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Lab Manual

The document provides instructions for laboratory experiments to analyze environmental samples, including preparing standard solutions, measuring pH, conductivity and ionic strength, and testing for acidity, alkalinity, turbidity, color, solids, hardness, dissolved oxygen, biochemical oxygen demand, and chemical oxygen demand.

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Hasam Tanveer H T M
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29 views

Lab Manual

The document provides instructions for laboratory experiments to analyze environmental samples, including preparing standard solutions, measuring pH, conductivity and ionic strength, and testing for acidity, alkalinity, turbidity, color, solids, hardness, dissolved oxygen, biochemical oxygen demand, and chemical oxygen demand.

Uploaded by

Hasam Tanveer H T M
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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ENVIRONMENTAL CHEMISTRY LABORATORY MANUAL

1. Standard Solutions, pH, conductivity, ionic strength

Group 1 Group 2 Group 3 Group 4


Prepare: Prepare: Prepare: Prepare:
1 N NaOH, 100 mL 1 N NaOH, 50 mL 2 N NaOH, 100 mL 2 N NaOH, 50 mL
1 N H2SO4, 100 mL 1 N H2SO4, 50 mL 2 N H2SO4, 100 mL 2 N H2SO4, 50 mL
10% (mass/mass) salt 25% (mass/mass) salt 50% (mass/mass) salt 35% (mass/mass) salt
solution, 100 mL solution, 100 mL solution, 100 mL solution, 100 mL

Dilute and prepare: Dilute and prepare: Dilute and prepare: Dilute and prepare:
0.02 N NaOH, 250 mL 0.02 N NaOH, 100 mL 0.02 N NaOH, 100 mL 0.02 N NaOH, 50 mL
0.02 N H2SO4, 250 mL 0.02 N H2SO4, 100 mL 0.02 N H2SO4, 100 mL 0.02 N H2SO4, 50 mL

Measure: Measure: Measure: Measure:


pH, conductivity, ionic pH, conductivity, ionic pH, conductivity, ionic pH, conductivity, ionic
strength of each solutions strength of each solutions strength of each solutions strength of each solutions

2. Acidity Test

 Measure 50 mL of sample using graduated cylinder and pour into an erlen


 Add 2-3 drops of methyl-orange indicator reagent
 Measure the pH value using a pH-meter
 Titrate the solution using 0.02 N NaOH and finish the titration when methyl orange turning point is observed.
 Repeat the steps using phenolftalein indicator reagent.
 Calculate the acidity types using the formula below.

3. Alkalinity Test

 Take 50 mL of sample
 Add 2 – 3 drops of phenol ftalein indicator reagent
 Titrate the sample with 0.02 N H2SO4 solution till the turning point.
 Add 2 – 3 drops of methyl ftalein indicator reagent.
 Titrate the sample with 0.02 N H2SO4 solution till the turning point.
 Calculate the alkalinity types using alkalinity dominant species table and the formula below.
4. Turbidity and Color Test

Turbidity Test:
 Homogenize (mix well) the sample, and add sample into the turbidimeter tube (25±1 ml).
 Wipe out the tube and place it into the turbidimeter, and close the lid.
 Read the value from the digital screen.
If turbidity value is > 1000 NTU:
 Homogenize the sample, and dilute the sample (For ex. 50%, 75% dilution).
 Add sample into the turbidimeter tube, place it into the turbidimeter and read the value.
 Multiply the value with dilution factor.

Color Test:
 Read the absorbance values of the colored standard solutions using a UV spectrophotometer.
 Draw a calibration graph using the measured points on the graph and generate the equation.
 Read the absorbance values of the unknown samples with spectrophotometer.
 Show the sample results on the graph and calculate the concentrations of the samples using the equation

5. Solid Matters Test

Total Solids (TS) Method


 Dry crucible at 103–105°C for 1 h and put it in a desiccator
 Weigh the crucible (A).
 Put a 50 mL of homogenized sample.
 Dry the sample at 103–105°C (usually it takes >3 h) and then put it in a desiccator.
 Weigh the sample + crucible (B).

TS (mg/L) = (B - A) / Vsample B = Weight of crucible + sample (mg, g, kg, …)


A = Crucible (mg, g, kg, …) Vsample = mL, L
Total Suspended Solids (TSS) Method

 Dry the crucible + filter paper at 103–105°C for 1 h and put it in a desiccator
 Weigh the crucible + FP (A).
 Filter a 100 mL of homogenized sample.
 Dry the crucible+FP at 103–105°C for 1 h and then put it in a desiccator.
 Weigh the sample + crucible + FP (B).

TSS (mg/L) = (B - A) / Vsample B = Weight of crucible + filter paper + sample (mg, g, kg, …)
A = Crucible + filter paper (mg, g, kg, …) Vsample = mL, L, m 3
Total Dissolved Solids (TDS) = TS – TSS

6. Hardness Test

 Take 50 mL of water sample (or take a sample which would consume <15 mL of EDTA and dilute to 50 mL).
 Add 1 mL of buffer solution to increase pH to 10,0 ± 0,1 (and finalize the titration within 5 minutes).
 Add a very small amount of eriochrome black T (EBT) indicator reagent (Color of the sample should turn pink).
 Titrate the sample with EDTA till the color turns from pink to blue.
 Calculate the hardness using the formula given below

VEDTA  N EDTA  50000


Hardness (mgCaCO3 / mL 
Vs (mL)
7. Dissolved Oxygen and Biochemical Oxygen Demand Test

 Apply dilution or add dilution solution to the sample and note the dilution factor.
 Fill two BOD bottles with sample (or diluted sample) and store one of them in the incubator immediately.
 Add 2 mL MnSO4 and 2 mL alkali iodide azid solutions into the BOD bottle, put BOD bottle for 10 min in dark
closet.
 Add 2 mL, 1 N H2SO4 into the bottle and mix it vigorously.
 Take 200 mL of sample into an erlene and start titration with 0.025 N sodium thiosulfate till light yellow color.
 Add 2-3 drops of starch and finalize titration when you reach the color of the sample.
 Repeat the procedure on the 5th day and calculate the BOD5 and ultimate BOD of the sample using the formula
below.
8. Chemical Oxygen Demand Test

 20 mL of sample (and 20 mL of blank) is filled into COD bottles (volumetric flasks).


o If sample is highly polluted, then the sample should be diluted with distilled water.
 A few number of boiling stones and 0.4 g of HgSO4 (mercury sulfate) are added.
o HgSO4 is added to prevent the interference of Cl.
 5 mL of Ag2SO4.H2SO4 (silver-sulphuric acid) is added and HgSO4 is dissolved.
 10 mL of standard K2Cr2O7 is added and mixed.
 COD bottles are placed into reflux system, and cooling water is started to run in the system.
 25 mL of Ag2SO4.H2SO4 is added from the top of the reflux system.
 Samples and blank are boiled for 2 hours in reflux system
 After boiling for 2 hrs, add 60 mL of distilled water into COD bottles and cool it till room temperature.
 After cooling, add 2–3 drops of ferroin indicator reagent.
 Samples and blank are titrated with standard iron ammonium sulfate (IAS) till the color changed from blue-
green to dark red.
 Calculate the COD of the sample using the formula below.

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