Chuyen e 2 NHNG NGUYEN TAC KY THUAT C BAN S DUNG CHO PHAN TCH THC PHAM

I/ NHNG PHNG PHAP PHAN TCH CO IEN

1/

PHN TCH TH TCH 1.1 Phng phap chuan o Axt Baz 1.2/ Phng phap chuan o phc cht 1.3/ Phng phap chuan o oxi ha kh 1.4/ Phng phap chuan o kt ta

2/

PHAN TCH BANG PHNG PHAP TRONG LNG

II/ PHNG PHAP PHAN TCH

HIEN AI
1/

Phng phap phan tch quang pho Quang pho hap thu nguyen t (AAS) Quang pho phat xa Plasma (ICP) 2/ Phng phap phan tch sac ky Phng phap phan tch bang sac ky kh (GC) Phng phap phan tch bang sac ky long (HPLC)

I/ PHAN TCH THE TCH ( chuan o Titrimetric analysis)

1/

Nong o cua dung dch dung trong phan tch 2/ Chuan o axt baz ( Acide- base titrations) 3/ Chuan o oxyhoa kh ( redox titrations) 4/ Chuan o ket tua ( Precipitation

Moi lien he gia 3 loai nong CM = C% . 10. d , o= C% .10. d CN

CN

= M. CM , CM = so mol . chat tan(n) so kg dung moi M : khoi lng mol phan t chat tan : ng lng g chat tan d : Ty trong rieng cua chat tan
CM

= a gam chat tan. 1000ml dung dch M .V M: khoi lng phan t chat tan

PHA DUNG DCH T CHAT RAN 1/ Tnh toan lng can 2/ Hoa tan 3/ nh mc 4/ Chuyen vao chai cha 5/ Hieu chnh nong o Mcan = CM . V. M 10. P% V : the tch tnh P% : o tinh khiet cua hoa chat M : phan t gam CM : nong o mol
V

du : Tnh lng can NaOH co P = 96% e pha c 200ml dung dch NaOH 0,1M mcan = 0,1. 200. 40 = 0,83g NaOH 10 . 96

1/

Tnh toan the tch can dung 2/ Pha loang 3/ nh mc 4/ Chuyen vao chai cha 5/ Hieu chuan lai nong o neu can
CM V

Pha dung dch t chat long

= C% . 10. d , V can lay = Ccan pha . Vcan pha M CM

du : Tnh the tch H2SO4 98%, d= 1,84 can lay e pha 200ml dung dch H2SO4 co nong o 1M CM = 10. 98. 1,84 = 18,4 M 98 V can lay = 1. 200 = 10,87 ml 18,4

Acide- base Titrations

1/ Chuan o axt baz ( Acide- base titrations)

Noi dung bai hoc

- nh ngha ve Axt Baz - Quan he gia Ka va Kb cua cap axt baz lien hp - Can bang dung dch - pH cua dung dch,thiet b o pH va ch th mau pH - Xay dng phng phap chuan o axt baz - Bai toan ng dung

nh ngha phan tch chuan o

Phan

tch chuan o la o the tch cua dung dch a biet c nong o chnh xac cua chat chuan va chat chuan o phan ng hoan toan vi dung dch a c chuan b t mau thc pham can phan tch. - e xac nh iem tng ng chnh xac ( point equivalent ) khi ket thuc chuan o phai s dung ch th hoa hoc khi mau cua ch thi thay oi

du : Xac nh o axt trong nc mam Dung dch chuan : NaOH 0,1N Ch th e xac nh iem tng ng : phenolphtalein : chuyen t khong mau tm o Mau phan tch : 20ml The tch chuan o c : 5 ml o axt = V x 0,1N x1000 = 25mldlg/l 20

CHUAN O AXT - BAZ

KHAI NIEM AXT BAZ 1.1. Cac luan iem can ban Theo ly thuyet ien ly cua Arrhenius : - axt la nhng chat trong nc ien ly cho cation H+ va anion goc axt - Baz la nhng chat ien ly cho anion hydroxyt OH va cation goc baz v du: HCl H+ + Cl NaOH OH - + Na+
1/

Chuan o axt baz la phan ng trung hoa cua axt va baz cho muoi va nc thc chat la phan ng ket hp cua proton vi anion hidroxyt HCl + NaOH = NaCl + H2O thc chat H+ + OH- H2O Nam 1923 ly thuyet Proton cua hai nha khoa hoc Bronsted va Lowry a m rong khai niem axt baz nh sau: Axt la tat ca phan t hoac ion co kha nang cho proton H+ Baz : la tat ca phan t hoac ion co kha nang nhan proton H+ Chat va co kha nang cho Proton, vua co kha nang nhan Proton goi la chat lng

du Axt : cho proton H+

_ H+ NH4+ HC2O_ H+ Baz : nhan proton OH- + H+ HCO3- + H+ H2 O + H+
CH3COOH

Baz lien hp CH3COONH3 C2O42Axt lien hp H2O H2CO3 H3O+

- H+


Proton

khong ton tai t do. Mot chat ch the hien tnh axt khi co mat mot baz e nhan proton. Ngc lai mot chat ch the hien tnh baz khi co mat mot axt e cho proton. Thc chat cua mot phan ng gia mot axt vi mot baz la s chuyen proton ( tc cho nhan proton) V du : CH3COOH + NH3 CH3COO- + NH4+ CH3COOH/ CH3COO- : mot cap axt baz lien hp, NH3// NH4+ mot cap axt baz lien hp th 2

du 2 : CH3COOH + OHO sang cho CH3COO2

CH3COO- + H2O H+ chuyen t H Tom

lai theo ly thuyet proton phan ng axt baz co s o sau:

Axt

(1) + Baz( 2) Baz (1) + Axt (2) Chuyen H+ t axt Baz Axt(1)/ baz (1) va Axt(2) / baz (2) la hai cap axt baz lien hp

1.2.

Khai niem o manh cua axt va cua baz

Bronsted Lowry o manh cua axt the hien kha nang cho proton , o manh cua baz the hien kha nang nhan proton , Phan ng : xay ra hoan toan khi HCl + H2O H3O+ + ClAxt HCl manh hn H3O+ Baz H2O manh hn ClTom lai axt cang manh bao nhieu th
Theo

1.3/ Bang o manh tng oi cua cac cap axt baz lien hp

Tnh axt giam dan Axt lien hp : HClO4 H2SO4 HCl HNO3 H3O+ H2SO3 Baz lien hp: ClO-4 HSO-4 ClH2O H2O HSO3 Tnh baz tang dan

xac nh cu the o manh cua axt hay baz ngi ta da vao hang so KA hoac hang so KB

1.4/ QUAN HE HANG SO KA VA KB

e

xac nh cu the o manh cua axt hay baz ngi ta da vao hang so KA hoac hang so KB Chon H2O lam dung moi e so sanh

Trng hp 1: dung dch n Axt

Axt : A + H2O B + H3O+ Ap dung nh luat tac dung khoi lng

K =

aB x aH3O+ aA x aH2O

K=

[B][H3O+] [ A] [H2O]

Rut ra :

K x [H2O] = [B][H3O+] = KA hay pKA = - lgKA

[ A]

d : CH3COOH co KA = 1,86.10-5 HCN co KA = 7,20.10-10 t pKA = - lgKA ( pKA ch s axt) suy ra pKA ca CH3COOH = 4,73 pKA ca HCN = 9,14 Kt lun: Hng s KA cang ln co ( tc ch so axt pKA cang nho ) th lc axt cang manh Chu y . Vi cac axt a chc yeu s ien ly xay ra qua nhieu giai oan V du : H3PO4 phai qua 3 giai oan H3PO4+ H2O H2PO4 + H3O+ K1 = 7,5.10-2 pK1 = 1,12 H2PO4+ H2O HPO4 + H3O+ K1 = 6,23.10-8 pK2 = 7,21 HPO4+ H2O PO4 + H3O+ K1 = 2,2.10-13 pK1 = 12,66

Trng
B

hp 2 :

dung dch n BAZ : B

+ H2O = A + OHAp dung nh luat tac dung khoi lng

aA x aOHneu dung dch loang K = [ A] [OH-] [ B] [H2O] [A][OH-] = KB [B]

K = aB x aH2O

Rut ra :

KB x [H2O] =

KB : Hang so baz:

Ch so baz :

pKB = - lg KB

 Ket

luan : Hang so baz cang ln (tc ch so baz pKB cang nho ) th baz o cang manh du : so sanh hai chat baz NH3 : KNH3 = 1,79x10-5, pKNH3 = 4,75 Anilin : K C6H5NH2 = 4.10-10, pK C6H5NH2 = 9,4 suy ra NH3 > C6H5NH2
V

1.5/ TCH SO ION CUA NC

Nc

la chat ien ly rat yeu va lng tnh H2O H+ + OHK = [H+].[OH-] , [H2O] K. [H2O] = [H+].[OH-], KH2O=10-14,pKH2O =14 nc trung tnh va nguyen chat nen [H+] =[ OH-]= 10-7

Da vaonong o cua ion H+ va ion OH- e biet c tnh chat moi trng

cua mot dung dch . e bieu th moi trng ngi ta s dung ai lng pH hoac ch so pOH vi quy c: Ch so hidro pH = - lg[H+] Ch so Hydroxyt pOH = - lg [OH-] pH + pOH = 14 suy ra pH = 14 - pOH Dung dch trung tnh : pH = 7 Dung dch axt pH < 7 Dung dch baz pH > 7

Lien he gia KA va KB cua mot cap axt baz lien hp KA = [B].[ H3O+] KB = [A] .[ OH-] [A] [B] Nhan vi ve cua hai phng trnh KA x KB = [ H3O+] . [OH-] = KH2O Vay pKA + pKB = pKH2O = 14
T

o cho thay axt cang manh th baz lien hp cang yeu va ngc lai baz cang manh th axt lien hp cang


Bai

tap :

1/ Tnh pH cua dung dch axt HCl, co nong o 0,001M HCl la axt manh ien ly hoan toan [H3O+] = 10-3 suy ra : pH =3
2/

Hoa tan 0,6g NaOH vao nc thanh 1l dung dch .Tnh pH cua dung dch Giai : Tnh nong o cua NaOH = 0,6g : 40g = 0,015M NaOH manh ien ly hoan toan [ OH-] = 0,015M [ H+ ].[OH-] = 10-14 T ay [H+] = 10- 14 : 0,015 = 6,6.10-13 pH = 12,18

TNH pH CUA CAC DUNG DCH

pH

dung dch axt manh

Ga s co mot dung dch axt manh HA nong o au la CA

HA H+ + AH2O H+ + OH-

luat bao toan nong o au : [A-] = CA nh luat trung hoa ien: [H+] = [A-] + [OH-] Tch so ion cua nc : Kw = [H+]. [OH-] Suy ra : [H+] = [A-] + [OH-] = CA + Kw [H+] [H+]2 - CA.[H+] Kw = 0
nh

[H+]2

- CA.[H+] Kw = 0

a/ CA << 10- 7 bo qua nong o [H+] [H+]2 = Kw hay [ H+ ] = Kw v du : tm pH cua dung dch HNO3 10- 9
10- 9 < 10- 7 do o [ H+ ] = Kw = 10-7 pH = 7 b/ CA 10- 7 dung dch co pH 7

c/ CA >> 10- 7 bo qua nong o [OH-] cua

nc
[ H+ ] = CA suy ra pH = pCA

pH dung dch baz manh

B + H2O HB+ + OH H2O H+ + OH

L bao toan nong o au: HB+ = CB L trung hoa ien : [OH-] = [HB+] + [H+] Tch so ion cua nc : Kw = [OH-].[H+] Suy ra : [OH-] = [CB] + [H+] CB + [H+] = Kw [H+]
Theo

[H+]2 + CB.[H+]- Kw = 0

Tng

t nh trng hp axt manh: a/ neu CB >> 10-7 co the bo qua H+ [OH- ] = CB hay pOH = - lgCB hay [ H+] = Kw

CB va pH = 14 pOH hay pH = 14 + lgCB Neu CB << 10-7 th co the bo qua CB va khi o [H+] = [OH-] = Kw va pH = 7
b/ c/

Neu CB = 10-7 giai phng trnh tren

du :Tm pH cua dung dch KOH 10-7

phng trnh : [H+]2 + 10-7[H+] 10-14 = 0 [H+] = 6,18 .10-8 , pH = - lg ( 6,18 .10-8) = 7,21
Giai

du : Tnh pH dung dch KOH co nong o 10- 5 [ OH-] = CB = 10-5 , pH = 14 lg10-5 = 9

V

pH cua dung dch n axt yeu

Ga

s co dung dch n axt yeu HA, nng u

l CA HA H+ + AKA = [H+ ].[ A- ] (1) H2O H+ + OH[HA] Do axt yu khong phan ly hoan toan cho nen trong dung dch s tn ti hai nng : CA : nng u HA + A- : nng phn ly v cha c phan ly ht Cho nen : CA = [ A- ] + [ HA] (2) [ HA]= CA- [ A- ] H+ = [A-] + [ OH-] (3) [A-] = [H+] [OH-]

(3) co : [ A- ] = [H+ ] - [ OH-] T (2)Co : [ HA] = CA - [A-] hay [ HA] = CA - [H+ ] + [ OH-] th [ HA] vao (1)
Ta

co : [H+ ] = KA . [ HA] = KA . ( CA - [H+ ] + [ OH-]) [A-] [H+ ] - [ OH-]

[H+ ] = KA (CA - [H+ ] + [ OH-] ) [H+ ] - [ OH-]

 Xet
a/

cac trng hp

Nu [H+] >> [ OH-] tc la axt tng i mnh ( pKA 3) th

V

[H+ ] KA (CA - [H+ ] [H+ ]

d : tnh pH ca dung dch axt salixylic 10-3 ( pKA = 3) [H+] = 10-3 x 10-3 [H+] [H+] T [H+]2 + 10-3 [H+] 10-6 = 0 Gii phng trnh : [H+] = 6,2 x10-4 pH=3,21

Nu [OH-] << [H+] << CA : s in ly ca nc khong ang ke , axt tng i yu

b/

[H+] = KA CA [H+] = KA . CA [H+]

pH = pKA lgCA

d 1 : Tm pH dung dch axt axetic 0,1M (pKA = 4,75) Gii : pH = 4,75 lg 10-1 = 2,87

Vd

2: Tm pH dung dch NH4 Cl 0,1M, biet pKB ( NH3) = 4,75 Giai : pKA (NH4+ ) = 14 pKB ( NH3) = 14 4,75 = 9,25 pH = ( 9,25 lg 10-1 ) = 5,13

pH dung dch n baz yu

B + H2O BH+ + OH- H2O H+ + OH- ( Kw) KB = [OH-].[BH+] (1) [B]

Ga s co mt n baz yu B, nng u CB

baz yeu cho nen s phan ly cua n chat baz xay ra khong hoan toan v vay nong o ban au CB bao gm c :

CB = [B] + [BH+] (2) [BH+] + [H+] = [OH-] suy ra [BH+] = [OH-] - [H+] [B] = CB - [BH+] = CB - [OH-] + [H+]

[OH-] = KB [B]
+

KB. CB [OH-] +[ H+]

-

Bit

ga tr ca [OH] ta tnh c [H+] va pH dung dch [H+] = Kw = pH = - lg [H+] [OH-] Xet cac trng hp sau:

Xt

cc trng hp: a/ [H+] << [OH-+] [OH-] = KB x CB [OH-] [OH-] V d : Tnh pH ca dung dch NH3 0,01M bit pKB = 4,75 NH3 + H2O = NH4+ + OH[OH-] = KB . (CB - [OH-]) [OH-] [OH-]2 + 10-4,75 [OH-] 10- 4,75 x 10- 2 = 0 [OH-] = 10- 3,38 suy ra [H+] = 10-10,62 vay pH = 10,62

[H+] << [OH-] << CB [OH-] = KB x CB [OH-] V d: Tnh dung dch KCN 0,01M, pKA(HCN) = 9,21 Gii: KCN K+ + CN CN- + H2O = HCN + OH pKB = 14- 9,21 = 4,89 CN- la mt baz trung bnh [H+] << [OH-] gi s CB = 0,01 >> [OH-] ta co
b/

= 10-4,89 x 10-2 = 3,58x10-4 [H+] = 10-14 / 3,58x10-4 = 2,79.10-11 , pH= 10,55

[OH-]

CONG THC TONG QUAT

= [B][H3O+] KB = [A][OH-] [A] [B] Kw = [H+] [OH-] = 10-14 pH + pOH = 14 suy ra pH = 14 pOH pKA + pKB = Kw = 14 pH axt manh pH baz manh [H+ ]2 - CA[H+] Kw = 0, [H+ ]2 - CB[H+] Kw =O a/ CA << 10-7 a/ CB << 10- 7 [ H+] = Kw [ H+] =[OH-] = Kw = 7
KA

b/

CA 10-7

b/ CB 10-7

[H+]2 -10-7[H+]-10-14 =0
C/

[H+]2 +10-7[H+]-10-14 =0
C/ CB >> 10-7 [OH-] = CB [H+] = Kw

CA >> 10-7 = CA pH= pCA

[H+]

CB

pH

dd n axt yu yeu
[H+ ] = KA x (CA - [H+ ] + [ OH-] ) [ H+ ] - [ OH-]

pH dd.n ca Baz
[OH- ] = KB x (CB - [OH- ] + [ H+ ) [ OH- ] - [ H+]

a/ [H+] >> [OH-] axt mnh mnh

[H+ ] = KA
x

a/ [H+] << [OH-] baz

[OH- ] = KB x (CB - [OH- ]

(CA - [ H+ ] [ H+ ]

[OH-]

b/ [OH-] <<[H+] << CA

b/

[H+] <<[ OH-] < CB

[H+] = KA CA = pKA lgCA

[ OH-] = KB .CB

Chun axt manh bang baz manh

Ga

s lay 100ml HCl 0,1N em chuan o bang dung dch NaOH 0,1N. T cong thc pH = -lg[H+] se tnh c pH thay oi trong qua trnh trung hoa axt manh bang baz manh. Trc khi chuan o dung dch HCl 0,1N : pH = -lg[H+] = -lgCHCl = -lg10-1 =1 Neu them 50mlNaOH 0,1N th dung dch con lai 50% HCl, khi them 99ml NaOH th dung dch con lai 1% HCL .trong qua trnh them NaOH th nong o H+ cua dung dch se b thay oi. e tnh nong o cua CHCl s dung cong thc :

CA = ( VA - VB). NA ( VA + VB) hay ( VHCl - VNaOH).NHCl / ( VHCl + VNaOH) VA : the tch ban au ng vi nong o NA VB : the tch the tch dung dch chuan ng vi nong o NB Khi them 50ml NaOH tc la HCl trung hoa c 50% CHCl = [H+]= ( 100 50) 0,1/ 150 = 3,3.10-2 M/l pH = -lg [H+] = 2 lg3,3 = 1,5 Tai iem tng ng tc la 100ml HCl = 100mlNaOH suy ra pH = 7

 Trng

hp chuan o qua 1001mlNaOH 0,1N th se tnh lng kiem d CNaOH = [OH-] = ( 0,1:200,1).0,1 = 5.10-5 pH = 14 pOH = 14 - 4,3 = 9,7 Luc au chuan o pH cua dung dch thay oi cham gan en iem tng ng thay oi rat nhanh sau iem tng ng lai thay oi cham

Chuan o axt yeu bang baz chuan o axt bang Tnh pH khac nhau khi manh
kiem V du: CH3COOH 0,1N chuan o = NaOH 0,1N Tnh pH iem 0 trc khi chuan o KCH3COOH = 1,82.10-5 pKCH3COOH = - lgKA = 5- lg 1,82 = 4,74 Thay ga tr pKCH3COOH,,va lgCCH3COOH vao cong thc pH = 4,74 + 1/2lg0,1= 2,37 + 0,5 = 2,87 Vay pH cua CH3COOH = 2,87 Trong qua trnh chuan o th pH cua dung dch se thay oi nh sau:

Trong

qua trnh chuan o trong dung dch ton tai co axt yeu CH3COOH , NaOH va muoi cua no tao thanh mot dung dch em Khi them 50ml NaOH : pH = 4,74 lgCH3COOH.0,1N + lg( 50/100).0,1N = 4,74
Khi

them 90mlNaOH : hon hp axt yeu va muoi cua no pH = - lg[H+] = pKA lgCA + lgCKhAn pH = 4,74 lg( 10/100)0,1 + lg( 90/100).0,1 = 4,74 +21,05 = 5,69 iem tng ng khong trung vi iem trung hoa tc la khong trunng vi thi iem xay ra s oi mau cua chat ch th b oi mau pH = 7 cho nen s ket thuc cua chuan o khong phai luon ket thuc pH=7

CHUAN O BAZ YEU BANG AXT MANH

pOH

= pKktOH - 1/2lgCKTOH

Khoang

chuyen mau cua mot so ch th thng gap Metyl da cam : 3,1 - 4,4 vang vang da cam Metyl o : 4,4 - 6,2 o vang Phenolphtalein : 8,0 -10 khong mau tm

DUNG DCH M
Dung

dch m l dung dch c to thnh khi trn ln mt axt yu vi baz lin hp ca n hoc mt baz yu vi axt lin hp ca n. V d: dung dch m : CH3COOH v CH3COO-, hay hn hp gm NH3 /NH4+ Dung dch m c c im l pH thay i rt t khi thm mt lng axt hoc baz HA + H2O H3O+ + A Khi thm mt lng axt (H3O+ ) : H3O+ + A- HA axt yu Ngc li khi thm OH- : OH- + H+ = H2O ba z yu

pH dung dch m: HA H+ + AKA = [H+] [A-] / [HA] NaA- Na+ + AH2O H+ + OHKw = [H+] [OH-] / [H2O] Ta c KA = [H+] [A-] [H+] = KA .[HA] [HA] [A-] Kw = [H+][OH-] + [Na+] = [OH-] + [A-] [H+]+ CB = [OH-] + [A-] Suy ra : [A-] = [H+] + CB [OH-] [HA] + [A-] = CA + CB [HA] = CA + CB [A-] [HA] = CA + CB - [H+] + CB [OH-] [H+] = KA [HA] = KA CA - [H+] + [OH-] [A-] CB + [H+] [OH- ]
[H+]

ton tai cua HA va A- trong dung dch ngan can s tao thanh H+ va OH- , khi tnh gan ung co the bo qua [H+] va [OH-]
S [H+]

= KA C A CB

suy ra pH = pKA lg CA CB

V d : Tnh pH ca dung dch CH3COOH 0,01M v CH3COONa 0,01M

Gii:

pH = pKA (CH3COOH) + lg 0,01 = 4,75 0,01 Gi thit thm 10ml dd NaOH 0,1M vo 1000ml dd m trn lc : [H+] = KA 0,01 - 0.001 0,01 + 0,001 pH = pKA lg 0,81 = 4,84

pH dung dch thay i : 4,84 4,75 x100% = 1,89% 4,75

PHA

DUNG DCH CHUAN AXT VA BAZ

NH NGHA CHT CHUN GC

1/

Cht gc C tnh n nh cao Bn vi mi trng ng lng ln Khi lng ng vi cng thc ha cht Phn ng nh lng H2C2O4.2H2O ,

C6H5COOH Na2B4O7.10H2O K2Cr2O7 ; NaCl KMnO4, ZnSO4.7H2O ; MgSO4.7H2O

2/

Chat goc dung e pha che cac dung dch chuan axt va baz - Chuan o cac baz phai co dung dch chuan axt HCl, H2SO4 . HCl thng hay c s dung hn ca v cac muoi cua no thng tan. Khi pha mau can un soi th hay s dung H2SO4 - Chuan o cac axt phai co dung dch chuan la baz NaOH, KOH, Nong o cua dung dch chuan thay oi t 0,01N en 0,2N . S dng dung dch 0,5N hay 1N sau pha long thnh cc dung dung dch c nng nh hn .

PHA CAC DUNG DCH CHUAN 1/ Neu axt hay kiem ban au la chat long
th ta o khoi lng rieng cua no, t o tra trong so tay hoa hoc se xac nh c nong o % cua chat co trong chat long 2/ Pha loang s bo dung dch am ac en the tch gan bang the tch pha , sau o xac nh lai chnh xac bang mot dung dch chuan khac. 3/ Neu axt hay baz ban au la nhng chat ran e pha dung dch chuan ta can mot lng can thch hp cua chat ban au trong mot the tch can thiet bang nc

XAC NH KHOI LNG RING CUA DUNG DCH

ngha : Khoi lng rieng (d) la ty so khoi lng cua vat(g) va the tch (V) cua no Khoi lng rieng c bieu dien : g/cm3 , g/ml d = g/V hay d = m/V Xac nh khoi lng rieng : ty trong ke, hoac phu ke
nh

PHA DUNG DCH HCl 0,1N

du : pha 2 lt dung dch HCl co nong o 0,1N - o khoi lng rieng cua HCl ac ban au bang ty trong ke : p = 1,179g/cm3. Tra bang tng ng HCl 36% - Trc het phai tnh neu HCl 100% e pha 2 lt dung dch HCl 0,1N lg HCl = 36,46N .0,1. 2 = 7,292gHCl - Sau o tnh cho dung dch 36% 100g -------36g gHCl -----7,292 suy ra : g (HCl) = 7,292.100/ 36 V (HCl) = m / d vay 7,292.100 / 36 / 1,179 = 17,2mlHCl ac Nh vay e pha 2 lt dung dch HCl 0,1N ta lay 17,2ml HCl (p=1,179g/cm3) bang ong ong cho vao bnh nh mc 2lt va pha loang bng nc cat
V

2/

Xac nh o chuan cua dung dch HCl 0,1N - Co 2 phng phap xac nh o chuan cua HCl 0,1N - Phng phap the tch bang kiem - Phng phap khoi lng a/ Phng phap the tch bang kiem Na2CO3 khan, Na2B4O7.10H2O, Na2C2O4.. NaOH 0,1N va ch th mau la phenolphtalein chuyen mau t trang xang tm hong

PHA CHE DUNG DCH KIEM NaOH 0,1N NaOH tinh the mau trang, rat hut am no b n ra trong khong kh va de dang phan ng vi CO2 cua khong kh. V vay thanh phan khong on nh nen khong s dung NaOH lam chat chuan goc e pha che dung dch chuan o c. Muon pha 2 lt dung dch NaOH 0,1N th can mot lng NaOH 100% la: NaOH = 40g, g (NaOH) = 40.0,1.2 = 8g Ga s khoi lng rieng p cua

pha thanh 2 lt dung dch NaOH 0,1N can lay lng can dung dch NaOH 26% la 100g ----------26g g NaOH--------8g suy ra g = 100.8/26 Vay the tch dung dch NaOH can lay: V= m/ d V = 100.8/26 / 1,285 = 24ml Xac nh lai o chuan cua NaOH 0,1N - Axt oxalic H2C2O4.2H2O loai PA - Axt Benzoic C6H5COOH loai PA

dnh o chuan cua NaOH 0,1N theo Axt oxalic H2C2O4.2H2O H2C2O4 H+ + HC2O4 HC2O4 H+ + C2O4 lg H2C2O4.2H2O = M H2C2O4.2H2O / 2 = 126,0662/2 = 63,033 iem tng ng pH = 8,55 , ch th mau la phenolphtalein t mau tm xang khong mau S co mat cua axt CO2 la axt co kha nang tham gia phan ng tao thanh Hydro cacbonat va cabonat gay can tr cho qua trnh chuan o bang axt oxalic do o khi pha dung dch chuan axt oxalic nc cat phai c un soi e ui het CO2
Xac

 Cong

thc tnh o chuan T

NNAOH =

VH2C2O4.2H2O . NNa2H2C2O4.2H2O / NNaOH NaOH 1000

VNaOH

TNaOH =

CHUN KT TA
Phng

phap chuan o ket tua la da tren phan ng hoa hoc cua chat can phan tch vi mot chat khac biet nong o ( chat chuan) va ket thuc chuan o tao ket tua hoan toan . Tai iem ket tua hoan toan tc la iem tng ng phai s dung chat ch th tao s chuyen oi mau . Phng phap ket tua gan lien vi s tao thanh hp chat t tan cua Ag, Ba, Hg, Pb, Zn..vi mot so nguyen to khac V d: chuan o Ba++ bang ion sunphat da tren phan ng Ba++ + SO4 BaSO4

Ngi

ta dung Natri rodizonat e xac nh iem tng ng khi d Ba++ dung dch dung dch se chuyen mau t o xang trang V d 2: Xac nh ham lng Cl- trong mu nc ung AgNO3 + Cl- AgCl + NaNO3 Xac nh iem tng ng nh ion Ag+ kt hp vi CrO4 d tao thanh Ag2CrO4 mu o gach cua

Phng

php kt ta cho php nh lng cc anion kt ta vi cc cation Ag, Ba, Hg, Pb, Znv d cc clorua, bromua, iodua.cng nh cc cation to kt ta t tan vi cc anion k trn Yeu cau oi vi phan ng c dung trong phng phap ket tua : - Phan ng tao ket tua hoan toan va phan ng xay ra nhanh - Ket tua c tao thanh co o tan thap nhat va co o tan cho phep khong c vt qua 10-5 M/ l

Tch so tan va o tan

1/

Tch so tan ien ly AgCl Ag+ + Cl ket tua Tong quat chat ien ly t tan ien ly AmBn mAn+ + nBm ket tua Ap dung nh luat tac dung khoi lng ta co TAmBn = [An+]m[Bm-]n = const TAmBn : tch so tan Tch so tan la mot hang so can bang , o ln cua no ch phu thuoc ban chat chat tan va nhiet o

2/

o tan : S
m+n

SAmBn=
V

[A+n ]m= [B-m]n = TAmBn

du : Tnh tch so tan cua BaSO4 , biet o tan cua no 200C la 1,05.10-5M Giai: T = [ Ba2+ ][SO42-] T = 1,0510-5 x 1,05.10-5 = 1,1.10-10

du 2 : Tnh tch so tan cua Ag2CrO4 biet rang 00C 100ml dung dch bao hoa cua no cha 0,002156g Ag2CrO4
Giai

: Tnh so mol cua Ag2CrO4 so mol = 0,002156 x1000 = 6,5 .10-5 331,73 x100 T = ( 6,5.10-5 )2 x 6,5.10-5 = 1,1.10-12

Theo

quy tac tch so tan , chat ien ly t tan se ket tua khi tch so tan nong o cac ion ( vi so mau thch hp) vt qua ga tr tch so tan nhiet o a cho Neu tch so [An+]m[Bm-]n trong dung dch ln hn ga tr TAmBn th se tao thanh ket tua Neu [An+]m[Bm-]n < TAmBn ket tua khong tach ra ma b hoa tan. S them bat ky ion nao tao thanh hp chat An+ B-m eu lam giam o tan. Viec them cac chat ien ly khac khong co ion chung vi hp chat An+ B-m lam tang o tan

S tao thanh va s hoa tan mot ket tua chat ien ly t tan

d : Trn 1l dung dch Pb(CH3COO)2 0,05M vi 1l dung dch KCl 0,5M. Hi kt ta PbCl2 co xut hin khong? Biet tch so tan cua muoi PbCl2 nhiet o thng la 1,6.10-5 Giai : Ta co CPb+2 = 2,5.10-2M , CCl = 2,5.10-1 CPb 2+ x CCl2 = 2,5.10-2 x ( 2,5.10-1)2 = 1,56.10-3 > 1,6.10-5 V tch so nong o cac ion vt qua ga tr tch so tan nen mot phan PbCl2 se ket tua Pb( CH3COO)2 + 2 KCl = PbCl2 + 2 CH3COOK

du 3: Tnh o tan cua AgCl khi them vao dung dch bao hoa cua no dung dch AgNO3 0,001N hay dung dch NaCl 0,001N Gai : o tan SAgCl = [Ag+] = [Cl-] = TAgCl = 1,7.10-10 = 1,3.10-5 M/l a/ o tan cua AgCl khi them AgNO3 0.001N ngha la trong dung dch d Ag+ bang SAgCl = [Cl-] = TAgCl 1,7.10-10 : 1.10-3 = 1,7.10-7 M/l [Ag] b/ o tan cua AgCl khi them NaCl ngha la d Cl SAgCl = [Ag+] = TAgCl 1,7.10-10 : 1.10-3 = 1,7.10-7 M/l [Cl] Nh vay o tan cua AgCl se giam i mot cach ong nhat khi them d ca ion Cl- va ion Ag+

CAC

PHNG PHAP PHAN TCH THC PHAM CO IEN

CHUAN O AXT BAZ KET TUA

THC NGHIEM PHAN TCH THC PHAM BANG PHNG PHAP CHUAN O AXT BAZ, KET TUA
I/

PHNG PHAP LAY MAU

Phng

phap chung cach lay mau phan tch Lay mau nguyen lieu hoac san pham thc pham e xac nh phan tch trong phong th nghiem la rat quan trong trong cong tac phan tch. Lay mau sai se lam c qua trnh phan tch sai
Cac

yeu cau ve lay mau

Lo

hang ong nhat : La lo bao gom nhng san pham cung ten goi , cung mot loai pham chat, ng trong cung mot loai bao b, cung mot kch thc, - Phai xem tnh trang cua bao b va c nghi nhan bang van ban -Mau hang lay em i kiem nghiem phai la mau trung bnh, ngha la sau khi chia thanh lo hang ong nhat , mau se c


oi

vi cac thc pham long nh nc tng , nc mam, dau an thng c cha trong cac thung to , hoac be to th dung ong cao su sach , kho cam vao v tr tren , di hay gia be e hut ra nen nh trc khi lay mau phai khuay ky cho eu , va bo i lt au va lt hai sau o mi lay mau chnh thc cho vao dung cu ng mau.
-

oi vi cac nguyen lieu va san pham thc pham the ran nh gao, bot, che, au..th lay mau phan tren, di , gia, ben canh cac bao hoac ong hang roi sau o tron eu cho ong nhat.

Lng lng thc va thc pham toi thieu can thiet e kiem nghiem
va thc pham che bien : 250 500g Ca, tom cua ca con : 250 500g Trng : 5 10 qua Nc mam, nc tng, dam : 500 750ml Dau m, Sa ti : 500 750ml Ru cac loai : 750 -1000ml Gao, bot, san pham che bie : 500 750g Banh mt keo : 250 500 g o hop, nv giai khat : 5 10 hop Pham mau : 50 100g
Tht

II/

phan tch tai phong th nghiem -Mau phai c tron eu, xay nhuyen( neu la mau dang ran nh au phong, gao) - Mau phai c ng trong bao b, co ma so ten goi - Mau cho phan tch vi sinh phai c ng rieng vao tui, chai..a c vo trung - Phai mo ta mau trc khi phan tch ( phan tch cam quan mui, v, trang thai ) - Vao so mau : ten mau,ngay gi nhan mau, ch tieu can phan tch, thi gian tra ket qua. Tien hanh kiem nghiem, neu trng hp cha phan tch c ngay th can phai bao

NGUYEN TAC GI MAU

Mau

thc pham gi kiem nghiem , hoac c gi trong bao b ban au cua no , hoac c ong goi trong ngng dung cu khong lam anh hng en chat lng thc pham Trng hp thc pham phai gi xa hoac mau co tranh chap phai ong goi ky pha ngoai co ong dau len nut buoc hoac kep dau xi can than , tranh mau b anh trao. Thc phan de b h hong th can phai gi gap en phong kiem nghiem Thc pham gi en phong kiem nghiem phai co phieu yeu cau kiem nghiem kem

quan hoac nha may san xuat - Ngay va gi lay mau, ni lay mau - ngi lay mau - yeu cau kiem nghiem Bien ban lay mau can co: Ten ho c quan ngi lay mau Ten ho a ch cua ngi co mau Ngay gi lay mau Ly do lay mau Loai hang va lng mau Ch ky hai ben Chu y : Phan mo ta mau . Mau kiem nghiem phai c gi lai 40% e lam oi chieu khi co khieu nai , thi gian lu mau t 01 tuan en 03 thang tuy theo tng loai mau bao quan

Chuan b mau cho phan tch

Khi

mau thc pham en phong th nghiem Can phai tien hanh trnh t sau: Kiem soat bao b co hp le khong Kiem tra lai phieu gi kiem nghiem : ten mau, ch tieu phan tch, ngay gi tra ket qua.. Vao so cua phong hoac kiem nghiem vien khi nhan mau Tien hanh phan tch Kiem nghien Hoa hoc gom 02 phan - Cam quan

I / XAC NH HAM LNG NaCl CO TRONG THC PHAMPhng phap nh

1/

lng trc tiep Phng phap Mohr

Nguyen tac cua phng phap

Co hai phng phap xac nh ham lng NaCl trong thc pham : Nguyen tac da tren phan ng ket tua cua ion Ag vi ion Cl- trong moi trng trung tnh, vi ch th KCrO4 . Mot giot d AgNO3 se ket hp vi CrO4-2 chuyen t mau vang sang mau o gach cua

NaCl

+ AgNO3 = AgCl + NaNO3 Ag+ + CrO42- = Ag2CrO4 mau o gach

2/

Cac yeu to gay anh hng cua qua trnh phan ng Trong mau phan tch khong c co nguyen to nh Ba, Sr, cac halogenua F, Br, se gay ket tua cung vi K2CrO4 cho ra mau o gach cua Moi trng axt va kiem se lam tan ket tua cua Ag2CrO4. Phai phan tch nhiet o thng , nhiet o cao se lam tan ket tua Ag2CrO4 Dung dch chuan AgNO3 tranh anh sang mat tri

Hoa

chat va dung cu - AgNO3 0,1N - Ch th K2CrO4 10% - NaOH 10%, HNO3 1:1 Bnh tam giac Pipet 10,20ml , Buret 10, 25ml X ly mau Neu mau thc pham dang ran th mau phai c nghien cho nhuyen , tron eu Neu mau dang long nh nc mam, nc tng..th mau phai c lac ky va pha loang trc khi phan


Tien

hanh phan tch - Mau ran sau khi nghien can mot lng ng vi o man cua muoi co trong mau t 1g- 20g cho vao bnh tam ga sau o cho them vao o 100ml nc cat c un nong cho vao mau va at tren may lac khoang 20 lay mau ra va, nh mc 100 ml sau o em loc
Lay

20ml t dch loc ( tuy thuoc vao lng NaCl co trong mau e lay mot the tch thch hp cho phan tch.) kiem tra lai pH co trung tnh hay khong bang giay th pH. Cho vao bnh tam giac 1ml K2CrO4 chuan o t t bang dung dch AgNO3 0,1N cho en khi xuat hien mau o gach ben vng.

Tnh

ket qua
= Vm 0,00585g. 0,1N . F. V1. 100% V2 . g

NaCl%

0,00585g

: he so g NaCl tng ng vi 1ml AgNO3 0,1N f : He so pha loang V1 : So ml AgNO3 tieu ton V2 : So ml mau lay phan tch Vm : the tch nh mc g : so gam mau lay phan tch

I / PHNG PHAP XAC NH NaCl

BANG PHNG PHAP GIAN TIEP VOHARD
Nguyen

tac Chuan o lng d cua AgNO3bang KSCN vi ch th phen sat amoni ( NH4)2 SO4.Fe2(SO4)3. Mot giot d KSCN se ket hp vi Fe3+ cho mau o. Moi trng cua phan ng la moi trng axt NaCl + AgNO3 = AgCl + NaNO3 AgNO3 + KSCN = AgSCN + KNO3 Dung cu va hoa chat - Bnh nh mc, pheu , Buret, pipet HNO3, dung dch KSCN 0,1N, AgNO3 0,1N Dung dch phen sat: ( NH4)2 SO4.Fe2(SO4)3 KOH 1N, AgNO3 0,1N

Chuan

b mau th : oi vi mau co cac thanh phan m, am khac nhau th phng phap x ly mau khac nhau: a/ Thc pham cha t beo < 5% : Can khoang 5 g mau thc pham a c nghien nat cho vao bnh tam giac cho them 200ml HNO3 4%lac trong 10-15. Sau o trung hoa = KOH 1N. Kh tap chat bang 5ml dung dch kaliferoxyanua va 5ml Zn(CH3COO)2 nh mc len 250ml = nc cat. Lac eu va loc qua giay loc bang vang . Lay 20 hoac 25ml dch loc va nh lng. b/ Thc pham cha nhieu chat beo > 5% Can mau vao khoang 1- 2g cho vao bnh tam giac cho them 20mlKOH 1N xa phong hoa . Chat beo se noi len tren mat. e nguoi va nh mc 100ml sau o loc. Lay 10 ml dch loc cho them 2giot dung dch metyl da cam 0,5% va trung hoa mau bang HNO3 6N sau o nh lng. Lam mau trang song song

c/

Thc pham cha nhieu am ong vat Can khoang 1g mau tht a c xay nhuyen cho vao bnh nh mc 250ml cho t nc cat co cha HNO3 tron eu vi mau sau o cho them 10ml HNO3 am ac va 20ml AgNO3 0,1N . un soi nhe va nho tng giot KMnO4 bao hoa cho en khi khong mat mau na. Lam mat mau KMnO4 bang vai giot NaNO3 60% hay H2O2 . e nguoi va nh lng AgNO3 d bang KSCN 0,1N cho en mau hong gach Tnh ket qua: % NaCl = 0,00585 ( Vt-Vm) 0,1N.Vm 100 m . Vm

II/ XAC NH O CHUA TRONG THC PHAM nh ngha : o chua bao gom : - Cac axt co trong thc pham. Cac axt nay hoac co san trong t nhien trong thc pham nh trai cay, axt hu c - Axt cho vao thc pham vi muc ch che bien : Siro, nc chanh, cam nhan tao - Cac axt sinh ra trong qua trnh chuyen hoa thc pham axt trong sa.. Do o xac nh o chua la xac nh ga tr thc cua thc pham hoac la xac nh o h hong cua thc pham V du : sa, bot , banh gao con tot hay a chua

Xac

nh o chua bao gom :

1/ Xac nh o axt toan phan

2/ Xac nh o axt de bay hi 3/ Xac nh o axt co nh 4/ Xac nh o axt t do cua dau m 5/ nh tnh cac axt vo c ( t hoc) 6/ nh lng mot so axt hu c ( t hoc)

1/ XAC NH O AXT TOAN

PHAN ngha : o axt toan phan la bao gom tat ca cac axt co the nh lng bang mot dung dch kiem chuan. Cac axt nay chu yeu la cac axt hu c: Axt axetic, malic, citric, tactric, lacticbao gom cac axt khong bay hi va cac axt de bay hi. Cac axt cacbonic va SO2 di the t do hay ket hp eu khong tnh trong o chua cua thc pham. Do o nhng thc pham nh bia, nc ngot co cha CO2 hoac SO2 eu c loai tr , trc khi chuan o e xac nh o chua
nh

Ch

th mau Hau het cac axt trong thc pham la axt hu c cho nen la cac axt yeu va khi c trung hoa chung la bang baz manh nh NaOH, KOH. iem tng ng th pH bao gi cung > 7 do o co the s dung phenolphtalein chuyen mau pH = 8,2 . Cung co the s dung cac ch th : Bromotymol xanh, metyl o pH tai d8iem tng ng la gan bang 7. Nguyen tac : Xac nh o chua toan phan cua thc pham la dung mot kiem chuan NaOH hay KOH e trung hoa het cac axt trong thc pham vi phenolphtalein lam ch th. Chuyen t khong mau sang mau hong

Dung

cu va hoa chat NaOH hoac KOH : 0,1N Dung dch phenolphtalein 1% pha trong con 900. Buret, Pipet, can 0,0001g Tien hanh th nghiem : Can chnh xac khoang 10g thc pham a c nghien nho cho vao bnh tam giac, them nc cat khoang 30ml cho vao may lac khoang 1h sau o lay ra cho vao bnh nh mc 50ml, trang bnh tam giac = nc cat cho them vao bnh nh mc en vach. e lang sau o dung pipet lay ra 25ml dch trong cho vao bnh tam giac e nh lng. Neu thc pham la chat long th lay V ml

Cho vao bnh non co cha san 25ml mau 5giot phenolphtalein chuan o t t dung dch NaOH 0,1N cho en khi dung dch co mau hong nhat ben vng. Tnh ket qua: o chua ( mllg/g) = K. VNaOH. 50.N 25 .m K : he so cua loai axt N : nong o ng lng cua NaOH m : lng can mau Tuy theo loai thc pham ket qua se bieu th bang mot so loai axt sau: K axt lactic = 0,09 ( Sa) K axt acetic = 0,06 (dam) Cac loai trai cay: Vi dau m : K axt malic = 0,076 K axt oleic = 0,282 K axt citric = 0,064 K axt tactric = 0,075

2/ Xac nh o axt de bay hi

nh

ngha : o axt de bay hi bao gom cac axt thuoc nhom axt axetic : HCOOH, CH3COOH, C2H5COOH, C3H7COOH di dang t do hoac di dang muoi. Cac axt sau: axt lactic, CO2, SO2 khong tnh vao o axt bay hi. Nguyen tac : Dung mot nguon hi nc nong i qua thc pham, keo cac xt bay hi khi gap lanh cac axt bay hi nay ngng tu lai chay vao bnh hng va c chuan o bang dung dch kiem vi ch th la phenolphtalein

Dung

cu va hoa chat - Dung cu cat axt de bay hi - dung dch chuan NaOH 0,1N -Phenolphtalein 1% trong con 900 - Can 0,0001g - Buret, Pipet, bnh non Tien hanh th Can chnh xac t 10 20g mau cho vao ong ng mau them vao ong khoang 50ml nc cat. at ong vao he cat . Cho hi nc nong suc qua ong ung mau va un nhe he cat. Hi thoat ra chay qua ong sinh han c lam lanh va chay xuong bnh hng. Cat khoang chng 300ml dch thu c th ngng . Lay bnh non ra un nhe cho bay hi het CO2 cho them 5 giot phenolphtalein va chuan o bang NaOH 0,1N en khi xuat hien mau hong ben vng.

ket qua : Tnh theo o bay hi cua axt axetc Axt % = VNaOH . 0,1N. 0,06 .100 m (g) Loai bo SO2 co trong mau hoac trong nc cat Sau khi nh lng axt de bay hi bang NaOH vi ch th Phenolphatalein cho them vao dch cat 1 got HCl tinh khiet, 2ml ho tinh bot, 1 hat tinh the KI va chuan SO2 t do bang dung dch iot 0,01N ( V1). Cho them 28ml natri borat bao hoa dung dch chuyen thanh mau hong nhat chuan o SO2ket hp bang dung dch Iot 0,01N cho en mau xanh
Tnh

Tnh

ket qua : Tnh so ml NaOH thc te dung e nh lng axt de bay hi: VNaOH = ( VNaOH - V1 - V2 ) 10 10
Trong

o : VNaOH : so ml chuan o cho axt de bay

hi V1 : so ml iot 0,01N s dung e nh lng SO2 t do V2 : so ml ot 0,01N s dung e nh lng SO2 ket hp Co the tnh o axt de bay hi bang cach :

3/ Xac nh o axt co nh
tac : o axt co nh bao gom tat ca cac axt khong bay hi. Sau khi mu c co can tren bep cach thuy e cac axt de bay boc het. Can c hoa tan vao nc cat va nh mc sau o lay ra chuan o vi baz NaOH 0,1 vi ch th phenolphtalein. Dung cu va hoa chat: Bep cach thuy Dung dch chuan NaOH hoac KOH 0,1N
Nguyen


Tien
Can

hanh th nghiem:

chnh xac khoang 10 -15g thc pham mau cho vao coc thuy tinh chu nhiet cho them t nc vao mau e mau dang set ( neu mau long th khong can cho them nc )at coc len bep cach thuy thnh thoang khuay eu un en can. Lay mau ra e nguoi sau hoa tan can bang nc cat nh mc 100ml . Roi lay ra 50ml chuan o vi NaOH 0,1N Tnh ket qua : Axt co nh mllg /g = 0,1N . Vm .VNaOH .K. m 50 Vm : the tch bnh nh mc VNaOH : So ml NaOH tieu ton trong chuan o K : he so chuyen oi ra axt cu the m : So lng gam mau lay phan tch 50: so ml mau hut ra e phan tch

 Hoac

co the tnh nh sau: Axt co nh mllg/g = K ( V1 V2 ) .N. m V1 : So ml NaOH 0,1N e nh lng axt toan phan V2 : So ml NaOH 0,1N e nh lng axt de bay hi K : he so chuyen oi ra axt cu the

4/ o axt t do cua dau m

Nguyen

tac : Dau m e lau b thuy phan va cho ra cac axt beo t do. Cac axt t do nay c chuan o bang dung dch KOH trong con moi trng ete-con o chua t do c bieu th bang ch so o chua ngha la so mgKOH can thiet e trung hoa cac axt t do trong 1g dau m. Hoa chat va dung cu: Ete : 1 the tch Con : 1 The tch , ete : Con theo ty le 1:1 Pha dung dch KOH 0,1N trong con 950 nh sau: Can 35gKOH trong 20ml nc cat , cho them con cho u 1l. ng trong chai mau nau va e 2148gi . Loc qua bong loc thuy tinh.

tra lai nong o KOH bang dung dch HCl 1N vi ch th phenolphtalein va ieu chng dung dch KOH 0,5N bang con. Muon co dung dch KOH 0,1N pha loang t dung dch KOH 0,5N . Lu y: Dung dch KOH trong con phai c xac d8nh lai nong o trc 12ngay . Dung dch KOH 0,5N s dung cho nh lng o axt t do trong chat beo cong nghiep. Dung dch KOH 0,1N s dung cho nh lng o axt t do trong chat beo thc pham co o axt thap.
Kiem

Tien

hanh th nghiem Cho vao bnh tam giac 250ml , 150ml dung dch hon hp con ete , cho them vao 5 giot phenolphtalein ( neu trng hp dung dch tren khong co mau th nho them tng giot KOH 0,1N trong con en khi mau hong xuat hien. Can chnh xac khoang 10g chat beo vao bnh tam giac khac hoa tan mau bang dung dch ete-con 20ml va chuan o bang dung dch KOH 0,1N ch th phenolphtalein cho en mau hong

ket qua : o axt t cua dau m tnh theo % % X dau m = K .VKOH. N. 100 m K : he so tnh ra cac loai axt beo, Neu la dau co K axt palmitic = 0,256, K axt oleic = 0,282 Ch so o chua ( so mg KOH dung e trung hoa 1g dau m) tnh bang cong thc Ia = 5,611. VKOH m 5,611: so mg KOH trong 1 ml KOH 0,1N VKOH so ml KOH 0,1N s dung e chuan o mau th m : so lng g mau em phan tch Lu y : Neu mau la chat beo co nc ket qua phai tnh tren chat kho
Tnh

5/ Phan tch protit (protein)

nh

ngha : Ve phng dien hoa hoc , protit la nhng chat hu c ma thanh phan cau tao gom C, H, O va N co khi trong thanh phan con co them S, P Protit bao gom cac axt amin va nhng hp chat ( peptit, protein) khi thuy phan cho 1 hay nhieu loai axt amin . Cong thc chung cua cac axt amin NH2CHRCOOH.

Peptit

la do mot so axt amin ket hp vi nhau bi day noi Peptit. Nhom chc cua axt amin nay ket hp vi nhom chc cua axt amin kia R CH CO OH + H NH CH R

NH2 COOH Protein la nhng protit khac ( khong co day noi peptit) chia thanh holoprotein khi thuy phan cho cac axt amin va heteroprotein. Thanh phan chnh cua protein la cac amino axt ngoai axt amin con cho nhng chat khong phai la protit goi la chat phi protit V du nh Alcaloit

PROTIT THO
nh

ngha: Protit tho trong thc pham c nh lng bang cach xac nh lng Nit toan phan va ket qua nhan vi 6,25. Nh vay protit luon co cha 16% la Nit. Thc te trong thc pham luon co ham lng nit cao hn 16% v co cac ni t khac trong thanh phan nh: alcaloit, amoniac, axt nitricNhng protit thc vat th ham lng nit < 16%. % Protit = % N .F F : he so e chuyen oi t N sang Protit

Thc

pham %N Hon hp 16 Tht 16 Bap 16 Sa va san pham sa : 15,66 Bot my 17,54 TRng 14,97 au nanh 17,51 Gao 16,81 Thc an gia suc

He so F 6,25 6,25 6,25 6,38 5,7 6,68 5,71 5,95 6,25

Cac phng phap xac nh Protein phap e xac Hien nay co nhieu phng
nh protit thc chat la xac nh ham lng Nit . Phng phap chon phu thuoc vao o ung o chnh xac cua phng phap va ieu kien san co cua phong th nghiem . Mot so phng phap e nh lng Ni t nh sau: - Phng phap kjeldahl - Phng phap chng cat trc tiep - Phng phap gia nhiet ( ot nhiet o cao) - Phng phap chuan o Formol - Phng phap phan tch quang pho

Phng phap Kendan ( Kjeldahl) Phng phap nay ra i t nam 1883 bi

ong Kjeldahl., ngi ng au cua mot cong ty san xuat ru bia Calsberg. ay la Phng phap nh lng Ni t toan phan va protein trong thc pham n gian ma chnh xac. Nguyen tac : Vo c hoa thc pham bang axt H2SO4 am ac va co chat xuc tac. Dung kiem manh NaOH e ay NH3 t muoi (NH4)2SO4 ra the t do . nh lng NH3 bang axt. H2SO4 N (thc pham) (NH4)2SO4 (NH4)2SO4 + 2NaOH Na2SO4 + 2H2O + 2NH3

NH3 + H2SO4 ( NH4)2SO4 Lng d H2SO4 + NaOH Na2SO4 + H2O

Hoa

chat va dung cu Bnh Kendan, bnh tam giac, bo ch cat H2SO4 am ac d=1,84 Hon hp cac nhom chat xuc tac : K2SO4, : 1000g K2SO4, : 50g CuSO4, : 30 g CuSO4, : 3,5g Selen : 30g

100g

K2SO4, : 100g CuSO4, : 10 g Selen : 1g

K2SO4, : CuSO4, : HgO :

10 g

30g

NaOH

: 50% khong cha cacbonat, HCl

0,1N Ch th mau: metyl o 0,016g + 0,083g bromocresol xanh nh mc thanh 100ml bang ethanol 96% u iem cua phng phap: - Phng phap nay dung e xac nh tat ca Ni t cac dang co the chuyen thanh amonium sulfat - Nitrat , nitric va hp chat nitroso khong the chuyen thanh dang amonium sulfat bang phng phap nay

Tien

hanh th nghiem Can chnh xac khoang 1g mau cho vao ong Kjeldahl ( khoi lng mau lay can nen cha khoang 0,03g nitrogen) . Them vao ong 25ml H2SO4 am ac them 10g hon hp xuc tac va cho vao bep pha mau ( he thong bep cua hang Foss) luc au pha cham e tranh trao ra . Sau khi mau a tr nen xanh trong tiep tuc un them 45 . e nguoi them vao ong khoang 100 200ml nc, e nguoi chuyen toan bo hon hp tren vao ong cat mau. Them 80 85ml NaOH 50% vao he thong cat chu y khong lam thoat amoniac. Chuan b bnh hng co san 25 100ml HCl 0,1N vi vai giot metyl o e hap thu amoniac . Khi dung dch khong chuyen mau na va lng dung

Trong

qua trnh cat neu dung dch hng chuyen sang mau vang cua kiem th cho them axt HCl 0,1N vao bnh hng( hoac dung 50ml dung dch axt boric 2% ) Chuan o lng d HCl bang dung NaOH 0,1N. Tien hanh lam mau trang song song Tnh ket qua % N = 14 . (V1 V2 ) . 0,1 .100 1000 . m V1 : The tch NaOH 0,1N cua mau trang V2 : The tch NaOH 0,1N cua mau th m : khoi lng mau lay phan tch % protein tho : % N x 6,25

MAY PHA MAU AM BANG PP.KJELDAHL

MAY CHNG CAT AM

Phng phap xac nh protein bang chng cat trc Nguyen tac : ay la phng phap da tiep co sa oi. e tren phng phap Kjeldahl
tranh s mat amoniac trong qua trnh phan huy mau bang axt manh va xuc tac th phng phap nay phan huy mau bang kiem manh nh NaOH va Na2SO4 . Amoniac thoat ra c hap thu trong bnh co san axt boric va aminiac chuyen thanh ammonium borate va chuan o lng d cua axt boric bang NaOH 0,1N . Phan tep theo lam giong nh Kjeldahl Tuy nhien phng phap nay khong c chnh xac nh phng phap tren va tiet kiem c thi gian pha mau

Xac nh Protein bang phng phap ot

Phng

phap nay c xay dng t nam 1830 bi ong Dumas. Nguyen tac : Da tren phan ng o mau phan tch nhiet o cao khoang 9500C. Vi kh ot la kh oxy. Kh mang la kh helium ( He). Ket qua c tnh ngay tren thiet b la Nit sau o tuy theo oi tng mau nhen vi he so e chuyen ve protein Dung cu va hoa chat Thiet b may phan tch , can giay goi mau, ong goi mau , Cu

Tien

hanh phan tch: Mau can chnh xac khoang 0,2g neu mau la chat long lay khoang 1ml. Mau ran c goi trong giay thiec, mau long th ng trong ong bang thiec. Mau c at vao trong autosampler sau o dung kh nen ay mau vao lo nung. ay lo nung c ot nong bang kh oxy len en 9500C. Mau se chuyen thanh dang kh mau c chuyen qua ong loc e gi lai cac kh khong can thiet nh HCl, SO2. Kh con lai bao gom CO2, Nox c kh mang He chuyen i tiep vao buong mau o may t ong trch ra 3mm3 kh cho i qua mot he thong loc tiep o co san bay va co bot Cu tinh khiet se hap thu mau kh va kh CO2 va NOX thanh Ni t t do i vao au do va t

Phng

trnh phan ng

NOx Tnh

+ Cu CuO + N2

ket qua : % Protein = % N x 6,25

May phan tch Nit - Phng phap Dumas

CHUAN O PHC CHAT

Trong phan tch the tch chung ta co the s dung cac phan ng hoa hoc thoa man nhng ieu kien sau: 1/ Chat tham gia phan ng phai phan ng theo ty le nh lng nhat nh ( ty le hp thc) 2/ Phan ng gia chat can xac nh vi dung dch chuan ( dung dch chuan o) cua thuoc th phai xay ra nhanh va hoan toan 3/ cac chat la co mat trong san pham nghien cu cung vi ch tieu can xac nh khong can tr s chuan o chat can xac nh.

5/ Phan ng phai co kha nang xay ra nhiet o phong 6/ S chuan o phai khong co phan ng phu kem theo gay sai lech ket qua Neu 6 iem neu tren ap ng c th nhan biet iem cuoi cua chuan o ( Tc la iem tng ng ) bang cach oi mau chat ch th , hoac dung ien cc ch th, hoac o o dan ien Tuy nhien co nhieu phan ng khong thoa man cac ieu kien tren hoac thoa man nhng phan ng khong ben b thay oi nhanh mau cua ch th kho nhan biet c iem cuoi cua chuan o do vay phai nghien cu phng phap mi o la : Chuan o bang dung dch chat tao

du : muon xac nh cac cation kim loai nh Ca, Mg, Alco trong cac mau thc pham th khong the s dung phng phap chuan o axt baz, hoac co the s dung c bang phng phap ket tua nhng ton thi gian, hoa chat, nhan cong va co kha nang ket qua cha c chnh xac. Dung phng phap tao phc co the nh lng c cac cation khac nhau va cac anion Phng phap tao phc: Phng phap tao phc da tren viec dung cac phan ng tao thanh cac phc chat tan hoac cac muoi t phan ly
V
+ -

lien quan gia phng phap ket tua va phng phap tap phc Phng phap ket tua lien quan chat che vi phng phap tao phc v nhieu phan ng ket tua kem theo s tao phc con s tao phc phai keo theo s ket tua cua chat kho tan V du:, [AgCl2]- ion phc tao thanh, khi d mot giot Ag len [AgCl2]- th AgCl ket tua ket tua, [Ag(CN)2]- ion phc tao thanh khi cho lng d Ag+ tac dung vi [Ag(CN)2]th se tao thanh ket tua AgCN. Phan ng tao phc se cho ra san pham cac muoi kem phan ly thanh cac ion: HgCl2, Hg(CN)2, Hg(SCN)2..
AgCN

Mot

trong nhng phng phap chuan o phc chat quan trong o la phng phap COMPLEXON . Hien nay trong chuan o complexon hau het dung cac axt aminopolycarboxylic lam chat tao phc , trong o etylendiamintetraaxetic (EDTA) chiem v tr quan trong nhat. Anion cua EDTA co the tao thanh cac vong cang nam canh vi ion kim loai Khai niem ve Complexon : Cac hp chat hu c la dan xuat cua axt aminopolycarboxylic thng c goi la cac complexon. Complexon n gian nhat la axt Nitrolotriaxetic (NTA complexon I H3Y)

Cong thc cau tao cua H3Y CH2COOH CH2COOH CH2COOH CH2COOH CH2COOCH2COOH

hay H N+

Co

ga tr hn ca la axt Etylendiamintetraaxetic (EDTA, complexon II H4Y)

HOOCCH2 HOOCCH2

N - CH2 CH2 N

CH2COOH CH2COOH

Hay

HOOCCH2 H
- OOCCH 2

CH2COO N+ - CH2 CH2 N+ H CH2COOH

Complexon

co cac nhom cacboxyl ( - COOH ) cha Nit amin (N) nh cau tao nh vay nen hp chat co kha nang tao thanh cung mot luc mot so lien ket phoi tr vi ion kim loai tap phc. Trong thc te thng dung muoi dinatri cua axt etylendiamintetra axetic( EDTA, HaEDTA complexon III hay trilon B viet tat Na2H2Y) HOOCCH2 CH2COOH

N - CH2 CH2 N

Phan ng cua comlexon vi cac ion kim loai tao phc xay ra theo theo ty le hp phc ng lng nghiem ngat. ieu o a m ra kha nang to ln cho viec dung complexon e nh lng nhieu cation nh Ca, Mg, Zn, Cu, Al Cac ac iem ac trng cua complexon 1/ De dang phan ng vi nhieu kim loai trong o co cation kiem tho la khong tao phc vi cac chat tao phc khac ) tao thanh cac phc ben tan trong nc 2/ Tan tot trong nc va cac dung moi hu c 3/ Co mot so tac dung chon loc oi vi ion nay hay ion khac

dung phng phap EDTA va cac complexon khac e che cac kim loai kiem , kiem tho , kim loai nang khi chung ngan can viec xac cac ion khac. Vi tnh chat nay complexon con c dung lam chat che. V du: S dung EDTA tao phc vi cac ion kim loai khac co trong mau khi can xac nh Be bang phng phap chuan o, o mau
S

Chuan o Complexon

Phng phap complexon la phng phap phan tch chuan o da tren viec dung phan ng cua ion kim loai tao phc vi cac complexon, tao thanh cac muoi noi phc ( vong cang) ben, t phan ly, tan trong nc Khi chuan o cac muoi kim loai tao phc bang EDTA xay ra cac phan ng sau trong giai oan ket thuc Na2H2Y 2Na+ + H2Y2Me2+ + H2Y2- MeY2- + 2H+ Me3+ + H2Y2- MeY2- + 2H+ Me4+ + H2Y2- MeY2+ 2H+

theo cac phng trnh tren cho thay 1mol cation phan ng vi 1 mol Na- EDTA ma khong phu thuoc vao hoa tr cua no .

 Xac

nh iem tng ng cua chuan o complexon nh cac chat ch th la cac pham mau hu c tao vi cac cation phc chat co mau cac chat ch th kim loai
Khi

chuan o bang EDTA cac hp chat mau nay dan dan se b phan huy do s tao thanh hp chat noi phc mi ben hn cua cation vi complexon. iem tng ng mau au tien cua phc chat tao thanh t kim loai can xac nh vi chat ch th , sau bien mat va xuat hien mau cua ban than cua ch th t do

CHAT CH TH
Trong

phng phap chuan o complexon chat ch th la cac chat mau hu c : Crom xanh en axt, Eriocrom Tencac chat ch th nay trong moi trng kiem co mau xanh . Cac ion Ca, Mg va nhieu ion khac tao vi chat ch th co mau o nho. Khi chuan o vi EDTA th cac ion kim loai se tach ra khoi ch th va tao phc ben vi EDTA va cho en khi ion kim loai tao phc ben hoan toan vi EDTA th chat ch th tr ve trang thai t do , mau ban au cua ch th. Me2+ + HInd2- MeInd- + H+ xanh o MeInd- + Na2H2Y + OH- Na2MeY + HInd2- + H2O

Cac loai phan ng c dung khi chuan o Complexon

1/ Phan ng tac dung trc tiep cua ion kim loai tao phc vi complexon Phng phap chuan o trc tiep Cach chuan o nay c dung e chuan o nhng ion kim loai khi chuan o thoa man ay u cac ieu kien cua phan ng chuan o the tch Nguyen tac : Dung dung dch chuan EDTA trong moi trng kiem vi chat ch th eriocrom T en hay trong moi trng axt vi ch th la xylen da cam. Trc khi chuan o a dung dch phan tch ve ga tr pH xac nh sau o dung dung dch em a vao dung dch phan tch e gi cho pH khong thay oi. oi khi a vao dung dch tac nhan tao phc nh tactrat, xitratmuc ch nhng chat nay lien ket vi mot so cation gi cac cation nay trang thai khong ket tua

du: Phan ng Ca vi Na2H2Y trong moi trng kiem KOH pH = 13-14 vi ch th mau huynh quang fluorexon chuyen t mau huynh quang sang mau hong

Ca2+

+ H2Y-

CaY2- + 2H+

2/Phng

phap chuan o

ngc Chuan o ngc c s

dung khi : - khong co ch th thch hp oi vi ion can xac nh - Cac ion tao thanh ket tua trong dung dch em - phan ng xay ra cham - Xac nh ham lng cation trong cac ket tua khong tan trong nc: Ca2+ trong CaC2O4, Mg2+ trong MgNH4PO4, Pb2+ trong PbSO4

2/Phng

phap chuan o

ngc :
Nguyen

tac : Them vao dung dch phan tch mot the tch chnh xac dung dch chuan Complexon , un en soi dung dch e thc hien phan ng tao phc , sau o lam lanh va chuan lai lng complexon d bang dung dch chuan muoi kim loai nh : ZnSO4 , MgSO4, Fe2SO3e xac nh iem tng ng dung ch th kim loai phan ng vi ion magie, hay kem

du: Xac nh nhom (Al) pH = 5, em axetat khi o them mot lng d complexon vao dung dch phan tch sau o chuan o lng d bang dung dch chuan o pH = 5 Al3+ + Na2H2Y AlY- + 2H+ + (n-1) H2Y2lng d pH = 10 ( n-1)Zn2+ + (n-1) H2Y2- (n-1)ZnY2- + 2H+ Lu y : Khi cho complexon vao mau trong mau a co san ch th Xylen da cam ma co mau hong th nh vay lng complexon la thieu phai cho them e dung dch chuyen ve mau vang ( iem tng ng t vang hong)

3/

Phng phap chuan o chat the :Phng phap da tren c s cation tao phc vi complexon kem ben hn la cation can xac nh , va xay ra phan ng trao oi cation kem ben o se c gai phong va cation can phan tch se the vao v tr cua cation o. Chuan o cation c giai phong ra vi EDTA. V du: Can phan tch cation Thori ( Th4+). Cho trc vao dung dch mot lng complexonat magie MgY2- . Sau o chuan o lai lng ion Mg2+ tach ra bang dung

 Phng

trnh phan ng xay ra nh sau: pH =2 Th4+ + MgY2- ThY + Mg2+ (a) Mg2+ + H2Y2- MgY2- + 2H+ (b) V Th tao phc vi complexon ben hn Mg , nen can bang chuyen dch ve ben phai Ket thuc chuan o , chuan o lai ion Mg bang EDTA vi ch th Eriocrom T en th co the tnh c ion Th co trong dung dch phan tch

Phan ng chuan o axt baz : Trong qua trnh tng tac cua phan ng complexon vi cation nao o lam tach mot lng tng ng ion Hydro. Chuan o lai lng ion hydro c tao thanh bang mot dung dch kiem chuan manh vi chat ch th axt-baz hay bang phng phap iot Me2+ + H2Y2- MeY2- + 2H+ 2H+ + 2OH- 2H2O ch th metyl o 3Me2+ +3H2Y2-+ IO3-+ 5I- 3MeY2-+ 3H2O+ 3I2 Iot tach ra c chuan lai bang thiosunfat S2O32- + 3I2 3 S4O62- + 6I4/

CHUAN O HON HP NHIEU ION CAC CHAT CHE Trilon B tap phc c vi nhieu ion kim loai do o muon chuan o mot ion kim loai ta phai tnm ieu kien thch hp e ch cation can xac nh phan ng vi trilon B , con cac ion la khong phan ng. Chat che phai thoa man cac ieu kien sau: Chat che khong tao phc vi cation can xac nh, hoac tao phc kem ben hn phc complexonat cua chung - Cac chat che thng dung: KCN dung e che Fe, Cd, Hg, Cu, Zn, Ag, Ni, Co

C s ly thuyet cua phng phap complexon

Cau

tao cua muoi noi phc c tao thanh Axt Etylendiamintetraaxetc ( EDTA) la mot axt bac 4 co 4 ion hydro linh ong va hai nguyen t nit vi tnh chat c ban la co 6 nguyen t co the tham gia phoi tr khi tao thanh cac vong 5 cua hp chat noi phc V du: ong glicocoliat 0 = C -----O O ------C = O Cu H2C ----H2N NH2----CH2 ____

Trong moi trng hp muoi noi phc c tao thanh khi cac ion kim loai tao phc the cac nguyen t hydro hoat ong cua nhom chc hu c , mat khac tac dung vi cac nhom nao o tao nen lien ket phoi tr. Cac nhom co ion hydro co kha nang b ion kim loai the va tng tac vi ion kim loai tao phc bang lien ket chnh la nhom carboxyl - COOH, nhom sunfoxilic SO3H, hydroxyt OH
HOOCCH2 HOOCCH2

CH2COOH N - CH2 CH2 N CH2COOH

Muoi

noi phc vi EDTA tao thanh mot mat la do s the cac nguyen t hydro hoat ong cua nhom caboxyl tao phc. ay EDTA ket hp vi ion kim loai tao phc bang hoa tr chnh mat khac do s tng tac cua nguyen t Nit co kha nang tao lien ket phu ( phoi tr) vi ion kim loi tao phc V du : muoi noi phc cua Canxi ( Na 2CaY) O=C----O O----C=O
NaOOCCH2

H2C N

Ca N

CH2

CH2 ---CH2

CH2COONa

Xac nh o chuan cua dung dch EDTA dung muoi dinatri Pha dung dch chuan EDTA s
cua axt etilendiamintetraaxetic Na2C18H14O8N2 . 2H2O, muoi c say 120 1400C trong 2 g se tr thanh muoi khan. Sau o lay ra e nguoi va can pha chuan. MEDTA = 372,24g , 1MEDTA = 372,24g/ 1l dung dch 1 N EDTA = MEDTA / 2 = 186,12/ 1l dung dch Xac nh o chuan cua EDTA bang ZnO, CaCO3, Zn kim loai tinh khiet hoa hoc , hoac ong chuan phicxenan nh muoi magie sulphat 0,1N, ),05N..

XAC NH HAM LNG CAN XI ( Ca) Xac nh Ca co nhieu phng phap :

- PP. trong lng CaC2O4 can dang CaCO3 hoac CaO - PP ket tua dang CaSO4 -PP Chuan o : Ca ket tua CaC2O4 sau o nh lng bang phng phap KMnO4 - Phng phap complexon Cac nhc iem cua phng phap: Thi gian lau, ket tua Ca b ket tua co nhieu tap dan en ket qua nh lng khong chnh xac cho nen hien nay s dung phng phap Complexon la hieu qua va chnh xac nhat

Xac

nh Ca bang phng phap complexon Nguyen tac: Da tren chuan o trc tiep ion Ca bang dung dch chuan EDTA trong moi trng kiem manh pH 12 14 vi chat ch th la murexit hay crom xanh en axt. Cach xac nh : Dung pipet lay 25ml dung dch Ca2+ cho vao bnh tam giac. Trung hoa dung dch bang NaOH sau o cho them 5 ml NaOH 20% e cho pH cua dung dch 12-14, cho them vai hat murext lac eu. Tien hanh chuan o nhanh bang dung dch EDTA en khi mau cua dung dch oi t xanh sang tm.

BAN CHAT VA PHAN LOAI CAC PHNG PHAP OXY HOA KH

nh

ngha : Phan ng oxy hoa kh la phan ng trong o co s thay oi so oxy hoa cua mot hoac vai nguyen to Chat oxy hoa la chat cha nguyen to nhan electron. Chat kh la chat cha nguyen to cho electron. V du: Sn2+ + 2Fe3+ Sn4+ + 2Fe2+ Sn2+ -2e- Sn4+ (S oxy hoa) Sn2+: Chat kh Fe3+ + e- Fe2+ ( s kh ) Fe3+ : chat oxy hoa

Ban

chat cua phng phap chuan o oxy hoa kh 1, Xac nh cac chat can xac nh ma co s thay oi ve hoa tr cua cac chat o khi phan ng ket thuc Fe2+ Fe3+ 2/Cac thuoc th tng tac vi chat can xac nh theo ty le hp thc trong phan ng b thay oi hoa tr Ca + C2O42- CaC2O4 5CaC2O4 + 2MnO4- +16H+ 5Ca2+ + 10CO2+2Mn2+ + 8H2O o o phng phap chuan o oxy hoa kh

Phng

phap c ng dung rong rai trong cac phong th nghiem . Phng phap cho phep xac nh nhieu chat vo c va huu c, cac hp chat c kim , cac chat sinh hoc va thc pham khac nhau . u iem cua phng phap - Cho o chnh xac cao -o lap lai tot - n gian, t ton thi gian phan tch -Cho phep xac dnh cac chat de b oxy hoa hoac kh va con co the xac nh cac chat khong b oxy hoa hoac kh - S chuan o oxy hoa kh xac nh tai iem tng ng co the dung ch th va cung co the khong dung ch th hoac dung cac phng phap dung cu

Y NGHA CUA PHNG PHAP OXY HOA KH

S chuan o xy hoa co the thc hien tat ca moi trng -Co the tien hanh xac nh bang cac phng phap chuan o trc tiep, gan tiep va chuan o ngc.

Phan loai cac phng phap chuan o oxy hoa kh Da tren ac tnh cua thuoc th c ban ( dung dch chuan o c ban ) c s dung cho tng trng hp cu the e chuan o cac hp chat rieng re hoac cac hp phan rieng biet cua hon hp chat can phan tch ma goi ten phng phap. V du: Phng phap da tren s oxy hoa cua Pemaganat goi la phng phap Pemaganat Phng phap da tren s oxy hoa cua iot goi la phng phap.Iot

 Phng

phap da tren s oxy hoa cua Crom VI goi la phng Cromat - Phng phap da tren s kh cua axt Ascobic goi la phng phap ascobic

Nguyen

tac cua pp. chuan o oxy hoa

kh Chuan o chat kh bang dung dch chuan la chat oxy hoa , chuan o cac chat oxy hoa hoa th bang dung dch chuan la chat kh V du : Xac nh Fe2+ la chat kh vay s dung chat chuan oxy hoa la KMnO4 Fe2+ + MnO4- Fe3+ + Mn2+ Kh cac hp chat co hoa tr cao xuong hoa tr thap bang cac chat kh manh Cu2+ + Sn2+ Cu0 + Sn4+ Thong thng trc tien kh chat oxy hoa can xac nh en hoa tr thap hn sau o chuan o bang dung dch chuan

CAC DUNG DCH CHUAN DUNG TRONG PHNG PHAP OXY HOA KH
Cac

dung dch chuan thng c su dung cho phng phap nay : Cac dung dch chuan la cac chat oxy hoa manh : KMnO4, K2Cr2O7, KI, Kali Bromat.. Dung dch co cac chat kh manh : Na2S2O3, Axt ascobic , Hp chat cua Cr2+ co tnh kh manh 1/ Kali permaganat : KMnO4 trong moi trng trung tnh, axt va kiem s thay oi hoa tr cua Mn trong cac moi trng o -Moi trng axt: MnO4- + 5e + H+ Mn2+ + H2O + H+

Moi trng kiem MnO4- + 3e + OH- MnO2+ OH- Moi trng trung tnh : MnO4- + 3e + H+ MnO2+ H2O MnO4- + e- + OH- MnO42- KMnO4 : la mot trong nhng chat oxy hoa manh nhat E0KMnO4/Mn2+ = 1,52V Phan ng oxy hoa kh cua KMnO4 phu thuoc vao moi trng e cho ra cac san pham khac nhau.e tang them toc o cua phan ng co cho them cac chat xuc tac nh muoi Mn, Fe, Cu e xac nh o chuan cua dung dch KMnO4 thng dung axt oxalic H2C2O4 , KI, muoi Mor ( NH4)2Fe(SO4)2 iem tng ng c xac nh bang d mot giot KMnO4 cho dung dch mau hong

- Cac hp chat cua Mn3+ va Mn4+ chu yeu e chuan o cac hp chat hu c Cac chat goc thng c dung e pha dung dch chuan la Mn3+ : Mn2(SO4).2Al2(SO4)3, , K2SO4.Mn2(SO4), 2/ Iod trong dung dch KI KI + I2 K(I3) I3 + 3e- 3IS dung dung dch Natri thiosunphat lam chat kh 2S2O32- + I3- S4O62- +3I-

Viec

chuan o bang iot tien hanh trong moi trng trung tnh hay trong cac dung dch em cacbonat, photphat, boratiem tng ng dung ch th ho tinh bot Phng phap chuan o bang iod c s dung rong rai e o cac chat vo c va hu c 3/ Kali cromat KMnO4 , bicromat K2CrO7 , anhidric cromomic , kali bromat ( KBrO3) la cac chat oxy hoa manh S chuan o c thc hien trong moi trng axt.Tai iem tng ng dung chat ch th hoac khong dung ch th Cac chat kh c s dung cho phng phap nay la cac kim loai t do, cac hp chat cua Fe2+

S Oxy hoa va tng tac axt baz

Khi

them axt hoac baz vao he oxy hoa kh co the gay ra s thay oi ac trng cua phng phap V du : khi them axt vao he oxy hoa kh cua AsO43- / AsO2- + I2/2I- xay ra s kh t As5+ As3+ H3AsO4 + KI + 2HCl HAsO2 + I2 + 2H2O + KCl Khi them kiem xay ra s oxy hoa As3+ As5+ AsO2- + I2 + 4OH- AsO43- + 2I- + 2 H2O

Hang so can bang cua phan ng hoa kh

Cac

phan ng oxy hoa kh thuan nghch . S can bang c thiet lap khi Eox bang Ekh . V du : MnO4- + 5Fe2+ + 8H+ Mn2+ + 5Fe3+ + 4H2O Ox1 Kh2 Kh1 Ox2 Bieu thc cua L tac dung khoi lng ( [Mn2+]/[MnO4-][H+]8 .([Fe3+]5 / [Fe2+]5+ = KMnO4-/ Fe2+ K:hang so can bang

ac

iem cua phan tch trong lng Phan tch trong lng la mot trong nhng phan tch quan trong nhat cua phan tch nh lng: Phan tch nh lng nc ng dung e xac nh thanh hoa hoc cua nhng oi tng nghien cu nh kim loai, silicat, vo c, hu c.. Phng phap xac nh trong lng co o chnh xac cao

C S PHAN TCH TRONG LNG

BAN CHAT CUA PHAN TCH TRONG LNG nh ngha: Phan tch trong lng la mot phng phap cua phan tch hoa hoc nh lng da tren s o chnh xac khoi lng cua chat can xac nh hoac cua thanh phan no c tach ra trang thai tinh khiet hoa hoc hoac di dang hp chat thch hp co thanh phan khong oi biet chnh xac. S tach trc tiep chat can xac nh hoac cac thanh phan cua no ra khoi san pham di dang tinh khi61t hoa hoc gap nhieu kho khan oi khi khong thc hien c do vay s dung phng phap ket tua

Phng

phap tach ket tua: Chuyen lng can mau thanh dang dung dch, them vao vao mau o lng thuoc th thch hp, thuoc th o se phan ng vi chat can phan tch thanh mot hp chat t tan. Khi o hp phan cua chat can phan tch ( cation , anion) c tach ra t dung dch di dang ket tua thc te khong tan. Ket tua c tao thanh c loc hoac ly tam, roi ra ket tua e loai tat ca nhng tap chat. Roi ket tua c say hoac nung en trong lng khong oi va c can tren can

PHAN LOAI CAC PHNG PHAP PHAN TCH TRONG LNG

lam 3 nhom ln : - Phng phap tach - phng phap ket tua - Phng phap cat
Chia

1/ Phng phap tach

Nguyen

tac cua phng phap: Cau t can xac nh c tach ra t chat phan tch di dang t do va c can tren can phan tch. V du : nh lng vang, bac, ong t hp kim hoac t quang Hoa tan hp kim trong cng thuy ( HCl : HNO3 1:3) thu c dung dch cha cac ion vang va ong. Them vao dung dch Hydro Peoxt ( H2O2) se kh ion vang en vang nguyen to va khong gay anh hng en ion Cu. Tat ca Au c tach ra trang thai vang kim loai. Loc vang c tach ra va ra no bang dung dch HCl loang sau o ra lai = nc cat Cho vang vao coc s em say va nung

o phan tach vang HP KIM

HNO3 + HCl 1:3

Oxyhoa H2O2

Ra ket tua = HCl loang

Say, nung Can Au tinh khiet

Cho dong ien mot chieu chay qua dung dch (nc ra va nc loc) trong ieu kien xac nh th Cu kim loai se c tach ra va bam tren catot Platin tr oi vi dung dch ( va a c can trc) da vao lng can cua catot se suy ra ham lng cua Cu trong hp kim. phng phap ien trong lng

2/ PHNG PHAP KET TUA

Nguyen

tac cua phng phap Ket tua nh lng cau t can phan tch bang cac phng phap hoa hoc di dang hp chat hoa hoc t tan. Ket tua c tach rara say hoac em nung , khi o ket tua thng c chuyen thanh mot chat mi co thanh phan biet chnh xac. Hp chat nay c can tren can phan tch. Phan biet dang ket tua va dang can Dang ket tua: la dang chat can xac nh c ket tua Dang can: la dang chat can xac nh c can V du: khi xac nh ion SO42- bang phng phap trong lng , ket tua chung bang ion
2+

+ Ba2+ = BaSO4 Chat can X dang KT dang can Trong mot so trng hp dang can va dang ket tua khac nhau 2Fe3+ + OH- Fe(OH)3 Fe2O3 Chat X dang KT dang can
SO42-

3/ Phng phap cat

Nguyen tac : Chng cat nh lng cau t can xac nh di dang hp chat bay hi. Phan can tach ra bang cach ot nong mau phan tch hoac bang tac dung cua thuoc th thch hp lam giai phong ra san pham bay hi. Co phng phap trc tiep va gian tiep.
PP.Trc

tiep: Cau t can phan tch c bay hi sau o hap thu vao chat hap thu phu hp, da vao s tang khoi lng chat hap thu ngi ta tnh c lng cau t can xac nh

du: Xac nh CO2 trong a cacbonat CaCO3 + H+ CO2 + H2O CO2 + 2NaOH Na2CO3 + H2O Mau Cacbonat c phan huy trong thiet b ac biet trong moi trng axt manh cho phep giai phong ra CO2. . Ham lng CO2 c hap thu vao hon hp dung dch CaO+NaOH. PP.cat gian tiep : Trong phng phap nay la xac nh phan con lai cua chat sau khi a tach hoan toan chat can xac nh.Hieu so trc va sau khi cat chat can xac nh ta se tnh c chat can xac nh V du: Tnh BaCl2.2H2O BaCl .2H O say kho BaCl + H O

 Nhng

u iem va nhc iem cua phng phap: - Xac nh o chnh xac cao at ti 0,01 0,005% vt xa o chnh xac cua chuan o - Xac nh c nhieu kim loai ( cation) va cac a kim ( anion), cac thanh phan cua hp kim, quang, silicat.. -Nhc iem: - Keo dai thi gian, khong kinh te nh ien tieu hao

Cach tnh toan trong phng phap trong lng Tnh lng can cua chat phan tch:
a/ ket tua dang tinh the V du : xac nh CaCO3 co trong mau cacbonat CaCO3 + 2H+ Ca2+ + H2O + CO2 Ca2+ + C2O42- Ca2C2O4 + CO2 Ca2C2O4 nung t0C CaO + CO + CO2 Rut gon: CaCO3 Ca CaO Tnh lc can phai can: MCaCO3 -----MCaO Xg ------- 0,5g Xg= 0,5x 100 = 0,9g 56 Vay oi vi ket tua tinh the dang can ( ket tua) nen co la 0,5g

b/

Ket tua dang vo nh hnh nh: Fe(OH)3 Khi nung len Fe(OH)3 Fe2O3 Vay lng can dang ket tua nen la 0,1g Cong thc tong quat: Ket tua tinh the : X = mMA.0,5/ nMA1 Ket tua vo nh hnh : X = mMA. 0,1/ nMA1

1/

Lay va hoa tan mau can Lng can cua chat phan tch cang ln, o chnh xac tng oi cua cac ket qua phan tch cang cao. - e tnh lng can can phai biet ham lng gan ung cua cau t - Lng can qua nho dan en sai so cang ln - Sai so cho phep can khong c vt qua 0,1% - S dung can co o chnh xac 0,0001g th lng can toi thieu co the can c vi o chnh xac cho phep la 0,1% - Neu can 1g vi sai so 0,0001g th sai so cho phep

KY THUAT PHAN TCH TRONG LNG

Neu can 0,1g sai so se la 0,1% Nh vay lng can toi thieu khong c nho hn 0,1g - Ham lng % cua chat can xac nh trong mau cang nho th lng can can phai cang ln 2/ Lay mau can e phan tch - Lay mau can chnh xac ong vai tro quan trong trong phan tch nh lng. - Tnh ung cua cac ket qua phan tch phu thuoc vao o chnh xac cua viec lay mau can phan tch

Neu mau la chat ran thng s dung coc thuy tinh, thuyen can bang kim loai, giay bac S dung muong inox nho e lay mau - Neu mau la chat long th dung ong nho giot e lay mau va cho vao coc thuy tinh e can - Neu mau la chat bay hi phai dung bnh nh mc nho co nut mai, hoac dung cu thuy tinh co nut mai e tranh bay hi cua mau. Trng hp s dung ngay coc can e x ly mau luon th tat ca dung cu lay mau phai c lam sach va say kho can trong lng khong trc sau o can mau . Hieu so cua trc va sau se la lng can

tan lng can : Mau sau khi can c hoa tan bang axt hoac nc cat trong coc thuy tinh chu nhiet hoac bang bat s nh phai ay bang nap knh ong ho , e mat lom quay xuong di. Ky thuat ket tua Phu thuoc vao chat nh ket tua dang nao th s dung thuoc th cho phu hp e ket tua c hoan toan. Lng dung moi : mau ran se c pha loang bang nc hoac hoa tan bang axt , tnh toan lam sao cho dung dch thu c co nong o khoang 0,1N
Hoa

Nh

vay trong dung dch co cha 0,1 ng lng gam chat can phan tch bang 1000ml The tch dung moi lat e hoa tan mau se la: 0,1g -------1000ml Xg -------Vml suy ra : Vml = 1000 a/0,1 = 100ml.Xg mau Ket tua cac ket tua tinh the : cac ket tua c ket tua khi un nong dung dch tren bep ien hoac bep cach thuynhng khong c un soi. Thuoc thu tao chat ket tua c nho t t va dung u thuy tinh khuay nhe sau o e nguoi va lang ket tu. Nho them vai giot thuoc th na neu khong thay tao ket tua th yen tam la ket tua a c hoan toan.

Ket

tua cua cac ket tua vo nh

hnh Nh Fe(OH)3, Al(OH)3 Ket tua cua cac ket tua vo nh hnh t dung dch nong, ac. Ket tua c tien hanh bang cach them nhanh chat ket tua e thu c ket co be mat nho nhat (tao bong cuc tap trung khong phan tan trong dung dch) Loc va ra ket tua Loc : Trong phan tch nh lng dung giay loc khong tro e loc ket tua Ra ket tua:

CAC IEU KIEN TOI U E KET TUA ieu kien ket tua dang tinh the
1/

Tien hanh ket tua t dung dch u loangbang dung dch thuoc th loang. Khi ket tua t dung dch loang se ket tua c tinh the ln hn 2/Them chat ket tua vao t t theo tng giot , neu cho vao nhanh se tao nhieu tam ket tua lam cho tinh the ket tua b nhuyen 3/ Khuay dung dch ket tua bang ua thuy tinh e tranh s qua bao hoa theo vung va tang ket tua ln 4/ Tien hanh ket tua bang dung dch nong se lam tang s ket tua ln

ieu

kien ket tua vo nh hnh Cac ket tua vo nh hnh co khuynh hng hap phu va tao thanh dung dch keo, do vay ket vo nh hnh dung dch nong , ket tua t dung dch ac khi o ket tua tao thanh de b co ac lai , de loc va de ra. Khi ket tua xong nen them mot the tch ln nc khoang 100ml muc ch cho phan hap phu ket tua chuyen vao dung dch tuy nhien khong nen keo dai va cho loc mau ngay

Cac phng phap tang o chnh xac cua phan tch trong lng
-

S giam o tan cua chat ket tua : them lng d thuoc th co cung ion cua chat ket tua. Tuy nhien khong nen dung lng d chat ket tua qua ln se an en s tao phc va lam tang o tan cua chat ket tua V du : BaSO4 neu ket tua Ba2+ th them SO42- va muong ket tua SO42- th them ion Ba2+ - Tm thuoc th ac trng cho phng phap muon xac nh, loai bo cac yeu to gay anh hng en qua trnh cong ket ket tua - Xac nh song song hai hoac ba mau e

Phan thc nghiem

Xac

nh ion Sunphat Nguyen tac : Da tren s ket tua BaSO4 khi cho ion Ba2+ tng tac vi SO4 co trong mau trong moi trng axt pH = 2 -3 Phng trnh phan ng BaCl2 + SO42- BaSO4+ 2ClBaSO4 nung 6000C BaSO4 + chat hu c bay hi Neu nung > 6000C BaSO4 BaO + SO3 Mot so anion gay can tr: SiO32-, SnO32- cung ket tua H2SiO3, H2SnO3 do o phai tach cac anion ngan can o ra trc , trc khi tien hanh ket tua SO42-

TNH TOAN LNG CAN

MNa2SO4

= 142,04 , MBaSO4 = 233,4 BaSO4 co cau truc tinh the nen lng can dang ket tua khoang 0,5g , vay lng can cho Na2SO4 = 0,5.142/233,4 0,3g mau Mau can va pha trong bnh nh mc en vach. 2/ Tnh lng BaCl2.2H2O cho vao mau e ket tua BaCl2.2H2O + Na2SO4 BaSO4 + 2NaCl+ 2H2O 242,2 ----- 142 X 0,3g X = 0,5g 1000 ml dung dch cha 121,1 BaCl2.2H2O

PHNG PHAP XAC NH SO4 TRONG THC PHAM Tnh ham lng SO4 co trong mau nc hoac thc pham co hai phng phap: 1/ Bang phng phap so mau 2/ Bang phng phap trong lng Nguyen tac cua phng phap ket tua va nung Vi ham lng SO4 trong thc pham t 0,5% tr len th dung phng phap trong lng Mau thc pham c xay nhuyen va can khoang 10g mau vao chen s cho vao lo nung nhiet o t 5500C 6000C.Dung H2SO4 loang chuyen cac chat khoang ve dang muoi sunphat

Tien

hanh th : Mau thc pham c xay nhuyen va can khoang 10g mau vao chen s at len bep ien than hoa mau sau o tro hoa cho vao lo nung nhiet o t 5500C 6000C nung trong 2gi cho en khi mau trang hoan toan. Lay mau ra e nguoi sau o hoa tan t nc, dung HCl hoa tan mau cho tan het va loc mau. S dung dch loc cho t t BaCl2 20% vao un nong nhe dung dch cho en khi mau ket tua hoan toan . Lay coc mau ra e qua em, hom sau loc bang giay loc bang xanh. Dung nc cat trang ra ket tua nhieu lan cho en khi het Clor th bang dung dch AgNO3.

Giay

loc cung chat ket tua c goi lai cho vao chen s nung loai nho at len bep ien than hoa, tro hoa trong lo nung nhiet o 5500C 6000C nung trong 30 cho en khi mau trang hoan toan. Lay chen s ra cho vao bnh hut am e nguoi va can ket tua.
Tnh

ket qua : BaSO4%= (G1 - G2 ).100.V.f m .Vm G1 : Chen khong + mau G2 : Chen khong V: the tch bnh nh mc M : lng can Vm : the tch hut mau % SO4 = %BaSO4 x MSO4 MBaSO4