PRACTICE OF ANALYTICAL CHEMISTRY

REPORT
LESSON 7:
QUANTITATIVE METHOD IN SILVER
QUANTITATIVE AgNO3 BY MOHR METHOD –
QUANTITATIVE CHLORIDE BY FAJANS METHOD
FULL NAME:
1. Nguyễn Đoàn Mỹ Uyên 23116040
GROUP: 5 CLASS: 241EACH210503E
TIME: 24/9/2024 DAY: TUESDAY

I. PRINCIPLES
- Prepare NaCl standard solution from pure, anhydrous NaCl solid
- Prepare a solution of AgNO3 ~ 0.02N from AgNO3 in water AgNO3
II. PREPARATION OF SOLUTION

1. Prepare AgNO3 0.02N standard solution

- Number of volumes of AgNO3 0.2N needed to make 100 mL of AgNO3 0.02N

solution: 10ml

- Description of preparation (briefly including necessary tools): use a pipette to suck

10ml of 0.2N AgNO3 into a 100ml volumetric flask, then add water up to the mark.

2. Prepare NaCl 0,02 N stock standard solution

- Number of grams of solid NaCl needed to make 100 mL of 0.02 N NaCl solution:
0.117g

- Number of grams of solid NaCl from actual weight: 0.1261g

- NaCl concentration calculated from the weight: 0.0215N
mrel 0 , 1261
Kcor = = =1, 077
mtheo 0,117
C N −NaCl =0 , 02× K cor =0 , 02× 1,021=0 , 021 N

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- Calculate measurement uncertainty:
0,0001 0 ,1
uweigh = ; ufiol ¿
√3 √6

√( )( )
u weigh 2 ufiol 2
uC (C N−NaCl ) = C N −NaCl × +
mweigh V fiol

√
2
0,0001 0,1 2
= 0 , 021 × ( ) +( ) =¿ 0,0000129
√ 3× 0 , 1261 √ 6 ×100
Infer the expanded measurement uncertainty: U C N−NaCl
=2× 0 , 0000129=0 , 000026

So: μ0 , 95=0 , 021± 0 , 000026

- Description of preparation (briefly including necessary equipment):

Use an analytical balance to weigh 0.1261g of NaCl then dissolve it in a 100ml

volumetric flask
II. EXPERIMENT RESULTS
Experiment 1. Re-determine the concentration of AgNO3 solution from the
0.02000 N NaCl stock standard solution using the mohr salt method
CN of NaCl is: 0.02
AgNO3 NaCl
Instruments Burrette pipette

σ instruments ± 0.03ml ± 0.05ml

Time 1 (mL) 5.45 10
Time 2 (mL) 5,65 10
Time 3 (mL) 5.75 10
Average (mL) 5.62 10

Representation CN of AgNO3 with measurement uncertainty

CN = (10*0.02)/5.62=0.036

√
n

Standard deviation: s = ∑ (X i −X )2
i=1
n−1

¿
√ (5 . 45−5 . 62)2+(5 . 65−5 . 62)2 +(5 .75−5 .62)2
2
=0 , 015

2
 s 0 , 015
 uA= = =0 ,009
√n √3

√
2
 uburette = ( 0 , 03 ) +0 , 0092=0 , 015
√6
0 , 05
 u pipette = =0,020
√6

√
2 2 2
u burette u pipette uC ,C
uC (C N− AgNO )=C N −AgNO × ( ) +( ) +( )
N −NaCl

3 3
V burette V pipette C N −NaCl

¿ 0 , 036 ×
√( 5. 62)( +
10
+ ) (
0 , 015 2 0,020 2 0 ,0000129 2
0 ,021
=0 , 0001221 )
Infer the expanded measurement uncertainty: U C N−AgNO 3
=2 ×0 , 0001221=0 ,0002442

So u0.95 = 0,036 ± 0,00024

ε 0,0000576
Accuracy: 1− p =1− =99 , 66 %
N 0,017

Experiment 2. Re-determine the concentration of AgNO3 solution from the

0.02000 N NaCl stock standard solution using the adsorption indicator method
CN of NaCl is: 0.02

AgNO3 NaCl
Instruments Burrette pipette

σ instruments ± 0.03ml ± 0.05ml

Time 1 (mL) 5.45 10

Time 2 (mL) 5,65 10
Time 3 (mL) 5.75 10
Average (mL) 5.62 10

Representation CM of AgNO3 with measurement uncertainty

CM = (10*0.02)/11=0.018

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 √
n

Standard deviation: s = ∑ (X i −X )2
i=1
n−1

√(11−11) +(11, 1−11)2 +(10 , 9−11)2

2
¿ =0 ,1
2

s 0,1
 uA= = =0,058
√n √ 3

→ uburette = (
√6√
0 , 03 2
) +0,0582=0 ,06

0 , 05
u pipette = =0 , 02
√6

√
2 2 2
u burette u pipette uC ,C
uC (C N− AgNO )=C N −AgNO × ( ) +( ) +( )
N −NaCl

3 3
V burette V pipette C N −NaCl

¿ 0,018 × (
√ 0 , 03 2 0 , 02 2 0,0000126 2
11
) +(
10
) +(
0,020
) =0,000062

Infer the expanded measurement uncertainty: U C N−AgNO 3

=2 ×0,000062=0,000124

So: μ0.95 , C N− AgNO3

=0,018 ± 0,000124

ε 0,000062
Accuracy: 1− p =1− =99 , 65 %
N 0,018

III. COMMENT/EVALUATION OF ANALYSIS RESULTS

Prepare NaCl 0.02N solution

Theoretically the NaCl concentration is: 0.02 N
According to the actual concentration of NaCl is: 0.0215 N
=> The error result is 1% different from theory..
Determine the concentration of AgNO3 solution again from the 0.02N NaCl stock
standard solution
According to theory, the concentration of AgNO3 is: 0,02N
According to reality, the concentration of AgNO3 is: 0.036N
 The error result differs from theory by 15%. The volume of AgNO 3
through measurements does not exceed 0.2, so the error results are
acceptable

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Cause of error
- Error due to tools
- Error due to chemicals not guaranteed pure
- Errors due to operation
 The experimental results are acceptable because the measured volume
does not exceed 0.1 (error results are not too large) and does not affect
the experimental process.

IV. QUESTION AND ANSWER

1:
In the silver quantitative method, the standard solution is usually 0.05N AgNO 3.
This solution can be prepared from precisely weighed amounts of repurified
AgNO3. However, the concentration of the AgNO3 solution changes over time, so it
is necessary to standardize its concentration with a NaCl standard solution.
2:
Precipitation in solution has the property of adsorbing ions on its surface, especially
ions contained in the precipitate.
- When determining Cl- with AgNO3, before the equivalence point, when there
is excess Cl- in the solution, Cl- is adsorbed on the AgCl surface, causing the
precipitated surface to have a negative charge.
- After the equivalence point, when there is an excess of 1 drop of AgNO3, the
precipitate adsorbs Ag+ and the surface of the precipitate carries a positive
charge.
- Absorption indicators are weakly electrolytic organic acids, the anions of the
indicator in the free state and the absorbed state have different colors.

Example: Fluorescein symbol (HE)

3:
In the Mohr method:
- The environment when titrating needs to be neutral, or weak acid, weak
alkaline, because in a strong alkaline environment Ag + decomposes, forming

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 Ag2O precipitate, in acidic environment K2Cr2O4 precipitates will dissolve,
affecting the determination. Equivalent scoring

In the Fajan method:

- Fluorescein indicator is only used in neutral environments because acidic
environments will reduce the dissociation of the indicator into anions.

4:
Ag+ + Cl- → AgCl
We have the tan product
TAgCl = [Ag+] [Cl-] = 10-10 ở 25oC
At equivalent point [Ag+] = [Cl-] = √ TAgCl = 10-10 ở 25oC
If you want Ag2CrO4 to precipitate, then:
[Ag+]2 [CrO42-] = TAg2CrO4 = 10-12
Inferred: [CrO42-] = TAg2CrO4/ [Ag+]2
At equivalent point [Ag+] = 10-5 , we have:
[CrO42-] = 10-12/ 10-10 = 10-2 M
0.2254
5:
Use Fluorescein (HE) for the determination of Cl- with Ag+ above:
- Before the equivalence point, because the surface of the precipitate has a
negative charge, it cannot absorb E-, E- is in a free state, so the solution is
green.
- After the equivalence point: because the surface of the precipitate has a positive
charge, it absorbs E-, E- is in an absorbed state, so there is a pink precipitate

6:
We have: CN KCl * VKCl = CN AgNO3 * VAgNO3
CN KCl * 25 = 0.105 * 34
 CN KCl = 0.1428
 m = (0.1428*250*74.5)/1000 = 2.65g

7:

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 a) HNO3, HCl react with NaOH to produce water, NO 3- , Cl- then react with
AgNO3 + K2CrO4

Ag+ + Cl- → AgCl (1)

After reaction (1) ends, the residual drop of AgNO3 + K2CrO4 will precipitate
brick red:
2Ag+ + CrO42- → Ag2CrO42-
b) We have: OH- + H+ → H2O

CN HNO3 + CN HCl = (35*0.1)/20 = 0.175 N

But CN H+ = CM H+ = 0.175M

 nH+= 0.175*20= 3.5 mmol

Ag+ + Cl- → AgCl

But CN Ag+ * VAg+ = CN Cl- * VCl-

0.1 * 17.5 = nCl- = nHCl = 1.75 mmol
 %VHCl = %VHNO3 = 50%

c) pH= -log(17.5*0.1/20)= 1.05