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Lab Manual-Total Alkalinity

1. This experiment aims to estimate the total alkalinity of water, which is defined as the amount of acid needed to lower the pH to 3.7. This involves determining the phenolphthalein alkalinity (to pH 8.3) and methyl orange alkalinity (to pH 4.3) separately. 2. The procedure involves standardizing HCl using sodium carbonate, then titrating a water sample with HCl using the two indicators to measure each alkalinity. 3. The total alkalinity is calculated as the sum of the phenolphthalein and methyl orange alkalinity values based on the titration results.

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Suvanka Dutta
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662 views

Lab Manual-Total Alkalinity

1. This experiment aims to estimate the total alkalinity of water, which is defined as the amount of acid needed to lower the pH to 3.7. This involves determining the phenolphthalein alkalinity (to pH 8.3) and methyl orange alkalinity (to pH 4.3) separately. 2. The procedure involves standardizing HCl using sodium carbonate, then titrating a water sample with HCl using the two indicators to measure each alkalinity. 3. The total alkalinity is calculated as the sum of the phenolphthalein and methyl orange alkalinity values based on the titration results.

Uploaded by

Suvanka Dutta
Copyright
© Attribution Non-Commercial (BY-NC)
Available Formats
Download as DOC, PDF, TXT or read online on Scribd
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Name of the Experiment: Estimation of Total Alkalinity

1. Theory:
Alkalinity of water is its acid-neutralising capacity. Alkalinity is a measure of an aggregate property of water and can be interpreted in terms of specific substances only when t the chemical composition of the sample is known. Alkalinity is significant in many uses and treatments of waters and wastewaters. Because of the alkalinity of many surface water is primarily a function of carbonate, bicarbonate and hydroxide content, it is taken as an indication of the concentration of these constituents. Hydroxyl ions present in a sample as a result of dissociation or hydrolysis of solutes react with additions of standard acid. Alkalinity thus depends on the end-point pH used. Alkalinity of water is the capacity of that water to accept protons. It may be defined as the quantitative capacity of an aqueous medium to react with hydrogen ions to pH 8.3 (phenolphthalein alkalinity) and then to pH 3.7 (total alkalinity or methyl orange alkalinity). The equation in its simplest form is as follows: Total Alkalinity is defined as the amount of acid required to lower the pH of the sample to the point where all of the bicarbonate [HCO 3-] and carbonate [CO3--] could be converted to carbonic acid [H2CO3]. This is called the carbonic acid equivalence point or the carbonic acid endpoint. These equations show what happens to carbonate and bicarbonate as acid is added: The equation in its simplest form is as follows: CO32 + H+ = HCO3(pH 8.3) i.e. phenolphthalein alkalinity From pH 8.3 to 3.7, the following reaction may occur: HCO3- + H+ = H2CO3

2. Interferences:
Free available residual chlorine markedly affects the indicator COlOUr response. The addition of minimal volumes of sodium thiosulphate eliminates this interference. Substances such as salt of weak organic or inorganic acids present in large amount may interfere. Oils and greases may also interfere by coating the electrode. Coloured or turbid samples may interfere in end point. Analyse such samples by potentiometric titration.

3. Apparatus Required:
3.1 Burette, 3.2 Pipette, 3.3 Conical Flask, 3.4 Measuring Cylinder
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4. Reagent required:
4.1 Hydrochloric Acid - Dilute 11.8 ml of concentrated Hydrochloric acid ( relative density l-84) to one litre with distilled water. i.e. 0.1 ( N) HCl 4.2 Phenolphthalein Indicator - Dissolve 0.5 g of phenolphthalein. in 100 ml, 1 : 1 (v/v), alcohol water mixture. 4.3 Mixed lndicatcr Solution - Dissolve 0.02 g methyl red and O-01 g bromocresol green in 100 ml, 35 percent, ethyl or isopropyl alcohol. 4.4 Standard Sodium Carbonate solution 1 (N)- Weight 10 g Na2CO3 and dry it 180oC in a hot air oven and cool in a desiccators, weight 5.3 g Na2CO3 and dissolve it with distilled water to a 100 ml volumetric flask. 4.5 Working Sodium Carbonate solution- 0.1 (N)

5. Procedure:
5.1 Step 1: Standardization of HCl by Na2CO3 1. Pipette out 10ml 0.1(N) Na2CO3 in 250 ml conical flask. 2. Add 1-2 drops of methyl orange indicator and a small amount of distilled water. 3. Titrate with the 0.1 (N) HCl. 4. At the end point the colour changes from yellow to pink. 5. Repeat the titration thrice. Observation No. Volume of Na2CO3 Burette readings taken(ml) V1 Initial Final Differenc e Mean volume of HCl (ml) V2

1 2 3 Table 1: Standardization of HCl 5.2.Calculation: (V1S1 = V2S2) Let the strength of Na2CO3 soln. =S1 =0.1 (N) Volume of Na2CO3= V1 =10 ml And volume of HCl soln. added= V2 =Mean volume from table 1 Strength of HCl soln. = S2=?

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5.3 Step 2: Estimation of Total Alkalinity a. Phenolphthalein alkalinity: 1. Take 100 ml tap water sample in 250 ml Conical Flask. 2. Add 1-2 drops of Phenolphthalein indicator. 3. If the solution is colourless, then Phenolphthalein alkalinity is zero. 4. If the solution turns to pink colour then titrate it with 0.1(N) HCl. 5. The Colour changes from pink to colourless at the end point. 6. Repeat the titration thrice.

Observation No.

Volume of tap Burette readings water taken(ml) V1 Initial Final Differenc e

Mean volume of HCl (ml) V2

1 2 3 Table: 2(i) Phenolphthalein alkalinity

b. Methyl Orange alkalinity: 1. Take 100 ml tap water sample in 250 ml Conical Flask. 2. Add 1-2 drops of Methyl Orange indicator. 3. The solution turns to yellow colour then titrate it with 0.1(N) HCl. 4. The colour changes from yellow to pink at the end point. 5. Repeat the titration thrice.

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Observation No.

Volume of tap Burette readings water taken(ml) V1 Initial Final Differenc e

Mean volume of HCl (ml) V2

1 2 3 Table: 2 (ii) Methyl Orange alkalinity 5.4 Calculation: a. Phenolphthalein alkalinity as (CaCO3) , mg/l= A B M 1000 S Where, A= Burette reading of mean volume of HCl solution B= Equivalent weight of CaCO3, i.e. 50 M= Strength of HCl, i.e. from table 1. S= Sample volume of tap water taken in a conical flask b. Methyl Orange alkalinity as (CaCO3) , mg/l= A B M 1000 S Where, A= Burette reading of mean volume of HCl solution B= Equivalent weight of CaCO3, i.e. 50 M= Strength of HCl, i.e. from table 1. S= Sample volume of tap water taken in a conical flask

Total Alkalinity = Phenolphthalein alkalinity + Methyl Orange alkalinity 6. Reference:

APHA (1995), Standard methods for the examination of water and waste water, 21st edn.; American Public Health Association, Washington, DC.

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