Tvefile 2013-09-05 6462811946

B GIO DC V O TO
TRNG I HC S PHM H CH MINH
KHOA HA HC
KHA LUN TT NGHIP
GIO VIN HNG DN: ThS. L NGC T
SINH VIN THC HIN: LI TH KIM BIN
LP: K35C
THNH PH H CH MINH- THNG 5 NM 2013

LI CM N
Trc ht, em xin trn trng cm n thy L Ngc T, ngi trc tip hng
dn, gip em v kin thc v phng php em hon thnh c kha lun tt
nghip ny.
Em cng xin trn trng cm n cc Thy C trong Khoa Ha hc trng i

hc S Phm thnh ph H Ch Minh hng dn, ging dy, cung cp kin thc
cho em trong sut bn nm hc qua.
Em cng xin gi li cm n su sc n gio vin ph trch phng thc hnh

ha phn tch tn tnh gip em trong vic mn ha cht v dng c phng
th nghim.
Ti cng xin chn thnh cm n cc bn sinh vin lp Ha K35A, K35B,

K35C, K36C gip ti hon thnh tt cc Phiu kho st phc v cho kha
lun tt nghip ny.
c s gip ca Thy C v bn b, cng vi nhng n lc ca bn

thn, em hon thnh kha lun tt nghip ti Thc trng v mt s bin
php nng cao hiu qu dy- hc phn thc hnh Phn tch nh lng Ha
hc, xin knh trnh Qu Thy C trong hi ng chm kha lun tt nghip. Do
trnh nghin cu v thi gian c hn nn chc chn khng trnh khi thiu st v
hn ch. Rt mong c s gp v ch dn ca Thy C.
Em xin trn trng cm n.
Thnh ph H Ch Minh, thng 5 nm 2013
Sinh vin thc hin
LI TH KIM BIN
MC LC
Trang
DANH MC BNG .................................................................................................. I
DANH MC HNH ................................................................................................. II
LI M U ............................................................................................................1
TNG QUAN ............................................................................................................2
CHNG 1:C S L LUN ...............................................................................3

1.1. Khi nim th nghim ha hc ....................................................................3
1.2. Mc ch ca vic thc hnh th nghim ....................................................3
1.3. Mt s gio trnh thc hnh Phn tch nh lng: ....................................5
1.3.1. Ti Khoa Ha Hc, Trng i hc S Phm Thnh ph H Ch Minh
hin nay ..............................................................................................................5
1.3.2. Ti cc trng i hc khc trong nc .................................................5
1.3.3. Nhn xt ..................................................................................................9
CHNG 2:C S L THUYT CC PHNG PHP NH LNG

HA HC ...............................................................................................................10
2.1. Phng php phn tch khi lng ...........................................................13
2.2. Phng php phn tch th tch .................................................................18
2.2.1. Phng php chun axit- baz .........................................................18
2.2.2. Phng php oxi ha-kh .....................................................................23
2.2.3. Phng php chun kt ta ..............................................................26
2.2.4. Phng php chun phc cht .........................................................28
THC NGHIM .....................................................................................................36
CHNG 3:KHO ST THC TRNG DY- HC PHN THC HNH

PHN TCH NH LNG HA HC ............................................................37
3.1. Kho st bng hnh thc phiu iu tra.....................................................37
3.1.1. Cch tin hnh .......................................................................................37
3.1.2. M t phiu iu tra ..............................................................................37
3.1.3. Phn tch kt qu iu tra ......................................................................37
3.1.4. Nhn xt ................................................................................................45
3.2. Kho st cc bi thc hnh c trong gio trnh .........................................48
3.2.1. Kho st bi 1: chun Axit mnh Baz mnh ..................................48
3.2.2. Kho st bi 2: chun axit yu .........................................................50
3.2.3. Kho st bi 3: chun baz yu........................................................51
3.2.4. Kho st bi 4: chun a axit ...........................................................53
3.2.5. Kho st bi 5: chun a baz..........................................................56
3.2.6. Kho st bi 6: nh lng Fe bng phng php pemanganat ............60
3.2.7. Kho st bi 7: nh lng Cu bng phng php iod .........................61
3.2.8. Kho st bi 8: chun kt ta ...........................................................62
3.2.9. Kho st bi 9: chun phc cht. .....................................................64
3.2.10. Nhn xt ................................................................................................66
3.3. xut chung ...........................................................................................67
CHNG 4:MT S GII PHP NNG CAO HIU QU DAY- HC

PHN THC HNH PHN TCH NH LNG HA HC ......................68
4.1. Chnh sa v b sung ni dung gio trnh ................................................68
4.1.1. Bi 2: Chun axit yu .......................................................................68
4.1.2. Bi 3: Chun baz yu .....................................................................68
4.1.3. Bi 5: Th nghim Chun hn hp Na 2 CO 3 v NaOH bng HCl ..69
4.2. Cc bi th nghim xut ........................................................................72
4.2.1. Bi 2: Xc nh hm lng st bng phng php Dicromat...............72
ii
4.2.2. Bi 3: Xc nh hm lng vitamin C trong vin nn bng phng
php chun iod .............................................................................................73
4.3. Xy dng phim minh ha cc bi thc hnh.............................................75
KT LUN- XUT ..........................................................................................77
TI LIU THAM KHO ......................................................................................79
PH LC .................................................................................................................81
iii
DANH MC BNG
BNG 2.1. Mt s ch th quan trng v khong chuyn mu ca ch th ..............21
BNG 2.2. Khong pH i mu ca ch th ERIOT ................................................32
i
DANH MC HNH
HNH 2.1. Phng php lc kt ta ..........................................................................16
HNH 2.2. Phng php chun th tch ...............................................................18
HNH 2.3. C ch i mu phenolphatalein .............................................................19
HNH 2.4. C ch i mu ca phenol ................................................................20
HNH 2.5. C ch i mu ca metyl da cam ..........................................................20
HNH 2.6. ng cong chun ion kim loi mn+ bng Na 2 H 2 Y .........................30
ii
LI M U
Phn tch nh lng c dng xc nh quan h nh lng gia cc

thnh phn ca cht nghin cu, trong phn tch ng vai tr l trung tm.
Trong xu th hi nhp khu vc v ton cu, chng ta ngy cng phi nng
cao cht lng ca mi loi hnh sn phm trong khng t sn phm c ng gp
ca chuyn ngnh Ho hc Phn tch. l phn tch nguyn liu v sn phm ca
qu trnh sn xut trong nng nghip cng nh trong cng nghip, phn tch cc
mu trong nghin cu khoa hc, phn tch lm sng, phn tch cc mu phc v cho
qu trnh iu tra ph n,... Mt khi lng khng l cc mu phn tch nh vy
khng t mu lin quan trc tip ti s thnh bi ca mt doanh nghip, sc kho,
v c bit l sinh mng ca con ngi. iu ni ln nhu cu thc t i hi tnh
chnh xc v tnh ng n ca cc kt qu phn tch. Chnh v vy cc sinh vin
Ha hc d i vo chuyn ngnh no u cn trang b nhng kin thc v Phn tch
nh lng.
Ngy nay, vi s tin b ca khoa hc k thut, Phn tch nh lng ngy
cng c quan tm nghin cu v ng dng thc t.
Qua so snh vi ni dung gio trnh thc hnh phn tch nh lng ha hc
ti mt s trng i hc nh i hc S phm Quy Nhn, i hc Bch Khoa H
Ni, i hc Khoa hc T nhin- i hc Quc gia H Ni, cho thy gio trnh
thc hnh Phn tch nh lng Ha hc cho cc i tng sinh vin khoa Ha,
trng i hc S Phm Thnh Ph H Ch Minh c thc hin t nm 2004 n
nay cn t bi thc hnh, cn c i mi v cp nht ph hp vi sinh vin v
theo kp nhng tin b mi v k thut.
T thc t bn thn trong vic hc tp phn thc hnh Phn tch nh lng
Ha hc v di s nh hng ca thy L Ngc T em tin hnh ti Thc
trng v mt s bin php nng cao hiu qu dy- hc phn thc hnh Phn
tch nh lng Ha hc.
1
PHN 1:
TNG QUAN
2
CHNG 1: C S L LUN
1.1. Khi nim th nghim ha hc [15]

Th nghim: Theo t in Ting Vit Nh xut bn khoa hc x hi 1992 th
th nghim c hai ngha. Ngha th nht: Gy ra mt hin tng, mt s bin i
no trong iu kin xc nh quan st, tm hiu, nghin cu, kim tra hay
chng minh. Ngha th hai: lm th rt kinh nghim. Theo i t in Ting
Vit Nh xut bn Vn ha thng tin 1999 th th nghim l: Lm th theo nhng
iu kin, nguyn tc c xc nh nghin cu, chng minh. Trong ti
nghin cu ny khi nim th nghim c gii hn trong mt phm vi hp hn l
thc hin cc phn ng, qu trnh ha hc
1.2. Mc ch ca vic thc hnh th nghim[13- 15]

Th nghim l phng tin trc quan
Th nghim l nn tng ca vic dy hc ha hc. Th nghim l phng tin
trc quan chnh yu, c dng ph bin v gi vai tr quyt nh trong qu trnh
dy hc ha hc. N gip sinh vin chuyn t t duy c th sang t duy tru tng
v ngc li. Khi lm th nghim sinh vin s lm quen c vi cc cht ha hc
v trc tip nm bt cc tnh cht l, ha ca chng. Mi ha cht thng c mt
mu sc khc nhau nh mu vng lc, lc nht, xanh lc, xanh l, xanh ve,nu
sinh vin khng quan st trc tip th khng th no hnh dung c cc mu sc
nh th no. Thc hnh th nghim cho sinh vin c c hi nhn thc v nhn ra
nhng v d thc hnh ca cc cht cp trong l thuyt, mt iu quan trng
l sinh vin Ha hc phi thy mt s cc phn ng. V vy, mc ch quan trng
ca cng vic th nghim l sinh vin thc hnh kho st qu trnh phn ng ca
cc cht.
Th nghim l cu ni gia l thuyt v thc tin
C th ni qu trnh nhn thc ca hc sinh, sinh vin l mt qu trnh nhn
thc c o. c o l ch h lun nhn thc c ci ng. Nhng tri thc m
h tip nhn c cc nh khoa hc, gio dc mit mi nghin cu, c kt t
3
thc nghim. Song khng phi nhng l thuyt a ra u c sinh vin chp
nhn d dng. S tht l th v nu bn thn h chng minh c nhng l thuyt
m h c hc l ng d rng l cng vic m nhng nh nghin cu trc
y lm. i vi b mn ha hc, thc hnh th nghim s gip cho sinh vin
sng t nhng vn l thuyt a ra. Hc i i vi hnh vi ngha thc
hnh th nghim gip sinh vin n tp v kim tra li cc vn l thuyt hc,
trn c s hiu su sc v nm vng nhng ni dung c bn trong gio trnh l
thuyt.
Nhiu th nghim rt gn gi vi i sng, vi cc quy trnh cng ngh. Chnh
v vy, th nghim gip sinh vin vn dng nhng kin thc hc vo thc t cuc
sng. Khi quan st cc th nghim sinh vin ghi nh li cc th nghim, nu sinh
vin gp li hin tng trong t nhin hay trong quy trnh cng ngh, sinh vin s
hnh dung li kin thc c v gii thch c hin tng mt cch d dng. T
sinh vin pht huy tnh tch cc, sng to v vn dng kin thc nhy bn trong
nhng trng hp khc nhau.
Rn luyn kh nng thc hnh
Trong tt c cc th nghim khoa hc, c bit l th nghim v ha hc, nu
khng cn thn s gy nguy him c khi dn n t vong. Khi thc hnh th
nghim, sinh vin phi lm ng cc thao tc cn thit, s dng lng ha cht
thch hp, pht tin cc k nng thc hnh nh k nng iu khin my mc, dng
c th nghim, k nng quan st hin tng v k nng thu thp s liu th nghim
nn sinh vin va tng cng kho lo v k nng thao tc, va pht trin k nng
gii quyt vn . T hc sinh s hnh thnh nhng c tnh cn thit ca ngi
lao ng mi: cn thn, ngn np, kin nhn, trung thc, chnh xc, khoa hc,y
l iu m th nghim o khng c c.
Pht trin t duy, tp lm nghin cu khoa hc
Th nghim ha hc gip sinh vin pht trin t duy, hnh thnh th gii quan
duy vt bin chng. Pht trin nhng k nng thit k, t chc, sp xp cc bc
tin hnh th nghim mt cch thch hp kim tra l thuyt. Hc x l v gii
4
thch s liu th nghim. Ngoi vic x l s liu thng thng, iu quan trng l
mun t trnh cao hn trong mt s mn i hc nn thit k nhng th
nghim nhm pht trin kh nng suy lun khoa hc cho sinh vin.
1.3. Mt s gio trnh thc hnh Phn tch nh lng:

1.3.1. Ti Khoa Ha Hc, Trng i hc S Phm Thnh ph H Ch Minh hin
nay [12]
Trn Th Yn (Ch bin), Ng Tn Lc, Nguyn Hin Hong,
Vn Hu, Nguyn Th Minh Hu, L Ngc T (2004), Thc hnh phn tch
nh lng, HSP TP.H Ch Minh.
Gio trnh gm 9 bi thc hnh
Bi 1: Chun axit mnh bng baz mnh v ngc li
Bi 2: Chun axit yu bng baz mnh
Bi 3: Chun baz yu bng axit mnh
Bi 4: Chun a axit vi hn hp axit (H 3 PO 4 + HCl) bng baz mnh
Bi 5: Chun a baz vi hn hp baz (Na 2 CO 3 + NaOH) bng axit mnh
Bi 6: Chun oxi ha kh. Phng php pemanganat
Bi 7 : Chun oxi ha kh. Phng php iod
Bi 8 : Chun kt ta
Bi 9: Chun complexon
1.3.2. Ti cc trng i hc khc trong nc
B mn Ha Phn tch (2004), Gio trnh Hng dn thc hnh
Phn tch nh lng, i hc S Phm Quy Nhn [1]
Gio trnh gm c 14 bi
Bi 1: Chun bazo mnh bng axit mnh
Bi 2: Chun baz yu v a baz bng axit mnh
Bi 3: Xc nh thnh phn Xt k thut
Bi 4: Chun axit mnh v axit yu bng baz mnh
Bi 5: Chun axit a chc H 3 PO 4 v hn hp HCl + H 3 PO 4 .
Bi 6: Chun oxi ha kh. Phng php pemanganat
5
Bi 7 : Xc nh Crom trong dung dch K 2 Cr 2 O 7
Bi 8 : Phng php iod
Bi 9: Phng php bicromat
Bi 10: Xc nh cng ca nc bng phng php Complexon
Bi 11: Xc nh mt s ion bng phng php Complexon
Bi 12: Phng php kt ta Xc nh hm lng Cl- trong mui n bng
phng php Mohr v phng php Volhard
Bi 13: Xc nh hm lng ion Fe bng Kaliferoxianua theo phng php kt
ta
Bi 14: Xc nh Cl-, Br-, I-, SCN- bng phng php FaJans
Nguyn Th Nh Mai, ng Th Vnh Ha (2002),Gio trnh
Hng dn thc hnh Phn tch nh lng bng cc phng php ha hc,
i hc Lt. [9]
Gio trnh thc hnh gm 8 bi thc hnh
Bi 1: Cch s dng cc dng c o khi lng v th tch
Bi 2: Phng php trung ha (Phng php chun Acid-Bazo)
Bi 3: Phng php trung ha
Bi 4: Phng php Oxy ha-kh php o Pemanganat
Bi 5: Phng php oxy ha-kh php o Dicromat v Iod
Bi 6: Phng php chun kt ta
Bi 7: Phng php phn tch khi lng
Bi 8: Phng php Complexon
Khoa Ha (2004), Gio trnh thc hnh Phn tch nh lng,
Trng i hc cng nghip [4]
Phn b thi gian: thc hnh 90 gi, mi bi 5 gi (18 bi)
Gio trnh gm 19 bi:
Bi 1: Pha ch cc dung dch
Bi 2: nh lng axit mnh - baz mnh
Bi 3: nh lng n axit yu-baz mnh nh lng n acid mnh-baz
6
yu
Bi 4: nh lng a acid v hn hp acid
Bi 5: nh lng a baz va hn hp baz
Bi 6: nh lng mui
Bi 7: Chun Pemanganat nh lng Fe2+, H 2 O 2 va NO 2 -
Bi 8: Chun Pemanganat nh lng Fe3+, Cr6+
Bi 9: Phng php Iod nh lng vitamin C, SO32-
Bi 10: Phng php Iod - Cromat nh lng H 2 O 2 , Cu2+, Pb2+
Bi 11: nh lng Ca2+- Mg2+
Bi 12: nh lng Zn2+, Fe3+, Al3+ v hn hp Al3++ Fe3+
Bi 13: nh lng hn hp Mg2++ Zn2+ v hn hp Mg2++ Ca2++ Fe3++ Al3+
Bi 14: nh lng Ba2+ v SO 4 2-
Bi 15: Phng php Mohr v Volhard nh lng ion Cl-
Bi 16: Xc nh SO 4 2- (hoc Ba2+)
Bi 17: Xc nh Fe3+
Bi 18: Xc nh Mg2+
Bi 19: Xc nh Photphat
Nguyn Vn Ri, T Th Tho (2006), Gio trnh Thc tp phn
tch Ha hc Phn 2 Phn tch nh lng Ha hc, Trng i hc Khoa
hc T nhin- i hc Quc gia H Ni [11]
Phn 1: Phn tch nh lng ha hc c bn
Bi 1: Chun n axit, n baz
Bi 2: Chun a axit
Bi 3: Chun a Baz
Bi 4: Chun trc tip xc nh cc ion kim loi
Bi 5: Cc k thut chun complexon
Bi 6: Cc k thut chun complexon (tip)
Bi 7: Xc nh hn hp Al3+, Ca2+, Mg2+ (bi kim tra)
7
Bi 8: Xc nh cc halogenua, SCN-
Bi 9: Phng php Pemanganat
Bi 10: Phng php Dicromat
Bi 11: Phng php chun iot-thiosunfat
Bi 12: Phng php chun Bromat, Iodat
Bi 13: Phng php phn tch trng lng xc nh Mg2+
Bi 14: Phng php phn tch trng lng xc nh Fe
Bi 15: Xc nh SO 4 2- bng phng php trng lng v complexon
Phn 2: Phn tch mu thc t
Bi 16: Xc nh hm lng Mn trong gang
Bi 17: Phn tch Al, Cu, Zn trong hp kim Devada
Bi 18: Xc nh Fe, Cr, Ni trong hp kim inox
Bi 19: Xc nh Cu, Sn, Pb, Zn trong ng thau
Bi 20: Xc nh hm lng Cu, Fe, Al, Zn trong hp kim nhm
Bi 21: Xc nh hm lng Al 2 O 3 , Fe 2 O 3 , CaO, MgO
Bi 22: Xc nh hm lng P 2 O 5 trong phn bn NPK
Bi 23: Xc nh Mn trong qung pirozulit
Bi 24: Xc nh mt s ch tiu ha hc ca nc b mt
Bi 25: Xc nh mt s ch tiu ha hc ca nc v nc thi
Bi 26: Phn tch mt s ch tiu ca nc mm
Bi 27: Phn tch hm lng cc loi ng trong sa c c ng
Bi 28: Phn tch mt s chi tiu ha hc ca cht bo
Bi 29: Xc nh mt s ch tiu ha hc ca ru ung
Bi 30: Xc nh hm lng foocmandehit, phenol trong nc ung
Xc nh hm lng KIO 3 trong mui iot
B mn Ha Phn tch (2007), Gio trnh Hng dn th nghim
Ha Phn tch, i hc Bch khoa H Ni. [2]
Bi 1: Xc nh SO4 2- (sunfat) theo phng php khi lng
8
Bi 2: Xc nh st theo phng php khi lng
Bi 3: Xc nh niken trong thp
Bi 4: Pha ch v chun dung dch HCl
Bi 5: Xc nh nng dung dch naoh bng dung dch HCl
Bi 6: Xc nh hm lng Na 2 CO 3 trong Na 2 CO 3 k thut
Bi 7: Xc nh nng NaOH v Na 2 CO 3 trong hn hp
Bi 8: Xc nh hm lng axit c trong dm v ru vang
Bi 9: Pha ch v xc nh nng dung dch KMnO 4
Bi 10: Xc nh hm lng canxi trong vi
Bi 11: Xc nh nng dung dch Fe2+ bng KMnO 4
Bi 12: Xc nh st trong dung dch FeCl 3 bng KMnO 4
Bi 13: Xc nh hm lng Mn trong thp hp kim
Bi 14: Xc nh nng Fe3+ bng K 2 Cr 2 O 7
Bi 15: Xc nh Crom trong thp hp kim
Bi 16: Chun dung dch Na 2 S 2 O 3 theo phng php it
Bi 17: Xc nh ng trong CuSO 4
Bi 18: Xc nh antimon trong antimon k thut
Bi 19: Xc nh Cl bng dung dch chun AgNO 3
Bi 20: Xc nh Cl bng dung dch chun Hg(NO 3 ) 2

Bi 21: Xc nh km bng feroxianua kali theo phng php kt ta
Bi 22: Xc nh nng complexon III bng dung dch ZnSO 4
Bi 23: Xc nh cng chung ca nc bng complexon III
Bi 24: Xc nh Ca bng phng php complexon
Bi 25: Xc nh Al bng complexon III theo phng php nh phn ngc
Bi 26: Xc nh Ni bng complexon III
Bi 27: Xc nh coban bng complexon III
1.3.3. Nhn xt
Qua nghin cu ni dung gio trnh thc hnh Phn tch nh lng ti mt
9
s trng i hc trong nc. Chng ta c th nhn thy c gio trnh thc
hnh Phn tch nh lng Ha hc hin c ca khoa Ha i hc S Phm H
Ch Minh c nhng c im sau:
V u im:
Minh ha c c bn ni dung chng trnh l thuyt Phn tch nh
lng Ha hc nh cc phng php chun axit-bazo, chun oxi ha-kh,
chun phc cht, chun kt ta.
V nhc im:
S lng bi th nghim cn hn ch.
Mt s phn l thuyt quan trng cha c bi thc hnh minh ha. V d:
thiu phng php phn tch khi lng, chun oxi ha- kh thiu phng
php Dicromat,
Mu phn tch ch yu l nhng mu n gin nh nh lng mt ion kim
loi, thiu nhng mu i hi kh cao nng cao tinh thn tm hiu ca
sinh vin.
Cc bi thc hnh phn tch mu thc t t c quan tm.
CHNG 2: C S L THUYT CC PHNG PHP NH LNG

HA HC
Phn tch nh lng [10]
Phn tch nh lng c nhim v xc nh lng ca cc cu t c trong i
tng phn tch (thng nh gi tng i theo %). Cc cu t y c th l cc
nguyn t (cn hoc khng cn xt n trng thi kt hp hoc trng thi oxi ha
kh trong cht phn tch, cc gc hoc cc nhm chc (trong phn tch hu c),
cc hp cht hoc c th l cc pha (n cht hay hp cht).
C th phn chia cc phng php nh lng thnh hai loi: cc phng php
ha hc, cc phng php vt l v ha l. Trong phm vi nghin cu ca ti
ny chng ta ch cp n cc phng php ha hc.
Cc phng php ha hc da ch yu trn vic p dng cc phn ng ha
hc c lin quan n cu t phn tch. S khc nhau gia cc phng php ha hc
10
l do s khc nhau v phng php o lng thuc th hoc sn phm to thnh
trong phn ng. Chng hn, xc nh hm lng ca cu t M c trong cht phn
tch ngi ta cho n tc dng vi mt thuc th R. Phn ng ha hc xy ra hon
ton v theo quan h hp thc M+nR=MR n . xc nh M c th dng d thuc
th R. Sau tch sn phm to thnh thng di dng kt ta t tan. Da vo
khi lng kt ta thu c c th tnh c hm lng M trong cht phn tch.
Phng php ny da ch yu trn vic cn lng sn phm phn ng nn thng
c gi l phng php khi lng.
xc nh M cng c th cho mt lng chnh xc thuc th R tc dng
va ht vi M. Thng thng ngi ta o th tch ca dung dch thuc th R c
nng chnh xc bit, v t tnh c lng cu t cn xc nh M. Phng
php phn tch nh vy gi l phng php phn tch th tch.
Sai s trong phn tch nh lng [7]
Sai s tuyt i
Khi nh lng mt cht, ta gp mt trong hai trng hp:
Lng tht s ca cht l , sau khi tin hnh nh lng ta c kt qu l x i
Hiu s = x i - gi l sai s tuyt i, biu th tnh ng ca kt qu tm ra.
c th dng hay m
Tuy nhin trong thc t, ngi ta khng bit gi tr thc ca i lng cn o
. Trong trng hp mun chc chn ta phi nh lng nhiu ln ri ly kt qu
trung bnh cng cc ln o . Mi kt qu ring bit em so snh vi ta c:
Hiu s d = x i - gi l lch tuyt i biu th tnh chnh xc cc kt qu
iu tra.
Sai s tng i:
Sai s tuyt i khng ni ln mt khi nim tng qut, nhng c khi li dn
ti nhng cch nh gi sai lch ng tic, do ngi ta thng thay bng cch
biu th sai s tng i. Sai s tng i l t s gia sai s tuyt i v kt qu
thc hoc t s gia lch tuyt i vi kt qu trung bnh.
11

S= hoc S =

Sai s h thng v sai s ngu nhin:

Sai s ngu nhin: Do mt nguyn nhn khng bit trc, khng trnh c,
bao gm cc yu t c th thay i bt thng qua mi ln nh lng.
Mun hn ch sai s ngu nhin, ta cn ch n cc iu kin c th khc
phc: lm nhiu ln phn tch, ly kt qu trung bnh, nu c sai lch qu ng th
b i. Ngoi ra cn x l kt qu bng thng k.
Sai s h thng: Do mt nguyn nhn xc nh, bin thin mt chiu (lun >
0, hoc lun < 0), ngha l gi tr th nghim lun lun ln hn hoc b hn gi tr
thc
Sai s h thng c th xut pht t:
Bn thn phng php phn tch
Do dng c phn tch km chnh xc
Do thuc th ha cht km tinh khit, nng khng ng,
Do c nhn ngi phn tch
X l kt qu phn tch theo phng php thng k:
Gi tr trung bnh cng x
L gi tr gn vi gi tr thc ca i lng cn o vi xc sut cao nht trong
s cc gi tr o c ca ai lng cn o.
Gi s ta tin hnh n php c lp i lng X vi cc kt qu: X 1 ,
X 2 ,....X n :
n
1
x = xi
n
i=1
Phng sai S 2

1
2 = ( )2
1
=1
lch chun S: L cn bc hai ca phng sai

Bin gii tin cy:
12

=

Khi o mt i lng no ta c , thay i ty ngi o, s ln o. Nhng vn
ta quan tm l t cho php ta nh gi c khong gi tr ca :

< < +

Kim tra thng k cc d liu thc nghim:
Chun Fisher (F): Chun F dng so snh lp li ca hai dy th nghim:
12
F= (chn sao cho 12 > 12 )
22
Sau tra bng F (p=0,95 ng vi k 1 , k 2 l bc t do ca hai dy th nghim)

Nu F TN < F (p, k1, k2) suy ra lp li ca hai phng php l ng nht ng
ng vi tin cy p
Chun t
Tm sai s h thng:
Tnh t TN v tra bng t (p, k)
Nu t TN > t (p, k) suy ra s sai khc gia v l ng k v do sai s h thng
gy ra.
2.1. Phng php phn tch khi lng[10]

Nguyn tc chung
xc nh khi lng cu t M c trong i tng phn tch X ngi ta tch
hon ton M ra khi cc cu t khc di dng mt hp cht ha hc c thnh phn
xc nh, v d M m A n . Da vo lng cn ca X v ca M m A n m tnh khi lng
M hoc hm lng % ca M c trong i tng phn tch.
C th tch cu t xc nh di dng hp cht t tan. Nu cu t xc nh d
bay hi hoc c th d dng chuyn thnh hp cht d bay hi nhng iu kin
thc nghim xc nh, th c th dng phng php ui bng cch un nng hoc
nung mu phn tch nhit cao v da vo khi lng hao ht khi x l phn
tch m suy ra hm lng cu t xc nh trong i tng phn tch.
13
Cng c th gi li cu t xc nh sau khi b ui ra khi mu phn tch bng
mt s cht hp ph thch hp. Da vo tng khi lng ca cc cht hp sau th
nghim m suy ra hm lng cu t xc nh c trong mu phn tch.
Phng php phn tch khi lng kt ta ng vai tr quan trng v c ng
dng rng ri nht. Cc giai on c bn c qu trnh phn tch khi lng kt ta
bao gm:
Cn mu v chuyn mu vo dung dch
Lm kt ta cu t xc nh di dng hp cht kh tan (dng kt ta).
Lc v ra kt ta
Sy, nung (nu cn thit) chuyn dng kt ta thnh dng cn.
Cn sn phm kh
Tnh kt qu phn tch.
Trong cc giai on ni trn th giai on lm kt ta ng vai tr quan trng
nht. Vic chn thuc th lm kt ta c ngha to ln i vi chnh xc phn
tch cng nh quyt nh n cc thao tc x l kt ta v sau. Vic chn thuc th
phi cn c vo dng kt ta v dng cn.
Yu cu i vi dng kt ta v dng cn
Dng kt ta l dng hp cht to thnh khi cho thuc th lm kt ta phn
ng vi cu t xc nh. Dng cn l dng cht m ta o trc tip khi lng ca n
tnh kt qu phn tch.Trong nhiu trng hp dng kt ta v dng cn l mt,
v d BaSO 4 , AgCl,Trong nhiu trng hp dng kt ta c thnh phn khng
xc nh nn khng th cn c vo tnh kt qu phn tch, nn sau khi lm kt
ta phi x l ha hc v x l nhit tnh kt qu phn tch, nn sau khi lm kt
ta phi x l ha hc v x l nhit chuyn thnh dng cn c thnh phn xc
nh v c th cn c.
Cc hp cht dng lm dng kt ta phi tha mn cc yu cu sau:
C tan b nht.
C tinh khit cao nht hoc ch cha cc tp cht c th ui d dng khi
sy v nung.
14
Kt ta to thnh phi d x l (khi lc, ra).
D dng chuyn thnh dng cn khi sy v nung.
Thun li nht l chn c kt ta trng thi tinh th to ht v t hp th
cht bn, d lc, d ra.
Dng cn phi tha mn cc yu cu sau:
C thnh phn ha hc ng ng cng thc
Bn ha hc ngha l khng b thay i trong qu trnh thao tc phn tch v
sau (khng b oxi ha bi khng kh, khng ht m hoc hp ph kh cacbonic v
khng t phn hy).
Cha cu t phn tch vi hm lng cng thp cng tt. iu ny nhm gim
n mc thp nht nh hng ca cc sai s thc nghim n kt qu cui cng.
La chn iu kin lm kt ta
Lng cht phn tch:
Khng nn ly lng cn cht phn tch qu b v s mc phi sai s ln khi
cn. Mt khc, cng khng c ly lng cn qu ln v s thu c qu nhiu kt
ta, lm mt rt nhiu th gi lc, ra v khng tin khi lm vic vi cc dng
dng c phn tch thng thng (phu lc, chn nung, cc). Thng thng khi
phn tch nhng hp cht xc nh trong ch cn phn tch hm lng mt cu t
chnh th ch cn phn tch hm lng cn t 0,2g (i vi cc kim loi nh) n
1g (i vi qung, silicat). Khi phn tch cc lng vt th ty theo mu m c
th ly lng cn ln t 10-100g.
Cht lm kt ta:
Cht lm kt ta thng chn sao cho tan kt ta to thnh l b nht, v
phi c tnh chn lc, ngha l khng lm kt ta ng thi cc ion khc c trong
dung dch phn tch. Phi chn cht lm kt ta v lng d ca n sao cho sau khi
lm kt ta, lng cu t xc nh cn li trong dung dch khng vt qu gii hn
chnh xc php cn (0,0002g). Thng thng nng thuc th lm kt ta bao
gi cng ln hn nhiu ln nng cu t cn xc nh.
Khi lm kt ta cc kt ta tinh th th nn tin hnh lm kt ta chm t cc
15
dung dch long bng cc thuc th long. Nu kt ta l v nh hnh (mt s
hidroxit, sunfua), nht l kt ta a nc, th tt nht l lm kt ta cc dung dch
c bng cc thuc th c nng cao v lm kt ta nhanh, nhm mc ch lm
gim b mt chung v gim th tch kt ta. Sau khi lm kt ta xong li pha long
vi nc trc khi lc gii hp mt phn ln cc ion l ra khi b mt kt ta v
lm cho vic lc c d dng.
Nhit
Ni chung, thng lm kt ta khi un nng. i vi kt ta tinh th th vic
un nng c tc dng lm tng tan, lm gim qu bo ha tng i v gim
c s trung tm kt tinh ban u, to c kt ta tinh th to ht.
i vi kt ta v nh hnh, vic un nng gip ng t v lm to ht.
i vi cc kt ta c tan tng khi un nng th trc khi lc phi lm
ngui v phi ra bng nc ra ngui. i vi kt ta keo c tan b nh Fe(III)
hidroxit th phi lc nng v ra bng nc ra nng trnh s pepti ha.
Lc v ra kt ta
Hnh 2.1. Phng php lc kt ta

Trong nhiu quy trnh phn tch khi lng ngi ta ngh lng dung dch
mt thi gian trc khi lc. i vi kt ta tinh th vic lng c tc dng thc
y qu trnh mui, do kt ta tch ra sch hn, to ht, d lc. Thi gian lm
mui c th ko di t na gi n 24 gi. Tuy vy cn xem xt tng trng hp c
16
th trnh sai s c th xy ra.
Lc l bin php nhm tch ta ra khi dung dch.
Nu ta c nung nhit cao: dng phu thy tinh v giy lc hu nh
khng tro (lng tro sau khi nung t 3x10-5 5x10-5g). Giy lc c kch thc l
xp thay i, thng gm 3 loi: l xp mn, l xp trung bnh v l xp kh ln,
v hp c mu khc nhau c qui c ty theo nh sn xut v c la chn
sao cho ta khng chui c qua giy lc m thi gian lc khng qu chm. V d:
c, giy lc bng xanh c s dng cho cc kt ta ht mn, giy lc bng
vng dng cho kt ta ht trung bnh v giy lc bng dng cho kt ta ht ln
hoc kt ta v nh hnh.
i vi kt ta d b kh trong qu trnh t chy giy lc hoc nung (do
carbon ca giy) hoc nu ta c sy di 2500C dng phu thy tinh c. Mng
lc l lp thy tinh c nh hay lp bt amiang. mn ca mng lc cng c
la chn ph thuc vo kch thc ta.
Ra ta: l dng dung dch ra lm sch ta. Dung dch ra thng c cc
c im:
Nng ( tng qu trnh gii hp)
Cha ion chung so vi ta chnh ( lm gim tan ta)
C th cha lng nh acid hay baz lm gim s thy phn
Cn thm cht in ly thch hp gim hin tng peptit ha (ta v nh
hnh sau khi ng t tr li dng keo). Thng dng NH 4 NO 3 hay cc acid d
bay hi khi chuyn sang dng cn.
Thc ra, qu trnh lc v ra ta thng c tin hnh song song. Vic ra
ta c thc hin nhiu ln bng cch lc gn ta vi cc lng nh dung dch
ra sao cho lng dung dch ra dng va lm sch ta nhng khng lm
tan ta v tn thi gian.
Chuyn kt ta sang dng cn
chuyn dng kt ta sang dng cn thng dng phng php sy kh v
nung nhm mc ch ui ht nc hp ph hoc nc kt tinh, hoc chuyn hon
17
ton thnh hp cht c thnh phn xc nh, hoc phan hy hon ton tp cht gi
li trn kt ta khi ra.
Phng php ph bin chuyn dng kt ta thnh dng cn l nung nhit
t 6000C 11000C.
Nu thnh phn ha hc cht kt ta khng thay i khi chuyn sang dng cn
(BaSO 4 , PbSO 4 , AgCl,) th khng cn nung nhit qu cao.
i vi cc kt ta b thay i thnh phn ha hc khi chuyn sang dng cn
(v d, kt ta Fe(III)hidroxit) th phi nung nhit cao.
Cn
Cn dng xc nh khi lng dng cn thu c l cn phn tch (chnh
xc 0.0001g hay hn na). Lun lun phi s dng php cn lp xc nh
khi lng ca ta: b (vt cha ta) c sy hay nung trc cng nhit s
sy v nung ta. ngui trong bnh ht m v cn, c khi lng m 0 (g). B
cng ta c sy (nung) ngui v cn, c khi lng m1 (g).
m1 = m 0 + m kt ta
Suy ra m kt ta = m1 m 0
2.2. Phng php phn tch th tch [10, 12]
Buert cha dung

dch chun
Bnh tam gic cha Dung

dch mu v ch th
Hnh 2.2. Phng php chun th tch

2.2.1. Phng php chun axit- baz
Mt trong cc phng php phn tch th tch quan trng l phng php
chun axit- baz, da trn s tng tc gia cc axit- baz v c dng nh
18
lng chng.
Ch th axit baz
Ch th dng trong chun axit baz phi tha mn yu cu c bn l s
i mu ca ch th phi thun nghch theo s thay i pH ca dung dch trong qu
trnh chun .
Ch th axit baz thng l cc axit hay baz hu c yu v mu ca hai
dng axit v baz phi khc nhau.
Dng tn ti ca ch th c th l HIn, HIn+, HIn-, (hay InOH) v c th chia
thnh 3 loi ch yu sau :
Cc ch th thuc loi phenolphtalein :
Phenolphtalein, Thymolphtalein, Naphtolphtalein
C ch i mu ca phenolphtalein :
Phenolphtalein c khong chuyn mu t pH = 8 (khng mu) n pH = 9,8
(mu tm hng)
OH OH OH OH
C H 2O C OH-
O OH
CO - H2O H+
COO-
Dng A: lacton, khng mu Dng B: Mui, khng mu

(pH < 8) (pH = 8)
O O- -O O-
Rat kiem
OH- C C
+ H+ OH
H COO- COO-
Dng C: quinon, mu hng Dng D: Cacbinol, khng mu

(pH = 8-12) (pH > 13,5)
Hnh 2.3. C ch i mu phenolphatalein [7]
Cc sulfophtalein: phenol , brom phenol xanh, crezol
C ch i mu ca phenol : phenol c khong chuyn mu t pH = 6,2
19
(mu vng) n pH = 8,0 (mu ).
+ -
HO OH O OH O O
-
C - C + OH C
+ OH
+
- + - +H -
SO 3 +H SO 3 SO 3
Mu (pK 1 = 1,5) Mu vng (pK 2 = 7,9) Mu

Hnh 2.4. C ch i mu ca Phenol [12]
Cc hp cht azo: metyl da cam, tropeolin, metyl , metyl vngc
mu vng trong mi trng trung tnh v kim, mu trong mi trng trong axit.
C ch i mu ca metyl da cam: Metyl da cam c khong chuyn mu t
pH = 3,1 (mu ) n pH = 4,4 (mu vng)
+ OH-
+
N(H3C)2 N N SO3- N(H3C)2 N N SO3-
H + H+
Mu (dng quinon) Mu vng (dng benzen)

Hnh 2.5. C ch i mu ca Metyl da cam [7]
Khong pH chuyn mu
Khong pH ti ch th i mu gi l khong chuyn mu ca ch th. Mi
ch th (dng axit) trong dung dch c cn bng phn ly nh sau:
HIn H+ + In- K* (Hng s cn bng iu kin)
H + In
K =
*
[ HIn ]
H + = K *
[ HIn ]
[ In ]
=
pH pK * + lg
[ In ]
[ HIn ]
Trong pK*
= pK + lg
f ( In )
. T s
[ In ] l gi tr quyt nh mu ca dung
f ( HIn ) [ HIn ]
dch.
Gi s dng In ca ch th c mu vng, dng HIn c mu th ta s thy
20
mu nu t s
[ HIn ] > 10 , v ta s thy mu vng nu t s [ In ] > 10 .
[ In ] [ HIn ]
Trong khu vc
1
<
[ In ] < 10 ta s thy mu trung gian ca hai mu v
10 [ HIn ]
vng.
1
Vy khong chuyn mu ca ch th l: pK * + lg < pH < pK * + lg10
10
Tc l: pK * 1 < pH < pK * +1
C nhng ch th axit baz c th i mu khi cha t c t l gia hai
dng axit v baz l 1/10 nn c khong chuyn mu nh hn 2 n v (V d:
metyl da cam c khong chuyn mu ch t pH = 3,1 n pH = 4,4)
i vi loi ch th ch c mt mu, tc l ch c mt trong hai dng axit hoc
baz lin hp c mu, v d: ch th c dng HIn m dng HIn khng c mu th
mu ca ch th s do dng In- quyt nh. Nu C l gi tr nng ca In- cn t
ti c th nhn bit mu ca n v C o l nng ban u ca n th pH ca dung
Co C
dch ti mu ca In- bt u xut hin l: =
pH pK * lg
C
Nh vy, pH lm i mu ph thuc nng cht ch th. V d: Trong dung
dch phenolphtalein bo ha, mu hng xut hin khi pH = 8 cn trong dung dch
long hn 10 ln th pH = 9 mi xut hin mu hng.
Bng 2.1. Mt s ch th quan trng v khong chuyn mu ca ch th [7]
c Mu
Nng Mu Khong
Ch th Dung mi tnh ch dng
% dng axit i mu
th baz
Alizarin vng Nc 0,1 axit vng tm 10,1- 12
Khng
Thimoltalein Cn 90% 0,1 - Xanh 9,3- 10,5
mu
0,1 v
Phenolphtalein Cn 90% - - 8,0- 10,0
1
21
Cn 20% 0,05 - - - 7,4- 9,0
trung tnh Cn 60% 0,1 Baz vng 6,8- 8,0
Phenol Cn 20% 0,1 Axit Vng 6,4- 8,0
Bromthimol
Cn 20% 0,05 Axit Vng Xanh 6,0- 7,6
xanh
Qu Nc 1 Axit Xanh 5,0- 8,0
0,1 v
Metyl Cn 60% Baz Vng 4,0- 6,0
0,2
Bromcresol lc Cn 20% 0,02 Axit Vng Xanh 4,2- 5,4
Metyl da cam Nc 0,1 Baz Hng Vng 3,1- 4,4
Bromphenol
Nc 0,1 Axit Vng Nu 3,0- 4,6
xanh
0,1 v
Tropeolin OO Nc Baz Vng 1,4- 3,2
0,01
Ch s chun pT ca ch th
Trong khong pH chuyn mu ca ch th c mt gi tr pH, ti mu ca ch
th chuyn i l r nht. Gi tr pH ny gi l ch s chun ca ch th v k hiu
l pT. Ch s chun pT ph thuc vo ch th v th t ca php chun .
V d:
- i vi phenolphtalein: khi chun axit bng kim, dung dch chuyn t
khng mu sang mu hng ti gi tr pH = 9 nn ch th c pT = 9. Khi chun
kim bng axit, dung dch chuyn t mu hng sang khng mu ti gi tr pH = 8
nn ch th c pT = 8.
- i vi metyl da cam: khi chun axit bng kim, dung dch chuyn t
mu sang mu vng ti gi tr pH = 4,4 nn ch th c pT = 4,4. Khi chun
kim bng axit, dung dch chuyn t mu vng sang hng cam ti gi tr pH = 4 nn
ch th c pT = 4. Ngoi ra, gi tr pT cn ph thuc vo nhit , dung mi, lc ion
ca dung dch.
22
Nguyn tc chn ch th cho mt php chun :
php chun c tnh chnh xc cao, ta phi chn cht ch th no c
khong chuyn mu trng vi khong bc nhy chun ca php chun , tt
nht l chn ch th c gi tr ch s chun pT gn trng vi gi tr pH ca dung
dch chun ti thi im tng ng.
Ch : Mun tng chnh xc ca mt php chun cn phi:
Chn ch th chnh xc (l nhng ch th c pT = pH t ca phn ng chun )
Lng ch th cho vo bnh chun phi ging nhau i vi cc ln chun
khc nhau.
Cho t ch th (2 3 git) v ch th axit baz l nhng axit hoc baz yu
dn ti tiu hao dung dch cht chun.
Chun n mu ging nhau (cn c bnh i chng)
Nn s dng mt ch th nht nh cho mt php chun c th.
2.2.2. Phng php oxi ha-kh
Trong phng php chun oxi ha kh ngi ta tin hnh phn ng chun
, l phn ng trao i electron gia dung dch chun cha cht oxi ha (hoc kh)
vi dung dch cht phn tch cha cht kh (hoc cht oxi ha). nhn bit im
tng ng ngi ta dng cc cht ch th.
ng chun oxi ha- kh
ng cong chun oxi ha kh biu din s ph thuc gia th ca dung
dch chun v th tch cht chun dng ( thi E V) hoc biu din s ph
thuc gia th ca dung dch chun v t s ng lng gia cc cht tham gia
phn ng chun ( th E P).
Khi cho mt th tch xc nh dung dch chun ca cht oxi ha (hay kh) vo
dung dch cn chun cha cht kh (hay cht oxi ha) th xy ra phn ng oxi
ha kh, lm thay i nng ca cc cht phn ng sao cho khi cn bng th oxi
ha ca hai cp oxi ha kh tr nn bng nhau ti mi im ca ng cong.
tnh th ti cc thi im chun ta c th dng phng trnh Nernst p dng cho
cc h oxi ha kh bt k tham gia trong phn ng. Tuy vy, thng s dng nh
23
sau:
Trc im tng ng: Tnh th ca h theo th ca cp oxi ha kh cht
phn tch cn chun .
Sau im tng ng: Tnh th ca h theo th ca cp oxi ha kh cht
chun.
Ti im tng ng: t hp cc biu thc tnh th ca c hai cp oxi ha
kh (cht phn tch v thuc th). Th ny l th hn hp ca c hai cp.
Cc cht ch th dng trong chun oxi ha- kh [8]
Trong chun oxi ha kh thng dng cc loi cht ch th sau y:
Cc cht ch th c bit phn ng chn lc vi mt dng no ca
cp oxi ha kh v gy ra s i mu (loi ch th ny khng nhiu).
V d: H tinh bt to mu xanh vi iot.
SCN- to mu vi ion Fe3+.
Bn thn cht oxi ha hoc kh trong php chun c mu v mu ca hai
dng oxi ha v kh ca n khc nhau. V d: MnO 4 - c mu tm cn Mn2+ hu
nh khng mu (phng php Pemanganat).
Ch th oxi ha kh: cht ch th c tnh oxi ha kh v mu ca hai
dng oxi ha v kh khac nhau. Mu ca ch th thay i ph thuc th ca cht ch
th v ca h chun . (Loi ch th ny c nhiu v c v tr quan trng trong
chun oxi ha kh).
Phn ng oxi ha kh ca ch th l phn ng thun nghch:
Inox + ne Inkh
Mu ca dung dch chun khi c cht ch th oxi ha kh ph thuc vo t
[Inox ]
s nng hai dng oxi ha v kh ca ch th, tc l ph thuc vo t s
[Inkh ]
trong phng trnh Nernst dng cho ch th:

RT [Inox ]
E = E0In + ln
nF [Inkh ]
Vi E0 l th thc ca ch th.
Nu cng mu ca hai dng xp x nhau th khong chuyn mu nm
24
[Inox ] 1
trong khu vc t s nng giao ng t n 10, khong th tng ng
[Inkh ] 10
bng:
0.059
E = E0In ( 250C)
n
0.060
E = E0In ( 300C)
n
i vi cc cht tham gia phn ng chun ta c th chuyn i trng thi

oxi ha ln cao hn hay xung thp hn chun cho thch hp. Cc giai on
oxi ha v kh trc chun ny phi theo ng cc yu cu nghim ngt l phn
ng phi xy ra hon ton vi tc nhanh v phi c kh nng loi b cc cht oxi
ha hay cht kh d. Phn ng ph ny phi chn lc, trnh lm nh hng cc
thnh phn khc trong mu phn tch.
Mt s cht ch th oxi- ha kh thng dng [8]:
Diphenylamin: C 6 H 5 NHC 6 H 5 , diphenylamin khng mu, u tin b oxi ha
khng thun nghch n diphenylbenzidin khng mu, cht ny b oxi ha tip tc
n benzidin mu tm. in th chun E0 hu nh khng ph thuc vo pH ca
dung dch, trong mi trng H 2 SO 4 0,5-1M th E0 = 0,76V. Ch th thng c
dng trong php chun dicomat, pemanganat, vanadat, Xeri(IV) bng Fe(II).
Feroin: l phc ca ion Fe2+ vi o-phenantrolin to thnh ion phctri-(1,10-
phenantrolin)Fe(II). Feroin c mu khi b oxi ha th chuyn thnh phc ca Fe3+
c mu xanh nht. Phn ng ca ch th l thun nghch. in th chun ca n
trong dng dch axit nng 1M (HCl hay H 2 SO 4 ) l 1,06V, s chuyn mu xy ra
r th 1,12V. Cht ch th ng dng chun Fe2+ bng Xe4+
Axit diphenylamin sunfonic
c dng vi dng mui Na hay Ba trong nc vi nng t 0,2% n
0,5%. Ch th khi b oxi ha c mu tm nh mu ca KMnO 4 . S chuyn mu
rt r nh trong trng hp diphenylamin. Th thc ca ch th pH = 0 l 0,84V.
C th dng cht ch th ny trong php chun cc cht oxi ha bng Fe2+.
Cc thuc th dng trong chun oxi ha- kh
Trong chun oxi ha kh c th dng thuc th (cht chun) l cc cht
25
oxi ha hay cc cht kh.
Cc cht oxi ha: KMnO 4 , K 2 Cr 2 O 7 , Ce(SO 4 ) 2 , I 2 , KIO 3 , Ca(ClO) 2 .
Cc cht kh: Fe2+, Na 2 S 2 O 3 , As 2 O 3 , H 2 C 2 O 4 , Na 2 C 2 O 4 , K 4 Fe(CN) 6 .
Cn c vo thuc th s dng, ngi ta chia ra cc phng php c tn gi
khc nhau nh: phng php Pemanganat, phng php icrmat, phng php
Iot, phng php Xeri
2.2.3. Phng php chun kt ta
Phn ng to thnh kt ta c s dng trong hai phng php phn tch,
l phng php chun kt ta (thuc phng php phn tch th tch) v phng
php phn tch khi lng.
S phn ng kt ta c dng trong phng php chun rt hn ch do:
Trong cc dung dch long cc phn ng kt ta xy ra rt chm. c bit
gn im tng ng, khi nng cc cht rt nh th vn tc phn ng nh
khng tha mn yu cu ca php phn tch th tch.
Phn ng to kt ta thng km theo phn ng ph, lm sai lch kt qu do
khng bo m c tnh hp thc. (v d: cc phn ng ph nh: hp ph, cng
kt, to dung dch rn)
Trong s cc phn ng kt ta c s dng, quan trng nht l cc phn ng
kt ta cc ion halogen bng AgNO3 v php phn tch s dng kt ta bng
AgNO3 thng gi l phng php bc (hay php o bc).
Phn ng chun
Phn ng chun l phn ng kt ta, v d:
AgNO 3 + NaCl NaNO3 + AgCl
Cc qu trnh xy ra trong h l:
Phn ng chnh l phn ng kt ta:
Ag+ + Cl- AgCl Ks-1
Phn ng ph l phn ng to phc hydroxo:
Ag+ + H 2 O AgOH + H+ (hay l *)
ng cong chun
26
Trong chun kt ta nghi ta xy dng ng cng chun l ng
biu din s ph thuc ca lg [Ag+] tc l P(Ag+) hay lg [Cl-] tc l P(Cl-) vo t
CV
s (k hiu l P).
C0 V0
tnh ton, thng s dng tch s tan iu kin: Ks = [Ag+][Cl-]

Trong : [Ag+] = Tng nng Ag+ cha b chun
= [Ag+] + [AgOH] = [Ag+](1+ h-1)
1 1
= [Ag+] vi Ag+ =
Ag+ 1+ h1
[Cl-] = [Cl-]
Ks
T ta c Ks = . Nu trong dung dch khng c s to phc ph khc
Ag+
th Ag+ ph thuc pH ca dung dch. xy dng ng cong chun ngi ta

tnh ton cc gi tr [Ag+] v [Cl-].
Theo nh lut bo ton nng ban u ta c:
CV
CAg+ = = [Ag+] + mAgCl (1)
V+ V0
C0 V0
CCl = = [Cl-] + mAgCl (2)
V+ V0
Trong mAgCl l s mol AgCl kt ta trong mt lt dung dch. T (1) v

(2) ta c
CV C0 V0
[Ag+] - [Cl-] = -
V+ V0 V+ V0
C0 V0
Chia c hai v cho ta s thu c :
V+ V0
V+ V0
P 1 = ([Ag+] [Cl-])
C0 V0
Ks
M P -1 =q (sai s cu php chun ) nn khi thay [Cl-] = th phng
[Ag+ ]
trnh trn s c dng:

C0 V0 V+ V0
q = ([Ag+] - )
V+ V0 C0 V0
y l phng trnh tnh sai s ti mt im bt k trn ng cong chun .

V+ V0 C+ C0
gn im tng ng th = do phng trnh s c dng:
C0 V0 CC0
27
C0 V0 C+ C0
q = ([Ag+] - )
V+ V0 CC0
Nu q = 2% th bc nhy chun (BNC) theo PCl ko di t PCl = 4

n PCl = 6 v theo PAg+ th s ko di t PAg+ = 6 n PAg+ = 4. ng cong
chun hon ton i xng.
Bc nhy chun ph thuc nng cc cht chun v tch s tan ca hp
cht t tan c to ra trong phn ng chun y.
Nu phn ng to hp cht t tan theo kiu M:2A hay 2M:A th ng cong
chun khng i xng qua im tng ng na.
2.2.4. Phng php chun phc cht
Phng php chun complexon
Phn ng to phc rt nhiu nhng s phn ng to phc c dng nh
lng bng phng php th tch khng nhiu, bi v phn ln cc phn ng ny
khng tha mn yu cu chung ca phn tch th tch l phi xy ra vi tc ln,
xy ra hon ton, ng t lng v khng c phn ng ph.
Trong chun complexon, cht to phc thng s dng l axit
etylendiamin tetraaxetic (cn gi l complexon II hay EDTA) c cng thc:
HOOC-CH2 CH2-COOH
N-CH2-CH2-N
HOOC-CH2 CH2-COOH
EDTA l axit 4 nc H4Y:
K 1 = 10-2, K 2 = 10-2,76, K 3 = 10-,16, K 4 = 10-10,26.
EDTA t tan trong nc, v vy hay dng di dng mui dinatri Na 2 H 2 Y 2 ,
thng gi l complexon III (thi quen vn gi l EDTA)
EDTA to phc bn vi cc ion kim loi v trong hu ht trng hp phn
ng to phc xy ra theo t l ion kim loi : thuc th = 1: 1
Mn+ + Y4- MY(n-4)+
Hng s to phc ph thuc vo nhiu yu t, trong c bn cht ca ion
kim loi Mn+ (ion kim loi to phc vi ion Y4-) v mi trng.
28
Thng th cc php chun complexon c tin hnh khi c mt cc cht
to phc ph duy tr pH xc nh nhm ngn nga s xut hin kt ta hydroxit
kim loi.
ng cong chun
Gi s chun V 0 ml ion M ( n gin khng ghi in tch) c nng C 0
mol/l bng dung dch EDTA c nng C mol/l v th tch tiu tn l V ml.
0 0
= [] + []
0 +

= [] + []
0 +
0 0
[] [] = =
0 +
0 0
Chia hai v cho v t hp cc h thc, ta c:
0 +
0 +
= 1 = ([] [] )
0 0
0 0
P= (phn ng xy ra theo t l 1:1 nn vn dng t s mol thay t s ng
0 +
lng).
q- sai chun .
0 +
Trc tng ng: p<1, [] > [] thiu chun , = []
0 0
0 +
Sau tng ng: p>1, [] < [] tha chun , = []
0 0
Ti tng ng: q=0 nn ta c:
1
[ ] =
0 0
ng cong chun cc ion kim loi M bng dung dch complexon III
(Na 2 H 2 Y) biu din s ph thuc ca i lng pM theo P, thng c dng sau:
29
pM
0 0
P=
0 +
Hnh 2.6. ng cong chun ion kim loi Mn+ bng Na 2 H 2 Y [12]
ng chun complexon cng c dng nh cc ng chun hc
(axit-bazo, oxi ha-kh), gn im tng ng c bc nhy chun , bc
nhy chun ph thuc vo cc gi tr , pH, C, C 0 (hng s bn iu kin ca
phc, pH ca mi trng, nng ca ion kim loi v ca EDTA).
Trong ta thy ph thuc pH v nng ca cht to phc ph, khi cho
thm dung dch m NH 3 + NH 4 Cl to pH = 9-10 th ion Mn+ s tc dng vi cc
phn t NH 3 to phc theo phn ng
Mn+ + NH 3 (3 )+

Ch th trong chun complexon

Trong chun complexon, xc nh im cui thng dng mt s loi
ch th nh sau:
Ch th mt mu: Loi ch th ny c mu nht hoc khng c mu,
to c vi ion kim loi phc c mu c trng. (V d: ion SCN- to vi ion Fe3+
phc c mu , ion Co2+ phc c mu xanh). Ty theo th t chun m mu
mt i hay xut hin vo im cui chun .
Ch th hunh quang: l loi ch th khi to phc vi ion kim loi lm
cho ch th c mu hay cng hunh quang ca ch th b thay i (c th lm tt
hoc lm mnh ln cng hunh quang ca ch th ti im tng ng do lc
phc vi ion kim loi ht, trong dung dch ch c phc ca ion kim loi vi
EDTA).
Ch th oxy ha kh: Nu ch th kim loi to phc c c hai dng
30
oxy ha v kh th s dng ch th oxy ha kh.
Ch th mu kim loi (ch th complexon) l cc thuc nhum hu
c, to c vi ion kim loi phc c mu c trng, khc vi mu ca ch th dng
t do. im cui chun c xc nh da theo s thay i mu ca phc kim
loi ch th (MIn) sang mu ch th ca dng t do (In) hoc ngc li.
Mt ch th mu kim loi s c s dng trong chun complexon khi tha
mn cc yu cu sau y:
C nhy cao: Ch cn mt lng v cng nh ca ch th lin kt vi ion
kim loi ngi chun cng c th nhn thy s thay i mu ti im cui chun
, nh vy phn ion kim loi lin kt vi ch th l khng ng k (10-5-10-6M),
khng cn tnh n khi tnh sai s ca php chun .
Phc gia ch th v ion kim loi (dng MIn) phi c bn tng i cao
trong phm vi ca php chun v phi km bn hn phc gia ion kim loi v
thuc th EDTA (dng MY):
104< MIn < MY .10-4
vic xc nh im cui chun c chnh xc, phn ng to phc gia
ion kim loi v ch th phi xy ra nhanh, hon ton thun nghch.
C ch i mu ca ch th trong chun complexon nh sau:
Phn ng to phc mu gia ion kim loi M v ch th In xy ra theo phn
ng:
M + In MIn MIn
Hai dng In v MIn c mu khc nhau. Khi chun bng EDTA, u tin ion
kim loi M t do (phn khng lin kt vi ch th) to phc vi EDTA, khi n
im tng ng, EDTA s tc dng vi phc gia ion kim loi v ch th (MIn),
to nn phc MY v gii phng ra ch th dng In c mu khc vi mu ca dng
MIn:

M In + Y4- MY + In =

Phn ng ny xy ra ti im tng ng v do dng MIn c mu khc vi
31
dng In nn ngi ta c th dng chun ng vi im tng ng (im
tng ng trng vi im cui chun ). Nu phc MIn khng chuyn hon
ton sang dng In th ta s c sai s chun .
V d: chun ion Mg2+ bng EDTA s dng ch th Eriocrom en T. Dung
dch Mg2+ ban u, sau khi iu chnh mi trng cho ph hp vi php chun ,
thm 3-4 git ch th th c mt phn v cng nh Mg2+ s tc dng vi ch th
Eriocrom en T to nn phc MgIn (MgIn c mu mn mi trng pH=10),
cn phn ln vn tn ti di dng Mg2+ t do. Khi chun bng EDTA, trc ht
ion Mg2+ t do s tc dng vi EDTA to phc MgY, khi ht ion Mg2+ t do,
EDTA s tc dng vi MgIn to nn phc MgY v gii phng ra ion ca ch th l
In c mu chm. Git dung dch chun EDTA cui cng phi lm mt nh ca
dung dch cn chun v ta dng php chun ..
Mt s ch th mu kim loi hay dng
Ch th Eriocrom en T (cn gi tt l ERIOT-k hiu ET-00)
ERIOT l mt thuc nhum azo, c cng thc l:
OH OH
HO3S N N
O2 N
Trong dung dch c s phn ly nh sau:

NaH 2 In Na+ + H 2 In-
H 2 In- H 2 In2- + H+ 1 = 106,3
HIn2- In3- + H+ 2 = 1011,5
Mu ca chit h ERIOT thay i ph thuc vo nng ca cc dng khc
nhau ca n (H2In-, HIn2-, In3-) tc l ph thuc vo pH ca dung dch.
Bng 2.2. Khong pH i mu ca ch th ERIOT
Dng tn ti H 2 In- HIn2- In3-
Khong pH pH <7 7< pH <11 11< pH
Mu Xanh Vng cam
32
Khi gi tr 7< pH <11 th ch th ERIOT dng HIn2- c mu xanh. Nhiu ion
kim loi (Ca, Mg, Ni, Cu, Al, Hg, Cd, Pb, Ti, Fe, Co, nhm Pt) to vi dng ny
ca ch th hp cht phc c mu vi nhy rt ln (10-6 10-7)
M2+ + HIn2- MIn- + H+ K = MIn .K 3
[ ] .[ + ]
K =
[2+ ] .[3 ]
Trong , [In3-] = C In = [H 2 In-]+ [HIn2-]+ [In3-] v K l hng s cn bng
iu kin.
[ ]
T s quyt nh s chuyn mu ca cht ch th, iu chng t s
[3 ]
chuyn mu ca ch th ph thuc vo pH ca dung dch.
Murexit
Murexit l mui amoni ca axit pupuric C 8 H 5 O 6 N 5 . Trong mi trng axit
mnh anion H 4 In-.
Anion H 4 In- ca murexit nm trong dung dch axit mnh. Axit pupuric l a
axit c pK 1 =0, pK 2 =9,2, pK 3 =10,9 nn mu ca cc dng cht ch th ph thuc pH
ca dung dch. Trong dung dch nc c pH < pK 2 cht ch th c mu tm, trong
khong pH t pK 2 -pK 3 c mu tm hoa c v khi pH = pK 3 cht ch th c mu xanh
tm. Murexit to vi Ca2+ pH = 12 phc c mu , to vi Co2+, Cu2+, Ni2+ pH
trong khong 7-9 (dung dch m amoniac) phc c mu da cam, to vi ion Ag+
trong dung dch m NH 3 c pH 10-15 phc mu .
Murexit l cht ch th tt cho vic chun trc tip cc ion Ca2+, Cu2+, Ni2+,
Ag+
Cc phng php tin hnh chun Complexon
Chun trc tip
Trong phng php ny ngi ta iu chnh pH cn thit ca dung dch cn
chun (thng l complexon III) cho n khi mu ca phc kim loi vi ch th
sang mu ca ch th dng khng to phc. ngn nga s to hydroxit kim loi
pH chun ngi thng thm cc cht to phc ph tng i yu, v d dng
33
hn hp m NH 3 + NH 4 Cl duy tr pH = 10 khi chun cc ion Zn2+, Cu2+,
Ni2+, gi cc ion ny trong dung dch dng phc amin
Chun ngc
Khi khng th chun trc tip c, v d khng c cht ch th thch hp,
hoc phn ng to phc gia ion kim loi v EDTA xy ra qu chm, c bn qu
nh hoc pH chun ion kim loi b kt ta di dng hydroxit, th s dng
phng php chun ngc.
Trong phng php chun ny, gi s phi chun ion kim loi M 1 ,
ngi ta thm vo dung dch cn chun mt lng chnh xc EDTA ly d v
thit lp cc iu kin cn thit ion kim loi M 1 tc dng ht vi EDTA. Sau
chun lng d EDTA bng mt dung dch chun ca ion kim loi M 2 cho n
khi dung dch i mu t mu cha ch th dng t do sang mu ca dng phc
gia ch th vi ion kim loi M 2 . Nu phn ng gia kim loi M 1 vi EDTA xy ra
chm th phi un nng v phi i cho phn ng xy ra hon ton, sau mi iu
chnh pH ca dung dch n gi tr thch hp cho php chun ngc ca ion kim
loi M 2 .
Khi phn ng to phc gia M 1 v EDTA xy ra khng chm th phi chn
sao cho hng s bn iu kin ca phc M 2 - EDTA (M 2 Y) b hn hng s bn
iu kin ca phc M 1 -EDTA (M 1 Y) nhng khng c nh hn 107
M 1 Y < M 2 Y < 107
Trong thc t hay chn Mg chun ngc v phn ln cc kim loi to
vi EDTA phc bn hn phc ca Mg vi EDTA v php chun c ch th tt l
ERIOT
Chun th
Nu phn ng ca mt ion kim loi to phc bn vi EDTA xy ra chm,
khng th chun trc tip c th ta c th thay M 1 bng mt ion M 2 c kh
nng to phc bn vi EDTA xy ra nhanh, c th chun trc tip bng EDTA
c theo phn ng:
M1 + M2Y M1Y + M2
34
Sau chun trc tip M 2 bng dung dch EDTA. Ta phi chn phc M 2 Y
sao cho tha mn iu kin M 2 Y < < M 1 Y nhng M 2 Y phi ln hn 107
bo m chnh xc ca php chun . Ngi ta thng dng phc MgY v sau
chun Mg2+ bng EDTA.
Chun gin tip
Nu cht phn tch khng c phn ng trc tip vi EDTA th dng phng
php chun gin tip.
V d: Ion SO 4 2- khng tc dng trc tip vi EDTA c, ngi ta cho SO 4 2-
tc dng vi mt lng Ba2+ chnh xc, Ba2+ s tc dng vi to kt ta. Lng d
s c chun bng dung dch EDTA t suy ra lng SO 4 2- cn phi tm.
xc nh lng ion PO 4 3- ngi ta cho dung dch phn tch tc dng vi
mt lng chnh xc Mg2+ trong mi trng NH 4 + to kt ta MgNH 4 PO 4 v sau
chun lng Mg2+ d bng dung dch EDTA t suy ra lng PO 4 3- cn
phi tm.
35
Kha lun tt nghip Thc nghim
PHN 2.
THC NGHIM
36
CHNG 3: KHO ST THC TRNG DY- HC PHN THC HNH

PHN TCH NH LNG HA HC
3.1. Kho st bng hnh thc phiu iu tra

iu tra thc trng v cc gi thc hnh Phn tch nh lng Ha hc ca
sinh vin khoa Ha trng i hc S phm H Ch Minh
3.1.1. Cch tin hnh
Chng em tin hnh iu tra vi cc sinh vin lp Ha 4A, 4B v 4C nm
hc 2012-2013.
S phiu pht ra: 150
S phiu thu v: 137; trong lp Ha 4A: 35 phiu, lp 4B: 33 phiu, lp
4C: 47 phiu v lp 3C: 22 phiu
3.1.2. M t phiu iu tra
Trong phiu iu tra chng em s dng 22 cu hi (gm 21 cu hi ng v 1
cu hi m). Ni dung cc cu hi tp trung vo 2 ch chnh l:
Thc trng vic hc thc hnh Phn tch nh lng Ha hc (t cu 1 n cu
15)
Nhu cu thay i hoc ci tin gi thc hnh Phn tch nh lng Ha hc (t
cu 16 n cu 21)
3.1.3. Phn tch kt qu iu tra
Khi vit phiu sinh vin th hin c thc xy dng, mong mun c
ng gp vo vic ci tin ni dung v phng php trong cc gi thc hnh Phn
tch nh lng Ha hc. Tuy nhin cng cn mt s phiu khng tr li ht cc cu
hi hoc nh du vo mc khng quan tm.
37
Sau y l kt qu phn tch phiu iu tra:

Cu 1: i vi cc gi thc hnh Phn tch nh lng ha hc bn cm thy:
Thi T l %
Rt thch 6,84
Thch 61,54
Bnh thng 21,37
Khng thch 10,26
Cu 2: Bn c nghin cu ti liu hng dn trc khi vo phng th nghim

hay khng?
Tnh trng T l %
Xem k 40,17
Xem s qua 55,56
Khng xem 4,27
Cu 3: Bn hy chn mc nhiu, t cho cc vn trong gi thc hnh

phn tch nh lng ha hc sau (1: rt t; 5: rt nhiu).
Mc (%)
Vn
1 2 3 4 5
a) Thi lng tin hnh th nghim
9,4 41,03 35,04 11,11 3,42
trong mt bui hc
b) Tng s bui th nghim 15,38 23,93 55,56 3,42 1,71
c) Tng s bi th nghim 15,38 21,37 58,97 2,56 1,71
38
Cu 4: Bn c cm thy hi lng vi ni dung cc bi th nghim ?

Thi T l %
Hon ton hi lng 52,99
Ch hi lng mt phn 43,33
Khng hi lng 3,68
Cu 5: Cc bui thc hnh phn tch nh lng ha hc gip bn rn

luyn: (c th chn nhiu phng n)
Ni dung rn luyn T l %
Thao tc s dng cc dng c th nghim 91.51
Thao tc chun b ha cht, tin hnh, quan st th nghim 86,01
Hiu r hn l thuyt hc 92,45
S dng ha cht vi liu lng chnh xc 83,34
Cch c th tch chnh xc 99,02
Kh nng t duy, tp lm nghin cu khoa hc 85.57
Cu 6: Khi tin hnh th nghim, bn thc s hiu r phn c s l thuyt

cha?
Mc T l %
10-20 % 0
30-40% 15,13
50-60% 30,03
70-80% 49,14
90-100% 0
39
Cu 7: Mc thnh cng cc bi thc hnh Phn tch nh lng ha hc ca

cc bn khong:
Mc thnh cng(%)
Tn bi 10- 30- 50- 70- 90-
20 40 60 80 100
Bi 1: Chun axit mnh bng baz mnh v
0 0 0 23,62 76,94
ngc li
Bi 2: Chun axit yu bng baz mnh 0 0 0 25,79 74,52
Bi 3: Chun baz yu bng axit mnh 0 0 0 27,56 72,39
Bi 4: Chun a axit vi hn hp axit
0 0 0 39,01 41,27
(H 3 PO 4 + HCl) bng baz mnh
Bi 5: Chun a baz vi hn hp baz
0 0 24,83 55,64 19,57
(Na 2 CO 3 + NaOH) bng axit mnh
Bi 6: Chun oxi ha kh. Phng php
0 0 24,30 64,18 11,52
pemanganat
Bi 7 : Chun oxi ha kh. Phng php
0 0 18,25 64,05 16,29
iod
Bi 8 : Chun kt ta 0 0 9,86 41,50 48,87
Bi 9: Chun complexon 0 0 7,29 30,59 61,05
Cu 8: i vi th nghim chun hn hp Na 2 CO 3 v NaOH bng HCl cc

bn thu c kt qu nh th no?
Kt qu T l %
Rt chnh xc. 6,84
Kh chnh xc 58,11
Khng chnh xc 35,04
40
Cu 9: Trong th nghim nh lng Fe bng phng php pemanganat, bn

c thu c kt ta Hg 2 Cl 2 dng di la mng?
Kt qu T l %
Thu c d dng 4,27
Thu c nhng phi sau vi th nghim. 60,43
Hon ton khng thu c. 35,3
Cu 10: Khi chun bn thng chun b bnh tam gic cha dung dch cn
chun nh th no?
Tnh trng T l %
Chun b bnh no th chun bnh . 33,33
Chun b tt c cc bnh ri chun cng mt lc. 10,26
Ty theo tng bi v ha cht s dng 51,03
Ty hng 5,38
Cu 11: S th nghim m bn cm thy hng th khi tin hnh vo khong:

S th nghim T l %
10-20 % 0,00
30-40% 0,00
50-60% 41,03
70-80% 58,97
90-100% 0,00
41
Cu 12: S th nghim m bn tin hnh thnh cng vo khong:

Mc T l %
10-20 % 0
30-40% 0
50-60% 17,61
70-80% 62,39
90-100% 21,45
Cu 13: Sau cc bui thc hnh phn tch nh lng ha hc bn cm thy:

Thi T l %
Rt vui v c hng th 31,37
Bnh thng 34.19
Mt mi 34,44
Cu 14: Theo bn s im bn t c cui hc phn c ph hp vi nng

lc ca bn khi thc hnh?
Thi T l %
Rt ph hp 58,97
t hn so vi kh nng 14,22
Nhiu hn so vi kh nng 26,24
Khng quan tm 1,45
Cu 15: Theo bn thang chm im ca gio vin trong mi gi thc hnh nh

th no?
Thi T l %
Qu kht khe 15.23
Rt tt 52,99
Kh d 32.65
42
Cu 16: Bn cha thch cc gi thc hnh phn tch nh lng ha hc ch:

(c th chn nhiu phng n)
Ni dung T l %
t c bi thc hnh hp dn 52,99
Cc bi thc hnh ch mang tnh minh ha l thuyt, ng dng thc t t 57,26
Mt s bi thc hnh n gin nhng phi lp i lp li nhiu ln 87,18
Mt s bi thc hnh kh, khng thu c kt qu nh mong mun 80,34
Cu 17: Bn thy c cn thit thay i ni dung gio trnh thc hnh phn tch
nh lng ha hc theo khng?
Mc T l %
Rt cn thit 5,13
Cn thit 41,03
Bnh thng 35,04
Khng cn thit 18,80
Cu 18: Bn thy c cn thay i hnh thc gio trnh thc hnh Phn tch
nh lng ha hc hay khng?
Mc T l %
Khng cn thit 18,03
Thm hnh nh minh ha, mu sc, hin tng th nghim 95,73
Cung cp clip thao tc s dng dng c th nghim 72,05
Cung cp cc clip hng dn thc hnh sinh vin d quan st 91,45
43
Cu 19: Bn hy chn mc cn thit trong vic thay i mt s th nghim

trong gio trnh thc hnh phn tch nh lng ha hc (1: rt cn thit; 5: hon
ton khng cn thit).
Mc (%)
S thay i
1 2 3 4 5
a) Thm th nghim phn tch khi lng
1,46 39,88 40,17 12,82 5,13
(v gio trnh ch c phn tch th tch)
b) Thm th nghim nh lng bng
50,42 20,51 9,40 7,69 11,97
phng php dicromat
c) Thm cc th nghim mang tnh ng
72,65 5,98 17,09 1,71 2,56
dng thc t
d) Thm vo giai on t cn, pha dung
19,66 46,50 21,62 9,40 2,82
dch th nghim.
e) Thm tnh khong tin cy trong phn x
4,55 52,07 39,11 2,56 1,71
l kt qu th nghim
Cu 20: Theo bn c cn tin hnh mt bui thi vo cui hc phn thc hnh
phn tch nh lng ha hc hay khng?
Mc T l %
Rt cn thit 4,27
Cn thit 52,14
Khng cn thit 43,59
Hon ton khng cn 0
44
Cu 21: Theo bn phn thi l thuyt cui k v trong mi bui nn tin hnh
di hnh thc no?
Hnh thc thi T l %
T lun 35,04
Trc nghim 26,50
Vn p 38,46
Cu 22: cc bui thc hnh Phn tch nh lng Ha hc mang li kt qu

tt hn theo bn cn phi?
Bn T Trn Kin sinh vin lp Ha 4C vit: Cn tng thm s bui hc,
s bi thc hnh, thi gian thc hnh mi bui thc hnh. Thm vo cc bi thc
hnh ng dng thc t
Bn Nguyn Th Dn An sinh vin lp Ha 4C vit Thi gian thc hnh
mi bui th nghim cn ngn nn khng thi gian lm .
Bn Hunh Th Nhn sinh vin lp Ha 4B vit Bi chun hn hp
NaOH v Na 2 CO 3 ti thu c kt qu cha tt d tin hnh k theo quy trnh
3.1.4. Nhn xt
V thi , tnh cm v nhn thc i vi gi thc hnh phn tch
nh lng ha hc (cu1, 4, 5, 11, 13, 14, 15)
C 68,38% sinh vin cm thy rt thch v thch bui thc hnh, ch chim 2/3
s kin, c n 10,26% sinh vin khng thch bui thc hnh.
C 52,99 % sinh vin cm thy hon ton hi lng vi ni dung cc bi th
nghim chim s kin, cn li cm thy ch hi lng mt phn hoc hon
ton khng hi lng.
Sinh vin ch cm thy hng th i vi 50-80% th nghim, tng ng 4 7
th nghim.
Sau gi thc hnh th nghim c khong 1/3 sinh vin cm thy vui v c
hng th, 1/3 cm thy bnh thng v cn li l thy mt mi.
Trn 85% sinh vin nhn thy c cc tc dng ca gi thc hnh phn tch
45
nh lng ha hc
C hn sinh vin cm thy im s nhn c l ph hp vi kt qu ca
bn thn tng ng cng c sinh vin cm thy thang chm im l rt tt, 1/3
sinh vin cho rng gio vin kh d nn im thu c cao hn so vi kh nng ca
bn thn. Cn li cm thy gio vin qu kht khe nn im thu c t hn so vi
kh nng bn thn.
Qua kt qu iu tra ta thy rng cc bui th nghim thc hnh Phn tch nh
lng ha hc to c tnh cm i vi a s sinh vin. Tuy nhin, t Ha Phn
Tch cn nghin cu a thm nhiu th nghim hp dn gy hng th vo gio
trnh thc hnh. Cn nhc nh sinh vin trong vic bo h lao ng (eo gng tay,
khu trang than hot tnh) gim bt mt phn c hi cho c th.
V cng tc chun b v tin hnh thc hnh Phn tch nh
lng Ha hc (cu 2, 3, 6, 10)
C khong 60% s sinh vin cha nghin cu k ti liu trc khi n phng
th nghim
C khong 80% s sinh vin hiu r 50-80% c s l thuyt.
C khong 80% s sinh vin bit cch chun b mu cn chun vo bnh
tam gic l ty theo tng bi v ha cht s dng, nhiu sinh vin cn thn c th
chun b bnh no th chun bnh . Bn cnh cng c 20% s sinh vin cha
bit cch c bn tin hnh chun dung dch. Gio vin cn hng dn r rng,
hn ch cho sinh vin v sm trc khi ht gi thc hnh, trnh tnh trng c lm
nhanh v sm, dn n thao tc v kt qu khng chnh xc.
C khong 41% s sinh vin cho rng thi lng tin hnh th nghim trong
mt bui hc l kh t(mc 2). C th do thao tc thc hnh cha c nhun
nhuyn nn cn chm chp mt thi gian; bi thc hnh di, nhiu th nghim; hay
gi ging l thuyt bi thc hnh ca gio vin di ln sang gi thc hnh ca sinh
vin;
V mc thnh cng v kt qu th nghim (cu 7, 8, 9, 12)
C khong 50-100% cc bi th nghim c sinh vin tin hnh thnh cng,
46
tc l khong 4-9 bi trn tng s 9 bi.

i vi th nghim nh lng Fe bng phng php Pemanganat c 65% sinh
vin thu c kt ta Hg 2 Cl 2 dng di la mng, nhng vn cn 35% s sinh vin
cha thc hin c giai on ny. Nguyn nhn c th l do: khng xc nh chnh
xc lng SnCl 2 khi cho vo, cho d hoc cho thiu.
100% sinh vin thc hin cc bi th nghim chun axit baz (bi 1-4) thu
c kt qu c chnh xc kh cao (70-100%). Tuy nhin bi 5 chun hn
hp NaOH v Na 2 CO 3 c khong 24% thu c kt qu cha chnh xc (50-60%).
C khong trn 90% sinh vin thc hin cc bi th nghim chun kt ta
(bi 8); chun phc cht(bi 9) thu c kt qu c chnh xc kh cao (70-
100%)
C khong trn 85% sinh vin thc hin cc bi th nghim chun
Pemanganat (bi 6) v chun iod (bi 7) thu c kt qu c chnh xc kh
cao (70-100%).
Khng c sinh vin no khng tin hnh c cc bi thc hnh (10-40%)
V nhu cu thay i hoc ci tin gi thc hnh phn tch nh
lng ha hc (t cu 16 n cu 22)
C nhiu nguyn nhn dn n vic cha thch gi thc hnh Phn tch nh
lng ha hc, tuy nhin c trn 80% sinh vin cho rng: mt s bi thc hnh n
gin nhng phi lp i lp li nhiu ln, mt s bi thc hnh kh, khng thu c
kt qu nh mong mun. y chnh l hai nguyn nhn chnh.
C 46% s sinh vin cho rng rt cn thit hoc cn thit thay i ni dung
gio trnh thc hnh phn tch nh lng ha hc. Ch c khong 18% s sinh vin
cho rng khng cn thit.
C khong 40% sinh vin cho rng nn thm th nghim phn tch khi lng.
C khong 60% sinh vin cho rng nn thm th nghim nh lng bng
phng php Dicromat.
Khong 77% sinh vin cho rng nn thm cc th nghim mang tnh ng dng
thc t
47
Khong 70% sinh vin cho rng cn thit thm giai on cn, pha ha cht vo
bi thc hnh.
Khong 56% sinh vin cho rng cn tnh khong tin cy ca kt qu thu c.
Khong 55% sinh vin cho rng cn tin hnh mt bui thi vo cui hc phn,
cn li cho rng khng cn thit.
Cc bn sinh vin ch yu xut v thi lng tin hnh mt bui thc hnh
l kh ngn khng th hon thin tt nht cc th nghim.
3.2. Kho st cc bi thc hnh c trong gio trnh

Ni dung tin hnh: thc hnh li 9 bi th nghim c trong gio trnh Phn
tch nh lng Ha hc.
3.2.1. Kho st bi 1: chun Axit mnh Baz mnh
Th nghim: Chun axit HCl bng NaOH 0,1N. Xc nh nng HCl
Kt qu thu c v x l kt qu
Nng HCl chun c tnh theo cng thc:
VNaOH .C N( NaOH)
C N(HCl) =
VHCl
i vi ch th Phenolphtalein
Thng s K hiu Kt qu
V NaOH dng (ml) V1 10,1
V2 10,1
V3 10,1
C N(HCl) tnh c C1 0,101
C2 0,101
C3 0,101
C N(HCl) trung bnh C 0,101
Khong tin cy
C 0,1010 0,0000
( tin cy 95%)
48
Ch th metyl
Thng s K hiu Kt qu
V1 10,0
V3 10,1
C1 0,100
C N(HCl) tnh c C2 0,101
C3 0,101
C N(HCl) trung bnh C 0,1007
Khong tin cy
C 0,1007 0,0014
( tin cy 95%)
So snh C N(HCl) trung bnh kho st c vi gi tr C N(HCl) mu thc

t vi tin cy 95%.
Mu HCl 0,1N
Ch th phenolphtalein
C N(HCl) trung bnh = 0,101N
|0,1010,1|
t TN = =1
tTN < t(0,95, 2)
t (0,95,2) = 4,3027
Ch th Metyl
|0,10,1|
t TN = =0

tTN < t(0,95, 2)
t (0,95,2) = 4,3027
S sai khc gia C N(HCl) trung bnh kho st c v C N(HCl) mu i vi c 2
ch th l ngu nhin
Kt qu C N(HCl) trung bnh thu c l tt
49
3.2.2. Kho st bi 2: chun axit yu

Th nghim: Chun CH 3 COOH bng NaOH. Xc nh hm lng
CH 3 COOH mu
Nng ca dung dch CH 3 COOH trong bnh nh mc (mu phn tch) c
tnh theo cng thc:
VNaOH .C N( NaOH)
C N(CH3COOH) =
VCH3COOH
Hm lng CH 3 COOH trong mu c tnh theo cng thc:

C N(CH3COOH) .100.60
a= (g/mu)
1000
Bng kt qu
Thng s K hiu Kt qu
V2 10,1
V3 10,1
CN(CH3COOH) tnh c C1 0,102
C2 0,101
C3 0,101
Hm lng CH 3 COOH a1 0,612
trong mu (g/mu) a2 0,606
a3 0,606
Hm lng CH 3 COOH trung bnh a 0,608
Khong tin cy
a 0,6080 0,0090
( tin cy 95%)
50
So snh 3 trung bnh kho st c vi gi tr 3 mu

thc t vi tin cy 95%.
Mu CH 3 COOH: 0,6g/mu
0,6080,6
t TN = = 2,3094

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
S sai khc gia kt qu kho st c ti phng th nghim v mu thc t l
ngu nhin.
3.2.3. Kho st bi 3: chun baz yu

Nng ca dung dch NH 3 trong bnh nh mc c tnh theo cng thc:

VHCl .C N(HCl)
C N( NH3 ) =
VNH3
Hm lng NH 3 trong mu c tnh theo cng thc:

C N( NH3 ) .100.17
a= (g/mu)
1000
51
Bng kt qu
Thng s K hiu Kt qu
V HCl dng (ml) V1 10,3
V2 10,2
V3 10,2
( ) tnh c C1 0,103
C2 0,102
C3 0,102
Hm lng NH 3 a1 0,1751
a3 0,1734
Hm lng NH 3
a 0.1740
Trung bnh
Khong tin cy
a 0,1740 0,0024
( tin cy 95%)
So snh 3 trung bnh kho st c vi gi tr 3 mu thc t

vi tin cy 95%.
Mu NH 3 : 0,17g/mu
0,6080,6
t TN = = 4,0414

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
ngu nhin.
52
3.2.4. Kho st bi 4: chun a axit

Th nghim 1: Chun H 3 PO 4 bng NaOH
Mu H 3 PO 4 : 0,1M
Nng H 3 PO 4 c tnh theo cng thc :
C( NaOH) .V1( NaOH ) C( NaOH) .V2( NaOH )
CM(H3PO4 ) = =
VH3PO4 2VH3PO4
C N(H3PO4 ) = 2C(H3PO4 )
Bng kt qu
Thng s K hiu Kt qu
V1 1 9,7
V1 NaOH dng (ml) V1 2 9,8
V1 3 9,8
C 1 (1) 0,097
( 4) nh c
C 2 (1) 0,098
Da vo V1
C 3 (1) 0,098
( 4) trung bnh C(1) 0,0977
Khong tin cy ca C(1)
C(1) 0,0977 0,0014
( tin cy 95%)
V2 1 19,9
V2 3 19,9
C 1 (2) 0.100
( ) nh c
C 2 (2) 0,099
Da vo V2
C 3 (2) 0,100
( 4) trung bnh C(2) 0,0997
C(2) 0,0997 0,0014
( tin cy 95%)
53
So snh ( ) trung bnh kho st c ti phng th nghim vi

gi tr( ) mu thc t ( tin cy 95%).
Mu H 3 PO 4 : 0,1M
Kt qu tnh tnh c da vo V1
|0,09770,1|
t TN = = 0,5773

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
Kt qu tnh tnh c da vo V2
|0,09970,1|
t TN = = 0,5773

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
ngu nhin i vi c 2 cch tnh
Th nghim 2: Chun hn hp axit HCl v H 3 PO 4 bng dung

dch NaOH
Nng HCl v H 3 PO 4 c tnh theo cng thc :
=Co2 C=
(
C( NaOH) . V2 V1 )
M(H3 PO4 )
V(H3PO4 + HCl)
=
Co1 C=
(
C( NaOH) . 2V1 V2 )
M(HCl)
V(H3PO4 + HCl)
Hm lng H 3 PO 4 v HCl c tnh theo cng thc :

a (H3PO4 ) = CM(H3PO4 ) .98.103.100
g/mu
a (HCl) = CM(HCl) .36,5.103.100
g/mu
54
Bng kt qu:
Thng s K hiu Kt qu
V1 1 9,8
V1 3 9,7
V2 1 14,5
V2 3 14,6
( ) 1 0,047
( ) nh c ( ) 2 0,048
( ) 3 0,048
( ) 1 0,460
Hm lng H 3 PO 4 (g/mu) ( ) 2 0,470
( ) 3 0,470
Hm lng H 3 PO 4 trung bnh ( ) 0,4667
Khong tin cy ca ( )
( ) 0,4667 0,0143
( tin cy 95%)
() 1 0,051
() nh c () 2 0,049
() 3 0,049
() 1 0,186
Hm lng HCl (g/mu) () 2 0,179
() 3 0,179
Hm lng HCl trung bnh () 0,1813
Khong tin cy ca ()
() 0,1813 0,0100
( tin cy 95%)
55
So snh kt qu trung bnh kho st c ti phng th nghim vi gi

tr mu thc t ( tin cy 95%).
Mu gm HCl 0,1825g/mu v H 3 PO 4 0,49g/mu
i vi HCl
|0,18130,1825|
t TN = = 0,2887

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
i vi H 3 PO 4
|0,46670,49|
t TN = = 4,0414

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
ngu nhin.
3.2.5. Kho st bi 5: chun a baz

Th nghim 1: Chun Na 2 CO 3 bng HCl
Nng mol ca Na 2 CO 3 c tnh theo cng thc sau:
C(HCl) .V1( HCl ) C(HCl) .V2( HCl )
CM( Na 2CO3 ) = hoc CM( Na 2CO3 ) =
VNa 2CO3 2VNa 2CO3
C(HCl) .V2( HCl )

=
C N( Na 2CO3 ) = 2CM
VNa 2CO3
56
Bng kt qu:
Thng s K hiu Kt qu
V1 1 9,8
V1 HCl dng (ml) V1 2 9,7
V1 3 9,8
C 1 (1) 0,098
( ) nh c C 2 (1) 0,097
Da vo V1 C 3 (1) 0,098
( ) trung bnh C(1) 0,0977

C(1) 0,0977 0,0014
( tin cy 95%)
V2 1 19,9
V2 3 19,9
C 1 (2) 0,100
( ) nh c C 2 (2) 0,099
Da vo V2 C 3 (2) 0,100
( ) trung bnh C(2) 0,099

C(2) 0,0997 0,0014
( tin cy 95%)
Mu Na 2 CO 3 : 0,1M
Kt qu tnh c da vo V1
|0,09770,1|
t TN = = 4,0414

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
57
Kt qu tnh c da vo V2
|0,09970,1|
t TN = = 0,5773

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
ngu nhin.
Th nghim 2: Chun hn hp Na 2 CO 3 v NaOH bng dung

dch HCl
Nng NaOH v Na 2 CO 3 c tnh theo cng thc sau:
C(HCl) . ( V2 V1 )
=Co2 C=
M( Na 2 CO3 ) ; C N( Na CO ) = 2CM( Na CO )
V( Na 2CO3 + NaOH) 2 3 2 3
C(HCl) . ( 2V1 V2 )
=Co1 C=
M( NaOH) ; C N( NaOH) = CM( NaOH)
V( Na 2CO3 + NaOH)
Hm lng NaOH v Na 2 CO 3 c tnh theo cng thc:

a ( Na 2CO3 ) = CM( Na 2CO3 ) .106.103.100 g/mu
a ( NaOH) = CM( NaOH) .40.103.100 g/mu
58
Bng kt qu
Thng s K hiu Kt qu
V1 1 9,8
V1 3 9,7
V2 1 14,6
V2 3 14,6
( ) 1 0,048
( ) nh c ( ) 2 0,050
( ) 3 0,049
( ) 1 0,5088
Hm lng Na 2 CO 3 (g/mu) ( ) 2 0,5300
( ) 3 0,5194
Hm lng Na 2 CO 3 trung bnh ( ) 0,5194
Khong tin cy ca ( )
( ) 0,5194 0,0263
( tin cy 95%)
() 1 0,050
() nh c () 2 0,047
() 3 0,048
() 1 0,2000
Hm lng NaOH (g/mu) () 2 0,1880
() 3 0,1920
Hm lng NaOH trung bnh () 0,1933
Khong tin cy ca ()
() 0,1933 0,0152
( tin cy 95%)
59

Mu Na 2 CO 3 0,53g/mu, NaOH 0,2g/mu
i vi Na 2 CO 3
|0,51940,53|
t TN = =1

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
i vi NaOH
|0,19330,2|
t TN = = 1,0910

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
ngu nhin.
3.2.6. Kho st bi 6: nh lng Fe bng phng php pemanganat

Hm lng ca Fe3+ trong mu c tnh theo cng thc:
( ) . ..
+ = (g/mu)
+ .
Bng kt qu
Thng s K hiu Kt qu
V1 9,4
dng (ml) V2 9,4
V3 9,3
a1 0,5264
Hm lng Fe3+ trong mu (g/mu) a2 0,5264
a3 0,5208
Hm lng Fe3+ trung bnh + 0,5245
Khong tin cy ( tin cy 95%) + 0,5245 0,0080
60

Mu FeCl 3 0,01M, + = 0,56g
|0,52450,56|
t TN = = 10,9697

tTN > t(0,95, 2)
t(0,95, 2) = 4,3027
S sai khc gia kt qu kho st c ti phng th nghim v mu thc t
khng phi l ngu nhin.
3.2.7. Kho st bi 7: nh lng Cu bng phng php iod

Hm lng Cu2+ trong mu phn tch c tnh theo cng thc:
( ) . ..
+ = (g/mu)
+ .
Bng kt qu
Thng s K hiu Kt qu
V1 9,5
dng (ml) V2 9,4
V3 9,4
a1 0,6080
Hm lng Cu2+ trong mu (g/mu) a2 0,6016
a3 0,6016
Hm lng Cu2+ trung bnh + 0,6037
Khong tin cy ( tin cy 95%) + 0,6037 0,0091
tr mu thc t ( tin cy 95%). Mu CuSO 4 0,01M, aCu2+ =0,64g
|0,52450,64|
t TN = = 9,8149
tTN > t(0,95, 2)
t(0,95, 2) = 4,3027
61
3.2.8. Kho st bi 8: chun kt ta

Th nghim 1: dng phng php Mohr xc nh nng
AgNO 3 bng dung dch NaCl chun.
Nng ca AgNO 3 c tnh theo cng thc:
.()
( ) =

Bng kt qu
Thng s K hiu Kt qu
V1 9,4
dng (ml) V2 9,5
V3 9,5
C1 0,0532
( ) tnh c C2 0,0526
C3 0,0526
( ) trung bnh C 0,0528
Khong tin cy
C 0,0528 0,0008
( tin cy 95%)

Mu AgNO 3 0,05N
|0,05280,05|
t TN = = 8,7179

tTN > t(0,95, 2)
t(0,95, 2) = 4,3027
62
Th nghim 2: p dng phng php Fajans xc nh nng

AgNO 3 bng dung dch NaCl chun
Nng ca AgNO 3 c tnh theo cng thc:
.()
( ) =

Bng kt qu
Thng s K hiu Kt qu
V1 9,4
dng (ml) V2 9,3
V3 9,3
C1 0,0532
( ) tnh c C2 0,0538
C3 0,0538
( ) trung bnh C 0,0536
Khong tin cy
C 0,0536 0,0008
( tin cy 95%)

Mu AgNO 3 0,05N
|0,05360,05|
t TN = = 10,8195

tTN > t(0,95, 2)
t(0,95, 2) = 4,3027
63
Th nghim 3: xc nh hm lng Cl- trong mu theo phng

php Volhard
Hm lng ca ion Cl- trong mu phn tch c tnh theo cng thc:
( ),
= (g/mu)
. .
Bng kt qu
Thng s K hiu Kt qu
V1 5,6
dng (ml) V2 5,6
V3 5,5
a1 0,3337
tnh c a2 0,3337
a3 0,3373
trung bnh a 0,3349
Khong tin cy
a 0,3349 0,0050
( tin cy 95%)

Mu NaCl: 0,01M, = 0,355g
|0,33490,355|
t TN = = 9,8150

tTN > t(0,95, 2)
t(0,95, 2) = 4,3027
3.2.9. Kho st bi 9: chun phc cht.

Th nghim 1: Xc nh nng EDTA theo dung dch MgCl 2
chun.
64
Nng ca dung dch EDTA c tnh theo cng thc:
.()
() =

Bng kt qu:
Thng s K hiu Kt qu
V1 10,3
dng (ml) V2 10,2
V3 10,2
() 1 R
0,0097
() tnh c () 2 R
0,0098
() 3 R
0,0098
() trung bnh () 0,0098
Khong tin cy
() 0,0098 0,0001
( tin cy 95%)

Mu EDTA 0,01N
|0,00980,001|
t TN = = 4,1453

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
ngu nhin.
Th nghim 2: Xc nh hm lng hn hp Canxi v Magie

trong mu phn tch.
Tng s mmollg (Ca2++ Mg2+) trong mu phn tch c tnh theo cng thc:
() 100 103
( ) =
1000
65
Bng kt qu:
Thng s K hiu Kt qu
V1 10,3
dng (ml) V2 10,2
V3 10,2
a1 1,0094
a tnh c a2 0,9996
a3 0,9996
A trung bnh a 1,0029
Khong tin cy
a 1,0029 0,0140
( tin cy 95%)

Mu th nghim: 100ml CaCl 2 0,05M + MgCl 2 0,05M
( ) = 1
|0,00980,001|
t TN = = 4,1453

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
ngu nhin.
3.2.10.Nhn xt
u im:
Thao tc tin hnh th nghim kh n gin

Dng c v ha cht th nghim thng thng, d kim.
Cc bi th nghim chun axit- baz (Bi 1- 5), chun phc cht thu
c kt qu tt. S sai khc gia kt qu thu c v mu thc l ngu nhin.
Nhc im
Cc bi th nghim chun st bng phng php Pemanganat (Bi 6),
66
chun ng bng phng php iod (Bi 7), chun kt ta (Bi 8) c kt qu

thu c cha tt. S sai khc gia kt qu thu c v mu thc khng phi l
ngu nhin.
Ha cht c pha sn, sinh vin cha c tip xc vi vic t tnh ton, cn
v pha ha cht.
Cng thc tnh ton c cung cp cui bi, sinh vin ch tnh ton th
ng. Vic tnh ton cn n gin cha c x l thng k.
bi chun Fe bng phng php Pemangant (bi 6) c nhiu hin tng
kh nhn thy. Kh xc nh c thi im mt mu ca FeCl 3 khi cho SnCl 2 . S
xut hin di la Hg 2 Cl 2 cng kh thnh cng, iu ny cng gy nh hng n
kt qu ca php chun .
3.3. xut chung

Kt hp nhng nhn xt, kt qu ca kho st bng phiu iu tra v kho st
li cc bi thc hnh trong phng th nghim, Ti a ra nhng xut sau:
Tin hnh thm mt s bi thc hnh phn tch mu thc.
Tin hnh thm mt s bi thc hnh v phn tch nh lng bng phng
php khi lng, phng php Dicromat
Thm giai on t tnh ton, cn, pha ha cht vo cc bi thc hnh
a phn gii quyt s liu thc nghim bng thng k ton hc vo gio
trnh thc hnh
Cung cp phim, hnh nh minh ha cc thao tc s dng dng c th nghim,
cng nh quy trnh tin hnh mi bi th nghim cho sinh vin quan st nh trc
bui hc, nhm thu c hiu qu tt nht trong gi thc hnh.
Khng cung cp cng thc tnh kt qu cui bi, sinh vin t vn dng
kin thc hc phn l thuyt vo vic tnh ton, p dng tnh khong tin cy cho gi
tr thu c.
Tng thi lng thc hnh mi bui, hoc gim bt thi lng tit l thuyt
trong gi thc hnh v a s cc l thuyt c hc k trong hc phn Ha phn
tch II.
67
CHNG 4: MT S GII PHP NNG CAO HIU QU DAY- HC

PHN THC HNH PHN TCH NH LNG HA HC
T kt qu v nhn xt phn thc trng dy- hc phn thc hnh phn tch
nh lng ha hc, Ti xut mt s gii php sau:
4.1. Chnh sa v b sung ni dung gio trnh

Qua kho st bng phiu iu tra c khong 70% sinh vin cho rng cn thit
thm giai on t cn, pha ha cht vo bi thc hnh. Vic t tnh ton lng cht
cn dng, cn, pha thnh dung dch c nng xc nh rn luyn cho sinh vin t
nhng bc c bn u tin ca nghin cu khoa hc, sinh vin phi t vn ng
to ra dung dch chun ban u mi c th p dng tnh ton cc th nghim tip
theo. Nh vy mun hon thnh tt bui thc hnh, sinh vin cn xem k ti liu
trc khi n lp, do va nng cao c k nng thc hnh va vn dng c
phn l thuyt hc.
T nhng l do trn ti tin hnh 2 xut 4.1.1. v 4.1.2.
4.1.1. Bi 2: Chun axit yu [10]

B sung vo phn I.3. Cch tin hnh xc nh nng NaOH chun bng
cht chun gc (Gio trnh trang 22)
Tin hnh cn, pha dung dch chun H 2 C 2 O 4 0,1M: Cn mt lng xc nh
H 2 C 2 O 4 (Lng H 2 C 2 O 4 sinh vin t tnh) c chnh xc 0,0001g trong cc.
Chuyn axit qua phu vo bnh nh mc 250ml. Trng cc 3 ln bng nc ct vo
bnh nh mc. nh mc n vch, lc k trn u, ta c 250 ml dung dch
chun axit oxalic 0,1M. Dng dung dch ny tin hnh xc nh li nng NaOH.
4.1.2. Bi 3: Chun baz yu [10]
B sung vo phn II.3. Cch tin hnh chun ha dung dch HCl (Gio trnh
trang 26)
Tin hnh cn, pha dung dch chun Na 2 B 4 O 7 0,1M: Cn mt lng xc nh
H 2 C 2 O 4 (Lng Na 2 B 4 O 7 sinh vin t tnh) c chnh xc 0,0001g trong cc.
Chuyn axit qua phu vo bnh nh mc 250ml. Trng cc 3 ln bng nc ct vo
68
bnh nh mc. nh mc n vch, lc k trn u, ta c 250 ml dung dch

chun axit oxalic 0,1M. Dng dung dch ny tin hnh xc nh li nng HCl.
4.1.3. Bi 5: Th nghim Chun hn hp Na 2 CO 3 v NaOH bng HCl
Qua kt qu kho st bng phiu iu tra, bi 5 th nghim chun hn hp
Na 2 CO 3 v NaOH c khong 24% s sinh vin t kt qu cha tt. Nguyn nhn
c th do ni dung cch tin hnh, do sinh vin thao tc cha tt, hay do dng lin
tip hai loi ch th phenolphtalein v metyl da cam nn kh nhn thy s thay i
mu sc, dn n qu chun . Do , ti b sung thm mt phng php na
xc nh hn hp NaOH v Na 2 CO 3 , t c th tin hnh so snh vi phng
php mt v rt ra phng php c kt qu chnh xc hn.
Phng php hai [2]:
Cch xc nh
Dng pipet ly chnh xc 10,00ml dung dch hn hp NaOH+Na 2 CO 3 cho
vo bnh nn, thm 1-2 git cht ch th metyl da cam ri chun bng dung dch
HCl cho n khi dung dch c mu da cam. Ghi th tch HCl tiu tn (V 1 ).
Li ly chnh xc 10,00ml dung dch hn hp nh trn, cho vo bnh nn sch,
thm 5-7ml dung dch BaCl 2 1M v 8-10 git cht ch th phenolphtalein. Khng
cn lc kt ta, chun bng dung dch HCl cho n khi mt mu hng. Ghi th
tch V 2 .
Sau khi tin hnh lm th trong phng th nghim ta thu c kt qu sau:
Nng ca dung dch NaOH c tnh theo cng thc:
. ()
() =

Nng ca dung dch Na 2 CO 3 c tnh theo cng thc:
( ). ()
( ) =

Bng kt qu:
69
Thng s K hiu Kt qu
V1 1 9,9
V1 HCl dng (ml) V1 2 9.9
V1 3 9,8
V2 1 5,0
V2 3 4,9
( ) 1 0,049
( ) nh c ( ) 2 0,050
( ) 3 0,049
( ) 1 0,5194
Hm lng Na 2 CO 3 (g/mu) ( ) 2 0,5300
( ) 3 0,5194
Hm lng Na 2 CO 3 trung bnh ( ) 0,5229
Khong tin cy ca ( )
( ) 0,5229 0,0152
( tin cy 95%)
() 1 0.050
() nh c () 2 0,049
() 3 0,049
() 1 0,2000
Hm lng NaOH (g/mu) () 2 0,196
() 3 0,196
Hm lng NaOH trung bnh () 0,1973
Khong tin cy ca ()
() 0,1973 0,0057
( tin cy 95%)
70

Mu Na 2 CO 3 0,53g/mu, NaOH 0,2g/mu
i vi Na 2 CO 3
|,,|
t TN = = 0,0163

tTN < t(0,95, 2)
t (0,95, 2) = 4,3027
i vi NaOH
|,,|
t TN = = 0,0981

tTN < t(0,95, 2)
t (0,95, 2) = 4,3027
ngu nhin.
Sai s tng i gia kt qu thu c bng phng php 1 v phng php 2

vi mu thc t. Mu Na 2 CO 3 0,53g/mu, NaOH 0,2g/mu
Phng php 1:
Kt qu thu c: Na 2 CO 3 0,5194 (g/mu); NaOH 0,1933 g/mu
Gi sai s tng i ca kt qu Na 2 CO 3 v NaOH ln lt l S 1 v S 2
,, ,,
S1 = = -0,02 S2 = = -0,0335
, ,
Phng php 2:
Kt qu thu c: Na 2 CO 3 0,5194 (g/mu); NaOH 0,1973 g/mu
Gi sai s tng i ca kt qu Na 2 CO 3 v NaOH ln lt l S 1 v S 2
,, ,,
S1 = = - 0,02 S 2 = = - 0,0135
, ,
Ta c: S 1 = S 1 suy ra kt qu hm lng Na 2 CO 3 thu c hai phng

php l nh nhau.
Ta c: S 2 = - 0,0335 v S 2 = - 0,0135 suy ra kt qu hm lng NaOH thu

c phng php hai gn ng vi mu thc t hn phng php mt.
71
4.2. Cc bi th nghim xut

4.2.1. Bi 2: Xc nh hm lng st bng phng php Dicromat
Qua kt qu phiu iu tra, c khong 70% sinh vin cho rng nn thm th
nghim nh lng bng phng php Dicromat. So snh vi cc gio trnh ca cc
trng i hc trong nc, cng nh do tm quan trng ca phng php chun
Dicromat, ti tin hnh xut bi th nghim Xc nh hm lng Fe bng
phng php Dicromat
Cch xc nh[2, 10]
Ly chnh xc 10,00ml dung dch FeCl 3 cho vo bnh nn nh, thm khong
5ml HCl 1:1. Thm 4-5 ht km (nghing bnh v cho km vo nh nhng, trnh
lm v bnh). t bnh ln bp in un gn si (lm trong t ht) cho ti khi dung
dch mt mu vng hon ton (nu thy c kt ta trng l mui baz ca km th
phi cho thm HCl ti khi tan ht).
Dng khong 10ml nc ct ngui cho thm vo bnh nn. Ly bnh nn ra
khi t ht v lm ngui nhanh dung dch, lc b km d bng giy lc chy nhanh,
hng dung dch vo bnh nn loi 250ml. Dng nc ct trng ra nhiu ln bnh
nn nh v phu lc. Thm nc ct ti khong 100ml (nu cn), thm vo 5-
7ml hn hp hai axit H 2 SO 4 +H 3 PO 4 v 1-2 git dung dch cht ch th
diphenylamin ri nh phn dung dch bng dung dch chun K 2 Cr 2 O 7 cho ti khi
xut hin mu xanh tm (cho thm nc ct l gim mu xanh ca Cr3+ , d nhn
thy s i mu ca cht ch th).
Hm lng ca Fe3+ trong mu c tnh theo cng thc:
( ) . ..
+ = (g/mu)
+ .
72
Thng s K hiu Kt qu
dng (ml) V1 9,7
V2 9.8
V3 9.8
Hm lng Fe3+ a1 0,5432
a3 0,5488
+ 0.5469
Khong tin cy
+ 0,5469 0,0080
( tin cy 95%)
So snh kt qu trung bnh kho st c ti phng th nghim vi

gi tr mu thc t ( tin cy 95%).
Mu FeCl 3 0,01M, + = 0,56g
|,,|
t TN = = 4,0414

tTN < t(0,95, 2)
t(0,95, 2) = 4,3027
4.2.2. Bi 3: Xc nh hm lng vitamin C trong vin nn bng phng php

chun iod
Khong 77% sinh vin cho rng nn thm cc th nghim mang tnh ng dng
thc t. ti tin hnh xut bi th nghim Xc nh hm lng vitamin C
trong vin nn bng phng php chun iod
Cch tin hnh[16,17]

Chun b mu:
73
Nghin v ha tan mt vin nn vitamin C vo bnh tam gic 250ml vi 40ml

H 2 SO 4 0,5M v 0,5g NaHCO 3 . Ta c mu vitamin C
Chun vitamin C:
Thm vo mu trn 25ml KIO 3 0,01M v 1g KI. Thm vo 5ml H 2 SO 4

0,5M v 0,1g NaHCO 3 . Lp tc chun lng I 2 sinh ra bng dung dch Na 2 S 2 O 3
0,1M cho n khi dung dch c mu vng rm, thm tip 2ml dung dch h tinh bt,
chun tip cho n mt mu xanh ca dung dch, ghi li th tch Na 2 S 2 O 3 . Lp
li th nghim t nht 3 ln.
Hm lng acid ascorbic trong mt vin nn c tnh theo cng thc:
= (. ( ) . , . ( ). ( ) ). (mg/mu)
Thng s K hiu Kt qu
V1 6,4
( ) dng (ml) V2 6,3
V3 6,3
a1 74,8000
Hm lng acid ascorbic a2 74,8000
trong vin nn (mg/mu) a3 73,9200
a 74,5067
Khong tin cy
a 74,5067 1,2621
( tin cy 95%)
So snh kt qu trung bnh kho st c ti phng th nghim vi gi tr mu
thc t ( tin cy 95%).
Mu: 1 vin nn My Vita ca cng ty c phn S.P.M cha 75mg acid ascorbic
|,|
t TN = = 0,9709

tTN < t(0,95, 2)
t (0,95, 2) = 4,3027
74

ngu nhin. Hm lng acid ascorbic c trong vin nn t ng hm lng ghi
trn bao b.
4.3. Xy dng phim minh ha cc bi thc hnh
Kt qu thu c tng cng 22 phim, bao gm

Bi thc hnh trong gio trnh gm 15 phim, c th nh sau:
Bi 1: Chun axit mnh, baz mnh gm 2 phim
Chun HCl bng NaOH vi ch th PhenolPhtalein
Chun HCl bng NaOH vi ch th Metyl
Bi 2: Chun axit yu gm 1 phim
Chun CH 3 COOH bng NaOH
Bi 3: Chun baz yu gm 1 phim
Chun NH 3 bng HCl
Bi 4: Chun a axit gm 2 phim
Chun H 3 PO 4 bng NaOH
Chun hn hp H 3 PO 4 v HCl bng NaOH
Bi 5: Chun a baz gm 2 phim
Chun Na 2 CO 3 bng HCl
Chun hn hp Na 2 CO 3 v NaOH bng HCl, phng php 1
Bi 6: Xc nh hm lng st bng phng php Pemanganat gm 1
phim
Bi 7: Xc nh hm lng ng bng phng php Iod gm 1 phim
Bi 8: Phng php kt ta gm 3 phim
Phng php Morh
Phng php Fajans
Phng php Volhard
Bi 9: Chun phc cht gm 2 phim
Xc nh nng EDTA bng MgCl 2 chun
75
Xc nh hn hp Mg2+ v Ca2+ bng EDTA

Bi thc hnh ngh gm 2 phim
Chun hn hp Na 2 CO 3 v NaOH bng HCl, phng php 2
Xc nh hm lng st bng phng php Dicromat
Hng dn s dng mt s dng c th nghim trong phn tch nh
lng ha hc gm 5 phim
ng o
Bnh nh mc
Buret
Pipet
Cn phn tch
76
Kha lun tt nghip Kt lun- xut
PHN 3.
KT LUN-
- XUT
77
KT LUN
1. Em tin hnh kho st thc trng dy- hc phn thc hnh phn tch nh
lng Ha hc bng phiu iu tra i vi cc sinh vin lp Ha 4A, 4B, 4C, 3C
nm hc 2012-2013. S phiu thu v: 137, chim 91,33%.
2. tin hnh kho st li tt c 9 bi th nghim c trong gio trnh Phn tch
nh lng Ha hc, trong 6 bi t c kt qu tt chim 66,67%, c 3 bi t
kt qu cha tt chim 33,33%.
3. chnh sa v b sung 2 bi thc hnh:
Bi 2: Chun axit yu
Bi 3: Chun baz yu
4. xut thm 2 bi thc hnh mi.
Bi 1: Xc nh hm lng st bng phng php Dicromat
Bi 2: Xc nh hm lng vitamin C trong vin nn bng phng php Iod
5. xy dng c 22 phim minh ha thc hnh. Trong : 15 phim v 9 bi
thc hnh c trong gio trnh, 2 phim bi thc hnh xut, 5 phim hng dn s
dng dng c th nghim.
XUT
Nhm nghin cu tip theo tin hnh cc bi thc hnh phn tch khi lng
cha thc hin c ti ny.
Thc hnh thm cc bi ng dng thc t lm phong ph hn cho gio
trnh.
78
Kha lun tt nghip Ti liu tham kho
TI LIU THAM KHO
TI LIU TRONG NC
[1]. B mn Ha Phn tch (2005), Gio trnh thc hnh Phn tch nh lng
ha hc, i hc S Phm Quy Nhn
[2]. B mn Ha Phn tch (2007), Hng dn th nghim Ha Phn Tch, i
hc Bch khoa H Ni
[3]. C Thnh Long (2008), Gio trnh ha hc phn tch 2: C s l thuyt
Phn tch nh lng, Khoa Ha trng i hc Khoa hc t nhin- i hc Quc
gia thnh ph H Ch Minh.
[4]. Khoa Ha (2004), Gio trnh thc hnh Phn tch nh lng, i hc Cng
nghip TP.H Ch Minh
[5]. Lm Ngc Th (2005), C s ha hc phn tch, NXB i hc quc gia H
Ni
[6]. L Th Mi (2006), Ha hc phn tch, i hc S Phm Nng.
[7]. Nguyn Hin Hong (2006), Ha hc Phn tch nh lng, i hc S
Phm thnh ph H Ch Minh.
[8]. Nguyn Thc Ct, T Vng Nghi, o Hu Vinh (1972), C s l thuyt
Ha hc phn tch, NXB Gio dc.
[9]. Nguyn Th Nh Mai, ng Th Vnh Ha (2002), Hng dn thc hnh
Phn tch nh lng bng cc phng php ha hc, i hc Lt
[10]. Nguyn Tinh Dung (2006), Ha hc Phn tch phn III cc phng
php nh lng ha hc, NXB Gio Dc
[11]. Nguyn Vn Ri, T Th Tho (2006), Thc tp phn tch Ha hc
phn 1 Phn tch nh lng Ha hc, i hc KHTN-HQG H Ni
[12]. Trn Th Yn (Ch bin), Ng Tn Lc, Nguyn Hin Hong, Vn
Hu, Nguyn Th Minh Hu, L Ngc T (2004), Thc hnh phn tch nh lng,
HSP TP.H Ch Minh.
[13]. Trnh Vn Biu (Ch bin), Trang Th Ln, V Th Th, Trn Th
Vn (2001), Thc hnh th nghim phng php dy hc ha hc, HSP TP.H
79
Ch Minh.
[14]. Trnh Vn Biu (Ch nhim ti), L Trng Tn, Trang Th Ln, V
Th Th, Trn Th Vn (2000), i mi ni dung v phng php dy hc hc
phn thc hnh l lun dy hc ha hc nhm nng cao cht lng o to gio
vin trong giai on mi, HSP TP.H Ch Minh.
[15]. V Phng Uyn (2009), S dng th nghim trong dy hc mn ha
lp 10, 11 trng Trung hc ph thng tnh Dk Lk, Lun vn Thc S Gio dc
hc
TI LIU NC NGOI
[16] Daniel C.Harris (2010), Experiment Quantitative Chemical Analysis, 8th
edition, W. H. Freeman and Company NewYork
[17] Lecturer Mr. Ateet Kumar Roshan (2011), Analytical Chemistry Laboratory
Manual
80
Kha lun tt nghip Ph lc
PH LC
1. PH LC 1: MU PHIU IU TRA
TRNG HSP TP HCM PHIU THAM KHO KIN

KHOA HA H v tn:
Sinh vin lp:..
TP HCM, ngythngnm 2012
Trong xu th pht trin khng ngng ca ha hc, nhm mc ch mang li
cc gi thc hnh HA HC PHN TCH NH LNG (HHPTDL) c hiu qu
tch cc hn na trong vic o to th h gio vin v c nhn ha hc tng lai,
xin bn cho bit kin v mt s vn di y (nh du cho vo thch hp).
Phn 1: Thc trng vic hc thc hnh HHPTDL ti trng HSP TP.HCM:
1. i vi cc gi thc hnh HHPTDL bn cm thy :
rt thch thch bnh thng
khng thch
2. Bn c nghin cu ti liu hng dn trc khi vo phng th nghim hay

khng?
xem k xem s qua khng xem
3. Bn hy chn mc nhiu, t cho cc vn trong gi thc hnh HHPTDL
sau (1: rt t; 5: rt nhiu). nh du cho vo chn.
Mc
Vn
1 2 3 4 5
a) Thi lng tin hnh th nghim trong mt bui hc
b) Tng s bui th nghim
c) Tng s bi th nghim
4. Bn c hi lng vi ni dung cc bi th nghim ?

hon ton hi lng ch hi lng mt phn khng hi lng
5. Cc bui thc hnh HHPTDL gip bn rn luyn (c th chn nhiu

phng n) :
Thao tc s dng cc dng c th nghim.
Thao tc chun b ha cht, tin hnh, quan st th nghim.
Hiu r hn l thuyt hc.
81
Kha lun tt nghip Ph Lc
S dng ha cht vi liu lng chnh xc

Cch c th tch chnh xc
Kh nng t duy, tp lm nghin cu khoa hc
6. Khi tin hnh th nghim bn thc s hiu r phn c s l thuyt cha?

10-20% 30-40% 50-60% 70-80% 90-100%
7. Mc thnh cng cc bi thc hnh PTDL ca cc bn khong:

Tn bi Mc thnh cng(%)
10- 30- 50- 70- 90-
20 40 60 80 100
Bi 1: Chun axit mnh bng baz mnh v
ngc li
Bi 2: Chun axit yu bng baz mnh
Bi 3: Chun baz yu bng axit mnh
Bi 4: Chun a axit vi hn hp axit (H 3 PO 4
+ HCl) bng baz mnh
Bi 5: Chun a baz vi hn hp baz
(Na 2 CO 3 + NaOH) bng axit mnh
Bi 6: Chun oxi ha kh. Phng php
pemanganat
Bi 7 : Chun oxi ha kh. Phng php iod
Bi 8 : Chun kt ta
Bi 9: Chun complexon
8. i vi th nghim chun hn hp Na 2 CO 3 v NaOH bng HCl cc bn thu
c kt qu nh th no?
rt chnh xc. kh chnh xc
khng chnh xc
9. Trong th nghim nh lng Fe bng phng php PEMANGANAT, bn c

thu c kt ta Hg 2 Cl 2 dng di la mng?
Thu c d dng
82
Thu c nhng phi sau vi th nghim.

hon ton khng thu c.
10. Khi chun bn thng chun b bnh tam gic cha dung dch cn chun
nh th no?
chun b bnh no th chun bnh .
chun b tt c cc bnh ri chun cng mt lc.
ty hng.
11. S th nghim m bn cm thy hng th khi tin hnh vo khong:
10-20% 30-40% 50-60% 70-80% 90-100%
12. S th nghim m bn tin hnh thnh cng vo khong:

10-20% 30-40% 50-60% 70-80% 90-100%
13. Sau cc bui thc hnh HHPTDL bn cm thy:

rt vui v c hng th Bnh thng Mt mi
14. Theo bn s im bn t c cui hc phn c ph hp vi nng lc ca

bn khi thc hnh?
Rt ph hp
t hn so vi kh nng
Nhiu hn so vi kh nng
Khng quan tm
15. Theo bn thang chm im ca gio vin trong mi gi thc hnh nh th

no?
Qu kht khe Rt Tt Kh d
Phn 2: Nhu cu thay i hoc ci tin gi thc hnh HHPTDL ti HSP

TP.HCM
16. Bn cha thch cc gi thc hnh HHPTDL ch:
t c th nghim hp dn
cc th nghim ch mang tnh minh ha l thuyt, ng dng thc t t.
Mt s th nghim n gin nhng phi lp i lp li nhiu ln.
mt s th nghim kh, khng xut hin hin tng nh mong mun.
17. Bn thy c cn thit thay i gio trnh thc hnh HHPTDL:

rt cn thit cn thit bnh thng
khng cn thit
83
18. Bn thy c cn thay i hnh thc gio trnh thc hnh HHTDL:
khng cn thit. thm hnh nh minh ha, mu sc,
hin tng th nghim.
cung cp clip thao tc s dng dng c th nghim.
cung cp cc clip thao tc thc hnh quy trnh tng bi th nghim sinh
vin d quan st.
19. Bn hy chn mc cn thit trong vic thay i mt s th nghim trong
gio trnh thc hnh HHPTDL (1: rt cn thit; 5: hon ton khng cn
thit). nh du cho vo chn.
Mc
S thay i
1 2 3 4 5
a) Thm th nghim phn tch khi lng (v gio trnh ch c phn
tch th tch)
b) Thm th nghim nh lng bng phng php dicromat
c) Thm cc th nghim mang tnh ng dng thc t
d) Thm vo giai on t cn, pha dung dch th nghim.
e) Thm tnh khong tin cy trong phn x l kt qu th nghim
20. Theo bn c cn tin hnh thi THPTDL vo cui hc phn hay khng ?
Rt cn thit Cn thit Khng cn thit lm
Hon ton khng cn
21. Theo bn phn thi l thuyt cui k v trong mi bui nn tin hnh di
hnh thc no?
T lun Trc nghim Vn p
22. cc bui thc hnh HHPTDL mang li kt qu tt hn theo bn cn phi?

Chn thnh cm n bn! Xin chc bn nhiu sc khe v nim vui.
84
2. PH LC HAI: BI TH NGHIM XC NH HM LNG ST

BNG PHNG PHP DICROMAT
Nguyn tc
K 2 Cr 2 O 7 l cht oxi ha mnh, c th dng lm cht khi u xc nh

nhiu loi cht kh khc nhau, lc Cr 2 O 7 2 chuyn thnh Cr3+:
Cr 2 O 7 2 + 14H+ + 6e = 2 Cr3+ + 7H 2 O
Th oxi ha tiu chun ca cp Cr 2 O 7 2/2Cr3+ = +1,36V (b hn th tiu

chun ca cp MnO 4 /Mn2+ = 1,51V)
So vi KMnO 4 th K 2 Cr 2 O 7 c nhng u im sau:
D dng tinh ch c K 2 Cr 2 O 7 tinh khit bng cch kt tinh li v sy

200oC. Do c th pha ch dung dch chun t mt lng cn chnh xc nh
trc. Dung dch K 2 Cr 2 O 7 ng trong bnh kn rt bn, khng b phn hy ngay c
khi un si trong dung dch axit, v vy nng dung dch K 2 Cr 2 O 7 khng thay i
trong thi gian bo qun.
C th chun cht kh trong mi trng HCl m khng s K 2 Cr 2 O 7 oxi

0
ha v 2
= +1,36V. Tuy nhin nu nng HCl >2N cng nh khi un si,
2
s oxy ha c th xy ra.
K 2 Cr 2 O 7 cng c nhc im: Trong qu trnh chun ion Cr3+ to ra c

mu xanh gy kh khn cho vic nhn bit im tng ng.
Trong phng php nh phn bng K 2 Cr 2 O 7 hay dng cht ch th

diphenylamin hoc axit phenylantranilic.
C th dng axit phenylantranilic (E0 = 1,08V) lm cht ch th (dung dch

t khng mu chuyn thnh ta) hoc diphenylamin (E0 = 0,76V) lm cht ch
th (dung dch chuyn t khng mu chuyn thnh xanh tm). Khi dng ch th
diphenylamin lm cht ch th cn ch :
85
Ch dng 12 git dung dch cht ch th, nu dng nhiu cht ch th s to

ra sn phm mu xanh khng thay i nn khng nhn bit c im tng
ng. c th dng diphenylamin, phi thm vo dung dch phn tch mt lng
H 3 PO 4 (xem thuyt v nh phn bng phng php oxy ha kh hc). Ngoi ra
cn to mi trng axit kh cao, v vy trc khi nh phn ngi ta thm vo dung
dch hn hp H 2 SO 4 +H 3 PO 4 .
C s ca phng php xc nh st
Sau khi ch ha mu (qung, hp kim v.v) st thng dng Fe3+. xc

nh, trc ht phi kh Fe3+ thnh Fe2+ bng SnCl 2 hoc Zn.
Fe3+ + Zn = Fe2+ + Zn2+
C th d dng lc b Zn d. Sau chun dung dch Fe2+ bng K 2 Cr 2 O 7.
Cch xch nh nng dung dch Fe3+
Ly chnh xc 10,00ml dung dch FeCl 3 cho vo bnh nn nh, thm khong
5ml HCl 1:1. Thm 4-5 ht km (nghing bnh v cho km vo nh nhng, trnh
lm v bnh). t bnh ln bp in un gn si (lm trong t ht) cho ti khi dung
dch mt mu vng hon ton (nu thy c kt ta trng l mui baz ca km th
phi cho thm HCl ti khi tan ht). Dng khong 10ml nc ct ngui cho thm vo
bnh nn. Ly bnh nn ra khi t ht v lm ngui nhanh dung dch, lc b km d
bng giy lc chy nhanh, hng dung dch vo bnh nn loi 250ml. Dng nc ct
trng ra nhiu ln bnh nn nh v phu lc. Thm nc ct ti khong 100ml
(nu cn), thm vo 5-7ml hn hp hai axit H 2 SO 4 +H 3 PO 4 v 1-2 git dung
dch cht ch th diphenylamin ri nh phn dung dch bng dung dch chun
K 2 Cr 2 O 7 cho ti khi xut hin mu xanh tm (cho thm nc ct l gim mu
xanh ca Cr3+, d nhn thy s i mu ca cht ch th).
Tnh ton kt qu: Hm lng ca Fe3+ trong mu c tnh nh sau:
( ) . ..
+ = (g/mu)
+ .
86
3. PH LC BA: BI TH NGHIM CHUN HN HP NAOH V

NA 2 CO 3 BNG HCl (PHNG PHP 2)
Nguyn tc
Dng dung dch HCl 0,1N chun hn hp NaOH+Na 2 CO 3 , dng
metyl da cam lm cht ch th. Ta bit c th tch dung dch HCl tiu tn
tc dng vi ton b NaOH v Na 2 CO 3
Sau ly mt mu khc, kt ta CO 3 2- bng dung dch BaCl 2 , CO 3 2- s
to kt ta BaCO 3
Na 2 CO 3 + BaCl 2 = BaCO 3 + 2NaCl
Dung dch cn li l NaOH. Khng cn lc kt ta, dng HCl chun
dung dch vi cht ch th phenolphtalein, bit c th tch dung dch HCl cn
tc dng vi ring NaOH.
T suy ra th tch dung dch HCl cn tc dng vi Na 2 CO 3 , phng
php ny chnh xc hn phng php 1.
Cch tin hnh v tnh ton
Dng pipet ly chnh xc 10,00ml dung dch hn hp NaOH + Na 2 CO 3
cho vo bnh nn, thm 1-2 git cht ch th metyl da cam ri chun bng
dung dch HCl cho n khi dung dch c mu da cam. Ghi th tch HCl tiu tn
(V 1 ).
Li ly chnh xc 10,00ml dung dch hn hp nh trn, cho vo bnh nn
sch, thm 5-7ml dung dch BaCl 2 1M v 8-10 git cht ch th phenolphtalein.
Khng cn lc kt ta, chun bng dung dch HCl cho n khi mt mu. Ghi
th tch HCl tiu tn cho php nh phn ny (V 2 ).
Nng ca dung dch NaOH c tnh theo cng thc:
2 ()
() =

Nng ca dung dch Na 2 CO 3 c tnh theo cng thc:
(1 2 )()
() =

87
88
NHN XT CA HI NG
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89

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B GIO DC V O TO

TRNG I HC S PHM H CH MINH

KHA LUN TT NGHIP

GIO VIN HNG DN: ThS. L NGC T

SINH VIN THC HIN: LI TH KIM BIN

THNH PH H CH MINH- THNG 5 NM 2013

Em cng xin trn trng cm n cc Thy C trong Khoa Ha hc trng i

Em cng xin gi li cm n su sc n gio vin ph trch phng thc hnh

Ti cng xin chn thnh cm n cc bn sinh vin lp Ha K35A, K35B,

c s gip ca Thy C v bn b, cng vi nhng n lc ca bn

Em xin trn trng cm n.

Thnh ph H Ch Minh, thng 5 nm 2013

Sinh vin thc hin

DANH MC BNG .................................................................................................. I

DANH MC HNH ................................................................................................. II

TNG QUAN ............................................................................................................2

CHNG 1:C S L LUN ...............................................................................3

CHNG 2:C S L THUYT CC PHNG PHP NH LNG

CHNG 3:KHO ST THC TRNG DY- HC PHN THC HNH

CHNG 4:MT S GII PHP NNG CAO HIU QU DAY- HC

KT LUN- XUT ..........................................................................................77

TI LIU THAM KHO ......................................................................................79

BNG 2.1. Mt s ch th quan trng v khong chuyn mu ca ch th ..............21

BNG 2.2. Khong pH i mu ca ch th ERIOT ................................................32

HNH 2.1. Phng php lc kt ta ..........................................................................16

HNH 2.2. Phng php chun th tch ...............................................................18

HNH 2.3. C ch i mu phenolphatalein .............................................................19

HNH 2.4. C ch i mu ca phenol ................................................................20

HNH 2.5. C ch i mu ca metyl da cam ..........................................................20

Phn tch nh lng c dng xc nh quan h nh lng gia cc

1.1. Khi nim th nghim ha hc [15]

1.2. Mc ch ca vic thc hnh th nghim[13- 15]

1.3. Mt s gio trnh thc hnh Phn tch nh lng:

Bi 19: Xc nh Cl bng dung dch chun AgNO 3

Bi 20: Xc nh Cl bng dung dch chun Hg(NO 3 ) 2

CHNG 2: C S L THUYT CC PHNG PHP NH LNG

Sai s h thng v sai s ngu nhin:

lch chun S: L cn bc hai ca phng sai

Sau tra bng F (p=0,95 ng vi k 1 , k 2 l bc t do ca hai dy th nghim)

2.1. Phng php phn tch khi lng[10]

Hnh 2.1. Phng php lc kt ta

2.2. Phng php phn tch th tch [10, 12]

Buert cha dung

Bnh tam gic cha Dung

Hnh 2.2. Phng php chun th tch

Dng A: lacton, khng mu Dng B: Mui, khng mu

Dng C: quinon, mu hng Dng D: Cacbinol, khng mu

Mu (pK 1 = 1,5) Mu vng (pK 2 = 7,9) Mu

Mu (dng quinon) Mu vng (dng benzen)

trong phng trnh Nernst dng cho ch th:

i vi cc cht tham gia phn ng chun ta c th chuyn i trng thi

tnh ton, thng s dng tch s tan iu kin: Ks = [Ag+][Cl-]

th Ag+ ph thuc pH ca dung dch. xy dng ng cong chun ngi ta

Trong mAgCl l s mol AgCl kt ta trong mt lt dung dch. T (1) v

trnh trn s c dng:

y l phng trnh tnh sai s ti mt im bt k trn ng cong chun .

Nu q = 2% th bc nhy chun (BNC) theo PCl ko di t PCl = 4

Ti tng ng: q=0 nn ta c:

Ch th trong chun complexon

Phn ng ny xy ra ti im tng ng v do dng MIn c mu khc vi

Trong dung dch c s phn ly nh sau:

CHNG 3: KHO ST THC TRNG DY- HC PHN THC HNH

3.1. Kho st bng hnh thc phiu iu tra