/l): s mol cht tan trong 1 L dung dch.
d) Nng phn triu (ppm = part per million) v nng phn t (ppb = part per billion):
khi lng cht tan cha trong 10
6
ln (i vi ppm) v 10
9
ln (i vi ppb) khi
lng mu c cng n v. Hai loi nng ny c s dng rt ph bin trong k
thut o lng nng cc cht gy nhim mi trng hay mt s c cht hin
din trong thc phm.
+ 1ppm = 1mg/10
6
mg = 1mg/kg = 1g/10
6
g = 1g/1000kg
GV: V Hng Thi 9
+ 1ppb = 1mg/10
9
mg = 1mg/10
3
kg = 1g/kg
Do cc loi nc thin nhin v nc thi c khi lng ring ~ 1(kg/l), do vy mt
cch gn ng th:
1ppm = 1mg/10
6
mg = 1mg/kg ~ 1mg/l
1ppm = 1g/10
6
g = 1g/1000kg ~ 1g/m
3
1ppb = 1g/kg ~ 1g/l = 1mg/m
3
e) Nng ng lng (C
N
hay N): l s ng lng gam (s ) hay s ng
lng (s ) cht tan trong 1 L dung dch (hay s mili ng lng gam / s mili
ng ng cht tan trong 1L/1ml dung dch). Loi nng ny c s dng ph
bin nht trong Ha phn tch nh lng.
A
N

a
C =
A
l khi lng ng lng ca cht A (mt s ti liu gi l
ng lng gam hay mol ng lng ca cht A)
a l s g ca cht tan A trong 1L dung dch
Sinh vin cn xem li trong phn l thuyt cc khi nim: ng lng, khi lng
ng lng (hay ng lng gam/mol ng lng) v nng ng lng
phn bit r. Xem li cch tnh khi lng ng lng (hay ng lng gam/mol
ng lng) ca cht trong cc phn ng khc nhau.
- Quy tc ng lng: trong mt phn ng ha hc tng s ng lng ca cc
cht phn ng phi bng nhau:
mA + nB = pC + qD
s
A
= s
B
= s
C
= s
D
Quy tc ny c s dng rng ri tnh ton kt qu trong cc php phn tch th
tch. tm s ng lng, c th:
+ Nhn nng ng lng vi th tch dung dch ha cht tiu th.
(C
N
)
A
.V
A
= (C
N
)
B
.V
B
+ Chia s g cht phn ng cho khi lng ng lng ca cht.
A
A

a
=
B
B

a
Suy ra (C
N
)
B
.V
B
=
A
A

a
hay (C
N
)
A
.V
A
=
B
B

a
Trong (C
N
)
A
v (C
N
)
B
l nng ng lng ca A v B.
V
A
v V
B
l th tch A v B tham gia phn ng (l).
a
A
v a
B
l s g ca A v B tham gia phn ng (g).
Ch : Nu V tnh theo ml th C
N
.V chnh l s mili ng lng = s ng
GV: V Hng Thi 10
lng/1000. Tng t, nu a tnh theo mg th a
A
/
A
= s mili ng lng.
- Mi quan h gia cc loi nng :
d
l g C
C
. 10
) / (
(%) =
M
l g C
C
M
) / (
= =
M
l mg C 1000 ). / (
M N
C n C . = (n l s mol ion hay nguyn t Hydro, s ion ha tr 1, s
electron c cung cp hay kt hp vi 1 mol cht. Mt s ti
liu cn gi n l h s ng lng v c th k hiu bng
ch z)
M
d C
C
M
10 . (%).
= (M l khi lng phn t ca cht)
(d l khi lng ring ca dung dch c nng %)

d C
C
N
10 . (%).
= ( l khi lng ng lng (ng lng gam) ca cht)
GV: V Hng Thi 11
BI CHUN B
I. Mc ch:
- Mt s iu cn bit khi tin hnh phn tch nh lng.
- Nm c mt s ch khi thao tc vi cc dng c o chnh xc trong Ha phn tch
nh lng.
- Cch x l s liu v biu din kt qu phn tch.
- Cch pha ch cc dung dch chun.
II. Ni dung:
II.1. Mt s iu cn bit khi tin hnh phn tch nh lng
II.1.1. Chun b th nghim
Mt th nghim phn tch nh lng thng bao gm nhiu giai on. Nu mi giai
on th nghim u c tin hnh cn thn, ng nguyn tc th kt qu cui cng
mi c th chnh xc.
Bi vy sinh vin phi chun b tht k trc khi lm th nghim:
- Nm vng c s l thuyt ca th nghim, hiu thu o ngha ca tng thao tc
th nghim.
- Nm vng cch s dng cc dng c th nghim, cch pha ch, chun b cc ha
cht cn thit.
- Trnh t th nghim.
- Cch ghi chp v tnh ton kt qu th nghim.
II.1.2. Tin hnh th nghim
Mun tin hnh th nghim c kt qu tt trong thi gian nh sn, khng lng ph ha
cht, lm h hng dng c, thit b, sinh vin cn ch mt s qui tc sau:
- Sp xp ch lm vic
Ch lm vic phi sch s, kh ro, cc dng c phi b tr thun tin
cho vic s dng, trnh xy ra va chm, v..
- Chun b dng c, thit b
Cc dng c thy tinh, s phi bo m sch s trc khi dng, cn kim tra
dng c thit b trc khi dng v bn giao y cho phng th nghim sau khi
hon thnh th nghim.
- Ghi chp
Mi hin tng, s liu trong khi th nghim u phi ghi vo s th nghim, khng
ghi vo mnh giy ri hoc ghi ln bn.
II.2. Ch khi thao tc vi cc dng c o chnh xc trong Ha phn tch nh lng
GV: V Hng Thi 12
II.2.1. Cn phn tch:
Trong cc PTN phn tch ha hc hin nay u s dng ph bin loi cn phn tch
in t. l thit b chnh xc, t tin v d hng. Trong PTN ca Khoa Mi trng
v CNSH, loi cn phn tch ang s dng cng l cn in t vi thng s k thut
nh sau:
- Trng lng ti a: 220g.
- chnh xc: 0,0001g.
Nguyn l hot ng ca cn in t:
Vt cn ko a
cn xung vi lc
F = m.g vi m l
khi lng ca vt
cn; g l gia tc
trng trng. Cn
in t s dng
mt lc phn hi
in t ko a
cn v v tr ban
u ca n. Khi t
vt cn vo a
cn, do khi lng ca vt cn ko a cn xung, iu s c detector pht
hin v gi tn hiu n b chnh dng, dng phn hi c sinh ra a ti ng
c tr. Dng in cn thit sinh ra lc phn hi t l vi khi lng ca vt v
c hin th trn mn hnh hin s.
Mt s nguyn tc c bn khi cn:
- Trc mi ln cn cn kim tra li trng thi ca cn. Dng vi mm lau sch bi
a cn.
- Tuyt i khng chm vo cn khi ang cn.
GV: V Hng Thi 13
- Quan st bng nc xem cn thng bng cha, nu cha sinh vin khng
c t chnh m bo cho cn b PTN bit.
- Tuyt i khng cn vt nng hn trng lng ti a cho php ca cn. Nu nghi ng
th cn cn trc vt cn trn cn k thut. Thc t ch nn cn mc tng khi
lng ca b ng v ha cht < 150g.
- Khng ha cht trc tip ln a cn m phi cn thng qua vt cha nh giy cn,
becse
- Nu nh ri ha cht ln a cn phi lau sch ngay.
- S thay i khi lng ca ha cht v b ng trong thi gian cn hay dn n sai s
khi cn, thng l do ha cht (cc ha cht rn dng bt ni chung ht m mnh) v
b ng b ht m (nh dng c thy tinh). V vy cn thao tc thi gian cn ch ko
di trong vi pht. Mt s ha cht nu dng lm cht chun cn c sy kh trc
khi cn.
- Sai s do chnh lch nhit gia cn v vt cn: Nu nhit vt cn cao hn nhit
cn th khi lng ca n s thp hn khi lng thc. V vy trc khi cn cn
lm ngui vt cn (tt nht l trong bnh ht m) cn bng vi nhit phng. Thi
gian lm ngui ph thuc nhit vt cn, kch thc v cht liu vt cn.
- Khi cn khng hot ng, tt nht nn m 2 ca 2 bn cn cn bng nhit gia
cn v nhit phng. Nhng khi cn, phi ng ht cc ca cn trc khi c kt
qu.
- Cch c kt qu: ghi ngay kt qu khi s hin trn cn va n nh.
- Khng c dng tay m phi dng gp kp vt cn t ln a cn.
- trnh nhm ln, tt nht khng ni chuyn trong khi cn.
II.2.2. Dng c o th tch:
- Nhn chung, cc dng c o th tch s dng trong phng th nghim u c ch
to t cc loi thy tinh khc nhau. Loi dng c lm t cht do c chnh xc km
hn v thng ch c s dng ti hin trng (on-site).
- Cc dng c o th tch u c chia thnh 2 loi: TC (To contain) hay In v TD (To
deliver) hay Ex.
+ Loi TC hay In (k hiu ny thng c ghi trn thn dng c): cc dng c c
ghi TC 20
o
C c ngha l dng c c nh chun (calibration) cha
chnh xc mt th tch ng vi ton phn cha trong dng c 20
o
C. Th tch m
dng c c kh nng cha c bao gm c lng ha cht s dnh bm ln dng
c nu trt lng ha cht trong dng c sang dng c khc.
Cc loi dng c TC cng thng p dng vi bnh nh mc, becse v erlen.
+ Loi TD hay Ex (k hiu ny thng c ghi trn thn dng c): cc dng c c
ghi TD 20
o
C c ngha l dng c c nh chun (calibration) dung tch
ca dng c ch ng vi phn dung dch chy ra v khng k git cui. Lng ha
GV: V Hng Thi 14
cht cn dnh bm ln thnh dng c sau khi trt ha cht ra c tr ra v
khng c tnh vo th tch trt b. Cc loi dng c TD cng thng p dng
vi buret, pipet v ng ong.
- Bnh nh mc: thuc loi TC. Ch dng pha ch cc dung dch c
nng chnh xc. Khi thm nc ti vch phi quan st mc m mt
cng mt phng vi vch. Khng c ra bnh nh mc bng
dung dch nh lng hay thuc th nh buret v pipet. Khng rt
thng cc dung dch nng hay lnh vo bnh nh mc m phi ch n
khi ngui v nhit phng mi rt vo bnh nh mc.
Khi lm vic vi bnh nh mc cn trnh tip xc tay vo bu bnh, ch
cm tay vo phn trn c bnh, v nhit t tay s truyn vo thnh bnh
lm thay i dung tch bnh. Trc khi lm y bnh nh mc, phi t bnh v tr
bng phng v c chiu sng r.
- Pipet: thuc loi TD. Pipet gm 2 loi: pipet bu (pipet chnh xc) v pipet chia .
gim sai s, cc pipet u phi sch v khng dnh du m. Khi lm vic vi pipet,
khng c chm tay vo phn gia ca pipet v nhit t tay s lm thay i dung tch
ca pipet.
Khi chuyn cht lng sang bnh chun phi cho chy t t th cht lng mi
chy ht khi pipet. Nu cho chy nhanh, do lc chy ca cht lng m mt
phn ng k s cn li trong pipet. Pipet phi v tr thng ng khi chy.
+ Pipet bu (bulb pipet): l loi pipet o mt th tch chnh xc do pipet quy
nh. KHNG BAO GI thi hay dng lc tc ng ngoi trng lc nhm
a git cui u pipet bu ra ngoi, v th tch trong pipet bu c
nh chun khng bao gm git cui. Do nu pipet bu b nt u hay m
u, phi loi b v pipet b sai s. Do c th ca pipet bu nn khi
cn ly mt th tch mu th chnh xc bng pipet bu, nht thit phi trng
n bng chnh mu th ti thiu 1 ln.
+ Pipet chia vch (measuring pipet): l loi pipet ch cho chnh xc tng
i. Ch nu trn c pipet c ch BLOWOUT hay c vin knh nhm
rng khong 3-5mm hay c 2 vin mu xung quanh c th khi thao tc, cn
thi git cui. Ch khng ln ln gia vin knh nhm (frosted band) vi
mt di mu rng (cng trn c pipet) v di mu l code ca nh SX dng
c. Cc pipet khng c 1 trong 3 c im trn th khi thao tc, khng
dng bt c tc ng no ngoi trng lc. Thng thng, pipet chia vch
c dng ht ha cht trong cc phn ng phn tch. Trc khi ht
ha cht, vic trng pipet chia vch bng nc ct (l ) hay phi bng
chnh ha cht em ht l ty thuc vo phng php phn tch c th.
Nguyn tc chung l nu cn mt lng th tch chnh xc (v d trong
phn ng chun ngc hay chun th) th cn trng pipet bng ha cht
em ht. Ngc li, nu lng ha cht khng cn chnh xc cao (v d to mi
trng hay to phc mu) th c th trng pipet bng nc ct l .
GV: V Hng Thi 15
- Buret: thuc loi TD. Ch nu buret b nt u hay m u, phi loi b v b sai
s do mt tc dng kim sat tc chy. chnh xc ca buret cao hn pipet nn
nu phn tch yu cu chnh xc cao, khng bao gi s dng pipet chun .
Mi ln nh lng nht thit mc ngang ca dung dch trong buret bt u t s 0,
tc l lun ch dng 1 phn ca buret. Tng t nh pipet bu, nht thit phi trng
buret bng chnh dung dch dng chun trc khi cha y dung dch trong
buret.
c buret ng dung dch trong sut c buret ng dung dch khng trong sut
c 24,87ml c 25,62ml
Khi lm vic vi buret, phi kp buret vo v tr thng ng. Trc mi ln chun
phi dung dch chun vo buret ti vch 0 v ch lm y c phn cui v c
kha buret. Khi c ch s trn buret, mt phi v tr ngang vi vch li. C th
c theo phn cong xung hay cong ln ca mt cong dung dch, nhng tt c cc ln
c k c khi c vch 0 v khi c mc dung dch sau khi chun u phi
ging nhau.
Ra buret xong nn dng thng trn gi v ngm nc ct trong buret trnh b
thay i th tch do gin n. p ngc ng nghim ln u buret hn ch s bay
hi ca nc.
- Becse, bnh nn, ng ong ch cho mc th tch rt tng i v khng bao gi s
dng cc vt dng ny vi mc ch o th tch chnh xc. Sai s ca cc dng c ny
c th ln ti 10%.
- Khng sy kh (trong t sy) cc dng c buret, bnh nh mc v pipet chnh xc v
s gy sai s do thy tinh gin n. Ch kh t nhin nhit phng hoc dng
lung khng kh sch lm kh dng c.
II.3. Cch x l s liu v biu din kt qu phn tch
GV: V Hng Thi 16
II.3.1. Khi nim v sai s ca php o
D vic phn tch c cn thn n u th kt qu thu c vn khc vi gi tr tht, tc l
vn c sai s. Gi tr ca mt php phn tch c nh gi ng v lp li ca
kt qu thu c.
- ng, lp li v chnh xc:
+ ng: phn nh s ph hp gia kt qu thc nghim thu c x vi gi tr
thc ca i lng o.
+ lp li: phn nh s khc bit trong cc gi tr xc nh x
i
cng iu kin th
nghim. Mun bit 1 php xc nh c lp li th no phi thc hin nhiu ln
php xc nh .
+ chnh xc: biu din ng thi ng tt v lp li tt ca php xc nh.
V d, khi kim tra dung dch HCl c nng chnh xc 0,1000M, kt qu thu c
trong cc th nghim c lp nh sau:
A: 0,1002 ; 0,0999 ; 0,1004 ; 0,0996 ; 0,1003
B: 0,1014 ; 0,1017 ; 0,1016 ; 0,1015 ; 0,1014
Chui kt qu A ng nhng lp li khng tt. Ngc li, chui kt qu B c lp
li tt hn nhng ng li km.
- Phn bit sai s h thng v sai s ngu nhin:
+ Sai s h thng hay sai s xc nh:
- C th xc nh c.
- nh hng mt chiu trn ng ca php xc nh.
- Do nhng nguyn nhn c th bit c nh: dng c o (buret, pipet, bnh
nh mc, cn..) hay ha cht c nng sai.
- Phng php xc nh c khuyt im.
- Ngi phn tch c khuyt im v cch nhn mu
+ Sai s ngu nhin hay sai s khng xc nh:
- Khng th bit hay xc nh c.
- nh hng c th hin trn lp li ca php xc nh khng theo quy lut
no.
- Do nhng nguyn nhn khng c nh v khng d on c.
- Ch c th gim bng cch tng s ln xc nh.
+ Sai s th: sai s trn gi tr ca 1 ln xc nh, c th qu ln hay qu nh so vi
cc gi tr x
i
khc ca chui n ln xc nh.
nh gi sai s ca cc php o:
GV: V Hng Thi 17
Thng thng kt qu phn tch c sai s tng i trong khong 1% v khi nh
lng dng vt th sai s c th ln ti 10%. Vi yu cu sai s thng thng trong
vng 1%, c th tin hnh lp li php nh lng vi ln v sau khi loi b sai s th
i, nu kt qu gn ging nhau l c. Nu php nh lng yu cu sai s nh
(0,1%) th cn lp li php nh lng nhiu ln rt ra thng tin ti u t kt qu
thc nghim v cn x l kt qu theo thng k (tham kho chi tit trong cc sch l
thuyt ha hc phn tch).
II.3.2. Trnh t nh gi sai s:
nh gi sai s ca kt qu theo cch n gin:
S =
x
d
i
trong : n l s th nghim lp li
Gi tr trung bnh
n
x x ........ x x
n
x
x
n 1 n 2 1
n
1
i
+ + + +
= =

x x d
i i
= ;
n
d
d
i
i

=
- Nu S nm trong khong 0,01 (1%) th lp li coi nh t yu cu.
- Nu S > 1% th c th lp li php nh lng thu thm kt qu ng thi
c th loi b cc gi tr qu cao hay qu thp so vi cc gi tr khc. Kim tra
li S S nm trong gii hn sai s cho php.
- Kt qu phn tch S x =
nh gi sai s ca kt qu theo thng k (tham kho):
- Kim tra dy s liu loi b sai s th i: dng chun Q
1 n
1 n n
tn
x x
x x
Q

=

Nu Q
tn
> Q
lt
(tra cu trong sch l thuyt ha PT) th cn b gi tr x
n
v ngc
li.
- Tnh gi tr trung bnh
n
x x ........ x x
n
x
x
n 1 n 2 1
n
1
i
+ + + +
= =

- Tnh lch chun

1 n
) x x (
s
n
1
2
i

=

- Tra bng tm t
lt
ng vi xc sut tin cy P (trong Ha phn tch, thng s
dng P = 0,95) v s ln th nghim n.
GV: V Hng Thi 18
- Tnh bin gii tin cy c hay chnh l sai s =
n
s . t
o
- Kt qu phn tch c = x
II.3.3. Ch s c ngha v cch ghi kt qu phn tch:
Ch s c ngha
Kt qu ca mt pho o trc tip hay thao tc phn tch phi c ghi chp sao cho
ngi s dng s liu hiu c mc chnh xc ca php o. Khng phi c ly
nhiu s l l tt. Nguyn tc chung l s liu c ghi sao cho ch c ch s cui
cng l bt nh. V d cn phn tch c nhy 0,1mg th kt qu cn phi ghi
1,2516g m khng ghi 1,251g hay 1,25160g (cc s 1, 2, 5, 1 l tin cy v c th c
c trn cc qu cn hay bn cn, cn s 6 l bt nh (c lng) v c c c
tnh trn thang chia hay l s bin i lin tc trn mt cn in t). Cc s tin cy v
s bt nh u tin gi l ch s c ngha.
- S ch s c ngha c xc nh nh sau:
+ Tt c cc s khng phi l s 0 (zero) u l s c ngha
+ Cc s 0 nm gia cc s khng phi l s 0 l cc s c ngha. V d s 1,012
c 4 ch s c ngha; s 1,0034 c 5 ch s c ngha; s 10,24 c 4 ch s c
ngha.
+ Cc s 0 nm bn phi s khng phi s 0 v bn phi du thp phn l ch s c
ngha do nhng s 0 vit cui cng khng bao gi c loi i nu chng l
nhng ch s c ngha. V d s 1,0120 c 5 ch s c ngha.
+ Ngc li, cc s 0 trc s khng phi l s 0 l s KHNG C NGHA. V d
s 0,0034 c 2 ch s c ngha (s 3 v s 4); s 0,24 ch c 2 ch s c ngha
(s 2 v s 4).
- Thng thng th i vi cc s phc tp nh trn ngi ta thng chuyn sang dng
lu tha thp phn v cc ch s phn nguyn c tnh vo ch s c ngha. V d
s 0,00520 = 5,20.10
-3
c 3 ch s c ngha; s 10920 = 1,0920.10
4
c 5 ch s c
ngha (nhng nu vit 10920 = 1,092.10
4
li ch c 4 ch s c ngha). Chuyn sang
dng lu tha thp phn nh vy rt quan trng v khng lm thay i s ch s c
ngha khi i sang cc n v tnh khc nhau. V d s liu 2,4g c 2 ch s c ngha.
Nu i ra mg th phi vit thnh 2,4.10
3
mg (2 ch s c ngha) m khng vit
2400mg (4 ch s c ngha).
Gi li bao nhiu ch s trong kt qu cui khi thc hin cc php tnh?
Trong cc php tnh khng c lm trn s cc giai on tnh trung gian m ch
lm trn s kt qu cui cng.
- i vi cc php tnh cng v tr: ch gi li kt qu cui mt s ch s thp phn
ng bng s ch s thp phn ca s hng c s ch s thp phn t nht.
V d: 6,145 + 13,24 + 34,7 = 54,085
GV: V Hng Thi 19
Kt qu lm trn l 54,1 (gi li 1 ch s thp phn)
- i vi cc php tnh nhn v chia: gi li kt qu cui cng mt s ch s c ngha
bng ng s ch s c ngha ca tha s c s ch s c ngha t nht.
V d: 1,2 x 3,145 = 3,774 th ghi kt qu l 3,8 (gi li 2 s c ngha).
00496 , 0
845 , 76
246 , 0 . 55 , 1
= (gi li 3 s c ngha)
- Gi tr ca sai s ca kt qu phn tch (S hay c) cng phi c lm trn v ghi vi
cng s ch s phn thp phn nh ca kt qu o. VD = 0,68 0,03 (d trc
tnh c sai s l 0,025).
- i vi cc php o c trn my th gi tr o c coi l cc s liu o trc tip v
vn c p dng cc quy tc trn.
II.4. Cch pha cc dung dch chun
II.4.1. Cht gc
Dung dch chun, dung dch gc l dung dch c bn trong phn tch th tch, khi chun
da vo n xc nh hm lng cc cht trong cht phn tch. Vic pha ch mt
dung dch c nng chnh xc cn phi tun theo nhng quy tc c bit v tnh chnh
xc v cn thn nghim ngt khi lm vic. Cch thng thng pha ch dung dch
chun l t cht gc. Cc cht gc cn tha mn cc yu cu sau:
- Phi c tinh khit cao (tinh khit phn tch tkpt).
- Thnh phn ha hc ca cht tn ti trong thc t phi ng ng vi cng thc
dng tnh ton lng phi cn.
- Cc cht gc phi bn vng, khng ht m, khng tc dng vi khng kh, khng chy
khi cn, khi pha thnh dung dch nng ca n phi khng i theo thi gian.
- Phn t lng ca cht gc cng ln cng tt v nh th s lm gim c sai s khi
cn.
thun li hn khi pha ch cc dung dch chun trn th trng c bn sn mt s loi
ha cht thng dng c cha trong ng thy tinh hay ng cht do gi l fixanal hay
ng chun. Trn mi ng chun nh sn xut ghi r dung tch cn pha thu c
nng xc nh.
V d: ng chun ng H
2
SO
4
trn c ghi 0,1N c ngha khi pha vo bnh nh mc
loi 1000ml s thu c dung dch H
2
SO
4
c nng 0,1N (trong hnh trn, cc im 1
v 2 trn hnh v l cc im phi chc thng bng a thy tinh chuyn dung dch
bn trong ng chun bng thu tinh vo bnh nh mc. Nu l ng chun bng cht do
th n gin ch vic ct mt u ng ri trt b dung dch trong ng vo bnh nh mc).
ng chun bng thu tinh
GV: V Hng Thi 20
II.4.2. Pha dung dch long t dung dch c
- Khi nng c biu th bng nng M, N
C
1
.V
1
= C
2
.V
2
V
2
= V
1
+ V
n
C
1
, C
2
: nng ca dung dch c v dung dch long ca cht cn pha.
V
1
, V
2
: th tch ca dung dch c v dung dch long.
V
n
: th tch nc cn phi thm vo V
1
ml dung dch nng C
1
c V
2
ml dung
dch nng C
2
.
- Khi nng c biu th bng nng %
C
1
.d
1
.V
1
= C
2
.d
2
.V
2
V
1
=
1 1
2 2 2
.
. .
d C
V d C
C
1
, C
2
; d
1
, d
2
; V
1
, V
2
: nng %, t trng v th tch dung dch c v dung dch long
cn pha.
- Quy tc ng cho pha dung dch
V d: Cn bao nhiu ml dung dch H
2
SO
4
96% v nc ct c dung dch
H
2
SO
4
30%?
Nh vy nu trn 30 gam dung dch H
2
SO
4
96% vi 66 gam nc ta s c dung dch
H
2
SO
4
30%.
Cu hi cui bui:
1. Phn bit cc loi nng v mi quan h gia chng.
2. Phn bit cc khi nim: mol, khi lng mol, nng mol, ng lng, khi lng
ng lng, nng ng lng.
3. Tnh h s ng lng n v khi lng ng lng ca cc cht (in nghing v
gch chn) trong cc phn ng sau:
a) Pb(NO
3
)
2
+ H
2
SO
4
PbSO
4
+ + HNO
3
b) Fe
2
(SO
4
)
3
+ Zn FeSO
4
+ ZnSO
4
c) KMnO
4
+ FeSO
4
+ H
2
SO
4
MnSO
4
+ Fe
2
(SO
4
)
3
d) H
3
PO
4
+ NH
3
(NH
4
)
2
HPO
4
4. Kt qu ca 4 php chun c lp nh sau:
C
HCl
(mol/l): 1,02 ; 1,04 ; 1,01 ; 1,06 ; 1,02
Tnh gi tr trung bnh v nh gi n gin sai s ca kt qu thu c.
5. Biu din cc kt qu sau (vit ng cc ch s c ngha):
GV: V Hng Thi 21
a) x =
3 , 1 . 15 , 22
00541 , 0 . 972 , 1
b) y = 1564 , 72 319 , 0 75 , 154 +
6. Cn ly bao nhiu ml dung dch HCl 12M c 250ml dung dch HCl 0,1M?
7. Cn bao nhiu ml dung dch H
2
SO
4
98% (d=1,84) pha 1lt dung dch H
2
SO
4
5%
(d=1,00)?
GV: V Hng Thi 22
BUI TH NGHIM 2
PHNG PHP PHN TCH HA HC
PHNG PHP PHN TCH KHI LNG
I. Mc ch:
- Nm c cc nguyn tc v thao tc c bn trong phng php phn tch khi
lng.
- Thc hnh phng php: lm bay hi nc ca mu ha cht m.
II. Ni dung:
- nh lng cu t X theo phng php phn tch khi lng, cn tch X ra di
dng nguyn cht, sau bng cch cn s suy ra hm lng ca X trong mu.
III. Thc hnh:
III.1. Xc nh hm lng nc kt tinh trong BaCl
2
.2H
2
O
a) Nguyn tc:
Cc tinh th BaCl
2
ngm nc nm cn bng vi hi nc theo cc qu trnh sau:
BaCl
2
. 2H
2
O BaCl
2
. H
2
O + H
2
O (hi)
BaCl
2
. H
2
O BaCl
2
+ H
2
O (hi)
Nghin cu cho thy c th dng nhit ui hon ton lng nc trong mui
BaCl
2
.2H
2
O bng cch sy mu mui 130
o
C. So snh khi lng mu trc v sau
khi sy tnh hm lng % nc kt tinh trong mui.
b) Ha cht, dng c:
- Mui BaCl
2
.2H
2
O
- L cn c np
c) Cch tin hnh:
- Trc khi thc hin th nghim, nht thit sinh vin phi nm vng cc ch
khi s dng cn phn tch (bui th nghim 1).
- Ra sch l cn. t l cn vo t sy 1302
o
C. Sau khi l cn kh, a l
cn vo bnh ht m. Sau khong 30 pht, l cn ngui th em cn chnh xc khi
lng l cn (khng cn np), gi l G
o
.
- Ly mt lng mui BaCl
2
.2H
2
O khong 3g v trt cn thn vo l cn xc nh
khi lng trn. Cn chnh xc l cn v mui (khng cn np), gi l G
1
.
- y np l cn v t l cn + np vo t sy, em sy 1302
o
C trong vng 1
gi. Sau , ly l cn ra, m np ri t l cn vo bnh ht m. Sau khi ngui
30 pht, cn chnh xc li l cn (khng cn np), gi l G
2
.
Ghi li kt qu phn tch vo bng sau (thc hin lp li th nghim 3 ln nhng tin
GV: V Hng Thi 23
hnh cng lc):
Kt qu cn (mg)
Vt cn
Ln 1 Ln 2 Ln 3
1. L cn - G
o
2. L cn + BaCl
2
.2H
2
O - G
1
3. L cn + BaCl
2
- G
2
d) Tnh ton kt qu phn tch:
- T cc s liu c v G
o
, G
1
v G
2
, sinh vin t lp cng thc tnh ton hm
lng nc kt tinh trong mu.
PHNG PHP PHN TCH HA HC
PHNG PHP PHN TCH TH TCH
I. Mc ch:
- Nm c cc nguyn tc v thao tc c bn trong phng php phn tch th tch.
- Thc hnh phng php: chun acid-base, chun oxy ha kh, chun to
phc, chun kt ta.
- Sinh vin p dng c kin thc l thuyt hc trn lp vo thc t, c th t lp
cng thc tnh ton hm lng cht cn xc nh theo cc phng php chun v
k thut nh lng khc nhau.
II. Ni dung:
aA + bB cC + dD
Nu cho B phn ng va ht vi V
A
(ml) dung dch A, ti im tng ng trong dung
dch khng cn d A hay B, v khi c th tnh c nng cht A nu bit nng
cht B l C
B
(N) v th tch cht B dng trong phn ng l V
B
(ml):
V
B
.C
B
= V
A
.C
A
Rt ra: C
A
=
A
B B
V
C V .
(N)
im ngng chun (c coi gn ng l im tng ng) l im m ti , cht
ch th i mu (phng php ha hc). Cch xc nh im tng ng bng dng c
(chun in th) s c gii thiu bui th nghim 4.
- Cc phng php chun da trn bn cht phn ng: trung ha; oxy ha kh; kt
ta v to phc.
GV: V Hng Thi 24
- Cc phng php chun da trn k thut nh lng: chun trc tip, chun
ngc, chun th. Trong cc phng php th chun trc tip l gim thiu
c sai s nht.
- Mi php chun cn lp li ti thiu 3 ln, vi cc kt qu chun gia cc ln
ch sai khc nhau ti a l 1%.
- Thc hnh phng php phn tch th tch trn 4 mu vi 4 phng php khc nhau:
+ Chun acid mnh bng base mnh
+ Chun oxy ha kh
+ Chun to phc
+ Chun to ta
III. Mt s thao tc cn ch khi tin hnh phn ng chun
Cc phn ng c s dng trong Ha phn tch, bao gm c cc phn ng chun ,
c tin hnh vi mc tiu cui cng l nh lng chnh xc nng cht trong
mu. V vy, tt c cc thao tc trong ton b qu trnh chun b cng nh lc chun ,
u phi c tin hnh rt cn thn, chnh xc gim thiu cc sai s do thao tc
khng chun pht sinh.
III.1. Tt c cc ha cht cn thit cho phn ng chun u c cha trong chai.
Tuyt i KHNG dng pipet ht trc tip ha cht t chai. Phi trt ha cht t
chai vo becse 100ml v rt tng lng nh trnh nhim bn ha cht (s dng
ti u trt ha cht ra becse ti ), sau mi dng pipet ht ha cht ln t
becse s dng. Ch : quy nh 1 becse v 1 pipet dng cho 1 loi ha
cht nht nh, KHNG c dng 1 dng c cho nhiu loi ha cht.
III.2. Phi trng ra buret bng chnh loi ha cht dng chun (ch thao tc
trng ra ging vin lm mu) trc khi cn mc ha cht trong buret. Ha cht
dng chun phi c rt ra becse 100ml sch v kh t chai cha, nu
becse cn dnh nc bn trong th phi trng li bec se bng ha cht chun
. Tng t, phi trng ra pipet dng ht ha cht trc khi ht ha cht
(ch thao tc trng ra ging vin lm mu).
III.3. Ha cht cn d li trong becse KHNG c trt b li vo chai ha cht m
GV: V Hng Thi 25
phi b. V lng ha cht l gii hn, khi s dng phi tit kim tin
hnh phn ng chun (k c phn ng lp li).
III.4. Khi chun , lc u c bnh nn (erlen) theo 1 hng, trnh mu vng ln
thnh dng c.
III.5. Sau khi kt thc chun , b phn ha cht cn d li trong buret. Trng li
buret bng nc ct t nht 2 ln, cha y nc ct trong buret v treo ln gi .
IV.Thc hnh: Chun dung dch NaOH bng dung dch HCl
a) Nguyn tc:
- Phn ng chun : H
+
+ OH
-
H
2
O
- Cn bng ch th mu: HInd H
+
+ Ind
-
Hng s phn ly K
HInd
=
] [
] ].[ [
HInd
Ind H
+
Nh vy, nng H
+
hay pH thay i khin t l [Ind
-
]/[HInd] thay i. Ty theo pH m nng dng Ind
-
hay HInd chim u th, quyt nh n mu sc c th
nhn bit, v mu ca dng Ind
-
khc vi mu dng
HInd. Ni cch khc, trong qu trnh chun , pH hn
hp dung dch thay i v s thay i ny c th nhn bit bng ch th mu.
Nghin cu cho thy: pH
chuyn mu
= pK
HInd
1.
Ti im tng ng: [OH
-
] = [H
+
] => pH
t
= 7.
- Ch th ti im tng ng hay ln cn tng ng: y l phn ng trung ha
base mnh bng acid mnh nn bc nhy ca ng chun kh di (t pH = 4
n 10). Do , v nguyn tc c th chn tt c cc cht ch th c kh nng chuyn
mu trong khong pH ny. 3 ch th thng dng bao gm:
+ Methyl da cam: t (dng acid) qua vng (dng base), im i mu ng vi pH
= 3,1 4,4.
+ Phenolphtalein: t khng mu (dng acid) qua hng (dng base), im i mu
ng vi pH = 8,0 9,8.
+ Bromothimol xanh: t vng (dng acid) qua xanh (dng base), im i mu ng
vi pH = 6,2 7,6.
Sinh vin nn xem li kin thc v nguyn tc chn cht ch th khi chun acid
mnh bng base mnh cc ngng nng khc nhau.
- V k thut nh lng: phn ng ny thuc loi chun trc tip.
- Ch : Khi thm dn H
2
SO
4
vo dung dch, lc u pH thay i chm nhng gn im
tng ng thay i rt nhanh nn cn chun chm lc mu sc c du hiu thay
i.
H
2
SO
4
GV: V Hng Thi 26
b) Ha cht
- Dung dch chun H
2
SO
4
0,1N.
- Ch th metyl da cam 0.1%/nc.
- Dung dch mu NaOH cha bit nng
c) Cch tin hnh:
- Buret: cha dung dch H
2
SO
4
0,1N.
- Erlen (bnh nn): Ht 10 ml dung dch NaOH cn xc nh nng , thm 3 git ch
th metyl da cam.
- Tin hnh chun bng cch nh dn H
2
SO
4
xung bnh mu mu chuyn
dn t vng sang cam.
- Lp li thao tc chun 3 ln vi 3 ln ht NaOH tnh V
tb
.
d) Tnh ton kt qu phn tch:
- T cc s liu c, sinh vin tnh V
tb
t kt qu ca 3 ln chun v t lp
cng thc tnh ton nng ca dung dch mu NaOH cn xc nh da trn cch
tnh ton t cc ti liu Ha hc phn tch.
IV. Cu hi ca bi thc hnh (tr li trong bo co th nghim)
1. Tnh th tch dung dch ha cht H
2
SO
4
m c c t trng 1,84 cha 98% H
2
SO
4
pha 1 lt dung dch H
2
SO
4
c nng 0,1N. Coi M
H2SO4
= 98.
2. Ti sao dung dch NaOH chun u phi c chun li trc khi s dng
hng ngy?
3. Nu mt i lng ha hc c th c xc nh bng c 2 phng php (trng
lng v th tch) th phng php no thng t c chnh xc cao hn?
Ti sao?
GV: V Hng Thi 27
BUI TH NGHIM 3
PHNG PHP PHN TCH HA HC
PHNG PHP PHN TCH TH TCH (tip theo)
I. Thc hnh: Chun oxy ha kh dng KMnO
4
a) Nguyn tc:
- Phn ng chun : MnO
4
-
+ 5Fe
2+
+ 8H
+
Mn
2+
+ 5Fe
3+
+ 4H
2
O
E
o
MnO4-/Mn2+
= 1,51V; E
o
Fe3+/Fe2+
= 0,77V
V bn cht, trong qu trnh chun , nng cc cht phn ng thay i sao cho ti
im tng ng, th oxy ha ca cp MnO
4
-
/ Mn
2+
v cp Fe
3+
/Fe
2+
bng nhau.
Th ti im ny l t hp ca cc th thc ca cc cp oxy ha kh. Ngay trc v
sau im tng ng c s thay i rt nhanh ca th dung dch, tng t nh s
thay i nhanh ca pH trong chun acid-base, v s thay i nhanh cng c
gi l bc nhy chun . Do c th xc nh im tng ng nh cht ch th.
- Mi trng acid cn to bng H
2
SO
4
long m khng s dng HCl hay HNO
3
.
- Ch th mu: trong phn ng ny, mu ca dng oxy ha MnO
4
-
khc vi dng kh
Mn
2+
, do vy c th li dng tnh cht ny nhn bit im dng chun : khi dng
d 1 git MnO
4
-
s c mu hng nht.
- V k thut nh lng: phn ng ny thuc loi chun trc tip.
- Sinh vin nn xem li cc khi nim v phn ng oxy ha kh, th in cc,
phng trnh Nernst
b) Ha cht
- Dung dch chun KMnO
4
0,05N.
- Dung dch H
2
SO
4
(1:5).
- Dung dch mu cha Fe
2+
cha bit nng
c) Cch tin hnh:
- Buret: cha dung dch KMnO
4
0,05N.
- Erlen (bnh nn): Ht 10 ml dung dch mu cha Fe
2+
cn xc nh nng , thm 5ml
dung dch H
2
SO
4
(1:5).
- Tin hnh chun bng cch nh dn KMnO
4
xung bnh mu mu chuyn dn
t khng mu sang hng nht, vn bn sau 30 giy.
- Lp li thao tc chun 3 ln vi 3 ln ht mu tnh V
tb
.
d) Tnh ton kt qu phn tch:
- T cc s liu c, sinh vin tnh V
tb
t kt qu ca 3 ln chun v t lp cng
thc tnh ton nng ca dung dch mu cha Fe
2+
cn xc nh.
GV: V Hng Thi 28
II. Thc hnh: Chun to phc vi complexon
a) Nguyn tc:
- Complexon III hay Trilon B (Na
2
H
2
Y) l mui di Natri ca acid etylen diamin tetra acetic
acid (EDTA), nhng vn quen quy c mui di Natri l EDTA. Cng thc ca EDTA
nh sau:
Trong nc: Na
2
H
2
Y 2Na
+
+ H
2
Y
2-
- Na
2
EDTA va d tan trong nc li c th to phc bn vi cc ion kim loi v t l
mol ion kim loi: mol thuc th = 1:1, do vy thng c s dng nh lng kim
loi. Nhn chung, phn ng thun li trong mi trng kim.
V bn cht, trong qu trnh chun , nng cht phn ng (ion kim loi t do) thay
i lin tc. Ngay trc v sau im tng ng c s thay i rt nhanh ca nng
ion kim loi t do, s thay i ny c gi l bc nhy chun .
- im cui: da vo s i mu ca ch th kim loi. Bn cht s i mu ny l s
thay i t mu ca phc gia ch th vi ion kim loi (MInd) sang mu ca ch th t
do (Ind) trong mi trng c pH thun li cho s phn bit gia 2 mu sc (m pH
10).
- Phn ng chun : xc nh Ba
2+
vi s c mt ca ion Mg
2+
. Thc t cc ion kim
loi Ba
2+
v Mg
2+
u to phc vi complexon III, c hng s bn xp x nhau, tuy
nhin Ba
2+
c kh nng to phc mu vi cht ch th (Eriochrome T en) kh phn
bit bng mu sc hn Mg
2+
. Khi chun hn hp Ba
2+
v Mg
2+
mi trng pH 10,
ti st im tng ng, phc MgInd cn li sau cng phn ng vi EDTA chuyn
thnh ch th t do c s thay i mu r rt lm cho php chun chnh xc hn.
Xa im tng ng: Ba
2+
+ H
2
Y
2-
2H
+
+ BaY
2-
Mg
2+
+ H
2
Y
2-
+ 2H
+
+ MgY
2-
Ti im tng ng th xy ra phn ng (do H
2
Y
2-
tc dng ht vi ion kim loi
t do v bt u tc dng vi phc BaInd v MgInd):
BaInd + H
2
Y
2-
BaY
2-
+ H
2
Ind (pH = 10)
(xanh tm) (xanh)
MgInd + H
2
Y
2-
MgY
2-
+ H
2
Ind (pH = 10)
( nho) (xanh)
GV: V Hng Thi 29
- Lu : Do cc ion khc nh Cu
2+
, Ni
2+
, Zn
2+
cng to phc bn vi EDTA pH
chun do nu trong mu c cc ion ny, cn loi nh hng ca chng bng
cch thm vo dung dch NH
2
OH.HCl kh cc ion kim loi ny v ha tr thp hn.
Mt s ion khc nh Ca
2+
, Pb
2+
, Mn
2+
cng to phc bn vi EDTA v khng th
loi chng bng NH
2
OH.HCl.
- Ch th s dng trong phn ng chun l Eriochrome T en (Eriochrome Black T),
thng k hiu l EBT hay ET-00.
- V k thut nh lng: phn ng ny c th coi l thuc loi chun th. Bi v
im tng ng c xc nh thng qua s chuyn mu ca phc MgInd.
- Sau khi to mi trng pH 10, phi chun cng nhanh cng tt trnh s to
kt ta cacbonat kim loi ca ion kim loi trong mi trng kim.
b) Ha cht
- Dung dch chun Na
2
EDTA 0,01 M.
- Dung dch MgCl
2
0,01M.
- Dung dch m pH 10.
- Dung dch NH
2
OH.HCl 10%
- Dung dch ch th Eriochrome T en (EBT hoc ET-00) 0,2%/ethanol.
- Dung dch mu cha Ba
2+
cn xc nh nng
c) Cch tin hnh:
- Buret: cha dung dch EDTA 0,01M.
- Erlen 100ml: ht chnh xc 5 ml dung dch mu. Thm chnh xc 5ml dung dch MgCl
2
,
tip tc thm 1 ml NH
2
OH.HCl v vi git ch th . Sau thm 1 ml dung dch m pH
10. C th trng thnh bnh bng mt t nc ct. Dung dch phi trong sut. Nu
dung dch b c, phi loi b v lm li mu khc.
- Tin hnh chun tht nhanh bng cch nh dn dung dch EDTA xung bnh mu
mu chuyn dn t mu sang mu xanh lam. Tuy nhin, trong khi chun , khi
thy dung dch bt u chuyn mu t sang xanh nh tm, thm tip 1ml dung dch
m pH 10 vo erlen v tip tc chun n khi mu chuyn hn sang xanh lam
(dng chun khi git EDTA cui cng lm mt hn nh tm ca dung dch).
- Lp li thao tc chun 3 ln vi 3 ln ht mu tnh Vtb.
d) Tnh ton kt qu phn tch:
- T cc s liu c, sinh vin tnh V
tb
t kt qu ca 3 ln chun v t lp cng
thc tnh ton nng ca dung dch mu Ba
2+
cn xc nh.
III. Thc hnh: Chun to ta theo phng php Volhard
a) Nguyn tc:
- Phng php Volhard l phng php dng dung dch AgNO
3
chun xc nh
GV: V Hng Thi 30
nng ion halogenua (Cl
-
, Br
-
, I
-
). Bn cht ca phng php chun to ta hay
chun kt ta l da trn phn ng to thnh hp cht khng tan.
- Phn ng chun :
+ Thm lng d xc nh dung dch AgNO
3
vo dung dch cha cu t cn xc
nh (X
-
) trong mi trng acid:
Ag
+
+ X
-
AgX+
+ Sau chun lng d Ag
+
bng dung dch chun SCN
-
:
Ag
+
+ SCN
-
AgSCN+
- V bn cht, trong qu trnh chun , nng cc cht phn ng (ion Ag
+
v ion
SCN
-
) thay i lin tc. Ngay trc v sau im tng ng c s thay i rt nhanh
ca nng Ag
+
v nng SCN
-
. S thay i ny c gi l bc nhy chun .
- im cui chun : dng ch th to phc l phn st ba, phc c mu cam c
to thnh gia ch th Fe
3+
v git d SCN
-
:
Fe
3+
+ SCN
-
FeSCN
2+
- V k thut nh lng: phn ng ny thuc loi chun ngc.
b) Ha cht
- Dung dch chun AgNO
3
0,05N.
- Dung dch chun KSCN 0,05N.
- Dung dch HNO
3
(1:1).
- Dung dch ch th phn st ba Fe(NH
4
)(SO
4
)
2
.12H
2
O bo ha
- Dung dch mu cha ion I
-
cn xc nh nng
c) Cch tin hnh:
- Buret: cha dung dch KSCN 0,05N.
- Erlen 100ml: ht chnh xc 5 ml dung dch mu. Thm vo 2 ml HNO
3
(1:1). Sau
thm chnh xc 15 ml dung dch AgNO
3
ri lc tht mnh dung dch. Thm vi git
ch th.
- Tin hnh chun bng cch nh dn dung dch KSCN xung bnh mu mu
chuyn dn t vng nht sang cam nht, bn trong vi pht. Trong khi chun
phi lc u v mnh dung dch.
- Sau khi kt thc chun , phi trng ra ngay erlen trnh hin tng hp
ph kt ta ln thy tinh.
- Lp li thao tc chun 3 ln vi 3 ln ht mu tnh V
tb
.
d) Tnh ton kt qu phn tch:
- T cc s liu c, sinh vin tnh V
tb
t kt qu ca 3 ln chun v t lp
cng thc tnh ton nng ca dung dch mu I
-
cn xc nh.
GV: V Hng Thi 31
IV. Cu hi ca bi thc hnh (tr li trong bo co th nghim)
1. Ti sao phi to mi trng acid tin hnh phn ng oxy ha kh bng H
2
SO
4
m
khng s dng HCl hay HNO
3
?
2. Ti sao phi cha dung dch chun ca KMnO
4
trong chai nu?
3. Ti sao ngi ta thng KHNG tin hnh phn ng oxy ha kh vi cht oxy ha l
KMnO
4
trong mi trng trung tnh hay kim?
4. Tnh lng ha cht Na
2
EDTA.2H
2
O pha 1 lt dung dch Na
2
EDTA c nng
0,01M. M
Na2EDTA.2H2O
= 372.
5. Ti sao phi tin hnh phn ng chun to phc khong mi trng pH 10? Nu
tin hnh mi trng c pH << 10 (v d pH = 7) th php phn tch c chnh xc
khng? Gii thch.
6. C th thm ch th phn st Fe(NH
4
)(SO
4
)
2
vo dung dch mu trc khi thm AgNO
3
trong bi chun kt ta xc nh nng I
-
trn c khng? Ti sao?
7. Ti sao phi tin hnh phn ng chun to ta theo phng php Volhard trong
mi trng acid? C th tin hnh trong mi trng kim hay trung tnh c khng?
(Gi : lin h n mi trng ion Fe
3+
c th tn ti)
GV: V Hng Thi 32
BUI TH NGHIM 3
PHNG PHP PHN TCH CNG C
PHNG PHP PHN TCH IN
Phng php phn tch o in th - Chun in th
I. Mc ch:
- Nm c nguyn tc o pH bng phng php o in th v ng dng ca n
chun in th.
- Nm c cc nguyn tc v thao tc c bn trong phng php chun in th.
- Thc hnh phng php: chun a base v xc nh cc im tng ng bng
phng php ni suy.
II. Ni dung:
- Sinh vin xem li cc loi in cc trong phng php o th (in cc ch th v in
cc so snh).
- Trong qu trnh chun , nng ion cn xc nh lin tc thay i, do vy in th
ca in cc ch th cng lin tc thay i. Ti ln cn im tng ng, nng ion
cn xc nh thay i t ngt, in th ca in cc ch th do cng thay i t
ngt.
- Gia in th ca dung dch v nng ion H
+
(hay pH) c mi tng quan:
E
o
= E
ch th
- E
so snh
= K 0,059.pH E
so snh
= o - 0,059.pH
Rt ra pH =
059 , 0
E
o
o
(o l hng s thay i ty theo loi in cc)
Khi chun , do pH dung dch hn hp thay i lin tc, in th ca dung dch cng
thay i. Do vy nu o c th in cc th c th bit c pH dung dch. im
tng ng l im ti c bc nhy pH.
- Sinh vin xem li trong cc ti liu l thuyt Ha Phn tch nguyn tc lm vic ca
my o pH.
- Khc vi chun dng ch th mu, vic
xc nh im tng ng bng chun
in th c th theo phng php th hay
phng php ni suy.
+ Phng php th: xy dng ng
cong chun th hy ng o hm
bc 1 ca ng cong chun hoc
ng o hm bc 2 ca ng cong
chun . Thng s dng giy k li
v ng chun c chnh xc.
Th tch dung dch chun (ml)
pH
dung
dch
chun

9,0
8,0
7,0
6,0
GV: V Hng Thi 33
+ Phng php ni suy: tnh ton v xc nh gi tr ca V
t
bng cch suy t th
tch ngay trc hay ngay sau im tng ng. Sinh vin tham kho cch tnh
trong phn ph lc II p dng.
III. Thc hnh: Chun dung dch Na
2
CO
3
bng dung dch HCl
a) Nguyn tc:
Na
2
CO
3
l mui di acid ca H
2
CO
3
nn th hin tnh base theo 2 chc:
Na
2
CO
3
+ HCl NaHCO
3
+ NaCl
NaHCO
3
+ HCl H
2
O + CO
2
+ NaCl
Hng s in ly ca 2 chc base ca Na
2
CO
3
khc nhau kh xa (pK
1
= 3,68 v pK
2
= 7,65), do vy c th nh lng ring tng chc base vi sai s 1%.
Nh vy th gi tr pH ca dung dch theo th tch HCl s dng s c 2 bc
nhy ng vi 2 th tch HCl l V
t1
v V
t2
. V
t1
tng ng vi th tch HCl cn
dng chuyn ton b lng CO
3
2-
thnh HCO
3
-
v V
t2
tng ng vi th tch
HCl cn dng chuyn ton b lng HCO
3
-
va to ra thnh CO
2
v H
2
O.
b) Ha cht
- Dung dch chun HCl 0,1N
- pH k (loi in cc t hp gm in cc thy tinh v in cc calomel bo ha)
- Dung dch mu cha Na
2
CO
3
c) Cch tin hnh:
Trc khi tin hnh th nghim, ging vin hng dn sinh vin cch s dng my o
pH (loi my sn c trong PTN thi im th nghim).
Bc 1: Chun ly s liu th
- Buret: cha dung dch HCl chun 0,1N.
- Becse 250ml: ht chnh xc 5 ml dung dch
mu, trng thnh Erlen bng khong 40 ml
nc ct.
- Cn thn nhng in cc ca pH k vo
becse.
- Tin hnh chun bng cch nh dn
dung dch HCl xung bnh mu, va lc
u dung dch trong becse. C sau 0.5 ml
HCl th ghi nhn gi tr pH 1 ln. Chun
n pH khong 2,2 - 2,3.
- Lp li thao tc chun 3 ln vi 3 ln
ht mu chc chn v kt qu.
T bng kt qu thu c, chn ra 2 khong
GV: V Hng Thi 34
th tch HCl m o hm bc 1 ca ng chun t cc tr ng thi o
hm bc 2 ca n i du (tham kho cch tnh ph lc 2). Da vo 2 khong th
tch th ny, tin hnh tm tip th tch chnh xc V
t1
v V
t2
.
Bc 2: Chun ly s liu tinh
- Buret: cha dung dch HCl chun 0,1N.
- Becse 250ml: ht chnh xc 5 ml dung dch mu, trng thnh Erlen bng khong 40
ml nc ct.
- Cn thn nhng in cc ca pH k vo becse.
- Tin hnh chun bng cch nh dn dung dch HCl xung bnh mu, va lc
u dung dch trong becse. Chun nhanh vi cc th tch HCl nm ngoi 2
khong th tch tnh c bc 1. i vi cc th tch nm trong 2 khong
ny, c sau 0.1 ml HCl th ghi nhn gi tr pH 1 ln.
- Lp li thao tc chun 3 ln vi 3 ln ht mu chc chn v kt qu.
T bng kt qu thu c, tnh ra 2 th tch HCl m o hm bc 2 ca ng
chun i du ng thi o hm bc 1 t cc i (tham kho cch tnh ph lc
2) chnh l V
t1
v V
t2
cn tm.
d) Tnh ton kt qu phn tch:
- T cc s liu c, sinh vin tnh V
tb
t kt qu ca 3 ln chun v t lp
cng thc tnh ton nng ca dung dch mu Na
2
CO
3
cn xc nh.
IV. Cu hi ca bi thc hnh (tr li trong bo co th nghim)
1. u im ca phng php chun in th so vi phng php dng ch th
mu.
2. C th dng ch th mu xc nh 2 im tng ng trong bi th nghim
c khng? Nu c th c th chn dng nhng ch th no?
3. Nu dung dch mu trong bi th nghim l hn hp ca Na
2
CO
3
v NaHCO
3
th c
th xc nh nng tng cu t bng cch chun vi dung dch chun HCl
c khng? Gii thch.
4. Tnh th tch dung dch ha cht HCl m c c t trng 1,174 cha 35% HCl
pha 1 lt dung dch HCl c nng 0,1N. Coi M
HCl
= 36,5.
5. Tnh lng ha cht Na
2
CO
3
tinh khit pha 1 lt dung dch Na
2
CO
3
c nng :
a) 0,5M v b) 0,5N. Cho M
Na2CO3
= 106.
GV: V Hng Thi 35
BUI TH NGHIM 5
BI 5: PHNG PHP PHN TCH CNG C
PHNG PHP PHN TCH QUANG
Phng php ph hp thu phn t vng sng UV-VIS
I. Mc ch:
- Nm c cc nguyn tc v thao tc c bn trong phng php o hp thu.
- Thc hnh phng php: xc nh nng SiO
3
2-
trong nc.
II. Ni dung:
- nh lut Lambert Beer:
Khi chiu mt chm tia sng n sc i qua mt mi trng vt cht th cng ca
tia sng ban u (I
o
) s b gim i ch cn l I.
I
o
: Cng ban u ca ngun sng
I
A
: Cng nh sng b hp thu bi dung dch
I: Cng nh sng sau khi qua dung dch.
I
R
: Cng nh sng phn x bi thnh cuvette v dung dch.
Gia I
o
, I, dy truyn nh sng (l) v nng (C) lin h qua quy lut Lambert
Beer:
KlC
o
10 . I I

=
Hay lC KlC
I
I
lg
o
c = =
K l h s hp th;
c l h s hp thu phn t hay h s hp th mol (l.cm
-1
.mol
-1
), c trng cho kh
nng hp thu nh sng ca dung dch. c ph thuc vo bc sng v cc iu kin
GV: V Hng Thi 36
th nghim c th.
l l chiu dy lp dung dch m nh sng truyn qua (cm);
C l nng ca dung dch (mol/l).
T s T
I
I
o
= gi l truyn qua ca dung dch.
T s D
I
I
lg
o
= gi l mt quang ca dung dch = hp thu A = tt E.
T : lC lC K D A

c = = =
T biu thc trn:
+ Nng ca cu t kho st trong dung dch t l thun vi hp thu nh sng.
+ nh lut ch ng vi nh sng n sc c bc sng xc nh.
+ Mt s hn ch trong vic p dng nh lut: sinh vin tham kho thm trong cc
ti liu l thuyt Ha phn tch.
- Ph hp th:
Dung dch hp th nh sng c tnh chn lc.
th biu din A = f() gi l ph hp th
nh sng ca dung dch. Trn ph hp th c
th c mt hay nhiu cc i: ti
max
c
A
max
.
Do , trong phn tch nh lng bng
phng php trc quang ngi ta chn mt
bc sng nht nh (thng chn
max
), chiu dy cuvet l nht nh v lp
phng trnh ph thuc ca hp th quang A vo nng C.
- Cu to v nguyn l hot ng ca my o quang vng sng t ngoi v kh kin
(UV-VIS): sinh vin tham kho thm trong cc ti liu l thuyt Ha phn tch.
GV: V Hng Thi 37
- Cc phng php xc nh nng cha cu t cn xc nh bng my o quang
c s dng gm phng php trc tip, phng php so snh, phng php thm
chun, phng php ng chun, trong phng php ng chun c s
dng rng ri nht. Sinh vin xem li trong sch l thuyt v phng php ny v cch
p dng (sinh vin c th tham kho phn ph lc I nguyn tc xc nh cc h s
ca phng trnh hi quy v h s tng quan R ca ng hi quy bng phng
php bnh phng cc tiu).
III. Thc hnh: Xc nh nng ca SiO
3
2-
ha tan trong mu nc bng phng
php ng chun
a) Nguyn tc:
Da trn phn ng xy ra gia silic v dung dch Ammonium Molybdate to thnh
phc cht Molybdosilicic c cng mu t l vi hm lng Silic tan.
c im ca phn ng:
- Phn ng trn ch dng xc nh Silic ha tan. Dng Silic khng ha tan phi
xc nh bng phng php khc.
- c th p dng phng php ny xc nh Silic ha tan trong mu nc,
nng ca n khng ln hn 10mg/l.
- Khi o phi i chiu mu o vi mu trng c tin hnh trn nc ct vi quy
trnh hon ton nh mu th.
- loi nh hng ca PO
4
3-
(do PO
4
3-
cng to phc vi Ammonium Molybdate),
s dng acid oxalic.
b) Ha cht
- Dung dch HCl 1:1.
- Dung dch acid oxalic H
2
C
2
O
4
10%.
- Dung dch thuc th Ammonium Molybdate 10% (AM).
- Dung dch chun gc ca SiO
3
2-
nng 1000mg/l pha dy chun.
- Dung dch mu cha ion SiO
3
2-
cn xc nh nng
c) Cch tin hnh:
- Sinh vin tnh ton v pha long dung dch chun gc nng 1000mg/l thnh
dung dch lm vic nng 50mg/l = 50g/ml trong bnh nh mc 100ml.
- Sau tin hnh pha lot dung dch chun v mu trng (M
B
) v cc mu th (M
1
,
M
2
, M
3
) trong bnh nh mc 100ml theo bng sau:
GV: V Hng Thi 38
Dung dch chun
(6 bnh)
Dung dch mu trng v
mu th (4 bnh)
Ha cht
C
o
C
1
C
2
C
3
C
4
C
5
M
B
M
1
M
2
M
3
V
SiO2
50mg/l
(ml)
0 4 8 12 16 20 - - - -
V mu (ml) - - - - - - - 20 20 20
V nc ct (ml) - - - - - - 20 - - -
V HCl 1:1 (ml) 2 2 2 2 2 2 2 2 2 2
V thuc th AM
(ml)
4 4 4 4 4 4 4 4 4 4
Lc k dung dch, yn 5-10 pht
V
H2C2O4
(ml) 5 5 5 5 5 5 5 5 5 5
nh mc ti vch bng nc ct. y np v o bnh vi ln.
yn dung dch trong 2-15 pht ri o mu bc sng 410nm
Nng C
(mg/l)
0 2 4 6 8 10 -
cn
tm
cn
tm
cn
tm
hp thu A 0 ? ? ? ? ? 0 ? ? ?
d) Tnh ton kt qu phn tch:
- T cc s liu o c, sinh vin tin hnh lp ng chun, xc nh cc h
s ca phng trnh hi quy tuyn tnh (yu cu ng chun phi c h s tng
quan R > 0,99 mi l t yu cu) t tnh kt qu ca 3 ln o mu t phng
trnh hi quy tuyn tnh t yu cu (sau khi hiu chnh vi mu trng) v ly gi
tr trung bnh.
IV. Cu hi ca bi thc hnh (tr li trong bo co th nghim)
1. Ti sao ch s dng duy nht 1 cuvet gia cc ln o?
2. Ti sao phi lc mu th trc khi em to phc so mu?
GV: V Hng Thi 39
PH LC
I. Phng php bnh phng cc tiu trong xc nh cc h s ca ng
hi quy
Gi s ta c cc cp kt qu th nghim (x
i
, y
i
) vi I : 1 n v cn xc nh a, b trong mi
quan h y = ax + b, ngha l gia x v y c mi tng quan tuyn tnh (trong gii hn
hp, mi tng quan gia nng C ca mu vi hp thu A ca n ti mt
bc sng n sc nht nh l tun theo tng quan ny).
Phng php bnh phng cc tiu cho ta gi tr ca a v b theo cng thc sau:


= =
= = =

=
n
1 i
2
n
1 i
i
2
i
n
1 i
n
1 i
i
n
1 i
i i i
) x ( x n
y x y x n
a


= =
= = = =

=
n
1 i
2
n
1 i
i
2
i
n
1 i
n
1 i
i i
n
1 i
i i
n
1 i
2
i
) x ( x n
y x x y x
b
Tuy nhin, vi bt k cc s liu (x
i
, y
i
) ta cng c th tnh c h s a v b tng ng.
Nh vy phng php ny khng cho chng ta thy c mi quan h gia x v y c
phi l tuyn tnh hay khng. xc nh xem x v y c quan h tuyn tnh vi nhau hay
khng ta dng h s tng quan R:
|
|
.
|

\
|
|
|
.
|

\
|

|
|
.
|

\
|
|
|
.
|

\
|

=


= = = =
= = =
n
1 i
2
n
1 i
i
2
i
n
1 i
2
n
1 i
i
2
i
n
1 i
n
1 i
i
n
1 i
i i i
y y n x x n
y x y x n
R
H s tng quan lun trong khong [-1, 1]. Khi r cng gn 0 th quan h cng lng lo,
ngc li khi r cng gn 1 hoc -1 th quan h cng cht ch (r > 0 c quan h thun v r
< 0 c quan h nghch). Trng hp r = 0 th gia x v y khng c quan h.
Trong ngnh ha hc phn tch nh lng, c th kt lun 2 i lng x v y c quan h
tuyn tnh khi R > 0.99. Cc ngnh khoa hc khc c th yu cu h s tng quan ln
hn hay v nh hn ty tnh cht chnh xc v mc yu cu. Khi xy dng cc mi quan
h gia cc i lng bng thc nghim, ta c th tin hnh nhiu ln (lp li), khi kt
qu no c h s tng quan ln hn s c u tin.
V d: ta c kt qu ca ng chun dng c nh sau
GV: V Hng Thi 40
n A = D (y
i
) C (mg/l) (x
i
) x
i
.y
i
y
i
2
x
i
2
1 0 0 000.00 0.0000 0
2 0.019 50 000.95 0.0004 2500
3 0.092 100 009.20 0.0085 10000
4 0.149 150 022.35 0.0222 22500
5 0.173 200 034.60 0.0299 40000
6 0.229 250 057.25 0.0524 62500
7 0.263 300 078.90 0.0692 90000
8 0.389 400 155.60 0.1513 160000
9 0.457 500 228.50 0.2088 250000
Tng 1.771 1950 587.350 0.5427 637500
NG CHUN
y = 0.0009x - 0.0084
R
2
= 0.9929
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0.4
0.45
0.5
0 100 200 300 400 500 600
Nng C (mg/l)

p

t
h
u

D

(
A
)
Ta s tnh c a = 0,0009 v b = -0,0084 hay A = 0,0009C 0,0084
H s tng quan R = 0.9929 > 0,99 l t yu cu
GV: V Hng Thi 41
II. Phng php ni suy s liu t kt qu chun in th
V d kt qu chun nh sau, ta s lp bng ni suy (ch AV trong v d = 0,1)
V (ml) pH V =
2
V V
1 i i +
+
pH A
V A
V
pH
A
A V A
A
|
.
|

\
|
A
A
V
pH
=
V
pH
2
2
A
A
1,1
1,2
1,3
1,4
1,5
1,6
3,66
3,88
4,66
6,32
6,8
7,02
1,15
1,25
1,35
1,45
1,55
0,22
0,78
1,66
0,48
0,22
0,1
0,1
0,1
0,1
0,1
2,2
7,8
16,6
4,8
2,2
56
88
-118
-26
Thc cht ca vic xc nh V
t
chnh l i tm honh im un trn ng cong
chun . C 2 cch xc nh gi tr V
t
ny:
Cch 1:
V
td
= V =
2
1 +
+
i i
V V
vi V
i
v V
i+1
l 2 th
tch c
V
pH
A
A
cc i, v d trong bng s
liu trn l V = 1,35 ml ng vi
V
pH
A
A
=
16,6. C s ton hc ca cch tnh ny
ch o hm cp 1 ca im un (ng
cong chun ) t gi tr cc tr ( th b)
Cch 2:
Chnh xc hn l cch ni suy bng gi tr
vi phn cp 2. C s ton hc ca cch
tnh ny l honh ca im un
(ng cong chun ) cng l im m
ti o hm cp 2 ca ng cong
chun t gi tr = 0.
Nh vy gi tr ca honh im un x
o
(chnh l V
t
ang cn tm) nm trong
khong m qua th o hm cp 2 i
du ( th c), v d trong bng s liu
trn th o hm cp 2 i du t
Th tch cht chun (ml)
V
pH
A
A
V
pH
2
2
A
A
Th tch cht chun (ml)
GV: V Hng Thi 42
1
2
2
|
|
.
|

\
|
A
A
V
pH
= 88 sang
2
2
2
V
pH
|
|
.
|

\
|
A
A
= -188 khi qua 2 im 1 v 2 tng ng, tc l V
t
cn
xc nh nm gia 2 gi tr tng ng vi 2 im 1 v 2 l 1,3 ml v 1,4 ml. Tip
theo cn tnh c th gi tr ca V
t
theo cng thc sau:
V
t
=
2
2
2
1
2
2
2
2
2
1 i
2
2
2
1
2
2
1
2
2
i
V
pH
V
pH
V
pH
V V
V
pH
V
pH
V
pH
V V
|
.
|

\
|
A
A
+ |
.
|

\
|
A
A
|
.
|

\
|
A
A
A =
|
.
|

\
|
A
A
+ |
.
|

\
|
A
A
|
.
|

\
|
A
A
A +
+
= 1.3 +
88 188
88
1 . 0
+
= 1.4 -
88 188
188
1 . 0
+
= 1.33 ml
GV: V Hng Thi 43
TI LIU THAM KHO
1. Trn T Hiu, 2008, Phn tch trc quang ph hp th UV-Vis, ti bn ln 2, H Ni,
NXB i hc Quc gia H Ni.
2. Nguyn Th Thu Vn (CB), 2006, Th nghim Phn tch nh lng, Tp H Ch Minh,
NXB i hc Quc gia Tp H Ch Minh.
3. Nguyn Tinh Dung, 2003, Ha hc phn tch nh lng, phn 3, ti bn ln 2, H Ni,
NXB Gio dc.
4. H Vit Qu, 2006, C s Ha hc phn tch hin i, tp 1, NXB i hc S phm.
5. H Vit Qu, 2006, Phn tch L-Ha, ti bn ln 2, H Ni, NXB Gio dc.
6. Phm Hi Tng, Phm Gia Hu, 1978, Ha hc phn tch, tp 2, H Ni, NXB Y hc.
7. Nguyn Thc Ct, T Vng Nghi, o Hu Vinh, 1985, C s l thuyt Ha hc phn
tch, H Ni, NXB i hc v Trung hc chuyn nghip.
8. L Xun Mai, Nguyn Bch Tuyt, 2000, Gio trnh Phn tch nh lng, Tp HCM,
NXB i hc Quc gia Tp H Ch Minh.
9. Hong Minh Chu (CB), 2007, C s Ha hc phn tch, ti bn ln 2, H Ni, NXB
Khoa hc v K thut.
10. Nguyn Th Xun Mai, 1998, Thc tp phn tch trc quang, Tp H Ch Minh, xng in
i hc Khoa hc t nhin.