Top Banner
ACKNOWLEDGEMENTS A formal statement of acknowledgement will hardly meet the ends of justice while writing these words, we feel obliged to all of them who extended their inconceivable co-operation towards the hard work whatever we have done. First of all, we feel very obliged to Director (Haryana Test House &Consultancy Services Panipat), who made our wish fulfilled to work out our Summer Training in Haryana Test House. We got an excellent opportunity to carry out our summer dissertation work under the honorable and encouraging guidance of Mr.T.L. MEHTA (Technical Manager Environment Dept). Their didactic, constant guidance, encouragement, inspiration and kind co- operation that they have shown towards us in completion of this endeavor are quite hard to match. 1
37
Welcome message from author
This document is posted to help you gain knowledge. Please leave a comment to let me know what you think about it! Share it to your friends and learn new things together.
Transcript
Page 1: Final TrainingReport

ACKNOWLEDGEMENTS

A formal statement of acknowledgement will hardly meet the ends of justice

while writing these words, we feel obliged to all of them who extended their

inconceivable co-operation towards the hard work whatever we have done.

First of all, we feel very obliged to Director (Haryana Test House

&Consultancy Services Panipat), who made our wish fulfilled to work out

our Summer Training in Haryana Test House.

We got an excellent opportunity to carry out our summer dissertation work

under the honorable and encouraging guidance of Mr.T.L. MEHTA

(Technical Manager Environment Dept). Their didactic, constant

guidance, encouragement, inspiration and kind co-operation that they have

shown towards us in completion of this endeavor are quite hard to match.

Words can never be able to express our heartiest thanks to Prof. C.P.

Kaushik, Chairperson and Dean of the Dept. and Mr. Jitender Pal Training

and Placement Incharge, Faculty of Non Conventional Sources of Energy

and Environmental Science, Department of Environmental Science and

Engineering, Guru Jambheshwar University of Science and Technology,

Hisar for their kind approval for our summer training work.

1

Page 2: Final TrainingReport

CONTENTS1. Introduction

i. Sources of Water…………………………………………….3

ii. Water Pollution……………………………………………....4

iii. Sampling……………………………………………………..6

2. Parameter studies in drinking water

i. Color…………………………………………………………8

ii. Turbidity……………………………………………………..10

iii. Odour………………………………………………………..11

iv. pH…………………………………………………………...12

v. Alkalinity……………………………………………………14

vi. Total dissolved Solids……………………………………….16

vii. Total suspended solids……………………………………….17

3. Parameters Studies in waste water

i. C.O.D…………………………………………………...22

ii. B.O.D……………………………………………….......

iii. Oil and Grease…………………………………………25

INTRODUCTION2

Page 3: Final TrainingReport

Chemical Properties:-

Chemically Active

Reacting with certain metals and metals oxides to form bases. And oxides of

non-metals to form acids. It reacts with organic compounds to from various

products e.g. Alcohols from alkenes.

Completely pure water is poor conductor of electricity, it is much better

conductor than most other pure liquids because of its self ionization i.e.

ability of two water molecules to react to form an OH and H3O+ions.

Sources of Water :-

Precipitation:-

The basic source of water is precipitation. This is the water falling from the

atmosphere to the surface of the earth as rain, snow etc.

Run off:-

Part of the rain and melted snow seeps into the soil. The rest becomes what

is called surface run off which flows down slopes and gathers in ravines that

discharge into rivers. Generally the term surface water indicates the water

that collects on or flows over the surface from rivers lakes, ponds, reservoirs,

canals brooks and creeks.

3

Page 4: Final TrainingReport

Ground Water:-

It is the accumulation of water below the surface ground. A portion of the

water falling or precipitation to the earth infiltration to the ground water

reservoirs. The ground water may be regarded as a temporary natural

reservoir. It emerges as springs or can be tapped by means of wells and in

filter galleries.

Importance of Water:-

1. Water is used for drinking, washing and irrigation purposes.

2. It is used in all metabolic reactions.

3. It is main constituent of blood plasma and 70% of our body weight is

water.

4. It is used I industries as a coolest and also as a solvent. It is also used

in constructions.

Pollution of Water:-

Any change in physical, chemical and biological properties of water by

human activity that imparts its use for different purpose is called water

pollution.

Sings of Water Pollution:-

1. Bad taste of drinking water.

2. Offensive odour from lakes.

3. Colour and turbidity and suspended solids.

4. Unchecked growth of aquatic weeds in water bodies.

5. Decrease in number of fist in fresh water, river water.

4

Page 5: Final TrainingReport

6. 0Oil and grease floating on water surfaces.

Types of Water Pollution:-

A. Point sources of pollution :- When a source of pollution can be

readily identified because it has a definite source and place where it

enters the water it is said to come from a point source e.g. municipal

and industrial discharge dices.

B. Non point source of Pollution:- When a source of pollution cannot

be readily identified such as agricultural run-off acid rain etc. are

called non-point source of pollution.

Pollutants:-

Organic Pollutants

Inorganic Pollutants

Sediments

Radio-active materials

Thermal Pollutants

Why Analysis of Water & Waste Water is necessary:-

To assess its quality to provides pure and wholesome water to the

public for drinking and other domestic purposes.

To find out whether water is suitable for the specific Industrial

purpose and if not to choose the most effective treatment.

To determine whether any pollution has occurred in a water course

and to trace the origin and extent of pollution and to suggest a

possible remedy.

5

Page 6: Final TrainingReport

To determine the efficiency towards natural purification when

industrial and sewage wastes and discharged in to water course.

To ascertain the effect of heavy rainfall or of long continued drought.

To measure the effect of pumping particularly when the wells are

constructed near sea or an estuary where the tidal influence is

possible.

To check the efficiency, uniformity and consistency of treatment and

purification processes.

To find out the possibility and extent of mixing water from two or

more sources.

To find out whether infection by microbial organisms has occurred

and if so, to find out the particular organism and to suggest preventive

measures and effective disinfection procedures.

SAMPLING:-

Samples are collected for various examinations under different conditions.

Whatever may be method of sampling, the samples must represent the

conditions existing at the pint taken. The sample must be of sufficient

volume to carry out the determinations.

Quality of Sample:-

Generally 2 liters of sample is sufficient for most of physical and chemical

examinations. For certain special determinations however larger volumes of

sample are necessary.

6

Page 7: Final TrainingReport

Sample Container:-

For most of the purposes, the ordinary stoppered Winchester Quart bottle of

2.5 liters capacity is enough generally glass container are preferable to those

made of polythene or other plastic materials. Polythene containers are

however used in some circumstances e.g. when the sample being examined

extracts substances from the glass or some of the constituents of the sample

adhere to the glass.

Samplers:-

A variety of special sampling devices are available to meet the specific

requirements among them displacement sampler for determination of

dissolved oxygen. When composite samples are to be collected, it is better to

use wide mouthed bottles of capacity 200-300 for the sub-samples. They are

particularly useful in transferring the contents without leaving any settle able

matter.

New glass bottles should be treated either with dil.Hcl or then

repeatedly washed with water and finally with distilled water. Subsequently

they may be cleaned using detergents.

If trace amounts of phosphates are to be determined do not use detergents for

cleaning. If chromium or sulphates are to be determined do not use acid for

cleaning.

Grab Sample of Composite Sample:-

Grab sample is a manually collected single portion of sample of water

or waste water.

7

Page 8: Final TrainingReport

When grab samples of particular water or waste water is collected at

regular intervals for a specific period and mixed, then the integrated sample

is known as ‘Composite Sample’.

Preservation of Samples:-

Preservative should be chosen with regard to the determinations that are to

be made. It should be noted that the preservative added for one constituent

should not affect the determination of other constituent keeping the sample

in the dark at low temperature is the best preservation.

PARAMETERS STUDIED IN

DRINKING WATER

1. Colour :-

IS: 3025 (P-4)

Units: Hazen

Colour is a common constituted of many natural waters and it is caused by

metabolic substances such as iron and manganese compounds, human

materials, peat tannins, algae, weeds and protozoa. The term colour means

the true colour solution ad due to the substances preset as fine colloids. For

true colour determination the sample has to be centrifuged to remove

8

Page 9: Final TrainingReport

turbidity. Apparent colour is colour due to both suspended ad dissolved

matters.

Interferences:-

Turbidity in excess of 5, seriously affects the true colour determination.

Hence it should be removed prior to determination by centrifugation ‘Do not

filter the sample to remove turbidity or suspended matter, since iteration has

a decolorizing effect’.

Reagents:-

Standard Colour Solution.

Procedure:-

Place 50 ml of the sample (centrifuged) in a 50 ml Nester tube compare the

colour of the sample with that of the working colour standards by looking

vertically downwards against a pure white surface placed at such an angle

that light is reflected up wards through the columns of liquid. If the colour

exceeds 70 units dilute the centrifuged sample with distilled water such that

the colour is within the range.

Limit:-

Desirable – 5 max.

Permissible – 25 max.

9

Page 10: Final TrainingReport

2. Turbidity: -

Is 3025 (P-10)

Units NTU

Method:- (Instrumental Method)

Turbidity is an important parameter for characterizing water quality. It is an

expression of optical property of a sample containing insoluble substances

which cause light to be scattered rather than transmitted in straight lines. The

amount and angular distribution of this scattered light is governed not only

by the quantity of the insoluble substances but also by their size shape and

refractive index. In most of the waters turbidity is due to colloidal and

extremely fine dispersions suspended matter such as clay, slit finely divided

organic and inorganic matter plankton and other microscopic organisms also

contribute to turbidity.

Regents:-

Stock Turbidity Suspension.

Standard Turbidity Suspension.

Working Turbidity Suspension.

Procedure:-

Follow the manufacturer’s operating instructions. If the instrument is

calibrated in terms of formalize turbidity units, use a series of working

turbidity suspensions to standardize the instrument, If calibrated in other

terms prepare a series of working turbidity suspensions covering the range

up to 40 units and measure the reading prepare a calibration curve relating

10

Page 11: Final TrainingReport

instrument reading to turbidity. Find out the turbidity of the sample either

directly from the instrument reading as from the calibration graph. The

calibration curve should be checked from time to time.

Following points should be born in mind while determining the

turbidity of the sample.

Shake the sample well to disperse the solids thoroughly. Pour the

sample into the turbid meter tube after all the bubbles have

disappeared.

If the sample is very cold allow it to reach the room-temperature

before testing.

If the turbidity exceeds 40 units, dilute the sample appropriately with

turbidity free distilled water.

Express the result in terms of NTU after rounding off them to the

nearest value as given in the schedule.

Limit –

Desirable – 5 max.

Permissible – 10 max.

3. Odour :-

IS: 3025 (P-5)

No water can be quite satisfactory for domestic and industrial purpose if it

possess any odour. Disagreeable odour and tastes in water are due to the

presence of a variety of objectionable substances particularly living

microscopic organisms or decaying vegetation including algae actinomy

cetes bacteria, fungi and weeds. Sewage and industrial waste also contribute

tastes and odour to receiving waters.

11

Page 12: Final TrainingReport

Qualitative Determination of Odour:-

Collect samples in glass bottles and determine the odour as-soon-as possible

after sample collection. Do not use plastic containers for collection of

samples for odour taste.

Place 250 ml of sample in 500 ml wide mouth earthen Meyer flask at

room temperature and sniff the odour. This is the cold odour quality. Some

odours may be missed at room temperature and it is better to determine. The

hot odour quality also.

Place 250 ml sample in 500 ml stoppered uncial flask and heat to

about 58-60oC. Remove the stopper and sniff the odour. Report the nature

and type of odour present.

Limit – Unobjectionable

4. pH Value :-

IS: 3025 (P-11) 1983

Method:- Electrometric Method

pH is a term used universally to express the intensity of the acid or alkaline

condition of a solution. It is a measure of hydrogen ion concentration as

mare precisely the hydrogen ion activity.

PH is defined as the “Logarithm (base 10) of the reciprocal of the

hydrogen ion concentration”. Thus if [H+] = 10-6 mole per liter, then pH=6.

pH is an important factor in water chemistry, since it enters into the

calculation of activity and alkalinity and processes such as coagulation,

disinfection, softening and corrosion control.

12

Page 13: Final TrainingReport

Principle of Electrometric Method:-

A pH meter is a high-impedance electrometer calibrated in terms of PH.

Electrometric determination of PH involves the measurement of the

electromotive force of a cell comprising an indicator electrode responsive to

hydrogen ions and a reference electrode both immersed in the test solution.

The indicator electrode commonly used is glass electrode and the reference

electrode is calomel electrode. Measurement of PH values above 10 and at

high temperature is made with special glass electrodes designed for such

purposes.

Reagents:-

pH-4 Buffer Solution:-

Dissolve 1.012 g anhydrous potassium hydrogen phthalate, KHC8H4O4 in

distilled water and make up to 100 ml in a volumetric flask.

pH-9 Buffer Solution:-

Dissolve 3.81 g sodium borate deca hydrate (borax) Na2B4O7. 10H2O in

distilled water and make up to 100 ml.

Procedure:-

Standardize the PH meter using standard buffer solution of PH 4.0 and 9.2

and then determine the PH of the sample of water or waste water.

Limit – No Relaxation

0

13

Page 14: Final TrainingReport

5. Alkalinity :-

IS 0 3025 (P-23) 1986

Method used:- Titrimetric

Alkalinity is the quantitative capacity aqueous media to react with

hydrogen ions. The alkalinity of natural and treated waters is normally due

to the presence of bicarbonates, carbonates and hydroxide compounds of

calcium, magnesium sodium and potassium.

Phenolphthalein and methyl orange are the indicators commonly used

for alkalinity titrations phenolphthalein gives pink colour in the presence of

hydroxide or normal carbonates. The change from pink to colour less occurs

at a PH 8.3. Methyl orange gives yellow colour in the presence of all the

three types of alkalinity and is orange in the presence of acid. The colour

change occurs at a PH value of about 4.5.

Principle:-

Alkalinity is directly determined by titration with 0.02NH2SO4 using

phenolphthalein and methyl orange indicators.

Ca (OH)2 + H2SO4 CaSO4 + 2H2O

2 CaCO3 + H2SO4 Ca (HCO3)2 + CaSO4

Ca (HCO3)2 + H2SO4 CaSO4 + 2CO2 + 2H2O

Reagents:-

Sulphuric Acid 0.02 N

Phenolphthalein Indicator

Mixed Indicator

14

Page 15: Final TrainingReport

Phenolphthalein Alkalinity:-

Place 25 ml or 50 ml volume of sample in a conical flask. Adjust the volume

to 50 ml with distilled water. Add phenolphthalein indicator solution. If no

pink colour ation occurs, there is no phenolphthalein alkalinity. If a pink

colour appears then titrate with 0.02NH2SO4 (to PH 8.3) until the solution

becomes colour less.

Total Alkalinity:-

Add 3 drops of mixed indicator solution to the solution in which

phenolphthalein alkalinity has been determined and titrate against

0.02NH2SO4 (to PH 4.6) to light pink.

General Calculations:-

If the sulphuric acid used for the titration is exactly 0.02N, Phenolphthalein

alkalinity as CaCO3 mg.

= Vol. of H2SO4 till end point (ml) x N x 1 x 1000

Ml of sample taken

Total Alkalinity as CaCO3 mg

= ml of H2SO4 used x N x 1 x 1000

Ml of sample taken

Limit –

Desirable – 200 max.

Permissible – 600 max.

15

Page 16: Final TrainingReport

6. Total Dissolved Solids (TDS) :-

IS 3025 (P-16)

Method Used:- Gravimetric Method

Solids:-

Solids is a term applied to all matter except the water contained in liquid

materials and thus the definition of solids refers to the matter that remains as

residue upon evaporation and drying at a definite temperature.

TDS:-

Filter a suitable volume of sample through filter paper or a glass fiber filter

paper. Evaporate the filtered sample in a tare dish. Use platinum dish for

water sample and porcelain dish for sewage and industrial effluents dry the

residue at 103 – 1080C or at 179-1810C. The increase in weight of dish

equals the total dissolved solids (TDS) It may also be obtained by the

difference between the total solids and total suspended solids.

General Calculation:-

Initial wt. of dish = W1g

Final wt. of dish = W2g

wt. of TDS = W2-W1 = W3g

TDS = W3g

Limit –

Desirable – 200 mg 1 lt.

Permissible – 2200 mg 1 lt.

16

Page 17: Final TrainingReport

7. Total Hardness :-

IS 3025 (P-21) 1984

Method Used:- EDTA Titrimetric Method

Hardness is deemed to be the capacity of water for reducing and destroying

the lather of soap. Hardness in water is due to the natural accumulation of

salts from contact with soil and geological formations or it may enter from

direct pollution by industrial effuluents. Calcium and magnesium are the

principle cautions causing hardness.

Principle:-

Calcium and magnesium ions react with EDTA to form soluble complexes

and the completion of reaction is indicated by the colour change of a suitable

indicator such as Erichrome black T(EBT)

Ca2+h2V2 Ca

Reagents:-

Standard EDTA titrant

Ammonia Ammonium Chloride (Buffer)

Erichrome Black T Indicator (EBT)

Procedure:-

Place suitable volume of sample in a conical flask and dilute to 50 ml.

Add 1 ml of buffer solution per 50 ml volume of sample. The PH of

the titre should be 10.0.

Add one drop of indicator solution or an appropriate amount of dry

powder.

17

Page 18: Final TrainingReport

Titrate with standard EDTA solution slowly, until a reddish tinge

appears and add the last few drops within 3-5 seconds. At the end

point the solution will be blue.

The whole titration procedures should be completed within 5 minutes after

the addition of buffer.

Calculation:-

Hardness as CaCO3 mg =

Ml EDTA titrant x E x 1000

Ml sample taken

Where E = CaCO3 equivalent to 1.0 ml EDTA.

Limit –

Desirable – 300 max.

Permissible – 600 max.

CLASSIFICATION OF HARDNESS:-

Hardness has been classified into ‘Temporary Hardness’ and ‘Permanent

Hardness’.

The portion of hardness that disappears o prolonged boiling is referred

as temporary hardness and is mainly due to the bicarbonates of calcium and

magnesium which are precipitated as normal carbonates by loss of CO2 on

heating. The hardness that remains after boiling is known as permanent

hardness and is due to the sulphates, chlorides and nitrates of calcium and

magnesium. Temporary hardness also called carbonates Hardness and

Permanent hardness called Non-carbonates Hardness.

18

Page 19: Final TrainingReport

Calculation of carbonate and Non-carbonate Hardness:-

Carbonates Hardness = Alkalinity (as CaCO3)

Non-Carbonates Hardness = Total Hardness – Alkalinity (as CaCO3)

Calcium – Hardness:-

IS 3025 (P-40) 1991

Method:- EDTA – Titrimetric Method.

Principle:-

The PH of the sample is made sufficiently high (12-13) to precipitate

magnesium as hydroxide and calcium only is allowed to react with EDTA in

the presence of a selective indicator.

Mg2 + 2 NaOH Mg (OH)2 + 2 Na+

Ca2 + 2 EDTA Ca (EDTA)2 + 2 Na+

Regents:-

NaOH (IN)

Murexide Indicator

Standard EDTA titrant 0.02N

Procedure:-

Place 50 ml of sample in a conical flask.

Add 2.0 ml of NaOH per 50 ml of sample to produce PH of 12-13.

19

Page 20: Final TrainingReport

Add 1 or 2 drops of indicator.

Titrate with EDTA to proper end point.

Calculation:-

If the EDTA is exactly 0.02 N mgIl calcium as CaCO3 =

Ml EDTA titrant x 1 x 1000

Ml sample taken

MgIl calcium as Ca =

Ml EDTA titrant x E x 1000

Ml sample taken x 0.40

Limit –

Desirable – 75 max.

Permissible – 200 max.

Magnesium Hardness:-

IS 3025 (P-46) 1994

Calculation:-

Magnesium as (MgCO3) mg1l =

Mg1l Total Hardness – Calcium Hardness as CaCO3

Magnesium (as Mg) mg1l =

Magnesium (as MgCO3) mg1l x 0.244

Limit –

Desirable – 75 max.

Permissible – 200 max.

20

Page 21: Final TrainingReport

8. Chloride:-

IS 3025 (P-32) 1988

Method:- Silver – Nitrate Method..

Chloride is the common anion found in water and sewage. The concentration

of chloride in natural water varies from foul milligrams to several thousand

milligrams per liter.

Principle:-

Silver nitrate reacts with chloride ions to form silver chloride. The

completion of reaction is indicated by the red colour produced by the

reaction of silver nitrate with potassium chromate solution which is added as

an indicator.

AgNO3 + Cl Ag Cl + NO3

2AgNO3 + K2CrO4 Ag2 CrO4 + 2KNO3

Reagents:-

Standard Silver Nitrate Titrant (0.0282N)

Potassium Chromate Indicator solution.

Sulphuric Acid

Sodium Hydroxide

Procedure:-

Place 100 ml sample in a porcelain basin of capacity 300 ml capacity. If the

PH of the sample is in range of 7 to 9.5 it can directly be titrated. If the pH is

not within this range. Adjust the PH to be within this range using sulphuric

21

Page 22: Final TrainingReport

acid or sodium hydroxide solution. Add 1 ml potassium chromate indicator

solution. Titrate against standard silver nitrate solution with constant stirring

until a slightest perceptible reddish colour action persists. Conduct blank

containing chlorine free distilled water wasted of sample.

Calculation:-

Mg 1l Chloride as CL =

S = ml AgNO3 used for sample.

B = ml AgNO3 used for blank.

Limit –

Desirable – 250 max.

Permissible – 1000 max.

PARAMETERS STUDIES IN

WASTE WATER –

1. C.O.D .

Is - APHA 21st Edition

Method:- Digestion Method.

C.O.D. – Chemical Oxygen Demand:-

This test is highly useful to find out the pollution strength of industrial

effluents and sewage. Chemical oxygen Demand as the name implies is the

22

Page 23: Final TrainingReport

oxygen requirement of a sample for oxidation of organic and inorganic

matter. As the oxidisable inorganic matter is usually negligible in

comparison with the quantity of organic matter, COD is generally

considered as the oxygen equivalent of the amount of organic matter

oxidisable by potassium dichromate.

Principle:-

The organic matter of the sample is oxidized to water, CO2 and ammonia by

refluxion with known excess of potassium dichromate in a 50% sulfuric acid

solution. The excess dichromate is titrated with a standard solution of

ferrous ammonium sulfate solution.

60Fe2+ + Cr2O72+ + 14H+ 6F3+ + 2 Cr3+ + 7 H2O

Reagents:-

Mercuric Sulfate Crystals

Potassium dichromate.

Ferrion Indicator

Ferrous Ammonium Sulphate.

Sulfuric Acid.

Procedure:-

Shake the sample well, so that the contents are mixed thoroughly

Place 50 ml sample in the reflux flask. Add mercuric sulfate according

to chloride concentration of the aliquot.

Measure suitable amount of sulfuric acid in a measuring cylinder.

From this amount initially transfer carefully and slowly 5 ml only to

23

Page 24: Final TrainingReport

the reflux flask ad mix thoroughly to dissolve the mercuric sulfate.

Cool while mixing to avoid possible loss of volatile matter in the

sample.

Pipette a pre-determined quantity of potassium dichromate solution in

to the flask and mix well.

Carefully add the remaining sulfuric acid in the measuring cylinder to

the reflux flask, cooling the flask simultaneously under tap.

Add a few antidumping granules and place the flask in position.

Attach the condenser and start the cooling water reflux for 2 hrs.

Remove the flame, allow the flask to cool and wash the condenser

with distilled water into the flask.

Transfer the contents of the flask to a 500 ml conical flask and cool it

well.

Add 2 to 3 drops of ferroin indicator and titrate with ferrous

Ammonium sulfate solution.

The end point is the sharp colour change from blue green to reddish

brown.

Conduct a blank using distilled water in place of sample.

Calculation:-

Mg1l COD =

B = Ml of FAS used in titration of Blank sample.

S = Ml of FAS used in titration of sample.

Limit – 250 mg 1lt. max.

24

Page 25: Final TrainingReport

2. Oil & Grease :-

IS 3025 (P-39)

Limit 10 max.

Method:-

Silver Extraction Method

The determination of oil and grease includes all the substances that are

extractable by the specified solvent. Generally the substances that are

extractable are oils, fats and waxes. It is to be noted that the results obtained

indicates only the non-volatile fraction of these materials. Determination of

the volatile fraction is beyond the scope of this book.

Principle:-

Oil and grease, and other extractable matters are dissolved in suitable

solvent and separated from the aqueous phase. The solvent layer is then

evaporated and the residue is weighed as oil and grease.

Reagents:-

Sulfate Acid.

Petroleum ether

Procedure:-

25

Page 26: Final TrainingReport

Place 1000 ml or appropriate volume of the sample in a suitable

separating funnel.

Add 5 ml sulfuric acid per liter of sample.

Rinse the sample bottle with 15 ml petroleum ether and add the

rinsing to the separating funnel. Add further 25 ml ether to the funnel

and shake vigorously for 2 minutes.

Draw the aqueous phase in to a clear container and transfer the ether

layer through a filter paper containing enough sodium sulphate wetted

with petroleum ether to a clean, tarred distilling flask.

Continue the extraction twice and add the ether extracts to the

distilling flask after passing through a cone of anhydrous sodium

sulfate Na2SO4 to remove traces of water.

Distill off the ether in the distilling flask until about 10 ml remains in

the flask. Dry on water bath.

26