Ethylenediamine tetra-acetic acid and its sodium salts (EDTA) form a chelated soluble complex when

added to a solution of certain metal cations. If a small amount of a dye such as Eriochrome black T is
added to an aqueous solution containing calcium and magnesium ions at a pH of 10 0.1, the
solution will become wine red. If EDTA is then added as a titrant, the calcium and magnesium will be
complexed. After sufficient EDTA has been added to complex all the magnesium and calcium, the
solution will turn from wine red to blue. This is the end point of the titration.
Apparatus
1. Burette
2. Pipette
3. Erlenmeyer flask
4. Bottle etc.
Reagents
1. Standard EDTA titrant (0.01 M)
2. Eriochrome black T indicator
3. Ammonia buffer solution
Procedure
1. Dilute 25 mL of sample (V) to about 50 mL with distilled water in an Erlenmeyer flask.
2. Add 1 mL of buffer solution.
3. Add two drops of indicator solution. The solution turns wine red in colour.
4. Add the standard EDTA titrant slowly with continuous stirring until the last reddish tinge disappears
from the solution. The colour of the solution at the end point is blue under normal conditions.
5. Note down the volume of EDTA added (V1).

Calculation
V1 x S x 1000
Hardness as CaCO3=

mg / L
V

where,
S = mg CaCO3 equivalent to 1 mL of EDTA titrant
= 1 mg CaCO3
1000 V1
Hardness as CaCO3=

= ..........mg / L
V

TABLE OF APPROXIMATE pH OF SOME COMMON ACIDS AND BASES

AT VARIOUS CONCENTRATIONS.
NORMALITY/
2N

1N

0.1N

0.01N

0.001N

36.5

3.65

0.37

0.037

0.11

1.08

Sulphuric acid g/l

49

4.9

0.49

0.049

H2SO4

pH

0.24

1.17

2.05

Formic acid

g/l

92

46

4.6

0.46

0.046

HCOOH

pH

1.61

1.79

2.32

2.85

3.42

Lactic acid

g/l

180

90

0.9

0.09

C3H6O3

pH

1.78

1.97

2.43

2.95

3.5

Acetic acid

g/l

120

60

0.6

0.06

CH3COOH

pH

2.18

2.4

2.87

3.37

3.89

T.S.P.P.

g/l

83

8.3

0.83

0.083

Na4P4O7

pH

10.5

10.15

9.25

9.01

Soda Ash

g/l

106

53

5.3

0.53

0.053

Na2CO3

pH

11.6

11.5

Ammonia

g/l

34

17

1.7

0.17

0.017

pH

11.72

11.59

11.16

10.64

10.15

g/l

98.6

49.3

4.93

0.493

0.049

Na3PO4

pH

12.8

12.3

11.4

11.1

10.95

Caustic soda

g/l

40

0.4

0.04

NaOH

pH

13.93

12.98

12

11

MATERIAL
Hydrochloric
acid
HCl

(Hydroxide)
NH4OH
Trisodium
phosphate

g/l

---

pH

---

11 10

9.8

Caustic Soda lye:

Take approximately 25 grams of caustic diluted to 500 ml. From this take 20ml and titrate with 1 N,
H2SO4 using phenolphthalein as indicator. Percentage Strength = V x 40 x 100/ 20 x 2 x wt where V
is the volume of H2SO4 consumed and wt = 25/500 x 20 grams.

Conversion of Caustic soda concentrations:

To convert a weight of a caustic soda solution to a weight of solid caustic soda, multiply by the %w/w
content and divide by 100.
Example: How much sold caustic soda should be used in place of 12 kg of 100TW caustic soda (% w/w
= 47.33)?
Calculation: 12 x 47.33/100 = 5.7 kg NaOH solid.
To convert a volume of caustic soda solution in to weight of solid caustic soda, multiply the volume, in
liters, by the g/l content of the solution.
Example: How much solid caustic soda should be used in place of 12 liters of 48.1Be (-710g/l NaOH)
caustic solution?
Calculation: 12 x 710 = 8520g = 8.5kg of NaOH solid.
Specific Gravity and concentration of Caustic Soda solutions at 20C

Specific Gravity and concentration of Caustic Soda solutions at 20C

SG

Be

TW

%W/W

G/L

1.000

1.05

10.6

1.050

6.7

10

4.68

48.9

1.100

13.0

20

9.19

101.1

1.150

18.8

30

13.73

157.9

1.160

19.8

32

14.64

169.8

1.170

20.9

34

15.54

181.8

1.180

22.0

36

16.44

194.0

1.190

23.0

38

17.35

206.4

1.200

24.0

40

18.26

219.0

1.210

25.0

42

19.61

231.8

1.220

26.0

44

20.07

244.9

1.230

26.9

46

20.98

258.0

1.240

27.9

48

21.90

271.5

1.250

28.8

50

22.62

285.2

1.260

29.7

52

23.28

299.0

1.270

30.6

54

24.65

312.9

1.280

31.5

56

25.56

327.1

1.290

32.4

58

26.48

341.6

1.300

33.3

60

27.41

256.2

1.310

34.2

62

28.33

371.1

1.320

35.0

64

29.26

386.2

1.330

35.8

66

30.20

401.6

1.340

36.6

68

31.14

417.2

1.360

38.2

72

33.06

449.6

1.370

39.0

74

34.03

456.0

1.380

39.8

76

35.01

483.2

1.390

40.5

78

36.00

500.4

1.400

41.2

80

36.99

518.0

1.410

42.0

82

37.99

535.6

1.420

42.7

84

38.99

553.6

1.430

43.4

86

40.00

572.0

1.440

44.1

88

41.03

590.8

1.450

44.8

90

42.07

610.0

1.460

45.4

92

43.12

629.6

1.470

46.1

94

44.17

646.2

1.480

46.8

96

45.22

669.2

1.490

47.4

98

46.27

698.2

1.500

48.1

100

47.33

710.0

1.510

48.7

102

48.30

730.4

1.520

49.4

104

49.44

751.2

1.530

50.0

106

50.50

772.4

Finding the strength of Soda Ash

Scope:

This test method covers the titrimetric determination of the total alkalinity of soda ash. This alkalinity
is normally expressed as percent sodium oxide (Na2 O).
Summary of Test Method
Total alkalinity is determined by titration with standard hydrochloric (or sulfuric) acid using methyl
orange or modi?ed methyl orange indicator solution.
Interferences
Alkalies other than soda ash (sodium carbonate) and compounds that consume acid will affect the
accuracy of this test method.
Reagents
1 Hydrochloric (or Sulfuric) Acid (1.0 N)Prepare in accordance with Practice E 200 (record
temperature of solution when standardized).
2 Modi?ed Methyl Orange Indicator Solution or Methyl Orange Indicator SolutionSee Practice E
200. 11.3 Water, carbon dioxide-free (freshly boiled and cooled).
Procedure
1. Weigh, to the nearest 0.1 mg, 4.4 +/- 0.1 g (Note 1) of the sample and transfer to a 500-mL
conical ask. Add 100 mL of water and swirl to dissolve the sample. Use of the spec ?ed weight of
sample requires a 100-mL buret for titration and is recommended. If a 50-mL buret is used, the
sample weight should be halved to 2.2 g. Add 3 drops of modi ?ed methyl orange indicator solution
2. Titrate this solution with standard 1.0 N acid to a gray end point.
3. Record the volume to the nearest 0.02 mL and temperature of the acid used. Correct the acid
normality for any difference from the standardization temperature by use of the factor DN/C 5
0.00035 between 20 and 30C. Add the correction when the temperature of use is below and subtract
when above the temperature of standardizatized.
If desired, 0.1 % methyl orange indicator solution may be used.
The analyst should end the titration at the same shade of color as was used for the end point in the
standardization of the acid.
Calculation
Calculate the total alkalinity as percent sodium oxide

Sodium Oxide Wt% =(A x B X 0.030990) x 100/B

where:
A = acid required for titration of the sample, mL,
B =corrected normality of the acid, and
W = sample used, g.
Alternatively, calculate the alkalinity as sodium carbonate as follows:
sodium carbonate, wt % = 1.7101 x Na2O weight %
If actual sodium carbonate content is desired, the sodium bicarbonate content must be determined
separately as:
sodium carbonate (actual), % = A -(B X 0.6308)
where:
A=Na2CO3 , % and
B= NaHCO3, % .
Ref : Courtesy http://en.blijoil.com/UserFiles/Uploads/E359.PDF

Analytical methods
H2O2 concentration
General remarks
This method describes the determination of hydrogen peroxide concentration in an aqueous solution.
We recommend that each sample is processed at least twice.
Procedure
Place approx. 50 ml 5 N sulfuric acid (H2SO4 , 2.5 mol/l ) in a flask and add an exactly weighed
sample of the H2O2 containing solution. Use an analytical balance (four decimal digits). A syringe
could be used to add the H2O2 sample. In this case, the syringe has to be rinsed thoroughly before
use. Calculate the amount by weighing the filled syringe before and after adding a few drops to the
flask.
For all procedures only deionized or distilled water should be used.
Titrate the sample with 0.25 N potassium permanganate solution (0.05 mol/l) while mixing vigorously.
If using visual/manual titration, titrate until a pale pink coloration persists for a while. If using
automatic titration equipment, the end point could be determined potentiometrically via a redox
electrode.
Note: Potassium permangante solutions must be standardized regularly.
Calculation
The content of hydrogen peroxide in the solution is calculated as follows:

The result gives the concentration of hydrogen peroxide in the solution expressed in weight percent (g
H2O2/100 g solution)
Stability
General remarks
This method describes the determination of hydrogen peroxide stability in an aqueous solution. A
sample of hydrogen peroxide is stored at 96 C for 16 hours. This treatment leads to a certain loss of
hydrogen peroxide content. The percentage loss of content gives the decomposition rate of the
sample.
The content of H2O2 before and after the treatment is analyzed with potassium permanganate in
acidic medium.
Clean equipment and a clean workplace along with high purity of the reagents are essential for this
analytical method. The flasks should be dedicated to this procedure. Otherwise, unreliable results
could be obtained. We recommend that each sample is processed at least twice.
Procedure
Each of three flasks of 100 ml volume is filled with exactly 50 ml (pipette) of the hydrogen peroxide
sample. To avoid losses by evaporation, the flasks are covered (e.g. with a condenser cap), but not
closed tightly. One of the flasks is used to determine the initial hydrogen peroxide content. This one is
stored at room temperature. The two other flasks are stored in a water bath for 16 hours at 96 C.
After that, all flasks are cooled to 20 C and filled up to the 100 ml mark with distilled or deionized
water. Now, the hydrogen peroxide content of these heated and unheated samples is determined. For
this, the titration method with potassium permanganate is applied (see above).
Calculation
The decomposition rate of the hydrogen peroxide sample is calculated as follows:

pH value
General remarks
This method describes the determination of the apparent pH value of hydrogen peroxide. The
measurement is carried out directly in the sample. A glass electrode and a common pH meter with a
resolution of 0.01 pH units is used.
Procedure
The pH equipment must be calibrated for acidic pH ranges using two different, well-defined standard
pH solutions. Calibration has to be repeated before every series of measurements.

Determination of the apparent pH of the hydrogen peroxide sample is carried out directly in the
sample. The value given by the pH meter represents the final result.

Determination of the strength of sodium hypochlorite

Sodium Hypochlorite: (NaOCl) Eq Wt 35.5
Determination of active chlorine in Commercial Sodium Hypochlorite:
Active Chlorine is not liberated as such from alkaline hypochlorite bleach liquors.
The effective amount of Chlorine liberated by acidification of hypochlorite solution is defined by the
equation as below.
NaOCl + 2KI + H2SO4 I2 + NaCl + K2SO4 + H2O
2Na2S2O3 + I2 2NaI + Na2S4O6
Procedure:
5 ml of concentrated hypochlorite is diluted to 100 ml with distilled water.
Pipette 10ml of the above solution in to a 500 ml conical flask containing about 200 ml distilled water
and 20ml Potassium Iodide solution ( approximately 166 g/l)
Add 50ml dilute (10%) Sulphuric acid and titrate with 0.1N Sodium Thiosulphate until the solution is
pale yellow color.
Add 5ml starch solution (soluble starch 1% w/w) and continue titration until the blue color formed is
discharged. Let the Titre value be A ml of 0.1N Sodium Thiosulphate.
Calculation:
1 ml 0.1N Sod. Thiosulphate = 0.00355 gram active chlorine
Gram/liter Active Chlorine = 0.00355 x A x 1000 x 100/(10 x 5)
Standardisation of Sodium Thiosulphate:
Na2S2O3. 5H2O Mol Wt: 248.18 g/mol Eq. Wt: 248.18
Standard Solution : 6.205 gram of Thiosulphate is dissolved in 250 ml of D.D.water (Alkaline proof)
7.pH.
For alkaline proof, we have to add some phenolphthalein indicator and add 0.1N NaOH lye until pink
colour appears.
Iodometric conversion table:
The table below provides easy conversion of titres to Sodium Hypochlorite or active chlorine content of
bleach liquor when a 10ml sample of the liquor has been titrated with 0.1N Sodium Thiosulphate
solution.

Volume of 01N
Na2S3O4

Active Chlorine
content of 100%

Active Chlorine
Active Chlorine g/l
content of 26% conc

conc solution

solution

0.22

0.88

0.35

0.45

1.76

0.71

0.67

2.64

1.06

0.90

3.52

1.42

1.13

4.40

1.77

1.35

5.28

2.13

1.58

6.16

2.48

1.80

7.04

2.84

2.03

7.92

3.19

10

2.26

8.80

3.55

11

2.48

8.68

3.90

12

2.71

10.56

4.26

13

2.93

11.44

4.61

14

3.16

12.32

4.97

15

3.39

13.20

5.32

16

3.61

14.08

5.68

17

3.84

14.96

6.03

18

4.06

15.84

6.39

19

4.29

16.72

6.74

20

4.52

17.60

7.10

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Testing Strength of Acetic acid, Hydrochloric acid , Sulphuric acid and

Oxalic acid -1
Standardisation of Sulphuric Acid: Mol Wt: 98.08 & Eq. Wt: 49.0
49 grams/litre of H2SO4 gives 1N acid.
Strength Testing of Sulphuric Acid:
Weigh accurately about 1 gram of the acid and transfer to a conical flask with D.D.Water. Add
phenolphthalein indicator and titrate against 0.5N NaOH to a permanent pink colour.
% of H2SO4 = (Vol. of NaOH x N of NaOH x 49) / (Wt of Acid x 10)
Standard Norms = 96.5% to 98% w/w.
Acetic Acid Strength Testing: Mol Wt: 60.05 Eq.Wt: 60.05 Freezing Point:16.6 and Boiling
Point:118C
Weigh accurately about 0.5 gram of the sample and transfer to a conical flask using D.D.Water. The
solution is titrated against 0.5N NaOH using phenolphthalein indicator. The end point is permanent
pink colour.
Calculation:
% of AcOH =
(Vol. of NaOH x Normality of NaOH x 60) / (Wt of acid x 10)
Standard Norms : 96 to 98% w/w

esting Strength of Acetic acid, Hydrochloric acid , Sulphuric acid and

Oxalic acid -3
Potassium Permanganate: Mol Wt: 158.04 Wq.Wt = 31.61
Preparation of Standard solution: 3.161 gram of KMNO4 in 500 ml of D.D.water boiled for 30 minutes
and made up to 1 litre gives 0.1N solution.
Determination of the strength of KMNO4: 20 ml of 0.1N Oxalic acid + 20 ml of 1N H2SO4 are heated
to a warm temp. and titrated against KMNO4.
V1N1 = V2N2 N1= V2N2 (0.1 X 20)/burette reading of KMNO4
Oxalic Acid Strength Testing: Mol Wt:126.07 Eq.Wt :63.02
Weigh about 0.5 gram of the acid and transfer to a conical flask containing 50 ml of distilled water.
Dissolve the acid completely and titrate against 0.5N NaOH using phenolphthalein as indicator.
% of HOOC-COOH.2H2O = (Vol of NaOH x N x 63)/ (wt of acid x 10)
Standard Norms = 94 to 98% w/w.
Strength of Sodium Bicarbonate: NaHCO3 :
About 1 gram of the sample accurately weighed is dissolved in distilled water and made up to 250 ml.
a 50 ml of the solution is titrated against 0.1N HCl using phenolphthalein as indicator and the reading
noted as Y.
Take another 50 ml of the solution and titrate against 0.1N HCl using methyl orange as indicator and
the Titre value be X.
Caluculation:
% of Sod.Bicarbonate =
[(X 2Y) x 0.0084 x 100 x Normality of HCl)]/wt of sample in 50ml
Standard Norms: 94 to 98%.
Strength of Citric acid : Eq Wt: 70 Melting Point:153C
Weigh accurately 0.5 gram of the sample and dissolve in 50 ml of distilled water. Add phenolphthalein
indicator and titrate against 0.5N NaOH to a permanent pink color.
Calculation:
% of acid = (Vol of NaOH x N x 70)/(Wt of acid x 10)
Standard Norms : 95 to 98% w/w.
Strength Testing of Hydro Chloric Acid: Mol Wt: = 36.46
Weigh accurately 0.5 gram of the acid and transfer to a conical flask with D.D.water. Add
phenolphthalein indicator and titrate against 0.5N NaOH to a permanent pink colour.
Calculation:
% of HCl =
(Vol of NaOH x Normality of NaOH x 36.5) / Weight of HCl x 10
Standard Hydrochloric acid strength will be 29 to 35

Tri Sodium Phosphate: Eq Wt: 82

About 5 grams of dried sample ( heated to 100C for 2 hours), accurately weighed is dissolved in 50
ml of distilled water. Add 2.5 gram of common salt (vacuum salt) and after to 15C, the solution is
titrated to a distinct red color with 1N HCl, using methyl orange as indicator.
Calculation:
% of T.S.P. = (Vol of HCl X Normality of HCl x 82)/(Wt of the sample x 10)