Acropolis Technical Campus, Indore

Department of Civil Engineering

Group/Title :Sampling techniques of
Environmental Engineering -I
Water
Evaluation Record Type/Session : Explorative / Jan-Jun.,2018
Name of the Student Enrollment No. 0875CE
Performing on First submission Second submission
Extra Regular

Grade and Remarks by the Tutor

1. Clarity about the objective of experiment
2. Clarity about the Outcome
3. Submitted the work in desired format
4. Shown capability to solve the problem
5. Contribution to the team work
Additional remarks

Grade: Cross the grade.

A B C D F
Tutor

1. Title:
Sampling techniques of water.

2. Outcome:
a) Students must understand the importance of sampling.
b) Students can collect the sample for determination of physical,chemical and biological
parameters of water.

3. Learning Objectives:
a) To know the procedure of sampling.
b) To collect the proper sample for determine the quality of water.
c) To confirm the presence or absence of contaminants in water.

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3. Theory:
SAMPLING

It is therefore important that all samples must be carefully collected, preserved, labeled and
immediately brought to the lab for prompt analytical work. Furthermore, choice of
sampling location, method of sampling and device, and frequency of sampling are all
important in obtaining representative sample.

METHOD OF SAMPLING:

Sampling may be grab, composite, or continuous measurement in situ. Grab samples are
single catch samples taken at a given time composite or integrated samples are taken at
constant time intervals usually over a 24- hour period, then pooled together to obtain one
representative sample of the day. Continuous measurement is done by installing measuring
device in situ.

GRAB SAMPLE:

When condition or quality remains relatively uniform over long periods. Examples are
lake, sludge digester, etc.

COMPOSITE SAMPLE:

Composite or integrated sampling is done to obtain the average quality data for the day.
Continuous sampler that removes the volume of sample in proportion to the flow is
desirable. Another type of composite sample removes sample within hour and deposits it
into different bottles. Volumes of sample from each bottle are mixed in proportion to flow
to obtain the composite average sample for the day. Individual hourly samples are the grab
sample representing the condition at that instant.

CONTINUOUS MEASUREMENT IN SITU:

Many measurements are taken continuously using inline measurement devices. Examples
of such measurements are velocity, flow, temperature, pH, conductivity, D0, chlorine
residual, ammonia, nitrogen, etc. Such measurement is generally recorded continuously,
and requires sophisticated measuring device or sensor, transmitter and recorded.

SAMPLING POINT AND FREQUENCY OF SAMPLING

Selection of sampling point is important in obtaining a representative sample accordingly.

The sampling points must be located where there is (1) good mixing of the flow to be
sampled, (2) uninfluenced by sludge or debris deposits, and (3) unaffected by other side
streams.

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The frequency of sampling depends on the flow rate and wastewater characteristics. If there
is low variability in flow and composition, manual grab samples suitable time intervals
may serve the purpose. For highly variable wastes the automatic samplers may be
necessary to collect samples at higher frequency.

SAMPLE SIZE AND HANDLINGS:

Approximately 2-litre portion of sample is sufficient for routine physical and chemical
analyses. Larger volumes may be necessary for special determinations. For microbiological
examination the samples should be collected separately since methods of collection and
handling are different.

All analyses should be conducted as so the following as possible. The following maximum
time durations between samplings and analytical work are suggested in the standard
methods.

Unpolluted water 72 hours

Slightly polluted waters 48 hours

Polluted waters 12 hours

The time and place of sampling and analysis should be recorded. If sample preservation is
used, the procedure for preservation should be fully described. The following results in
particular are sensitive to sampling handling techniques.

Microbiological, BOD, DO, Nitrogen- organic, ammonia, 𝑁𝑂2 and 𝑁𝑂3 ,Phosphorus-
organic and inorganic

Carbon dioxide- this may also change pH, alkalinity, and acidity

Certain cautions (Cu and Fe) may be lost due to absorption on the glass bottle.

WORK INSTRUCTIONS FOR SAMPLE WATER/ WASTE WATER RECEIVING:

1. SAMPLE LABELING AND CHAIN OF CUSTODY: - Sample labels, seals, field

logbook, chain of custody record, sample analysis request sheet, sample delivery to the
laboratory, receipt and logging of samples and assignment of sample for analysis.
2. All the sample should be received as soon as possible.
1. For unpolluted waters- 48 hrs.
2. For slightly polluted waters- 24 hrs
3. For polluted waters- 6 hrs

All the analysis should be conducted within 6-12 hrs. Depending upon the pollutants.

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WORK INSTRUTIONS FOR SAMPLE OF WATER/WASTEWATER DISPOSAL:

After testing all the sample are kept in air tight containers for 7-10 days and dispose them
in server line after giving proper treatment to remove polluted ingredients depending upon
the type of pollutants in the samples.

WORK INSTRUCTIONS FOR HANDLING OF LAB CHEMICALS:

All the lab chemicals should be handled with great care after wearing hand gloves, eye
glass and full sleeve shirt shoe which are not loose.

Self- assessment - 1
a) What are the types of sampling?
b) Define frequency of sample ?
c) What is sampling?
d) Describe handling of sample?

Cautions:
 Collect sample, where water is well mixed.
 Avoid large non-homogenous matter such as leaves, rags, twinges and other floating
material in the sample.
 Sample preferably collect at particular depth.
 Provide complete information on the source and conditions under which the sample was
collected.
 Attach a record tag to the sample container by noting sample number, source of sample,
analytical required, temperature and name of person taking the sample.

References:
 EPA(Environmental Protection Agency).
 NEERI (National Environmental Engineering Research Institute).
 WHO (World Health Organization).

4. Tutorial Questions/ Additional Questionnaire:

a) Why proper sampling is essential?
b) How are samples stored and preserved?

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Stepwise Procedure:
Following table gives the preservation required for some commonly required parameters.

Table
Parameters Container Preservative Max. holding
period
1 2 3 4
Acidity Glass(bsgb) Refrigeration at 40C 24 hours
Alkalinity Glass(bsgb) - do - 4 hours
BOD - do - - do - 24 hours
Calcium Plastic Not required -
COD Glass(bsgb&pec.) 2 ml H2SO4/ l pH -2 24 hours
Colour Refrigeration 24 hours
Cyanide PH -10 by NaOH 24 hours
DO Glass(BOD bottle) Fix on site 6 hours
Metals, total Plastic 5 ml HNO3/l 6 months
Dissolved metals - do - 40 filtrate : 3m11:1 6 months
HNO3/1
Ammonia Nitrogen - do - 40 mg HgCl2 / liter 24 hours
40 0 C
Kjeldahl Nitrogen - do - - do - Unstable
Nitrate – Nitrite Glass / plastic 40 mg MgCl2 / litre 24 hours
40 0 C
Oil & Grease 2 ml / litre H2SO4 – 24 hours
40 0 C
Organic carbons Glass To add HCl to – (pH 4 hours
-2)
Phenolics 1 g CuSO4 + H3PO4 24 hours
(pH: 4)
Phosphorus Glass 40 mg MgCl2/ l -40C 7 days
Sulphates Plastic / Glass 40C 7 days
Sulphide 2ml Zn Acetate /l 7 days
Silica Plastic Filter on site then - do -
40C

Polluted Liquid Sampling: -

When the liquid to be sampled contains oily or tarry matter or solids like those in sewage, it
is difficult to collect representative samples. At sewerage works, sampling should not be done
before screening. It should be done at a point in sewer where considerable turbulence is

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present. Oily substances form a film over the liquid and special procedure showed be followed
under these circumstance.

Sample for physical and Chemical Analysis: -

Samples should be collected in containers of Pyrex glass or other inert material like
polythene. Sample bottles must be carefully cleaned before use. Glass bottles may be rinsed
with a chromic acid cleaning mixture, made be adding one liter of concentrated sulphuric acid
slowly with stirring to 35 ml saturated sodium dichromate solution, or with an alkaline
permanganate solution followed by an oxalic acid solution . After having been cleaned, bottles
must be rinsed thoroughly with tap water and then with distilled water.

About 2.5 liters of the sample is required for analysis prior to filing, the sample bottle should
be rinsed out two or three times with water to be collected. Care should be taken to obtain a
sample that is truly representative of existing conditions and to handle it in such a way that it
does not deteriorate or become contaminated before it reaches the laboratory.

The sample should reach the place of analysis within 72 hours of collection. The time elapsed
between collection and analysis should be record of the laboratory report.Some determinations
are likely to be affected by storage of samples. Walls of glass containers are likely to-absorb
cations like aluminum, cadmium, chromium, copper, iron, lead, manganese ,silver or zinc
which are best collected in a separate bottle and acidified by concentrated hydrochloric or
nitric to a pH approximately 3.5 to minimize precipitation and absorption on the walls of the
container.

1. Sample collection from different sources ( for chemical analysis ) : -

The sample device consists of a hollow cylinder of about one or two liters capacity with
hinged flaps at either ends. Tape is fitted to the lower flap for withdrawing water from the
cylinder to other smaller bottle. The sample is attached to a cable of about 50 meter long
would over a width and provided with a depth recorder. Sometimes a thermometer is also
fitted for recording the temperature of water. The sample is lowered to the desired depth
with both flaps open. Now with some mechanical arrangements the flaps are closed. The
sample is hauled up and the sample is transferred to number of other sample bottles.

1.1 Sampling from water works system: -

In order to find out whether the processes of treatment are satisfactory, the proper sampling
points at different situations of water works system are selected. The sampling points
should be located from the place of entry of the raw water into the water works up to rising
main in the pumping station.

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1.2 Distribution system: -

For this the samples should be drawn from different mains and periphery of the
distribution system. For taking samples sterilized stand pipe must be used. Before taking
sample the pipe line should be flushed for a sufficient period to get a representative
sample.

1.3 Frequency of sampling: -

Test of free ammonia, nitrite, phosphate and silicate and chloride should be made once
in a week and complete analysis of raw and finished water once a fortnight or month. In
case of local contamination is suspected, radio chemical examination of the source of
raw water should be carried out at least once in a month.

1.2 Sampling for dissolved gases: -

Free C02, Dissolved H2S and residual chlorine special care and special bottles are
needed for testing each of the above gases. There should be minimum agitation of water of
contact with air. A piece of glass tubing is attached to the tap by means of a rubber tube.
The glass tube is taken upto the bottom of the bottle. The tap is opened and the bottle is
gently filled completely and allowed to overflow and then the stopper is replaced without
forming any air bubble. Analysis should be made at the spot of collection.

1.5 Special sample: -

Special sample is required for estimating Az, Cd, Cr, Cu, Fe, Pb, Mn, Ag and Zn
sample should be acidified immediately with concentrated HCL and HNO3 to a pH
values of about 3.0 in order to minimize the precipitation and absorption is the walls of
glass container.

1.5 Sample for Bacteriological Analysis : -

1.5.1 Sampling bottles: -

Sterilized glass bottles provided with ground glass stopper having an overlapping rim
should be used. The stopper and the neck of the bottle should be protected by brown
paper. The sterilization is carried out in an autoclave at 1kg/cm2 pressure for 15 minutes
or two hours under steam.

1.5.2 Dechlorination: -
Dechlorination is necessary for chlorinated water samples for this , sodium thiosulphate
should be added to the clean , dry sampling bottles before sterilization in an amount to
prove an approximately concentration of 100mg/l in the sample. This can be done by

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adding 0.2 ml of 10% thisosulphate solution to a 250 ml bottle. The bottle is then
sterilized by either dry or moist heat.

1.5.3Size of the sample:-

The volume of the sample should be sufficient for carrying out all the tests required and
in no case; it should be less than 200 ml.

1.5.4Preservation and storage: -

Water samples should be examined immediately after collection. However, this is seldom
practical and hence it is recommended that the samples should be preferably analyzed
within. One hour after collection and in no case this time should extend 24 hours. During
transit, the temperature of the sample should be maintained as close as possible be that of
the source of the sample, at the time of sampling. The time and temperature of storage of all
samples should be recorded since they will be considered in the interpretation of the
laboratory results.If they cannot be analyzed within 24 hours, the samples must be preserved
in ice until analysis. No sample is fit for bacteriological analysis after 72 hours.

6. Quizzes and Viva Questions:

1. What do you mean by grab sample?
2. What do you mean by composite sample?
3. How would you select the sampling point?
4. What guidelines should be followed while taking samples?
5. What are the time duration between sampling and analytical water are suggested?

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