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Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BO CO TH NGHIM PHN TCH THC PHM


BI 2.XC NH CHUA V MN TRONG THC PHM
1. Xc nh chua trong Yomost
a) Nguyn tc
DngdungdchNaOH0.1Ntrunghalngacidctrongmuvicht
chthphenolphtalein1%.
b) Cc bc tin hnh
Bc 1.Chomuvocc.
Bc 2.Chuyn10mlmusangbnhnhmc10ml,nhmctivch.
Bc 3.Chuyn50mlmusangcc250ml+ct.
Bc 4.incc,raschbngncct,nhngngpvodungdchkhngchm
voyccmu.
Bc 5.Citthngschun.
Chnchmy
Titratinonready Mnhnhmcnh

ngha
Snsngchun

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

pHtitration

Dynamic(EQ) D pH tng ng: Chn phng


phpdpHttheophngphptip
tuyn
Dynamiccontrol
Kim sot qu trnh d: Chn d
Steepjump
theotngbcnhy
Endoftitration
iukindngchun:Chntheo
ml
thtchtiutn
Totalcomsumpt,
Tng th tch tiu tn kt thc
Ex:10ml
titrafinal
chun:vdchn10ml(nghal
consumpt,ml
khichuntithtch10mlthskt
thcqutrnhchun)
Driftcontrol
Tcchun:Chnnhanh
Fast
Waitingtime 1s
Nhp gi tr thi gian bt u tin
(s)entervalue
hnh chun sau khi hon tt ci
t
Ext,trtrapt,burettle No
Chchuntrc(nhmtitkim
thigian):ChnNo
Reactiontime 1s
Thi gian phn ng: Chn 1s (xem
(s)waitingtime
nhphnngtcthi,nuphnng
thun nghch, chm cn chn thi
gianlnhn)
Predosing
Bm trc: Chn No (Do khng
No
chuntrc)
Filldosineunit
Gitrthtchdungdchchuncn
Fill
bmychoburet:Chnbmy
Newcaculation
Formular
Tnhton:Chncngthctnhton
selection
choimtngng.
EQ(equipvalent)

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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:

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Lng nc o c (ml)

Khi lng mu (g)

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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)

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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.

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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).

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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.

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 3 : XC NH TRO TON PHN Ca, Mg TRONG THC PHM


I.

Xc nh tro ton phn trong sa bt:

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

Bc 3: Tro ha trong l nung 60 pht vn cn tro en ly a thy tinh


nghinnhalivolnungnungtip30phtchonkhictrotrng
lyravnguitrongbnhhtm.

Bc 4 : Sau khi ngui trong bnh ht m30 pht, ly ra mang cn cn


phntch

Khilngchnnungvmusaukhinungm2 = 22.7156g
4.Tnh kt qu
-Hmlngtrotonphntrongsabt:
=

. 100 (%) =

22.7156 22.6647
. 100 = 2,4428%
2,0837

Trong:
-

G1lkhilngcachnnungvmusautroha(g)

12

Bo Co TN Phn Tch Thc Phm

Glkhilngchnnungbanu(g)

Plkhilngmusdngtroha(g).

GVHD. ThS V Hong Yn

II.

Xc nh Ca, Mg trong sa bt hoc phomat.

1. Cch tin hnh.


Bc 1: Chunbmu.
ngnhtmu.
Cnmuvochnnung:5-6gsa
Than ha : Chuyn chn nung + mu than ha trn bp in cho n khi ht bc
khi.
Troha:Chuynchnnung+thanmuvolnung6500Cnkhitrotrng,nu
tro cha trng thi ch chn ngui thm 3 git HNO3 hoc 3 git H2O2 30%,
nungtipchonkhitrotrng.
Cnbngnhittrongbnhhtm30pht.Saukhilychnracalnung5pht.
Lytrobctrn+5mLHCl2Nunnhchonkhisigncn,thm10mL
nccthailn,khuynhrichuynvoBM300ml,rachnnung,ncra
vdchtrngcnhpchungvoBM300ml,cuicngdngncct2ln
nhmcnvch.DungdchnydngxcnhCa2+,Mg2+(chunbmucho
clp).
Bc 2: XcnhtngCa2+vMg2+:
Buret:RatrngvnpydungdchEDTA0,02N.
Bnhtamgic250ml(3bnh):10mlmu+thmtnggitNH310%tipHkhong
8(thbnggiypH)+5mlmpH=10+3gitchthETOO.
ChunbngdungdchchunEDTAnkhidungdchchuyntmunho
sangxanhchm.
GhithtichEDTAtiutnchotngCa2+vaMg2+lVI.

13

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Hm lng Ca2+
Cngthc

X Ca 2

(V 2 V m 0,004 )
100
Vm p

Ths
X (%)

Ktqu

(0,7 300 0,004 )


100
10 6,4131

1,3098(%)

Hm lng Mg2+
Cngthc

X Mg

(V V 2 ) V m 0,0024
1
100
Vm p

Ths
X (%)

Kt
qu

(1,43 0,7 ) 300 0,0024


100 0,8196
10 6,4131

(%)

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Bi 4. XC NH KHONG VI LNG TRONG THC PHM


I.

Xc nh st trong thc phm (sa bt hoc Fomat).

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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.

Xc nh P trong thc phm (sa hoc Fomat).


Nguyn tc :
P trong dung dch kt hp amonimolybdovanadate to thnh mt phc
chtmuvngbntrongmitrngpH=39.

2.

Cch tin hnh :


Bc1:nhlngmu
Bc2:phadungdchPchun
+ Pha long 20 ln t dung dch chun P 2000ppm thnh dung dch
chunP100ppm.

19

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Bc3:thmlnltcchachtvobnhnhmc25mlnhbng
sau:

Dung dch (ml)

B1

B2

B3

B4

B5

Bmu

DD chun P 100ppm

DD mu

0.1

Amonilybdovanadate

5 ( lc 1
pht)

H2O ct 2 ln

Lc nh, sau 5 pht mi dng nc ct nh mc ti vch

Cp(

100

200

300

400

Cx

Sau 10 pht em o = 400nm

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 5: XC NH M TNG TRONG THC PHM BNG PHNG


PHP KJELDAHL
1/ Nguyn tc:
+un370390oC
+KhitnngmuncmmviH2SO4mcccchthucboxihato
thnhSO2,CO2,H2O.CnnitsaukhicgiiphngdidngNH3kthpvi
H2SO4tothnh(NH4)2SO4tantrongdungdch.
H2SO4 m c, to, xc tc
Hpchtchanit,protein....(NH4)2SO4+SO2+CO2+H2O

+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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

(18,6 17) 0,1 10

1000 6,25

14 1 1000 6,25
1

= 14

Ln 2:

10

14

(18,6 17,1) 0,1 10

1000 6,25

14 1 1000 6,25
1

= 13,125

23

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 6. XC NH M TNG TRONG NC MM BNG PHNG


PHP NESSLER ( Phng php o quang)
I.

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Nunittngs(mtng)khngtinhschthnngcanittngs(mtng)
ctnhtngithpph.
2.

Quy Trnh x l mu:


Nguyn tc hot ng ca my Kjeldahl:
Mu c a vo bn t (h thng v c ho mu) thng qua cc ng

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

(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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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)

0,000 0,045 0,124 0,233 0,407 0,558 0,049

thdychun

27

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

nngnittngsvihpth: y 0, 0213 x 0, 0092

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

Bo Co TN Phn Tch Thc Phm

K=f/mu(f=6,25)=>K=

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 7: XC NH M THI (NH3) V M AMIN (M FORMON)


1. nh lng Nito acid amin (phng php formon):
a) Mc tiu:

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:

Ht chnh xc 10ml mu nc mm cho vo cc nh mc 100ml, thm vo

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

tchNaOHtiutn.
d) Tnh kt qu:
Nitoformon

0, 0014 VNaOH 100 f 0, 0014 3 100 100

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Hnh 1. B ct m Kjeldahl
Bc 3:
ChunlngH2C2O40.1NdtrongbnhhngbngNaOH0.1N

Np y buret bng NaOH 0.1N ly bnh tam gic hng ng sinh hn ra v

emichunbngdungdchnynkhidungdchtrongbnhtamgicchuynt
muhngnhtsangmuxanhlthdnglivghithtchNaOH0.1Ntiutn.

Trc khi chun

Sau khi chun

d) Tnh ton kt qu
Tac: % NH 3

(V1 V2 ) 103 N 17 F 100 (20 5).103 0,117 100

0, 255%
m
10

Trong :
V1:ThtchdungdchH2C2O40.1N(ml)
V2:ThtchdungdchNaOH0.1N(ml)
N:nglngdungdch
F:HsiuchnhdungdchNaOH
m:Khilngmucn(g)

34

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 8. NH LNG LACTOZA TRONG SA C C NG BNG


PHNG PHP BERTRAND
1. Nguyn tc
- Phng php ny da trn mi trng kim, cc ng kh(glucoz,fru ctoz,
mantoz)ddngkhng(II)oxitthnhng(I)oxit,kttangmtcmu
gch,quatnhclngngkh.nhlngngkhthngdngthuc
thfehling.
-Thuckhfehlinglhnhpca2dungdch:dungdchngsunfatgilfehling
Avdungdchkimcamuiseignett(muikalinatritactrat)gilfehlingB.
- Khi trn hai dung dch fehling A v fehling B vi nhau th xy ra phn ng gia
chngxyratheohaigiaion.
-utintokttacanghidroxitmuxanhdatri.

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Tnhton:
Hmlnglactoza/100gsa=

mDg lactoza .( NV ) KMnO4 .100 Vdm

.
mmau
Vmau

Vdm:Thtchnhmc(ml)
Vmau:Thtchdungdchemxcnh(ml)
Mmau:Khilngmu(g)
VKMnO4:ThtchKMnO4tiutntrongchun(ml)
NKMnO4:NngnglngcaKMnO4
Hmlnglactoza/100gsa=

mDg lactoza .( NV ) KMnO4 .100 Vdm 103.342.(0,1.2).100 100


.

.
58, 0522
mmau
Vmau
2,3565
5

38

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 9: NH LNG NG TNG TRONG TRI CY BNG


PHNG PHP FEROCYANUR V PHNG PHP IOD.
I.

nh lng ng saccaroza trong sa c c ng bng phng php Lane


Eynon (phng php chun cn bng).
1. Nguyn tc.
ngkhtrongdchthuphnngtanvthuphntinhbtckhnngkh
Cu tronghnhpFehlingvCu+(Cu2O)khngtan,mu.Thtchdungdch
ngkhcnthitkhhontonmtthtchnhtnhhnhpFehlingcxc
nhbngphngphpchunvichtchthxanhmetylen.Hmlngtinhbt
ctnhbnghmlngglucozatrongdchthyphntinhbtnhnvihschuyn
i0,9.Phmvipdng:Quitrnhnypdngchoccloihtngccnhgo,m,
ng...cngnhccsnphmcangccvquynhphpthxcnhhmlng
ngtngsvtinhbtbngphngphpLane-Eynon.
2+

2. Cch tin hnh.


Chun b mu v thuc th:
Mu:50mldungdchIbi8chovobnhnhmc100ml+5mlHCl,cho
vobpcchthynhit750C,sau2pht,nhittrongbnhphit68
700C.Ginhitnyng5pht.Lmnguinhanhdivinc,trunghadung
dchbngNaOH20%(khong4ml),saudngNaOH1%trunghavichthPP.
Saunhmcn100ml(dungdchII).
Thuc th:
-

Feling A: 8,75g CuSO4.5H2O + 12,5ml H2SO4 ha tan bng nc ct v nh


mcn250ml.

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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=

(10 11,1 13,9) 0,005

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 10: XC NH TNG S CHT BO LIPID.


I. Xc nh tng bo trong sa bt bng phng php soxlet.
Nguyn tc.
Dngdungmihuchatanttcchtbotdoctrongthcphm,sau
uidungmihuc,sykhvcnchtbothuc,tnhrahmlngcht
boctrongthcphm
Cch tin hnh.
- Mugiylccsytrong15pht1021050C.
Nhn xt:
Ktquthnghimvhmlnglipittrongsabtmnhmocl18,85%
so vi thc t cho thy sa bt c hm lng bo kh cao khong 26-46% trng
lngkhivisabtnguyncht.Nhvytrongqutrnhlmthnghim
bmcsais.
II. Xc nh bo tng s trong phomat mm hoc b bng phng php Adam
Rose.
Nguyn tc.
mitrngammoniacvcnchitxutlipitbngeteveteduha,cnlipitt
tnhrahmlnglipittrong100gamthcphm.
-Ammoniaccnhimvhatanprotein,lmthayisccngbmtcacccht
bo,bgylinktbo-mcamnglipit-proteinlipithotanddnghn.
-Diethyleterctnhchthatanlipitnhngcnghatanccchtkhcnhnc
v cc cht ha tan trong nc nh lactozo, mui khongdo chng ta dng
thmeteduha.
-

Eteduhahtnchnetethng,ctnhchtyncvccchthatan

trongncrakhietethnglmchoetethngchcchachtbovetedu

42

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

ha.Ngitacngkhngthdngeteduhathaythchoetethngvetedu
hakhnghatanccchtbocnc.
-

Hn hp sau khi b sung dung mi v khuy o tch thnh 2 pha : pha nh

nmtrngmdungmivbo,phanngnmdigmncvccchtha
tantrongnc.Tathuphanhgmdungmivbo,lmbayhidungmitathu
ctngbotrongmusa.

Cch tin hnh.

Ht5mlsatikhngngvophuchitqul,saucho5mlestevo.

Tiptheochothm10mlcnammoniac(208,5mlC2H5OH900+7,5mlNH325%+
H2Oct=250ml)+1gitPP1%.
-

Lcphuchit,sauyntrong30pht.

Tchblpdi,gililptrn(lpeter+bo).
-

Thmtip5mleterduha,lcmnh2pht,yntrong15pht,tiptctch

b lp di, x b phn eter + bo vo cc 50ml ( c sy kh v cn khi


lng).
-

Chobayhietertrnbptrongtht.

Cnccxcnhkhilngchtbom1.

Tnh ton kt qu:

%bo=

( m1 m0 ) 100
mm

Trong:

m1=46,85glkhilngccvchtbosaukhiuntrnbptrongtht.

m0=46,78glkhilngccbanu.

mm=5glkhilngmubanu.

43

Bo Co TN Phn Tch Thc Phm

%bo=

GVHD. ThS V Hong Yn

=1,4%.

Nhn xt.
Hmlngchtbothuctrongthnghimtngithpsovithct.Nguyn
nhncldothaotctrongqutrnhchangvhachtkhngctinhkhit.

44

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 11. XC NH CH S AXIT, CH S PEROXID V CH S IOD


TRONG DU N
I.

Xc nh ch s axit

1.

Mc tiu
-

ChsaxitlsmgKOHcnthittrunghaaxitbotdoctrong1gcht
th.

Xcnhchsaxittrongdumngthcvtbngphngphptrungha.

2.

Nguyn tc thc hin

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

5, 61.V 2, 085 V 2, 085 0, 4

0,1668
2mm
mm
mm

Trong :
-

5.61:smgKOHtngngvi1mldungdchNaOH0.1N(Dotrongbily
nngNaOH0.05Nthinntaphichiacho2dimus).

V:SmlNaOH0.05Nsdngtrongnhlng(ml)

mm:Trnglngchttheminhlng(g)

45

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Gii thch kt qu

Dumcnglmitrngthunlichomtsvikhun,nmmcpht

trin.Ngoiranhngyutnhsng,nhit,nc,kimloi,oxycngtc
ngnccdynikhngbohalmchodumbbincht.Nhvynu
mchsacidcnglnchngtlngchtboctrongthcphmcngcao
chonnccsnphmnydbhhngdoccvisinhvttncng
II.

Xc nh ch s Iod (phng php Wijs)

1.

Mc tiu

Xcnhccaxitbokhngnoctrongchtbo.

2.

Nguyn tc thc hin

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

dchhtinhbtvochunchonkhidungdchmtmuhonton.Ghili
thtchNa2S2O30.1Ntiutn.
4.

Tnh kt qu
ChsI2(gI2/100g)

a=40,7ml

b=14.6ml

m=1g

(a b) 0, 01269 100 (40 14, 6) 0, 01269 100

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

1 lng d Iod phn ng cng vi du bo, ri i chun Iod cn li nh vo


Na2S2O3,suyralngIodcngvodubo.
III.

Xc nh ch s peroxid

1.

Mc tiu

GiiphngI2ctrongmuiKIranhdungdchNa2S2O3.
2.

Nguyn tc thc hin

Khicoxikhngkhccaxitboctrongthnhphncadunhtlccaxit

bokhngnosddngboxihamtphnvtothnhperoxid.

Vicxcnhchsperoxidcthdavoccphnngsau

LngIodgiiphngracthchunbngdungdchNa2S2O3.Vichthl

htinhbt

47

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

2Na2S2O3+I2=>2NaI+Na2S4O6

TheolngNa2S2O3cnIodgiiphngracthtnhcchsperoxid..

3.

Cc bc tin hnh
Muth:
-

Cnvobnhtamgiccntnhmcsykh:1gmu+1gNa2CO3+
15mlCH3COOHmc,ynplcnkhiNa2CO3tanht.

Mnpchonhanh10mlCHCl3volcchonkhitanht,thmnhanh1mlKI
bohalctrongti5pht,thm75mlncctlcduvchunbngdung
dchNa2S2O30.02Nvihtinhbt1%lmchth.

Mutrng:
-

B vo bnh tam gic c nt nhm c sy kh: 1g Na2CO3 + 15ml


CH3COOHmc,ynplcnkhiNa2CO3tanht.

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

(Vm VB ) N 1000 (3, 6 1, 2) 0, 02 1000

48
mm
1

Trong :
Vm:smlNa2S2O3tiutnchomu
VB:smlNa2S2O3tiutnchomutrng
mm:Khilngmuemlmthnghim(g)
N:nglngdungdchNa2S2O30.02N
KT QU BN LUN

48

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

Cnphitinhnhchunnhanhvdungdchdbayhidntimudung
dchsbcchonnktquchunskhngtrnhkhisaist.
CnynpbnhtamgicvI2dbthnghoachonncnphiynpv
trongbngtivoxikhngkh+nhsngsoxihaccaxitbokhngnotothnh
peroxidedntiktqubsai.

49

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

BI 12: XC NH NITRIT V NITRATE TRONG THT.


I. Xc nh nitrite
Chun b mu:
- Cn10,03gxcxchvtnnhuyntrongcis.Sauchovobnhnn250mlc
np,thm100mlncctnng(70800C).Chothm5mlddBorate5%,un
cchthykhong30pht,dngakhuyvlc15pht.Chnguithm3mldd
Ferocyanur10%+2mldungdchAcetatekm10%chuynvobnhnhmc200
mlquaphu,trngcc3ln,miln5mlH2O,saudngncct2lnnh
mctivch,lctrnu,yn30pht,cnthngnphntrongquamtbnh
nhmckhccphu+giylcbngxanhxpgp.(Lcnhiulncngtt).
- DchqualcdngxcnhNitritevNitrate(dungdchI).
Xy dng ng chun v o mu
ThmcchachtlnltvoccBM25mltheobngsau:

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

Bo Co TN Phn Tch Thc Phm

CH3COOH4N

GVHD. ThS V Hong Yn

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

Bo Co TN Phn Tch Thc Phm

GVHD. ThS V Hong Yn

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 )

C 1x .100.250 1,1548 100 250

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 )

C x2 .100.100.250 1,8095 100 100 250

902,044
25.20.m
25 20 10,03

52

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