02-412-106

.
2557


(Basic of analytical chemistry laboratory)

1. (significant figure)




2

1.6
1
6
0.1

1.68
1 6
8
0.01

(scale)

1.1
-

2.76 2 2 7 6
3
-
108 3 1 0 8

2 |

0.501 3 5 0 1

0.0050003 5 5 0 3
3
-

8.0
2
2.50
3
0.0050000 5
1.2

) 5 2.78
2 8 8 5 2.78 = 2.8
) 5 2.72 2
2.7
) 5
(1) 5 5 2.85 = 2.8
(2) 5 5 2.75 = 2.8

2.65834 2 5 6
8, 3 4 2.65834 = 2.65 = 2.6
1.3
1.3.1
(absolute
uncertainty)

1.3.2

8 10

(uncertainty)

 | 3

(relative uncertainty)

2.
2.1
(precision)


(average standard deviation)
( x )

SD=

(x -x)
i

n-1

(1)

xi
x
n

1
(mol/L)

(mol/L)
1
0.12
0.00
2
0.15
0.03
3
0.10
0.02
0.37/3 = 0.12
= 0.05/3 = 0.02
= 0.12 0.02 mol/L 0.02 mol/L
3
2.2
(accuracy)
(experiment value) (true accepted value)

4 |

(error)

(relative error)


2.3
(error) (true value, )
(accepted value)
(absolute error, AE)
(relative error, RE)
(absolute error)

absolute error = x i -
(2)

absolute error = x -
(3)
(relative error)

%relative error =

x-
x 100

(4)

 | 5

3.



(function) (line graph)
(linear) (non-linear)
(best-fit line)

microsoft excel

1) (x) (y)
2) x y
3) ()
4)
5) ( 1)
6) (best-fit line)
( 2)
7) y (y-intercept)
y

()
()
1 () () (bestfit line)

6 |

3.1 (linear curve)

Ax + By + C = 0 A, B , C
A B 0 (two variable linear
equation)
y = mx + b
(5)
y y 2 -y 1
m (slope)
=
x x 2-x 1
b y (y-intercept) y (0, b)

y


(Laboratory technique)

1.
(filtration)

Whatman

1
2
3
4
5
40
41
42
43

Qualitative
Qualitative
Qualitative
Qualitative
Qualitative
Quantitative (Ashless)
Quantitative (Ashless)
Quantitative (Ashless)
Quantitative (Ashless)

Medium crystalline
Crystalline
Coarse and gelatinous precipitate
Crystalline
Crystalline
Crystalline
Fine crystalline
Fine crystalline

Ashless

2
1) 1/4 1/4

3 ()
2) 1/16 3 ()

8 |

()

()
3 () () (fluted)
) (vacuum filtration)
suction
buchner funnel filter pump aspirator 3
4 buchner funnel
vacuum filter flask

 | 9

1)
5 ()







()

2) (sintered glass)



0-5 3
4
()
4 (BaSO4)
5 () ()
2.

2 transfer pipet measuring pipet
6
1. Transfer pipet transfer pipet 25 mL
25 mL transfer pipet 1 mL 100 mL

2. Measuring graduated pipet

transfer pipet transfer pipet

10 |

1 blow-out pipet
2
3
4
5 (A B)
6
7
6 transfer pipet volumetric

1.
2.
3. ( 7)

()

 | 11

4.

5.

3. (titration)

(buret) -
stop-cock
10 mL 100 mL

()

()
titrant

titrand

8 () ()
8()

(titrant)
(titrand) stop-cock

12 |

1.
2.
stop-cock
3. 5
mL
4.
( 10)


(

)
5.
stop-cock


( 11)
6. stop-cock

stop-cock


7.

8. 2
0.2 mL
0.2 mL
3

10

11
stop-cock

(Reagents and preparation)

1.
(reagent)

1) ACS reagent
(American Chemical Society ACS)

2) (analytical reagent (AR)/reagent grade) 99%

(ACS)
AR (ACS) reagent
3) USP U.S. Pharmacopoeia

4) purified/practical grade

5) C.P. (chemical pure) (reagent
grade)
6) (lab practical) 95%

7) NF National Formulary (NF)

(impurities)

8) (technical commercial)

(impurity)

14 |

1. (chemical name)
2. (formula weight, formula structure)
3. , (molecular weight- Mr, MT, M.W., F.W.)
4. (grade- AR, lab, technical)
5. (company suppliers)
6. (% assay)
7. (impurities)
8. (catalog number)
9. (risk phrases) (safety phrases)
10.
11. (hazard pictogram)
12.





1.

2.

3.
4.

 | 15

12
A =
B =
C =

D =
E =
F =

G =
H = Lot. NO.
I =

J =
L = ,
O = MSDS

13 Trifluoroacetic acid

16 |

(Material Safety Data Sheet, MSDS)

MSDS
MSDS
( )


MSDS
16
1.
2. /
3.
4.
5.
6.
7.
8. /
9.
10.
11.
12.
13.
14.
15.
16.

MSDS (SG)

1. MSDS (
MSDS )
2.
3. MSDS
http://msds.pcd.go.th,
http://www.msds.com, http://www.chemtrack.org

 | 17

(Hazard pictogram)

(European Economic Council, E.E.C)
NFPA (National Fire Protection
Association)
1.

EEC 67/548/EEC

14

14 EEC
2. (UN)
(International Maritime Organization, IMO) ()
9
45 15

15 UN
3. NFPA (National Fire Protection Association)

18 |

16 NFPA
4
0-4 4
Diamond Shape
4
(Flammability)
(Health)
(Reactivity)
()
() 0 4 0
4

 | 19

2.





0.0001
(volumetric flask) (measuring pipet)
2.1

W (g)
MW (g/mol)
W (mg)
mmol =
MW (g/mol)

1 L = 1 dm3 = 1000 mL = 1000 cm3

mol =

(6)
(7)
(8)

2.2
2.2.1 (percentage) 3
1) (%w/w)
100 (%w/w)
(g)
%w/w =
x 100
(9)
(g)
15%(w/w) NaCl NaCl 15 85
2) (%w/v)
100 mL (%w/v)
(g)
%w/v =
x 100
(10)
(mL)
5% (w/v) KCl KCl 5 100 mL
3) (%v/v) mL
100 mL

20 |

%v/v =

(mL)
x 100
(mL)

(11)

30% v/v ethanol 100 mL 30 mL

2.2.2 (molarity, molar, M)
1 (1000 mL) (mol/L)
(M) =

(12)

0.5 M NaOH 1 NaOH 0.5

2.2.2 (normality, normal, N) (equi. gram)
1
(N) =

(13)

1 N HNO3 1 HNO3 1

(equi. gram) =

(14)

(15)

(equi. wt.) =
H equivalent H

-
Al2(SO4)3 = 2x3 = 6
- H+ OH- H2SO4 = 2
KOH = 1
-

 | 21

1 0.10 N Na2S2O35H2O 100 mL

0.10 N Na2S2O35H2O 1000 mL Na2S2O35H2O
0.10
Na2S2O35H2O = 248.18 g/mol
248.18 (g/mol)

equi. wt. =
= 124.09
2
W (g)

0.10 equi. gram =

124.09
W (g) = (0.10 equi. gram)x(124.09) = 12.409
1000 mL Na2S2O35H2O 0.10 = 12.409 g
100
100 mL Na2S2O35H2O = 12.409 x
= 1.2409 g
1000
Na2S2O35H2O 1.2409 g 100 mL
2.2.3 (part per million, ppm)
(ppm = mg/kg mg/L)
ppm =

(g)
x 106
(g)

(16)

ppm =

(g)
x 106
(mL)

(17)

2 100 ppm Fe3+ 100 mL FeCl3 (MW.=162.2

g/mol)
gsolute
ppm =
x 106
mL solution
(100 ppm)(100 mL)
gsolute =
= 0.010 g
106
Fe3+ 0.010 g
FeCl3 162.2 g Fe3+ = 55.9 g
162.2 x 0.010
Fe3+ 0.010 g FeCl3 =
= 0.0290 g
55.9
FeCl3 = 0.0290 g 100 mL

22 |

2.2.4 (dilution ratio)

2 : (A : B)
(A) (B)
HCl (1:1)
2.3

( /mL)
(conc.)

2
conc. HNO3 MW = 63.01 g/mol (d) = 1.420 g/mL
= 70% (w/w)
HNO3
m
m
(d) = 1.420 g/mL d = v =
d
v
1g
= 0.7042 mL
HNO3 1 g =
1.420 g/mL
HNO3 100 g = 0.7042 x 100 = 70.42 mL
70% (w/w) HNO3 100 g HNO3 70 g
HNO3 70 g mol
70 g
mol HNO3 =
= 1.11 mol
63.01 g/mol
HNO3 70.42 mL HNO3 1.11 mol

1000
HNO31000 mL HNO3 = 1.11 mol x
= 15.8 mol/L
70.42

70% 1000 mL 1.420 g 1 mol
M=

= 15.8
100% 1 L 1 mL 63.01 g/mol
HNO3 15.8 mol/L

 | 23

2 -

(glacial)

(g/mol)

(g/mL)

H2SO4
HNO3
CH3COOH
HCl
HCOOH
H3PO4

98.08
63.02
60.05
36.46
46.03
98.00

1.84
1.42
1.05
1.18
1.205
1.70

NH4OH

35.05

0.9015

H2O2

34.02

%w/w

(mol/L) approx.

95.95
71.01
99.6
37.08
90
85
30 (NH3),
58 (NH4OH)

18
15.8
17
12
23.6
14.7

30

2.4
1)

W (g) 1000 (mL)

(18)
M (mol/L) =

MW (g/mol) V (mL)
M = (mol/L)
W = (g)
MW = (g/mol)
V = (mL)
3 AgNO3 0.1 mol/L 250 mL
250 mL
W(g) = 0.1 mol/L x 169.87 g/mol x
1000 mL
= 4.25 g
AgNO3 0.1 mol/L 250 mL AgNO3 4.25
250 mL

24 |

2)

(M, mol/L)

M1V1 = M2V2
(16)
V1 = A (mL)
V2 = B (mL)
M1 = A (mol/L)
M2 = B (mol/L)
4 0.5 M HNO3 100 mL 70% (w/w) HNO3
HNO3 15.8 mol/L
2 0.5 M HNO3 100 mL 15.8 mol/L HNO3
M1V1 = M2V2
0.5 mol/L x 100 mL
V1 =
= 3.16 mL
15.8 mol/L
conc. HNO3 3.16 mL 100 mL

(Gravimetric analysis)

(gravimetric analysis)

2
(precipitation) (volatilization)
(precipitation)
(10-20%)
100 (macro quantitative analysis)



(weighing form) (S)
(BaSO4)

1.
2.

3.
4.
5.

6.
7.

26 |

- (precipitant)
-
-
-

Ba2+(aq) + SO42-(aq) BaSO4(s)

BaSO4 SO42-

g gfw.SO
SO 2- =
4

BaSO4

gfw.BaSO4

gfw.SO42
gravimetric factor (GF)
gfw.BaSO4
g x GF
% SO42- = BaSO4
x 100
sample (g)

2-

 1 | 27

(volatilization)


NaHCO3
H2SO4
2NaHCO3(aq) + H2SO4(aq) 2CO2(g) + 2H2O(l) + Na2SO4(aq)
2
1) (direct method)

2) (indirect method)

w i-w f
x 100
wi
wi = ()
wf = ()

(%) =

28 |

1.1

1)
2)

BaCl2
(digest)
Ba2++ SO42- BaSO4 BaSO4(s)
(BaCl2)

()

()

BaCl2

1) 4
2)
3)
4)

- (5 % w/v BaCl2)
- (0.1 M AgNO3)
- (conc. HCl)

1.
105C 1
2. 0.30-0.35 400
mL
3. 25 mL conc. HCl 0.5 mL ( 10 )
200-250 mL
4. hot plate BaCl2 10-12 mL

5. 2-3 BaSO4
BaCl2

 1 | 29

BaCl2 3 mL
BaSO4
() 1
6. 42 (
) (
AgNO3 )
7. 1.1

1.2

1.1
8.
( 1.2)

600C 1
9.

10.

30 |

1.2

1)
2)

(moisture content)

(dehydrating agent)
(total volatile matter)
(total solid)

(hot air oven method)

1) 4
2)
3)
4)

1)

1) 105C 30-60
2)
3) 2.xxx
4) ( ) 105C 3

5) () 30
6)
7) 30

(Preparation and standardization of reagents)

( )

1. (%)
1) (%v/v) 100

mL
%v/v = solute x 100
mL solution
2) (% w/v) 100

g
%w/v = solute x 100
mL solution
2. (molarity, M) 1 L
mol
gsolute
M = solute =
1000 mL (MW.)x1000 mL
(mol/L) (mol/dm3)

(18) ( 23)
3. (formal, F) 1 L
mol
gsolute
F = solute =
1000 mL (FW.)x1000 mL
4. (molal, m) 1
mol
gsolute
m = solute =
1000 g (MW.)x1000 g

32 |

5. (normal, N) 1 L
( 20)
equi. molsolute
equi. gsolute
N=
=
1000 mL (MW.)x1000 mL

2
1)

2
2

1.

2.

standardization
2)

(4 )

(volumetric flask)

1)
2)
3)

 2 | 33

4)

2.1

(standardization)
(secondary standard)
(primary standard)

34 |

aA + bB cC + dD
A
A titrant ()
B titrand ()
b x mmolA = a x mmolB
a
mmolA = mmolB
b
a mgB
MA VA =

b gfw.B
a mgB
MA =

b VA x Mw.B
M mol/L
V mL
Mw.

 2 | 35

2.1 : NaOH

1)
2) NaOH

1) (NaOH) (Mw = 40.0 g/mol)

2) 0.1% (w/v)
phenolphthalein 0.1 30 mL 70 mL
()
3) (KHC8H4O4, KHP) (Mw. = 204.224 g/mol)
110C 2 ()

1. NaOH
NaOH 2 ( 2 ) 500
mL ( ) (
) (** )
2. standardization NaOH
1. KHC8H4O4 0.5xxx g 50 mL 25.00 mL (
25 mL) ( 2 )
2. 2-3 25 mL
3. NaOH
NaOH ()
4. NaOH

KHC8H4O4 + NaOH KNaC8H4O4 + H2O

36 |

2.2 : HCl

1) HCl
2) HCl

- 36%(w/w) HCl (Mw.=36.46 g/mol, d=1.18 g/mL)

- Methyl orange ()
- Na2CO3 (Mw.=106) 120C 2

1. HCl
conc.HCl 3.0 mL 250 mL 147 mL
* 600 mL
**
2. standardization HCl
1. Na2CO3 ( 110C 2 .) 0.0132 50 mL
25.00 mL ( 25 mL) ( 2 )
2. Methyl orange 2-3
3. HCl
HCl ()
4. HCl

Na2CO3(aq) + 2HCl(aq) CO2(aq) + 2NaCl(aq) + H2O(l)

2 HCl 1 Na2CO3

 3
-

(Acid-base titration)

(titrimetric analysis) (volumetric analysis)

- (neutralization)
(precipitation)
(complexation)
- (oxidation-reduction)

(analyte) (titrant)
(standard solution)
+
(equivalent
point)
(stoichiometry)

=

= (stoichiometry ratio) x
stoichiometry ratio
(indicator)

(end point)

38 |

1. (99.9%)

2.
3. (side reaction)

4.

 3 - | 39

3.1 :

1. -
2.

1.
2. NaOH ( 2.1)

1.
10.00 mL () 100 mL
dilution factor
2.
1 NaOH ( 2.1)
2 (%w/v)
1. 25.00 mL 250 mL
2. 2-3
3. NaOH
NaOH
()

CH3COOH(aq) + NaOH(aq) CH3COONa(aq) + H2O(l)

40 |

3.2 :

1. -
2.

1. ()

1 HCl ( 2.2)
2
1. 0.25 - 0.35
50 mL ( 2 )
2. HCl 2.2
3.

Na2CO3 + 2HCl CO2 + 2NaCl + H2O

(Titrimetry)

1) (precipitation titration)
2) (redox titration) -

3) (complexometric titration)
EDTA
eriochrome black-T

(precipitation titration)
(insoluble precipitate)
(very slightly soluble substance)


(Ag+)
(argentometric
method)
(Cl-), (Br-), (I-)
(SCN-)

(Ksp)

BA ( )
B+ A-
BA(s)
B+(aq) + A-(aq)

Ksp = [B+][A-]

42 |

Ag+ Cl- AgCl AgCl

Ag+ Cl-
AgCl(s)
Ag+(aq) + Cl-(aq)

Ksp = [Ag+][Cl-]
Ksp (solubility product constant) Ksp
Ksp

1) (ion product)
Ksp (
)
< Ksp
= Ksp
> Ksp

1.

2.
3. 2

- (oxidation-reduction reaction)
(redox reaction) ()
( )

2
(oxidation reaction)

Fe2+(aq) Fe3+(aq) + e-

 4 | 43

(reduction reaction)

MnO4-(aq) + H+(aq) + 5e- Mn2+(aq) + 4H2O(l)

complexing agent
physical method chemical method

gravimetric method


1)
2)
3)
(Kf)
4) sharp end point

5)

(ligand) (chelating agent) (complexing agent)

- (central atom)

- 1
(unshared pair of electron) ligand
(NH3)
- O, N, X (halogen) S
- -NH2 COO-
- lewis base

44 |

4.1 : Mohr

1)
2)

0.15-10 (AgNO3) (titrant)
(Cl-) (K2CrO4) Ag+
Ag+ CrO4 AgNO3 NaCl
(AgCl)
Ag+ (aq) + Cl- (aq) AgCl(s)
AgCl
Ksp = [Ag+][Cl-] = 1.6 x10-10)
(end point)
(CrO4-) (Ag2CrO4)

indicator error blank

AgNO3
Ag+
CrO4- Ag2CrO4
2Ag+(aq) + CrO42-(aq) Ag2CrO4(s)
()

1. AgNO3 (MW=169.87 g/mol) AgNO3 2.39x 50 mL

1000 mL
2. NaCl (MW=58.44 g/mol) NaCl 0.8240 ( 120C 2
.) 50 mL 1000 mL

 4 | 45

3. (K2CrO4) K2CrO4 4.00 100 mL

AgNO3 12

4. 2 mol/L NaOH
5. 0.1 mol/L H2SO4

1 AgNO3
1.1 NaCl 10 mL 250 mL
1.2 K2CrO4 0.5 mL (10 )
1.3 AgNO3
AgNO3 ()
()
2
2.1 100 mL 250 mL (.
) 3
2.2 7-8 1 mol/L NaOH 0.1 mol/L H2SO4
2.3 K2CrO4 1 mL (20 )
2.4 AgNO3 ()
3 Blank
2 100 mL ( Blank
0.2-0.4 mL)
Cl - (mg/L)=

A-B N 35450
mLSample

A = AgNO3
B = AgNO3
N = AgNO3
(Cr)
Cr3+/Cr6+

46 |

4.2 :

1)
2)

(dissolved oxygen, DO)

14.6 mg/L 0C 7 mg/L 35C

1
(DO meter)
()
(azide modification of iodometric method)

(redox reaction)

(Mn(OH)2)
MnSO4(aq) + NaOH(aq) + O2(g) Mn(OH)2(s)

Mn(OH)2 (I2)
Mn(OH)2(s) + 4H+(aq) + 2I-(aq) Mn2+(s) + I2(aq) + 3H2O(l)

(Na2S2O3)
I2(aq) + 2S2O32-(aq) 2I-(aq) + S4O62-(aq)

1. 300 mL

1. (manganese sulfate) MnSO44H2O 48.0

100 mL ()
2. (alkaline-iodide-azide) NaOH 50 NaI 13.5
100 mL (NaN3) 1 (
4 mL) ()

 4 | 47

3. 1.6 0.2 100 mL

4. 0.025 N Na2S2O35H2O (MW=248.18 g/mol)
Na2S2O35H2O 3.10xx 50 mL NaOH
0.4 1000 mL
5. 0.025 N KH(IO3)2 (MW=398.92 g/mol)
KH(IO3)2 4.986 ( 105C) 50 mL
1000 mL

1 Na2S2O3
1. KI 2 50 mL 250 mL 100 mL
2. conc. H2SO4 0.5 mL 1 mL
2. KH(IO3)2 20 mL
3. Na2S2O3
1 mL (20 )

4. Na2S2O3 ()
5. Na2S2O3

IO3(aq) + 6H3O+(aq) + 5I-(aq) 3I2(aq) + 9H2O

2S2O32-(aq) + I2(aq) S4O62-(aq) + 2I-(aq)
3
(1)
mol I2 = mol IO31
1
(2)
mol I2 = mol S2O322
1
3
mol S2O32- = mol IO32
1
6
mol S2O32- = mol IO31
6 MK(IO ) x VK(IO3 )2
MNa2S2O3 = 3 2

1 VNa2S2O3

(1)
(2)

48 |

2
1. BOD ( )
2. MnSO4 1 mL 1 mL
BOD (
) 15

Mn2+(aq) + 2OH-(aq) Mn(OH)2(s)
(4.1)
Mn(OH)2 (IV)
(MnO(OH)2)
Mn(OH)2(s) + O2(aq) MnO(OH)2(s)
(4.2)
3. (
)
4. conc. H2SO4 1 mL
(IV) (I-)
(I2)
MnO(OH)2(s) + 4H+(aq) + 2e-(aq) Mn2+(aq) + 3H2O(l)
(4.3)
I (aq) I2(aq) + 2e
(4.4)
+
2+
MnO(OH)2(s) + 4H (aq) + 2I (aq) Mn (s) + I2(aq) + 3H2O(l)
(4.5)
5. 201 mL ( 100 mL pipet 1 mL)
250 mL
6. Na2S2O3
1 mL (20 )

I2(aq) + 2S2O32-(aq) 2I-(aq) + S4O62-(aq)

(4.8)
7. Na2S2O3 ()
8. ( mg/L)

 4 | 49

4.3 :

1)
2)

Ca2+ Mg2+ Al3+, Fe2+, Mn2+,
Sr2+, Zn2+ Ca2+ Mg2+
Ca2+
Mg2+ (mg/L ppm) (CaCO3)
, , 0-75, 75-150,
150-300 300 mg/L as CaCO3

ethylene diamine tetraacetic
acid (EDTA) eriochrome Black-T
EDTA

pK1=2.0, pK2=2.67, pK3=6.16,
pK4=10.26 EDTA H4Y
4.2
4.2 EDTA
EDTA
EDTA
4 EDTA 6
EDTA hexadentate ligand
1:1 (1 EDTA : 1 )
Ca2+ +

2 H2NCH2CH2NH2
(EDTA)

EDTA

eriochrome black-T

50 |

1. (ZnO)
ZnO 0.2000 ( 105C 1 ) 50 mL
4 mol/L HCl 250 mL

2. EDTA (MW=372.24 g/mol)

Na2EDTA2H2O 3.725 ( 80C 1 )
700 mL NaOH ( 5 )
1000 mL
3. 1% w/v eriochrome black-T eriochrome black-T 1.0 100 mL (20:20:60
v/v ethanol : ethanolamine : H2O)
4. pH 10 (NH4Cl-NH3) NH4Cl 6.8
57 mL 100 mL

1 EDTA
1. ZnO 25.00 mL 250 mL
2. NH3 Zn(OH)42+ NH3
( Zn(NH3)42+) NH3 2 mL
3. eriochrome black-T 2-3
4. EDTA
Zn2+ + Y4- ZnY21 Zn2+ 1 EDTA
2
1. 100 mL 250 mL 2 mL
2. eriochrome black-T 2-3 ( )
3. EDTA
4. ( mg/L as CaCO3)

molEDTA x MW.CaCO3
(mg/L as CaCO3) =
x106
Volume of sample

(Potentiometric titration)

(potentiometric method)

-

(glass electrode) H3O+ Ag/AgCl
CI- Ag+
- pH meter pH

5.1
-


-
1. (titration curve)
pH
(pH jumped)
HCl NaOH 5.2
( A)

52 |

() B

pH

NaOH (mL)
5.2 HCl NaOH
2. (derivative curve)
pH (pH/v)
HCl NaOH
(derivative) 5.1
5.3
5.2 pH

(first derivative)
dpH pH

dV
V

1
5.3 ()
2 (second derivative)

d(

dpH
)
2
2
dv d pH pH 0
dv
(dv) 2
( v) 2

2
2 5.3 ()

 5 | 53

- 1
2

5.1 1 2 0.05 M HCl 0.1010 N NaOH

4.00
8.00
10.00
11.00
11.50
11.60
11.70
11.80
11.90
12.00
12.10
12.20
12.30
13.00
14.00
16.00
20.00

pH
1.70
2.00
2.30
2.70
3.15
3.35
3.80
5.00
6.85
8.55
9.55
9.95
10.20
10.85
11.30
11.65
11.85

pH

pH/v

0.20
0.45
1.20
1.85
1.70
1.00
0.40
0.25

0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10

2.00
4.50
12.00
18.50
17.00
10.00
4.00
2.50

NaOH (mL)

(pH/v)

2.50
7.50
6.50
-1.50
-7.00
-6.00
-1.50

2pH/v2

0.10
0.10
0.10
0.10
0.10
0.10
0.10

2.50
75.0
65.0
-15.0
-70.0
-60.0
-15.0

NaOH (mL)

5.3 () 1 () 2 HCl NaOH

54 |

5.1 potentiometric titration

1) pH meter
2)

1. (pH meter)
2. magnetic stirrer
3.

1. (KHC8H4O4)
2. (NaOH)
3. HCl CH3COOH

1 NaOH ( 2.1)
2 HCl
1. (*) pH
(calibration)
4, 7 10 (
)
2. HCl 25.00 mL 250 mL
75 mL ( )

3.

4. NaOH
5. x y (scale)
6. pH NaOH
1.0 mL pH ( 5.2) NaOH

7. 2 mL
NaOH 0.10 mL pH ( 5.3)

(Quantitative analysis based on spectroscopy)

200 300 780 1000

380 780







1.

2.
3. pH

4.

5.
(absorption) (species)

1.

2.
3.
(cell) (cuvette)
(blank)

56 |

(calibration curve)

6.1

6.1

 6 | 57

6.1

1)
2)
3)

()
Fe2+ 1,10-phenanthroline
pH 3-9 pH 3.5

(II) (hydroxylamine
hydrochloride) (II)
4Fe3++ 2NH2OH 4Fe2++ N2O + 4H+ + H2O
Fe2+(aq) + 3PhH+ Fe(Ph)32+ + 3H+

1,10-phenanthroline
Fe-phenanthroline complex
Kf 2.5x10 25C pH
3.5

1. UV-Vis spectrophotometer
2. (cell)
3.

58 |

1. 10 ppm ( stock 1000 ppm) 25 mL

2. 10%(w/v) NH2OHHCl
3. CH3COONH4 250 100 mL
700 mL 1000 mL
4. 1% (w/v) 1,10-phenanthrolien

1 (max)
1. 1 mL 10 ppm Fe 25 mL
2. NH2OHHCl 1 mL acetate buffer 1 mL
3. 1,10-phenanthrolien 2 mL
10
4. 800-400 nm
5.
2 (standard calibration curve)
1. 25 mL 6 10 ppm Fe 0, 0.5,
1.0, 2.0, 3.0, 4.0 5.0 mL () (** 1 )
2. 1 510 nm
3.

3
1. 25 mL 3 10 mL (
)
2. 1 510 nm
3.

 6 | 59

6.2 -

1.
2.

1. UV-Vis spectrophotometer
2. (cell)
3.
4. 25 mL

1. 100 ppm 0.100

10 mL 0.5 mol/L NaOH 100 mL
2. 0.1 M Fe3+ FeCl3 (anhydrous) 1.62
100 mL
3. 0.5 mol/L NaOH 1 mL
10 25 mL

1 (max)
1. 25 mL 1 1.0 mL Fe3+ 4.0 mL

2. 800-400 nm
3.
2
1. 25 mL 6 0, 1.0,
1.5, 2.5, 4.0 5.0 mL () (** 1 )
Fe3+ 4.0 mL
2. 530 nm
3
1. 25 mL 3 10 mL
2. Fe3+ 4.0 mL
3. 530 nm
4.