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EnterF3:TitrationparametersMethod
creation
ChnphmF3vochcit
ccthngsvomythchinqu
trnhchun.Tophngphp
Chncitccthngschun
H thng chun : Chn chun
pH
Gi tr ban u ca qu trnh chun
.ChnNo
Chn knh truyn tn hiu. Chn
knhA
Titrationparameters
Typeoftitraation
pH
Initialmeasurement No
value
Selectchanel
Measuring
chanel
A
Inputdelay
No/Water
Thigianchthitlpcnbng
pHtitration
EnternoofEQs
Nhpsimtngng:Chn1
1
CaculationEQ EQ
Cng thc tnh cho im tng
(s)
ngthnht:ChnEQ
Formularselection MlxF1xF2/Q Chn cng thc tnh: Chn cng
thctnhcisnnhghi
EnterF1
Entervalue:0.1 Nhp F1: F2l nng dung dch
chunNaOH:chn0.1
EnterF2
Entervalue:Ex:
0.95
EnterQ(ml)
Enterunit
Entervalue:Ex:
10
Mg/L
Enterindetifer
XDDC
Next
Endselection
Start
F1
Nhp gi tr F2 l h s bao gm
mllactic,hshiuchnh,hspha
long(nuc)
Nhp th tch mu xc nh: V d
chnthtchmul10ml
Nhp n v tnh ca kt qu cui
cng:mg/lit
Nhp tn cho im tng ng:
chnXDDC(xcnhchua)
Bcktip
Ktthccit
Btuchun:NhnF1
Bc 6. Chun
c) Kt qu v tnh ton
Ktquchun:
V1(ml)
4,488
V(ml)
100
Vdm(ml)
100
Vm(ml)
10
chuatnhbngg/ltheocngthcsau:
Cngthc
K . V1
X (g / l)
Vdm
Vm
Ths
0,009 4,488
1000 X
100
Ktqu
100
10 1000
X=4,0392(g/l)
Vi:
Vm:lthtchmu(ml)
V:lthtchmumangchun(ml).
V1:lthtchNaOH0.1Ntiutntrongchun(ml).
K:lhscaloiacid,llngacidtngngvi1mlNaOH0.1N.Trongtrng
hpnymusaktqubiuthlacidlacticK=0,009
2. Xc nh m trong Fomat mm
a) Nguyn tc
Dng dung mi hu c thch hp chng ct li cun theo nc trong thc
phm. Dung mi v nc ngng t trong mt ng ong c khc vch thnh hai lp
ringbit.cthtchnclngphadi,ttnhracmcamuthc
phm.
Yucudungmi:
-
Cnhitsicaohnncmtt,khidungmibayhiskotheonc
trongthcphm.
Khngtantrongnc,dungmivncstchthnhhailpringbitkhi
otrongngong.
Nhhnnc,lpncdilpdungmitrongngong.
Dung mi thng s dng l toluen tinh khit nhit si 1000C hoc xylen
nhitsi138-1440C.
b) Cc bc tin hnh
Bc 1.Chunbmu
Becher100mlsch,kh+20gctsch,kh(sykh1800Ctrong1gi)+
10gmu,trnu.Chuynvobnhcuchngctcahthng.
Dngdungmitrng3,4ln,chuynvobnhcu,milnkhong1020ml.
Thmtipvobnhcu80100mldungmi.
Bc 2.Lprphthng
Bc 3.Chngctnkhithtchnckhngtngna.
Bc 4.cktqu
c) Tnh ton kt qu thu c
Kt qu:
Lng nc o c (ml)
5,1
10,38
Tnh ton:
100 =
5,1
100 = 49,133(%)
10,38
Trong:
mH 2O :Lngncoc(ml).
mmau :Khilngmu(g).(1mlnctngngvi1gnc).
3. Xc nh mn ca nc mm
a) Nguyn tc
DavokhnngphnngcaionAg+viionCl-tothnhAgClkttamu
trngvionAg+ viionCrO42- tothnhAgCrO4 mugchtinhnhxcnh
lngNaCl.
Phngtrnhphnng:
NaCl+AgNO3AgCl+NaNO3
ChodungdchchunAgNO3vdungdchtrungtnhchaNaCl,khiNaCltrong
dungdchkthphtviAgNO3,mtgitAgNO3dskthpviK2CrO4 cho
kttagch(qutrnhxcnhktthc).
2AgNO3+K2CrO4Ag2CrO4+2KNO3
TlngAgNO3tatnhclngNaCl.Phnngnythchintttrongmi
trngtrungtnh.
VnumitrngkimthmtlngionAg+sbhaoidophnng:
2Ag++2OH-2AgOHAg2O+H2O
NumitrngacidthcschuyntCrO42-thnhbicromatCr2O72-.
2CrO42-+2H+Cr2O72-+H2O
KttaskhngphilAg2CrO4mugchmlAg2CrO7muvngrt
khphthinimtngng.Doktqusthiuchnhxc.
NutrongdungdchcionCO32-,S2-thcngtothnhcckttaviion
Ag+lmsais.
b) Cc bc tin hnh
Bc 1.Cho2mlncmmvobnhnhmc100ml,dngnccttrngvnh
mctivch.
Bc 2.Lcquagiylc.
Bc 3.RavtrngnpyburetbngdungdchAgNO30.1N
Bc 4.Cho5mldchlc+vigitPP+2gitK2CrO410%
Bc 5.Chunnkhinobnhxuthinkttagch.
c) Kt qu v tnh ton
Kt qu:
Vmau
(ml)
2
Vdm(ml)
V1(ml)
100
Bnh1
4,6
VAgNO3tiutn(ml)
Bnh2
Bnh3
4,2
4,9
4,57
Tnh ton:
mn ca nc mm c xc nh bng cng thc:
Cngthc
Ths
Ktqu
X(g/l)=
X=
267,345(g/l)
Trong:
a :TrungbnhthtchAgNO30,1Ntiuhaotrong3lnchun(ml).
Vmau:Thtchmuthcphm(ml).
Vdm:Thtchbnhnhmc(ml).
V1:Thtchdungdchemichun(ml).
0,00585lsgamNaCltngngvi1mldungdchAgNO3.
Cu hi:
1. Nguyntcxcnh,ccphnngcho3chtiutrn.
2. Trnhbycngthctnh:chuaquyvacidlactic(%m/v),m(%m/m)v
mn(%mNaCl/l).
3. Trnh by nhng nguyn nhn gy sai s khi tin hnh lm 3 ch tiu trn, cch
khcphc?
4. Vsaocnphitrohamuncmmtrckhiphntchmn?
5. GitrpHEQhinthitrnmychunnmtrongkhongnolhpl?
6. Trnhbygiiphpspxp,btrtrnhtcccngviccnthchinhontt
bithnghimnhanhnht?
Tr li:
1. Nguyn tc xc nh, cc phn ng cho 3 ch tiu trn?
Xc nh chua trong Yomost: Dng dung dch NaOH 0.1M trung ha
lngacidctrongmuvichthlphenolphthalein1%.
XcnhmtrongFomatmm:Dngdungmihucthchhpchng
ctlicunnctrongthcphm.Dungmivncngngttrongmtng
ongckhcvchthnhhailpphnbit.cthtchlngphadi,t
tnhracmcamuthcphm.
Yucuvdungmi:
C nhit si cao hn nc mt t, khi dung mi bay hi s ko theo nc
trongthcphm.
Khngtantrongnc,dungmivncstchthnhhailpringbitkhio
trongngong.
Nhhnnc,lpncdilpdungmitrongngong.
Xcnhmntrongncmm:DavokhnngphnngcaionAg+vi
ion Cl- to thnh AgCl kt ta mu trng v ion Ag+ vi ion CrO42- to thnh
Ag2CrO4mugch,(xcnhimtngngktthcqutrnh chun
).
NaCl AgNO3 AgCl NaCl
ChodungdchchunAgNO3vodungdchtrungtnhchaNaCl,khiNaCl
trongdungdchkthphtviAgNO3,mtgitAgNO3dskthpviK2CrO4
chokttamugch(qutrnhchunktthc).
2 AgNO3 K 2CrO4 Ag 2CrO4 2 KNO3
TlngAgNO3tiutntatnhclngNaCl.Phnngnythchintt
trongmitrngtrungtnh.
NumitrngkimthmtlngionAg+sbhaoidophnng:
2 Ag 2OH AgOH Ag 2O H 2O
NumitrngacidthcschuyniCrO42-thnhionbicromatCr2O72-,kt
takhikhngphilAg2CrO4mugchmlAg2Cr2O7muvng,rtkhxc
nhimtngngdnnsaisvktqukhngchnhxc.
2CrO4 2 H Cr2O72 H 2O
NutrongdungdchcionCO32-.S2-thcngtothnhkttaviionAg+gy
sais.
2. Cc cng thc
chuaquyvacidlactic:
chua=
V1.K . f .1000
(g/l)
Trong:
V1:ThtchNaOH0,1Ntiutntrongchun(ml).
V:Thtchmumangchun(ml).
K:Hscaloiacid.TrongbilloiacidlacticnnK=0,009.
f:hsphalongmu.
m
mtheophntrmtnhtheocngthc:
m=
mH2O
mmau
.100 (%)
Trong:
mH2O:Lngncoc(ml).
mmau:Khilngmu(g).
mn:
mntnhbngNaClchatrongthcphmbngcngthcsau:
a. V dm .0, 00585.1000
Vmau
NaCl
V1
(g/l)
Trong:
a :TrungbnhthtchAgNO30,1Ntiuhaotrong3lnchun(ml).
Vmau:Thtchmuthcphm(ml).
Vdm:Thtchbnhnhmc(ml).
V1:Thtchdungdchemichun(ml).
0,00585lsgamNaCltngngvi1mldungdchAgNO3.
3. Nguyn nhn sai s
TN1: Saiscthdo:
Dngpipetvchhtkhngchnhxcthtchdungdchmuvthtchnc
ctcnphadungdch=>htchnhxcthtchdungdchmuvthtchncct.
TN2: Saiscthdo:
Cn mu thiu chnh xc, th tch dung mi trong bnh cu, c kt qu khi
ncvtoluenetrongngongchachiara2phnrrt=>cnmuchnhxc,dng
khngiykh(htm)gimu mukhngdnhvothnhbnh,cktqukhi
ncvtoluenechiathnh2phnrrt.
Do trong qu trnh cn mu khng chnh xc => nn s dng cn phn tch
chnhxcn0,0001g.
KhisdngbnhchngctXylen,dokhakhngchtlmncvotolueneb
chyrangoi=>kimtrakha,nubnhhnnthaythphngphphocdngc
khc.
TN3:Saiscthdo:
Chunbngtaydovicxcnhimtngngchachnhxc.
Mt mu do trong qu trnh chuyn t dng c ny sang dng c khc => s
dngtrctipmtdngctinhnhthnghim.
4. Tro ha mu lm mt nc, v cc cht hu c d chy ch gi li mui
khongcnxcnh.
5. pHEQhintrnmyhplkhong78,5.
6. Giiphpspxp,btrtrnhtcccngviccnthchinhonttbith
nghimnhanhnht.
Htchnhxc1mlncmmchovochnnungschkh,emitroha(v
thigiantrohadi)ht10mldungdichmuYomost+30mlncctkhuyu
+ct,raincc,nhngngptrongdungdchkhngchmyccmu,cit
thngschuntrnmychunghiktqusykhngiychohtm
ca khn cn mu phomat, dng khn giy gi mu lp rp h thng chng
ctchuynmuvobnhcuchngct,chodungmivobnhcuchngct(i
nkhincvdungmichiathnh2phnrrt)kimtramuncmm,nu
tro ha thnh tro, ht khi cho vo l nung 6600C tro ha thnh tro trng h
10
thngchngct:khithtchH2Okhngtngna(ncvtoluenchiara2phnr
rt),ghithtchnctrongngolymutrotrngncmnchovobnhnh
mc dng nc ct 2 ln nh mc ti vch ra, trng v np y buret bng dd
AgNO3 chun b 3 bnh tam gic vi ha cht cn thit chun ln lt tng
bnhvghiliktqu.
11
1. Nguyn tc
Dng sc nng 550-6000C un chy hon ton cc cht hu c, phn cn li
emcnvtnhraphntrmtroctrongthcphm.
2. Ha cht v thit b
-
Hacht:khngsdnghacht
Thitb:bpin,lnung,cn
Dngc:chnnungmingrng,dungtch50ml
3. Quy trnh xc nh
-
Bc 1:Chunbmu
+Cnchnnung:22.6647g
+Cnmu :2.0837g
Khilngchnnungbanumc = 22.6647g
-
Bc 2:Thanhatrnbpinnkhimuhtbckhi
Khilngchnnungvmusaukhinungm2 = 22.7156g
4.Tnh kt qu
-Hmlngtrotonphntrongsabt:
=
. 100 (%) =
22.7156 22.6647
. 100 = 2,4428%
2,0837
Trong:
-
G1lkhilngcachnnungvmusautroha(g)
12
Glkhilngchnnungbanu(g)
Plkhilngmusdngtroha(g).
II.
13
Bc 3 :XcnhringMg2+:
Buret:RatrngvnpydungdchEDTA0,02N.
Bnhtamgic250ml(3bnh):10mlmu+NH310%(sgitbngthnghimxc
nhtngCa+Mg)+2mlNaOH2N+chthMurexide1%.
ChunbngdungdchchunEDTAnkhidungdchchuyntmuhng
sangtmhoac.
GhithtchEDTAtiutnchotngCa2+lVII.
Bc 4:tsliuthuctnhktququyvmg/100gmu.
2. Tnh kt qu.
S liu ban u:
Khilngmup
ThtchnhmcVm
6,4131g
300ml
Kt qu chun .
Trungbnh
V1
1,4ml
1,4ml
1,5ml
1,43ml
Trungbnh
Lnchun
V 2
0,7ml
0,8ml
0,6ml
0,7ml
Lnchun
EDTAtiutn(: Xcnh
tngCa2+vMg2+)
EDTAtiutn(: Xcnh
ringCa2+)
14
Hm lng Ca2+
Cngthc
X Ca 2
(V 2 V m 0,004 )
100
Vm p
Ths
X (%)
Ktqu
1,3098(%)
Hm lng Mg2+
Cngthc
X Mg
(V V 2 ) V m 0,0024
1
100
Vm p
Ths
X (%)
Kt
qu
(%)
Vi:
2+
2+
V1 :thtchtrungbnhEDTAtiutn(XcnhtngCa vMg )
2+
V 2 :thtchtrungbnhEDTAtiutn(XcnhringCa )
Vm:thtchnhmc.
Vm:thtchdungdchmuemixcnh.
p:khilngmu
Cu hi.
1. Tthcnghimvitnguyntcxcnh,ccphnngchoccchtiutrn.
2. Trnhbycccngthcvgiithch.
3. Trnh by nhng nguy c gy ra sai s khi tin hnh phn tch cc ch tiu trn,
cchkhcphc?
4. TrongtrnghpnothcnphicmutrngkhixcnhCa,Mg?
5. Phnbthigianhplvtrttcccngviccnthchinchobithnghim,
15
giithchchospxpmAnh(Ch)chn?
Tr li
1. Nguyntcxcnh,ccphnngchoccchtiu.
Xc nh tro ton phn trong sa bt: Dng sc nng (550 6000C) nung chy
hon ton cc cht hu c. Phn cn li em cn v tnh ra % tro c trong thc
phm.
2. Nguynnhngysais.
Cthdotrongqutrnhcnmukhngchnhxc=>nnsdngcnphntch
chnhxcn0,0001g.
Mtmudotrongqutrnhchuyntdngcnysangdngckhc=>sdng
trctipmtdngctinhnhthnghim.
Mtmudotrongqutrnhthanhagilmthtthotmu=>ngcatrnhgi
khithanha.
Saisdngcchunbngtaynnvicxcnhimtngngchac
chnhxclm=>chunbngmy.
Hachtlungytrongphngthnghim=>sdnghachtmi.
3. Trongtrnghpkhicnxcnhcngcancthcnphicmutrngkhi
xcnhCa,Mg.
4. Phnbthigianhplvtrttcccngviccnthchinchobithnghim:
Sychnnunghtmcnchncnmuthanhatrnbpintro
trng trong l nung 6600C ht m trong bnh ht m cn trng lng chn
mu sau khi nung cho tro vo bnh nh mc 3ml HCl nh mc ti vch
chunb3bnhtamgicthmhachtnhyucura,trngnpyburetbng
dungdchEDTA0,02Nchunlnltvghiktqutngbnhchotngtrng
hp.
Giithch:nungchntrcxcnhtrnglngchntrc,thanhatroha
vthigianthanhavtrohadi,chunbhachtkhitrohaxong.
16
1. Nguyn tc
Saukhitroha,musacnliFevP,emomubcsng=510nm
ivixcnhFev=400nmivixcnhP.Sau lpthng
chunsuyrahmlngFevPctrongsaquyvmg/kg.
Fe(II) trong dung dch kt hp voi81 1,10-phenaltroline thnh mt phc cht
mu cam bn trong mi trng pH 3-9. Nu mun mu ny khng b nh
hngcathucthdvcmtcaccionkhc,phnngcntinhnh
pH3,5-4,5.
Phcchtnygm3phnt1,10-phenaltrolinekthpvi1ionFe(II).Phn
ngchiuchoFe(II)nnphichuynhtFe(III)vFe(II)bngcchkhvi
hydroquynonhayhydroxylaminclohydric.
2NH2OH+4Fe3+N2O+4Fe2++4H++H2O
2. Cc bc tin hnh xc nh hm lng Fe c trong sa
Bc 1.Cn6.01gmusatrongchnnungsch,kh.
Bc 2. Thm 10ml glycerol:etanol (1:1) v than ha t t trn bp in n ht
khi,trnhchythnhngnla.Sauembchnnungchamuvothitb
htkhinkhinohtkhi.
Bc 3.avolnung6500Ctrong1gi,lmngui,thm1mlHNO3mc,
tiptcavolnungtip30pht.
Bc 4.Chngui,thmtip1ml6Nvotrounnhtrnbpincliamiang
nkhivacn,thm5mlncct2ln,khuynhbngathytinh,chuyn
sangcc100ml,rachnnung2n3ln, nhpchungncra vocc.Dng
NH3 10% chnh tng git cho n khi pH= 3,5 5 ( th bng my pH), sau
chuynvobnhnhmc100ml,dngncct2lnnhmctivch.Tac
dungdchmu:dngxcnhtngFevP).
17
Bc 5.Thmlnltcchachttheobngsau:
Xc nh Fe
Dungdch(ml)
B1
B2
B3
B4
B5
Bmu
DDFe(II)10ppm
DDmu
10
DDHydroxylamin
10%
1(lc1
pht)
DDmpH=5
1,10-phenaltroline
0.1%
H20ct2ln
CFe(II)(g)
Lcnh,sau5pmidngncctnhmctivch
0
10
20
30
40
Cx
Sau15phtemo=510nm
3. Kt qu v tnh ton
Ktquthnghim:
CFe (g)
B1
0
0
B2
10
0,078
B3
20
0,16
B4
30
0,24
B5
40
0,329
Bmau
x
0,254
Tnhton:
18
0,35
y = 0,008x - 0,002
R = 0,999
0,329
0,3
0,25
0,24
0,2
0,16
0,15
0,1
0,078
0,05
0
0
0
10
15
20
25
30
-0,05
35
40
45
CngthctnhhmlngFe
Tacphngtrnhngchun:
y=0,008x0,002
0,254=0,008x0,002
x=CFe=32(g)
II.
1.
2.
19
Bc3:thmlnltcchachtvobnhnhmc25mlnhbng
sau:
B1
B2
B3
B4
B5
Bmu
DD chun P 100ppm
DD mu
0.1
Amonilybdovanadate
5 ( lc 1
pht)
H2O ct 2 ln
Cp(
100
200
300
400
Cx
3.
Kt qu v tnh ton
Ktquthnghim:
CP (g)
B1
0
0
B2
10
0,331
B3
20
0,675
B4
30
1,108
B5
40
1,445
Bmau
x
0,37
Tnhton:
20
1,6
y = 0,003x - 0,021
R = 0,997
1,4
1,2
1
0,8
0,6
0,4
0,2
0
-0,2
50
100
150
200
250
300
350
400
450
CngthctnhhmlngP
Tacphngtrnhngchun:
y=0,003x0,021
0,37=0,003x0,021
x=CP=130,33(g)
21
+yNH3khimui(NH4)2SO4bngbazmnh
(NH4)2SO4+NaOH2NH3+2H2O+Na2SO4
+nhlngNH3bayrabng1acid
2NH3+H2SO4(NH4)2SO4
NaOH+H2SO4dNa2SO4+H2O
2/ Cch tin hnh:
+Ly1mlncmm+2gxctcCuSO4.K2SO4+10mldungdchH2SO4mc
+Tinhnhvchomuchonkhong1h30pht,khidungdchchuynmuxanh
ltrongsut
+ngui,chovobnhnhmc100mlvnhmctivchbngncct.
+LprphthngbctmKjeddahl.Tastinhnhchngctct3lnvi2mu
ncmmv1mutrng(ncct).
Ln 1:Cho20mldungdchmu+vigitchthphenolphtalein+10mldung
dchNaOH0,1Nvophucabctm.Mvanttchodungdchtrnchyvo
bnhct,trngraphubngncctvkhovanli
Chunbbnhtamgicgm:20mldungdchH2SO4+vigitchthTashirov
hngvoungcabsinhhnngphntrongdungdchcabnhtamgichng,
dungdchtrongbnhtamgiccmutmnht.
22
Tinhnhctkohinctrongkhong15pht
Nngungsinhhnrakhimtdungdchtrongbnhtamgic,dngbnhtiara
ungsinhhn,tiptccttrong30giy.DnggiypHkimtra,nudungdch
khnglmimugiypHlc
LybnhhngemichunbngdungdchNaOH40%,dungdchchuynttm
sangxanhnht.ThtchNaOHtiutnl17ml
Ln 2:Lmtngtnhln1.ThtchNaOHtiutnl17,1ml
Ln 3:Thaydungdchmubngncct.Tinhnhccbckhcnhln1.Th
tchNaOHtiutnl18,6ml
3/ Tnh ton kt qu:
Ln 1:
10
14
1000 6,25
14 1 1000 6,25
1
= 14
Ln 2:
10
14
1000 6,25
14 1 1000 6,25
1
= 13,125
23
Cc bc thc hin
1.
Nguyn tc
Ttcccdngnitctrongcthhaytrongccmcgilnittngs
(mtng).NitctrongthnhphnaxitamincaproteinlNprotein.Nitkhngc
trongthnhphnproteinnhccmuimvc,axitnitric,ccaxitamintdo,ure
v cc dn xut ca ure, cc alcaloit, cc baz purin v pyrimidinl cc nit phi
protein.
Nittngs(mtng)=Nitprotein+Nitphiprotein
MucvchobngH2SO4()nhitcaovcchtxctc.Ccphn
ngcaqutrnhvchomuxyranhsau:
2H2SO42H2O+2SO2+O2
Oxytothnhtrongphnnglioxyhoccnguyntkhc.Ccphntcha
nitditcdngcaH2SO4tothnhNH3.Ccproteinbthuphnthnhaxitamin.
CacbonvhydrocaaxitamintothnhCO2vH2O,cnnitcgiiphngdi
dngNH3kthpviaxitH2SO40,1Ndtothnh(NH4)2SO4tantrongdungdch.
2NH3+H2SO4(NH4)2SO4
CcnguyntkhongkhcnhP,K,Ca,Mg,chuynthnhdngoxit:P2O5,
K2O, CaO, MgOtuy tn ti trong dung dch mu nhng khng nh hng n kt
quphntch.
Pht hin v o nit tng s (m tng): Phng php n gin nht o nng
nittngs(mtng)trongdungdchlhpthtiacctmcan.Nunittng
s (m tng) tinh sch th nng tuyt i ca n c tnh theo gi trc o.
24
Nunittngs(mtng)khngtinhschthnngcanittngs(mtng)
ctnhtngithpph.
2.
Kjeldahl.Saukhivchomuxong,tonbmu+ngKjeldahlclmnguiri
tinhnhquytrnhlnmumu.
a. V c ha mu:
QutrnhnycthchinhontontrongtHotte.
0,2mlncmmvongKjeldahl
+0,4ghnhpxctc
Dngpipetht3mlH2SO4mc
(d=1,84)chovongtrn
t0=2000C
Lpngtrnvohthngvc
homukhong20phtthxem
mu 1 ln cho n khi mu c
muxanhtrongthngngvlm
nguimu
Vicvchomuhontonkhitonbdungdchtrongngvchomuhon
tontrng.
Bc 1: Cho 0,2ml nc mm vo tn y ca ng Kjeldahl +0,4g hn hp xc tc
25
(chkhngdnhtrnthnhng)thucktqucaonht.
Bc 2:Dngpipetht3mlH2SO4mc(d=1,84)chovongvchomuc
chahnhptrn.H2SO4mcnhmtchyhnhphuc(khitnngmu
viH2SO4(),cchpchthucctrongmuboxihatothnhSO3,SO3phnli
thnhSO2voxinguynt.Oxicthirasoxihahydrovcacboncahpcht
hu c c trong mu to thnh CO2 v H2O.Cn N2 s c chuyn thnh dng
NH3.
Bc 3:Lpngtrnvohthngvchomuphmu(cimykhong20
phtnusau20phtmuvncnmuthtiptccithm20phtnachonkhi
mucmuxanhtronglc)rilmngui.
b) Xy dng chun:
Chunb6bnhnhmc25mlsch,khrithmhachttheobngsau:
Becher
B1
B2
B3
B4
B5
B6
DungdchN20ppm(ml)
0,1
0,3
0,6
0,9
1,2
Ncct2ln(ml)
2,9
2,7
2,4
2,1
1,8
mpH=6(ml)
ttNessler(git)
N(g)
12
18
24
Ncctva,nhmctivch
Sauoquang=440nm.
MubnhnhmcnhtmdntB1nB6
otngtheothttbnhB1nbnhBmu
26
TrngcuvetbngDDB1,rirtDDB1vovcchmingcuvet5mm.Cho
cuvetvomyUV-VISvoghiliktquo.
Lu : trnh cc bt kh c trong cuvet khi rt dung dch vo.
Lmlnltvicc bnhcnli(trngcuvetbng DDtiptheo)vghikt
quo:
c) Ln mu mu:
Chuynmuclmngui(saukhivcha)vobnhnhmc100ml,
nhmctivchbngncct2ln(lcu).
Sauht1mldungdchmuphalongchovobnhnhmc25ml+0,9mlH2O+
1,1mlNaOH1%+2mlmpH=6+5gitthucth(dungdchNessler),sauo
quang=440nm.
d) Tnh ton kt qu:
3. Kt qu:
Becher
B1
B2
B3
B4
B5
B6
Bmu
N (g)
12
18
24
hp th quang A
(= 440nm)
thdychun
27
4. Tnh ton:
a. Phng Php ng Chun:
C s nh lng
nhlutBougher-Lampere-Beer:khichiumtchmphotonnscquadung
dchthmchpthcadungdchtlthunvicngsutchmphotonvnng
ccphnthpth
Cngthc:A=.l.C
Quy trnh
-
PhamtlotdungdchchuncCtctngdnmtcchun(thng58Ctc)(Cc
dungdchchunphiccngiukinnhdungdchxcnh)
TinhnhoAhocTcadychunchn.
DngthAX=f(Cx).VitPTHQtuyntnhcangchun.
Tinhnhphachdungdchxcnh.
oAhocTcamu.
CncvoPTHQtuyntnhcadychunvAXmxcnhnngcachtX
trongmu.
thA=f(Ctc)tutheocchotathuc2dngngchun:
Dng1:iquagcta
Dng2:khngiquagcta
Khichnvngnngxydngngchunphich:
VngnngcadychunphibaogmcCX
VivngnngchndungdchphituntheonhlutBeer
28
CcgitrAtcngvinngchnphisaochokhiotrnmyc
lplicaovbomstuyntnhA=f(C).
StngquangihpthquangAvnngCkhil=constlnidungca
nhlutBeer.Khongnngthamnnhlutnykhir>0,999.
Hstngquanrbinitrongkhong-1r1(R2=01)
-
Khir1cstngquanchtchgiaxvytheotlthun.
Khir-1cstngquanchtchgiaxvytheotlnghch.
Khir0haiilngnykhngcntngquan.
b. Xc nh Nit Tng S (m tng)Trong Thc Phm:
Tbiutrntacphngtrnhngchunthhin miquanhgia
Hstngquan:R2=0,9615=>R=0,9806
Trong:
xlnittngs(mtng)
ylhpth.
Tachpthcamuocl:y=0,049.Suyranngcanittng
sctrongmul 0, 049 0, 0213 x 0, 0092 x 2, 732 gN
Trong0,2mlc2,732gN
Vysuyratrong1mlc13,66gN(C)= 13, 66103 gN
Tnh % m:
%m = K 0, 01 C
29
K=f/mu(f=6,25)=>K=
6, 25
=31,25
0, 2
CsgNtrongmu
%mtrong1ml= 31, 25 13, 66.103 0, 01 0, 4268%
Trong1mlc%m=0,4268%
Vytrong100mlc%m=42,68%
c. Nhn xt kt qu:
Sovithctmtrongncmml450nhngthcttaemphntch
ktquchl42,680.Vytrongqutrnhthnghimmcsaisln.
Nhng yu t c th nh hng n kt qu th nghim, sai s
NngH2SO40.1Nkhngmbochnhxc
Lymukhngidin
Cnmukhngchnhxc
NgunncctcthbnhimN
Trongqutrnhlmvicvimykhngcnthntrongvicamuvodnh
trnmingngvlpngblch.
Phng php gim thiu sai s l:
Cnphikimtrahacht.
Cnthntrongthnghimhnvthaotcvthchin.
30
XcnhlngNitoacidaminctrongncmm.
b) Nguyn tc thc hin:
Acidamintrongdungdichncmmthtrungtnh,khigpformon,ccacid
amin b mt tnh kim, tnh acid ca COOH tri ln. Do c th nh lng nhm
COOHbngdungdchkim.
c) Tin trnh th nghim:
Bc 1:
50mlncctkhuyu,thm2gBaCl2sautlnmykhuttkhuyusau
thmtnggitBa(OH)2bohatrongCH3OH,iuchnhpHbngmytipH=8.3.
Chuynvobnhnhmc100mlridngncctnhmctivch.
Bc 2:
-
TinhnhsonghnhcngvichiuchnhnngNaOH0.1Nvidungdch
chun H2C2O4 0.1N, ch th PP 0.1% 3 ln, mi ln 10ml dung dch H2C2O4
0.1N
Ly10mldchlcchovobnh250ml,thmtip10mldungdchHCHO20%
trungtnhkhuyubngcttrong15pht.
Nhnginccthytinhngptrongdungdch,trnhsty,khuyutrong
5pht.
Chun t buret bng dung dch NaOH 0.1N n khi pH=8.3 v ghi li th
31
tchNaOHtiutn.
d) Tnh kt qu:
Nitoformon
0, 42 g / l
Vm
10
10
Trong :
0,0014gamnitngvi1ldungdchNaOH0.1N
VNaOH:ThtchdungdchNaOH0.1N
f:HsiuchnhdungdchNaOH
Vm:Thtchmuemlmthnghim
Gii thch kt qu
N-formolphnnhphnNitocaccacidaminvcaAmmoniactc
lccchtdnxutcaqutrnhproteinclnmen.ChsN-formol/N-ton
phnthcchtlongucancmm.
2. nh lng m NH3 (m thi): (phng php Kjeldahl):
a) Mc tiu
XcnhlngmNH3(mthi)ctrongmmnm.
b) Nguyn tc thc hin
Dnghinckoamonicgiiphngrathtdosangbnhchun
vkthpvimtlngdaxitH2C2O40.1N.Chunsaukhichngctxongbng
dungdchNaOH0.1N.
c) Tin trnh th nghim
Bc 1:Xlmu
Cn10gmummnmsauchovocisvcho25mlncctvov
nghinnh.Saulcquagiylcthudchmmnm,dchlcthuc
32
csdngchobctiptheo.
Bc 2:Tinhnhchngct
Tinhnhlprpbchngctm,chovobnhcukhong2/3ncct
vrabchngctmchonkhinctrongngsinhhnchyxung
khong20mlthttbp,hnhitlmschhthngriktthcqu
trnhra.
Chuyntonbdchlcthucvohthngchngct,dngncct2
lntrng.
Trongqutrnhctchothm25mlNaOH2Nquaphusauxttcho
nkhicn1ml,thm5mlncctxnkhicnkhong2mlthkhali.
Chovobnhtamgichng20mlH2C2O40.1N+3gitchthTashiro.
Nhng u ng sinh hn ca b chng ct m ngp trong dung dch ca
bnhtamgichng.
Mncvongsinhhn.
Tinhnhctkohinckhong30pht.
Saukhiht30phtthtanngungsinhhnlnvtrngungbngnc
ctsaudngqutmhnggitncthotraungsinhhn.Nugiyqui
thnhmuxanhchngtcnkhNH3thtatinhnhchngcttip,cnnugiyqu
khngimucnghahtkhNH3vktthcqutrnhct.
33
Hnh 1. B ct m Kjeldahl
Bc 3:
ChunlngH2C2O40.1NdtrongbnhhngbngNaOH0.1N
emichunbngdungdchnynkhidungdchtrongbnhtamgicchuynt
muhngnhtsangmuxanhlthdnglivghithtchNaOH0.1Ntiutn.
d) Tnh ton kt qu
Tac: % NH 3
0, 255%
m
10
Trong :
V1:ThtchdungdchH2C2O40.1N(ml)
V2:ThtchdungdchNaOH0.1N(ml)
N:nglngdungdch
F:HsiuchnhdungdchNaOH
m:Khilngmucn(g)
34
e) Bn lun
Trong thc t ta thy m thi ch chim mt lng kh nh so vi lng
mctrongmmnm.
N-Ammoniac phnnhphnNitoaminbphnhothnhNH2vNH3(c
mi khai, c i vi c th, thng c gan chng ta kh c nh chc nng
sinhUr,tchn,trckhithiranctiu).TlNH3cngcaothmmcng
thi.
35
CuSO4+2NaOHCu(OH)2+Na2SO4
-SauddCu(OH)2tcdngvimuiSeignetttothnhmuiphchatan,ddc
muxanhthm.
Muiphctrnlmthpchtkhngbn.Ccngcchanhmandehit
hocxetonddngkhCu2+thnhCu1+,torakttang(I)oxitmugchv
ngboxihakhitcdngviddfehling.
nhlngng(I)oxit:
-
OxithanbngFe2(SO4)3hocbngamonistkpsunfattrongmitrng
acidsunfurit,Cu1+boxhtrliCu2+,Fe3+bkhFe2+
+
) +
+2
xcnhlngFe2+:
-
BngcchoxhnhddKMnO4trongmitrngacid:
36
10FeSO4+2KMnO4+8H2SO45Fe2(SO4)3+2MnSO4+K2SO4+8H2O
TlngKMnO40.1Ntiutntrongchuntrabngccsml
nglactoza,glucozo,maltozo,saccarozo...rinhnvihsphalongtachm
lngngtrong100gsa.
2. Tin hnh th nghim
Bc 1.Cn2-2.5g saccngvoccthytinh 50ml,hatanvi mt
lngncmsauchuynvobnhnhmc100mldngncnngtrnccri
nhp vo BM n 75ml. ngui. Sau cho 5ml K4[Fe(CN)6] + (CH3COO)2Zn
30%vo,lcu,lmnguinhmctivch,lcquagiylc.cddI.
Bc 2:Chovobnhtamgic250ml10mlddfelingA+10mlddfelingB.un
si,khiangsichovo5mlddIv10mlncct,si2p.Lybnhranghin
choCu(I)dnv1gcc5-10p.
Bc 3. Lc gn bng nc nng qua phu G4 di p sut thp, dng lc khi
nctrongbnhhtmuxanh,trnhngchoCu(I)rivophuvkhngtatip
xcvikhngkh.
Bc 4.Hatantatrongbnhtamgicbng10mlddFe2(SO4)35%,chuynht
ddvophurihthtttcvomtbnhtamgicmi.
Bc 5.Sauchovo10mlH2SO46NriemichunbngddKMnO40.1N
chonkhisuthinmuhngnht.
3. Kt qu v tnh ton
Ktquthnghim:
Khilng
mu(g)
ThtchKMnO4tiu
tntrongchun
(ml)
Thtchdung
dchemxc
nh(ml)
Thtchnh
mc(ml)
2,3565
100
37
Tnhton:
Hmlnglactoza/100gsa=
.
mmau
Vmau
Vdm:Thtchnhmc(ml)
Vmau:Thtchdungdchemxcnh(ml)
Mmau:Khilngmu(g)
VKMnO4:ThtchKMnO4tiutntrongchun(ml)
NKMnO4:NngnglngcaKMnO4
Hmlnglactoza/100gsa=
.
58, 0522
mmau
Vmau
2,3565
5
38
FelingB:37,5gKalinatritactrathatantrong100mlncct+25gNaOHhatan
vnhmcn250ml.
Dung dch Feling (ch pha trc khi s dng): 15ml dung dch Feling A + 15ml
dungdchchunglucoza0,005g/ml,unsi15giyCu2Ohnhthnh+5git.
MB1%(trongH2O),unsithm1giy.
Chunbngdungdchglucozachun0,005g/mlnkhimtmuxanh,ghiV1(ml)
tiutn.
39
20mldungdchFelingvobnhnn250mlkhc,thmchnhxcV1mldungdch
II,unsidungdch15s,thm5gitMB1%,chunbngdungdchglucozachun
nkhimtmuxanh.GhiV2(ml).
3. Tnh kt qu.
Kt qu chun
Thtchglucozatiutn(V1)
Thtchglucozatiutn(V2)
11,1(ml)
13,9ml
Hm lngSaccaro
Cngthc
Ths
Ktqu
Saccaro/100gX=
11,1
0,00324(g/ml)
10 V1 V2 0,005
V1
Vi:
-
X:llngglucoza(g/ml).
Vy:lngglucozactrongdungdchIIl:100XvtrongdungdchIl200X.
Lngglucozadolactozanghchchuynl:Y
Lngglucozadosacarozal200XY
%Sacaroza=Z
M glucoza
M lactoza
M glucoza
M lactoza
=Z.
100
0,95 .
25
Cu hi.
1. ChobitvaitrcaHCl?Vitccphngtrnhphnng.
2. Thitlpcngthctnhhmlngngsaccaroza.
Trli:
40
X:llngglucoza(g/ml).
Vy:lngglucozactrongdungdchIIl:100XvtrongdungdchIl200X.
Lngglucozadolactozanghchchuynl:Y
Lngglucozadosacarozal200XY
%Sacaroza=Z
M glucoza
M lactoza
M glucoza
M lactoza
=Z.
100
0,95 .
25
Theophpchuncnbngth:
(10+V1)0,005=V1x+V20,005x=
10 V1 V2 0,005
V1
KT QU BN LUN
Hmlngsaccarozamnhmtnhcchothygitrhmlngsaccaroza
trongsachimmttlnh,vcschnhlchrtnhiusovihmlnglactoza
ctrongsa.Nguynnhnlvsaccarozacngtcaohnccloingkhcc
trongsa,vimtlngthchhpsgpphnnngcaongtcasa.Ngoira,
mt s trng hp c th ngi khng c kh nng dung np lactoza do khng c
enzyme phn gii, v vy vic b sung thm saccarozo l iu cn thit
41
Eteduhahtnchnetethng,ctnhchtyncvccchthatan
trongncrakhietethnglmchoetethngchcchachtbovetedu
42
ha.Ngitacngkhngthdngeteduhathaythchoetethngvetedu
hakhnghatanccchtbocnc.
-
nmtrngmdungmivbo,phanngnmdigmncvccchtha
tantrongnc.Tathuphanhgmdungmivbo,lmbayhidungmitathu
ctngbotrongmusa.
Ht5mlsatikhngngvophuchitqul,saucho5mlestevo.
Tiptheochothm10mlcnammoniac(208,5mlC2H5OH900+7,5mlNH325%+
H2Oct=250ml)+1gitPP1%.
-
Lcphuchit,sauyntrong30pht.
Tchblpdi,gililptrn(lpeter+bo).
-
Thmtip5mleterduha,lcmnh2pht,yntrong15pht,tiptctch
Chobayhietertrnbptrongtht.
Cnccxcnhkhilngchtbom1.
%bo=
( m1 m0 ) 100
mm
Trong:
m1=46,85glkhilngccvchtbosaukhiuntrnbptrongtht.
m0=46,78glkhilngccbanu.
mm=5glkhilngmubanu.
43
%bo=
=1,4%.
Nhn xt.
Hmlngchtbothuctrongthnghimtngithpsovithct.Nguyn
nhncldothaotctrongqutrnhchangvhachtkhngctinhkhit.
44
Xc nh ch s axit
1.
Mc tiu
-
ChsaxitlsmgKOHcnthittrunghaaxitbotdoctrong1gcht
th.
Xcnhchsaxittrongdumngthcvtbngphngphptrungha.
2.
DngdungdchNaOH0.1Ntrunghaccaxitbotdotrongchtcnth
vphenolphtaleinlmchthmu.
3.
Cc bc tin hnh
-
Cn5gduchovobnhtamgic250mlcsykh,thm25mlC2H5OH
950 trung tnh + 25ml ete trung tnh, lc cho n khi cht bo tan ht, thm 3
gitchthphenolphtalein1%.
ChunttbngNaOH0.05Nnkhidungdchcmuhng,ghithtch
NaOH0.05NtiutnlV=0.4ml
4.
Tnh kt qu
ChngtadngNaOH0.05Nchunnnktquctnhtheocngthc
sau:
Chsaxit
0,1668
2mm
mm
mm
Trong :
-
5.61:smgKOHtngngvi1mldungdchNaOH0.1N(Dotrongbily
nngNaOH0.05Nthinntaphichiacho2dimus).
V:SmlNaOH0.05Nsdngtrongnhlng(ml)
mm:Trnglngchttheminhlng(g)
45
Gii thch kt qu
Dumcnglmitrngthunlichomtsvikhun,nmmcpht
trin.Ngoiranhngyutnhsng,nhit,nc,kimloi,oxycngtc
ngnccdynikhngbohalmchodumbbincht.Nhvynu
mchsacidcnglnchngtlngchtboctrongthcphmcngcao
chonnccsnphmnydbhhngdoccvisinhvttncng
II.
1.
Mc tiu
Xcnhccaxitbokhngnoctrongchtbo.
2.
Nhnglinktkhngbohacaccaxitbokhngnockhnnggnvi
Iodhoccchalogenkhcdotaxcnhcccaxitbokhngnoctrongcht
bo.
3.
Cc bc tin hnh
Cnhiuphngphpxcnhchsnynhngtrongbithnghimnyta
chnphngphpWijs.
Mudun:
-
Cn1gdunchovobnhtamgiccntnhmcsykh.
Cho20mlCCl4+30mlthucthWijs(dungdchcloruaIod)lctrong1pht
riyntrongbngti1gi.
Thm20mlKI10%+90mlncct.
ChunbngNa2S2O30.1Ngncuiqutrnhchunchothm2mldung
dchhtinhbtvochunchonkhidungdchmtmuhonton.Ghili
thtchNa2S2O30.1Ntiutn.
Mutrng:
-
Cho1mlncctvobnhtamgiccntnhmcsykhemtrong
bngti1gi.
Thm20mlKI10%+90mlncct.
ChunbngNa2S2O30.1Ngncuiqutrnhchunchothm2mldung
46
dchhtinhbtvochunchonkhidungdchmtmuhonton.Ghili
thtchNa2S2O30.1Ntiutn.
4.
Tnh kt qu
ChsI2(gI2/100g)
a=40,7ml
b=14.6ml
m=1g
32, 23
m
1
Trong :
m:Lngthucthxcnh(g)
a:ThtchNa2S2O30.1Nemichunmutrng(ml)
b:ThtchNa2S2O30.1Nemichunmuth(ml)
5.
Bn lun
ChsIodnilnmcchanocadubo.Chsnycnghakhikim
trachtlngchnghnyucucaloidudal...,nudngphnngkimtrach
s Iod thy khng t th c th kt lun khng t ch tiu cht lng.
VphnngochsIodngitadavophngphpthatrtclcho
Xc nh ch s peroxid
1.
Mc tiu
GiiphngI2ctrongmuiKIranhdungdchNa2S2O3.
2.
Khicoxikhngkhccaxitboctrongthnhphncadunhtlccaxit
bokhngnosddngboxihamtphnvtothnhperoxid.
Vicxcnhchsperoxidcthdavoccphnngsau
LngIodgiiphngracthchunbngdungdchNa2S2O3.Vichthl
htinhbt
47
2Na2S2O3+I2=>2NaI+Na2S4O6
TheolngNa2S2O3cnIodgiiphngracthtnhcchsperoxid..
3.
Cc bc tin hnh
Muth:
-
Cnvobnhtamgiccntnhmcsykh:1gmu+1gNa2CO3+
15mlCH3COOHmc,ynplcnkhiNa2CO3tanht.
Mnpchonhanh10mlCHCl3volcchonkhitanht,thmnhanh1mlKI
bohalctrongti5pht,thm75mlncctlcduvchunbngdung
dchNa2S2O30.02Nvihtinhbt1%lmchth.
Mutrng:
-
Mnpchonhanh10mlCHCl3volcchonkhitanht,thmnhanh1mlKI
bohalctrongti5pht,thm75mlncctlcduvchunbngdung
dchNa2S2O30.02Nvihtinhbt1%lmchth.
4.
Tnh kt qu
Chsperoxidlsmilinglngcaperoxidctrong1kgmuchtbo.
Chsperoxid(mgH2O2/kg):
Vm=3.6(ml)
VB=1.2(ml)
mm=1g
48
mm
1
Trong :
Vm:smlNa2S2O3tiutnchomu
VB:smlNa2S2O3tiutnchomutrng
mm:Khilngmuemlmthnghim(g)
N:nglngdungdchNa2S2O30.02N
KT QU BN LUN
48
Cnphitinhnhchunnhanhvdungdchdbayhidntimudung
dchsbcchonnktquchunskhngtrnhkhisaist.
CnynpbnhtamgicvI2dbthnghoachonncnphiynpv
trongbngtivoxikhngkh+nhsngsoxihaccaxitbokhngnotothnh
peroxidedntiktqubsai.
49
Bnh25ml
Mu
Mu
Nitri
Nitra
te
te
DungdchI(ml)
Cdht
3ht
CH3COOH1:1
0.5
1.5
(ml)
NO2g/ml :20
ppm
GiressA(ml)
50
CH3COOH4N
GiressB(ml)lc 1
(ml)
Ncct1ln
NO2(g)
12.5
25
37.5
50
Cx1
Cx2
0.224
0.450
0.601
0.860
0.027
0.038
Ghich:
Dungdchmucthly1,2,5,10,15mltyhmlngnitritetrongmu.
KhilyCdht,cnlcthtnhanh,saukhilyphilptcykntrnhCd
httipxcvikhngkh.
SaukhichothucthGiressAvophilcutrongvng5pht.
KhichoCH3COOH4Nvophilcu.
KhichothucthGiressBvophilcutrong5pht,trnhdnhln
tay.
emosau15pht =540nm.Dngkthutngchuntnht
tnhCx.
51
1
0,9
y = 0,016x + 0,007
R = 0,995
0,8
0,7
0,6
0,5
0,4
0,3
0,2
0,1
0
0
10
20
30
40
50
60
thchun
Tacphngtrnhngchunl:y=0,0168x+0,0076
Tnh C 1x ? vibnhmu1,y=0,027
C 1x x
0,027 0,0076
1,1548
0,0168
C1 (mg / kg )
287,836
10.m
10.10,03
Tnh C x2 ? vibnhmu2,y=0,038
C x2 x
0,038 0,0076
1,8095
0,0168
C 2 ( mg / kg )
902,044
25.20.m
25 20 10,03
52