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أساسيات الكيمياء التحليلية
أساسيات الكيمياء التحليلية
أساسيات الكيمياء التحليلية
W
K
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W
K
W K
KKKKK
E F
K
K
K
K
W
KW .
W
.
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KW .
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.
K
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--
W
W
K .
K .
W
K
W
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EF
EF
W
W K
K
WQualitative Analysis
FQualitative analysis
WKE
W
.
F
KE
W .
KKKK
K
WQuantitative Analysis
Quantitative analysis
Quantitative chemical analysisW
KQuantitative instrumental analysis
--
yY + xX P
XReagentY
KP
E FX
KVolumetric analysis
PX
KGravimetric
WK
E
. Atomic Absorption Spectrometry
Physico-chemical Methods
K2CrO4Cr3+
--
W
W
K .
K .
K .
K .
K .
K .
K .
W .
K K
K K
K K
K K
W .
K K
K K
K K
K K
K K
--
WSampling
Bulk
HomogeneousKMaterial
Heterogeneous
KEKKKF
WWater sampling
K
WEKKKF450EPyrexF
K24
PTFEWJ
Kpolytetrafluoroethylene
WKE45F
KBiodegradation 4
K(pH = 2)
WSoil sampling
E 10FE30F
E2 1F
KPolyethylene
--
WSample preparation
110100
WWeighingDrying K
KDessicator 21
K
WSample ashing K
EF
WEF
700400WDry ashing
K24
WWet ashing
SulfuricNitric acid
WSample dissolution K
K
K
--
EaF
KK2S2O5
EbF
KNa2CO3
EcF
KNa2O2
K
WEliminating interferences
.Electrodeposition
Ion ExchangeChromatography .
KExtraction
KMasking .
WMeasurements
K .
K .
K .
--
W
.
KAutomatic methods
Kmillion
Replicate analysesE F
KMeanStandard deviation
--
K
K K
K K
K K
K K
K K
K K
--
KEFEF
WEKKKFJ
450EPyrexF
K24
PTFEW J
Kpolytetrafluoroethylene
WKE45F
KEbiodegradationF4
K(pH = 2)
K
- -
W K
E
F
2. G.D Christian: Analytical Chemistry, 5th edition, John Wiley &Sons, Inc, International
edition, 1994.
3. G.H. Jeffrey, J. Bassett, J. Mendham, R.C. Denney: Vogel's Textbook of Quantitative
Chemical Analysis, 5th edition, Longman Scientific & Technical, 1989.
4. D.A. Skoog, D.M. West and F.J. Holler, Analytical Chemistry An Introduction,
Saunders College Publishing 6th edition, International edition, 1994.
- -
- -
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F
KE
W
W
K .
K .
.
K
K .
K .
W
K
W
K??
- -
W K
E
F
W
KEF
W
K
()
)
(
- -
WK
KEF .
KpH-meter
WEquivalence point
Stoichiometric
W
W
KE1:1FNaOHHCl
W
W
2NaOH + H2SO4 Na2SO4 + 2H2O
FNaOHH2SO4
KE2:1
- -
W K
K .
K .
KEF .
K .
W .
A+B C+D
WStandard solutions K
W
KPrimary standard .
KSecondary standard .
WPrimary standard
K
K .
K .
K .
K .
K .
K .
W
W .
KC6H5COOH K
WSecondary standard
EF
KStandardization
NaOH
NaOH
NaOH
KH2SO4
W K
W .
W
KAcid-base titrations .
KPrecipitation titrations .
KComplexometric titrations .
KOxidationreduction titrations .
- -
W K
E F
EFEF
E
F EF
M1 V1 = M 2 V2
W
0.1FH2SO4 NaOH10
W9E
K K
KNaOH K
W
K
K
number of mmoles of NaOH 2
=
number of mmoles of H 2SO 4 1
M NaOH VNaOH 2
=
M H SO VH SO 1
2
M NaOH 10 2
=
0.1 9
1
0.1 9 2
= 0.18 M
M NaOH =
10 1
- -
W
WMole
WEF
KW
.
58.49 .
158.04
NaCl
.
KMnO4 .
194.20
K2CrO4
40.00
NaOH
W K
K23=
K16=
K1=
40K 40=
KNaOH
W K
46=23C2=NaC2
12=12C1= CC1
48=16C3 = OC3
K106=
- -
W K
KOH-H+
NaOH + HCl NaCl + H2O
Na+ + OH- + H+ + Cl- Na+ Cl- + H2O
OH- + H+ H2O
W
KpH
pH-
Kmeter
W K
WArrhenius definition
Arrhenius
Arrhenius
KOH-
WBrnsted-Lowry definition
Brnsted and Lowry
KEF
H+
HA
H+
A-
BH+
HA +
BH+
A-
WLewis definition
W Lewis
Electron acceptor
KElectron donor
W
H3N: +
- -
W K
pH
K
W
0.150HCl
WK
K10090605551504840200
W
K0=NaOH
K0.1= HCl
pH = log[H + ]
pH = log(0.1)
pH = log(101 )
pH = (1) = 1
KNaOH20
WReacted HClmillimoles
Reacted HCl (millimoles) = 20 0.1 = 2 mmoles
KHCl
no. of HCl mmoles = 0.1 50 = 5 mmoles
- -
WHCl
no. of mmoles
volume(ml)
3
Molar HCl =
= 0.04 M
70
Molar HCl =
WpH
pH = log(0.043)
pH = (1.37) = 1.37
pH
WEFNaOH
NaOH + HCl NaCl + H2O
0
pH
20
40
60
80
100
14
14
12
12
10
10
(8.3-10)
(3.3-4.4)
2
0
0
20
40
60
( )
- -
80
2
0
100
NaOHHClW
Equivalence point
K
K10.73.3
KMethyl OrangePhenolphthaleinW
K
W K
KEFW
CH3COOH + NaOH CH3COONa + H2O
14
12
10
pH
6
4
2
0
0
20
40
60
80
( )
W
- -
100
WCH3COONa
CH3COONa + H2O
10.77.7
K
W K
KEFW
pH
4
2
0
0
20
40
60
80
100
( )
- -
H+
NH4Cl
NH4OH + H+ + Cl-
NH4Cl + H2O
K
W K
KEF W
CH3COOH + NH4OH CH3COONH4 + H2O
12
10
pH
6
4
2
0
0
20
40
60
80
100
( )
- -
KMethylene blueNeutral blue
W K
K
K
FW
E
K
W
A + B
C + D
FDCEFBAW
KE
W
v1 = k1 X [A] X [B]
v2 = k2 X [C] X [D]
k2k1
Wv1 = v2
k1 [ C][ D ]
=
k2 [ A ][ B]
Kk2k1
KChemical equilibrium constant
W
cC + dD
aA + bB
Kdcba
[ C] [ D]
K=
[ A ] [ B]
c
W
Le ChatelierK
KW
W
W
H+
HIn
EF
In-
EF
- -
K In =
[H + ] [In ]
[H In ]
KOH-H+
W
KH+H+
KEFln-
H+
+ In EFH+EF
HIn
HIn H+ OH-
KEF
H+
+ In EFOH-EF
HIn
W
K
W
W
OHIn
OH-
- -
In+
OH-H+W
In+ OHIn
In+OH-W
OHIn
K
W
K
W
.
. .
2.9 . Methyl .
4.0
yellow
3.1 . Methyl .
4.4
orange
6.8 . Phenol .
8.4
red
.
.
.
Phenolphthalein
7.2 . Cresol .
8.8
red
8.3 .
10.0
- -
Precipitation Titrations
W K
BAK
KC,
A + B C + D
Silver nitrate, AgNO3
W K
K
Mohr's W
Chromate ion,CrO42-
K E
KEF
- -
Ag+
Cl-
Cr2O42-
KMohr's methodW
E F
K
E F
K
(1)
EFEF
E2FE1FK
- -
(2)
W
WpH = 8
.
.
K
K
Fe3+
W
KEF
- -
SCN-
Ag+
Fe3+
KW
E F K
KAg+
-
SCN + Ag AgSCN
(3)
Ag+
WEFFe3+
Fe3+
+ SCN-
Fe(SCN)2+
(4)
KEFE3F
W
Chloride, Cl-Halides
KEF
- -
K
KBack titration
W
SCN- + Ag+ EF AgSCN (s)
WEF
W
W
F W
0.1234E
12.2E F
MillimolesK0.930Molarity
K300
- -
W
W
aA
EF
bB
EF
cC
EF
+A
()
EF
+
dA
EAF
()
WBA
Number millimoles A = ( volume A Molar A ) ( volume C molar C
Number millimoles B = number millimoles A
b
a
b
Number millimoles A atomic weight A 100
a
%B =
Sample weight
KWCWBWAW
W
Number millimoles AgNO3 = ( 40 0.1234 ) (12.2 0.093)
Number millimoles AgNO3 = 4.94 1.13
Number millimoles AgNO3 = 3.81 millimoles
W
1
1
Number millimoles Cl = 3.81 millimoles
- -
W
3.81 35.4 100
300
% Cl = 44.96%
% Cl- =
WFajan's method
F
Fluorescein indicatorE
KEF
Ag+
Cl-
In-
KW
KIn-
- -
Cl- W
Adsorbed
KEF
Cl- Cl- Cl- Cl- Cl- Cl- Cl- Cl- Cl- Cl- Cl- Cl- Cl-
Na+
Na+
Na+
Na+
Na+
Na+
Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+ Cl-Ag+ ClCl- Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+
KW
AgCl
Ag+
KEFIn-
In- In- In- In- In- In- In- In- In- In- In- In- In+
Ag Ag Ag Ag Ag Ag Ag Ag Ag Ag
Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+ Cl-Ag+ ClCl- Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+ Cl- Ag+
KW
- -
Reduction-Oxidation Titrations
W .
K
K
EFW
EFEF EF EF
K
EFEFW
2+
Zn Zn + 2e
W
WReduction
K
Cu2+ + 2e- Cuo
- -
WReducing agent
Bred Box + ne
WOxidation number .
S2-Fe2+
WK
KS8P4,Ar, Cl2
Peroxides)(2-)
K(1-)
KH2O, Fe2O3W(2-)
H2O2, Na2O2W(1-)
K(1-)(1+)
KH2S, NH3W(1+)
BaH2, LiHW(1-)
- -
KClO4- Cl W
KCl=x
(4*-2) + x = -1
(-8) + x = -1
x = +7
KCr2O72- Cr W
KCr=x
(2x) + (7*-2) = -2
2x 14 = -2
2x = -2 + 14
2x = +12
x = +6
WHalf-reactions .
W
Fe3+ Fe2+
Fe3+ + e- Fe2+
Cl2 ClCl2 2ClCl2 + 2e- 2Cl-
W
WPermanganate ion (MnO4-)J
MnO4- Mn2+
MnO4- + 8H+ Mn+2 + 4H2O
MnO4- + 8H+ +5e- Mn+2 + 4H2O
- -
Cr2O72- Cr3+
Cr2O7-2 + 14 H++ 6e- 2Cr3+ + 7H2O
Cr2O7-2 +14H++ 6e- 2Cr3+ + 7H2O
W
WW
(i)
(ii)
W(ii)(i)
WW
MnO4- Mn2+
Fe2+ Fe3+
+
2+
MnO4 + 8H + 5e Mn + 4H2O
Fe2+ Fe3+ + e-
W
(i)
(ii)
W(ii)
(iii) 5Fe
2+
3+
5Fe + 5e
W(iii)(i)
MnO4- + 5Fe2+ + 8H+ Mn2+ +5Fe3+ +4H2O
WW
MnO4- Mn2+
C2O42- CO2
- -
2+
MnO4 + 8H + 5e Mn + 4H2O
C2O42- 2CO2 + 2e-
W
(i)
(ii)
W(ii)(i)
2MnO-4 + 16H+ + 10e- 2Mn2+ +8H2O
5C2O42- 10CO2 + 10e-
(iii)
(iv)
W(iv)(iii)
2MnO4- + 5C2O42- + 16H+ 2Mn2+ + 8H2O +10CO2
WW
Cr2O72- Cr3+
Fe2+ Fe3+
W
Cr2O72- + 14H+ + 6e- 2Cr3+ + 7H2O
Fe 2+ Fe3+ + e-
(i)
(ii)
W(ii)
(iii)
W(iii) (i)
Cr2O72- + 6Fe2+ + 2Cr3+ 7H2O + 6Fe3+
- -
W .
KCe4+100Fe2+100
KNernst equation
RT [Ox ]
ln
nF [Re d ]b
a
E = E0 +
[Ox ]
0.0591
log
n
[Re d ]b
a
E = E0 +
K=E
K=E0
8.314 JK-1mol-1=R
K=[Ox]
K=[Red]
K96485 C (coulombs)=F
K=T
Klog2.303==ln
K=n
WCe4+ Fe3+
- -
WFe2+Ce4+10
E = 0.75 + 0.0591log
10
90
E = 0.69V
WEF
1.5
E, Volt
1.3
1.1
0.9
0.7
0.5
0
20
40
60
80
Cerium (IV), mL
Ce4+W
W .
WPotassium permanganate
%2
StandardizationK
KFe2+
K
- -
W(i)
W (ii)
MnO4-
W(iii)
MnO4- + e- MnO42-
W
K1500 .
K .
F .
E
K .
.
K
E F .
K
WCerium (IV)
Ce4+ + e-
Ce3+
- -
Sn
K, H2O2 , Fe , V , Mo, W , Ti , U
WPotassium dichromate
K2Cr2O7
KEF
K
WPotassium bromate
KBrO3
WBr2
BrO3- + 5Br- + 6H+ 3Br2 + H2O
Br2
KBr
K
WKI
-
2I + Br2 I2 + 2Br
Na2S2O3
K
- -
WIodine
WI3-Potassium iodide, KI
I2 + I -
I3-
KW
WDirect methods
As(III)
SO32-H2SSn(II)Sb(III)
K
WIndirect methods
KI
Aox + I- Ared + I2
KA
W
I2 +
2S2O32-
2I +
S4O62-
KCr3+Cu2+ClO-Br2Cl2Cr2O72-
W
Cr2O72-Cr3+0.2
E
I-FKI
- -
0.1SCN-
KK22.15
W
+
Cr2O72-
3+
(i)
(ii)
W3C(ii)
(iii)
K KI-EiiiF
W
(iv)
(v)
WEvFEivF
2-
2-
2S2O3 + I2 S4O6 + 2I
(vi)
W
2Cr3+ Cr2O72- 3I2 6S2O32Cr
2
1
3+
:
:
:
S2O32-
6
3
- -
KS2O32-
22.15
0.1
1000
moles = 2.215 103 moles
KCr3+
1
number of Cr 3+ moles = number of S2O3 2- moles
3
1
number of Cr 3+ moles = 2.215 103
3
3+
number of Cr moles = 7.38 10 4 moles
Cr 3+ (%) =
Cr 3+ (%) =
Cr 3+
WIron (II)
Fe2+Fe(NH4)2(SO4)2.6H2O
0.5F
KE
- -
Fe2+
K
WPotassium thiosulfate
WNa2S2O3
K .
K .
WS4O42-
K
WRedox titration indicators .
K
K
WSelf indicator
KMnO4
WMn2+Fe2+
+
+2
E FFe2+E F
Mn2+MnO4-
- -
MnO4-Fe3+Fe2+F
KMnO4-
WSpecific indicators
K
E F
K
EFFe3+KSCN-
E FTi3+
Ti3+Fe(SCN)2-
W
Fe3+SCN-Fe3+
W
Fe (SCN)
2+
3+
Fe
+ SCN
E F
K
K
-
Inox + ne Inred
EFEF
E = E 0In
[ In ]
0.0592
log red
n
In ox
- -
EF(II)10,1
K(Phen)3Fe2+
N
Fe
2+
(II)10,1W
1.06 V
(Phen)3Fe3+ + e-
W
K
KE
EFCe4+Fe2+
1.10 V
KEF(II)10,1
- -
+1.1V
II{
+0.85V
+0.28V
E0ln
- -
W
Complexometric Titrations
W .
Complexing
agent
KELFLigands
L
KKMLn
EDTA
K
W .
Lewis acidK
KLigands Lewis base
WUnidentate ligands
: NH 3 H 2 O :
HN3: + M H3N: M
- -
WBidentate ligands
K
EFEthylenediamine
ChelationKEF
KChelating agents
H2
C H2
KEthylenediamineW
H2
C H2
N
H2
N C
Co
N C
H2
H2
H2
- -
WPolydentate ligands
HOOCCH2
N
CH2
CH2
N
CH2 COOH
HOOCCH 2
W .
EDTA .
KWEDTA .
M2+ + H2Y2-
MY2- + 2H+
FNa2H2YH4Y .
KEDTA E
- -
CH2COONa
HOOCCH2
N
CH2
CH2
N
CH 2 COONa.2H2 O
HOOCCH 2
Na2H2YW
WEDTA .
EDTA
K
KpH
KKMYEF
- -
KMYEDTAW
KMY .
KMY .
KMY .
5.0 .
4.2 .
1.0 .
Bi3+ .
Ca2+ .
Ni2+ .
10
18
23
x 10
x 10
x 10
4.9 .
3.2 .
1.3 .
Mg2+ .
Zn2+ .
Fe3+ .
8
16
25
x 10
x 10
x 10
MY
K Y
M + Y
H+}~
HY, H2Y,
MY
W Y
K
KFe3+Bi3+
KBuffer solutions
- -
W .
EDTA
K .
K .
K .
KKMEDTA>>KInd .
WEriochrome black TK
KEFErio-T .
KNaH2D .
W .
pH = 6.3
pH =11.6
2