T 264
Standard Method of Test for
Collection and Preservation of Water Samples
1. SCOPE
1.1 The objective of sampling is to
collect a portion of material small enough
in volume to be conveniently transported
to and handled in the laboratory while
still accurately representing the material
being sampled. This implies, first, that
the relative portions or concentrations of
all pertinent components must be the
same in the sample as in the material
being sampled, and second, that the
sample must be handled in such a way
that no significant changes in
composition occur before the tests are
performed. Complete and unequivocal
preservation of samples, either domestic
sewage, industrial waste, or natural
waters, is a practical impossibility.
Regardless of the nature of the sample,
complete stability for every constituent
can never be achieved. At best,
preservation techniques can only retard
the chemical and biological changes that
inevitably continue after the sample is
removed from the parent source.
1.2 The values stated in SI units are to be
regarded as the standard.
2. TYPES OF SAMPLES
2.1 Grab or Catch Samples-Strictly
speaking, a sample collected at a
particular time and place can represent
only the composition of the source at that
time and place. However, when a source
is known to be fairly constant in
composition over a considerable period
of time or over substantial distances irr
all directions, then the sample may be
said to represent a longer time period or a
larger volume, or both, than the specific
point at which it was collected. In such
circumstances, some sources may be
quite well represented by single grab
samples. Examples are some water
supplies, some surface waters, and rarely
some wastewater streams.
When a source is known to vary with
time, grab samples collected at suitable
intervals and analyzed separately can be
of great value in documenting the extent,
frequency, and duration of these
variations. Choose sampling intervals on
the basis of the frequency with which
changes may be expected, which may
METHODS OF SAMPLING AND TESTING
AASHTO DESIGNATION: T 264-78
vary from as little as 5 minutes to as long
as 1 hour or more.
When the composition of a source varies
in space rather than time, a set of samples
collected from appropriate locations with
less emphasis on timing may provide the
most useful information.
Use great care in sampling wastewater
sludges, sludge banks, and muds. No
definite procedure can be given, but
every possible precaution should be taken
to obtain a representative sample.
2.2 Composite Samples-In most cases,
the term composite sample refers to a
mixture of grab samples collected at the
same sampling point at different times.
Sometimes the term time-composite is
used when it is necessary to distinguish
this type of sample from others. Time-
composite samples are most useful for
observing average concentrations that are
used, for example, in calculating the
loading or the efficiency of a wastewater
treatment plant. As an alternative to the
separate analysis of a large number of
samples, followed by computation of
average and total results, composite
samples of this type represent a
substantial saving in laboratory effort and
expense. For these purposes, a composite
sample representing a 24-hour period is
considered standard for most determina-
tions. Under certain circumstances,
however, a composite sample represen-
ting one shift, or a shorter time period, or
a complete cycle of a periodic operation,
may be preferable. Evaluation of the
effects of special, variable, or irregular
discharges and operations may require
composite samples representing the
period during which such discharges
occurs.
For determination of components or
characteristics subject to significant and
unavoidable changes on storage,
composite samples cannot be used.
Perform such determinations on
individual samples as soon as possible
after collection and preferably at the
sampling point. Analyses for all
dissolved gases, residual chlorine, soluble
sulfide, temperature, and pH are
examples of determinations of this type.
Changes in such components as dissolved
oxygen or carbon dioxide, pH, or
temperature may produce secondary
changes in certain inorganic components
such as iron, manganese, alkalinity, or
hardness. Use time-composite samples
only for determining components that can
be demonstrated to remain unchanged
under the existing conditions of sample
collection and preservation.
Take individual portions in a widemouth
bottle having a diameter of at least 35
mm at the mouth and capacity of at least
120 mL. Collect these portions each
hour-in some cases half hour or even
every 5 minutes-and mix at the end of the
sampling period or combine in a single
bottle as collected. If preservatives are
used, add them to the sample bottle
initially so that all portions of the
composite are preserved as soon as
collected. Analysis of individual samples
may sometimes be necessary.
It is desirable, and often absolutely
essential, to combine the individual
samples in volumes proportional to the
volume of flow. A final volume of 2 to 3
liters is sufficient for sewage, effluents,
and wastes.
Automatic sampling devices are available
but should not be used unless the sample
is preserved as described below. Clean
sampling devices, including bottles, daily
to eliminate biological growths and other
deposits.
2.3 Integrated Samples-For certain
purposes, the information needed is
provided best by analysis of mixtures of
grab samples collected from different
points simultaneously, or as nearly so as
possible. Such mixtures sometimes are
called integrated samples. An example of
the need for such sampling occurs in a
river or stream that varies in composition
across its width and depth. For evaluation
of average composition or total loading, a
mixture of samples representing various
points in the cross-section, in proportion
to their relative flows, may be useful. The
need for integrated samples also may
exist if combined treatment is proposed
for several separate wastewater streams,
the interaction of which may have a
significant effect on treatability or even
the composition of the mixture.
Mathematical prediction of the
interactions may be inaccurate or
impossible and testing of a suitable
integrated sample may provide more
useful information.
Both natural and artificial lakes often
shown variations of composition with
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T 264
both depth and horizontal location.
However, under most conditions, neither
total nor average figures are especially
significant in these situations. The local
variations are of more importance, and
the samples are examined separately
rather than integrated.
The preparation of integrated samples
usually requires special equipment to
collect a sample from a known depth,
without contamination by the overlying
water. Prior knowledge about the
volume, movement, and composition of
the various parts of the water being
sampled usually is required. Therefore,
the collection of the integrated samples
becomes a complicated and specialized
process that cannot be described in
complete detail here.
3. FREQUENCY AND DURATION
OF SAMPLING
3.1 A reasonably accurate estimate of the
composition of a raw water piped from a
large body of water, such as the Great
Lakes, far enough from the shoreline to
avoid variation from inflowing tributaries
and waste discharges, may be made by
taking individual samples at infrequent
intervals, such as biweekly or monthly,
sufficient to cover seasonal changes. If
samples are taken from near the shoreline
of such a body of water or from a river,
take them at shorter intervals, for instan-
ce daily, to provide more exact know-
ledge of the variations in composi-tion
where these are of importance in the use
to which the water is to be put. If greater
variations or cycles of pollution occur or
closer surveillance of plant intake water
is required, collect more frequent
samples, for example, at hourly intervals.
3.2 Water undergoing continuous or
intermittent treatment must be sampled
with such frequency that adequate control
is assured. The interval between samples
is directly related to the rate at which
critical characteristics can reach
intolerable limits.
4. POINT OF SAMPLING
4.1 Choose the point of sampling with
extreme care so that a representative
sample of the water to be tested is
obtained. Avoid surface scum.
4.2 Because of a wide variety of con-
ditions found in streams, lakes, reservo-
irs, and other bodies of water, it is not
possible to prescribe the exact point of
sampling. Where the water in a stream is
mixed so as to approach uniformity, a
sample taken at any point in the cross
section is satisfactory. For large rivers or
METHODS OF SAMPLING AND TESTING
for streams not likely to be uniformly
mixed, more samples are desirable and
are usually taken at a number of points at
the surface across the entire width and at
a number of depths at each point. Take
care, when boats are used, to avoid
collecting samples where the turbulence
caused by a propeller or by oars has
disturbed the characteristics of the water.
Ordinarily, samples are taken at these
points and then combined to obtain an
integrated sample of such a stream of
water. Alternatively, test the single grab
samples, for example, to determine the
point of highest bacterial density.
4.3 Choose the location of the sampling
point with respect to the information
desired and in conformity to local condi-
tions. Allow sufficient distance downs-
tream, with respect to stream flow at the
time of sampling, from a tributary or
source of pollution to permit thorough
mixing. If this is not possible, it is better
to sample the stream above the tributary
or source of pollution and, in addition, to
sample the tributary or source of pollu-
tion. In general, a distance of 1.5 to 5 km
(1 to 3 miles) below the tributary is
sufficient.
4.4 Collect samples at least 0.8 km (0.5
miles) below dams or waterfalls to allow
time for the escape of entrained air.
When lakes, reservoirs, or other bodies of
water are sampled, it is necessary to
avoid non-representative areas such as
those created by inlet streams, more
stagnant areas, or abrupt changes in
shorelines, unless determining the effect
of such local conditions is a part of the
sampling program.
4.5 It is desirable to take a series of
samples from any source of water to
determine whether differences in
composition are likely to exist before
final selection of the sampling point.
5. SAMPLE CONTAINERS
5.1 Sample containers shall be made of
materials that will not contaminate the
sample and, before use, shall be cleaned
thoroughly to remove all extraneous
surface dirt. Chemically resistant glass
and polyethylene are suitable materials
for the containers. Only polyethylene
containers shall be used for samples in
which small amounts of hardness, silica,
sodium, or potassium are to be
determined. The collection, storage, and
subsequent analytical determination in
plastic containers will result in erroneous
pH values due to the permeability of
plastic to gases such as CO2.
NOTE-New chemically resistant glass
containers shall be conditioned by allowing
them to stand full of distilled water for several
days. Conditioning may be hastened by a
preliminary treatment with dilute hydrochloric
acid solution.
5.2 The closures for the sample
containers shall be glass stoppers that
have been thoroughly washed, or plastic
caps with suitable liners.
5.3 Refer to Table 1 for the
recommended container for individual
parameters.
6. GENERAL PRECAUTIONS
6.1 For sampling of unconfined water at
any specified depth in ponds, lagoons,
reservoirs, etc., during which contact
with air or agitation of the water would
cause a change in concentration of
characteristics of a constituent to be
determined, use a sampling apparatus so
constructed that the solution at the depth
to be sampled flows through a tube to the
bottom of the container, and that a
volume of sample equal to 4 to 10 times
the volume of the receiving container
passes through it. When no determi-
nations of dissolved gases are to be made,
any less complicated apparatus may be
used that will permit the collection of a
sample at a desired depth, or of an
integrated sample containing water from
all points in a vertical section.
6.2 Some test methods require adjust-
ment to other than ambient temperature.
Such adjustment should be carried out
when indicated.
6.3 Normally, samples are taken without
separation of particulate matter. If cons-
tituents are present in colloidal or
flocculent suspension take the sample so
that they are present in representative
portion.
6.4 Volume of sample:
6.4.1 Collect a minimum volume of 2
liters; 4 liters is preferable.
6.4.2 The estimates in Table 1 cover
the volume of sample required for the
usual determinations that are made on a
water sample as well as for several tests
that are made for special purposes.
6.4.3 The sample volume required for
bacteriological analysis varies greatly
with the bacterial density of the water.
Serial dilutions are necessary for high
density samples.
6.5 When samples are to be shipped, do
not fill the bottle entirely in order to
allow some room for expansion when
subjected to a change in temperature. An
air space of 10 to 25 mL usually suffices
for this purpose, although this does not
protect against bursting of the container
due to freezing.
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T 264 METHODS OF SAMPLING AND TESTING

6.6 If contact with air would cause a TABLE 1 Recommendation for Sampling and Preservation of Samples According to
change in the concentration or Measurement6
Volume
characteristics of a constituent to be Measurement
Req., mL
Container Preservative Holding Time°
determined, secure the sample without Acidity 100 P,G2 Cool, 4°C 24 hours
contact with air and completely fill the Alkalinity 100 P, G Cool, 4°C 24 hours
container. Arsenic 100 P, G HNO3 to pH < 2 6 months
BOD 1000 P. G Cool, 4°C 6 hours'
6.7 Microbiological samples: Bromide 100 P, G Cool, 4°C 24 hours
6.7.1 When taking a sample from a COD 50 P. G H2SO4 to pH < 2 7 days
Chloride 50 P, G None required 7 days
sample line or tap, allow the water to run
Chlorine req. 50 P, G Determine on site No holding
for at least 5 minutes or long enough to Color 50 P, G Cool, 4°C 24 hours
flush, with 6 to 10 times its volume, the Cyanides 500 P, G Cool, 4°C 24 hours
entire part of the system that has been NaOh to pH<2
stagnant for 2 hours or more. Dissolved oxygen:
Probe 300 G only Determine on site No holding
6.7.2 Turn off the sample outlet and Winkler 300 G only Fix on site 4 to 8 hours
empty it of water without touching the Fluoride 300 P. G Cool, 4°C 7 days
inside. Flame the outlet with a suitable Hardness 100 P. G Cool, 4°C 7 days
HNO3 to pH < 2
torch or other devise that will avoid the Iodide 100 P, G Cool, 4°C 24 hours
deposition of soot, which is undesirable. MBAS 250 PG Cool, 4°C 24 hours
This flaming procedure may be omitted Metals:
if the outlet is carefully cleaned by use of Dissolved 200 PG Filter on site 6 months
HNO3 to pH < 2
a swab of cotton or other suitable Suspended Filter on site 6 months
material thoroughly saturated with Total 100 HNO3 to pH < 2 6 months
denatured ethyl alcohol (70 percent). Mercury:
Dissolved 100 P. G Filter 38 days (glass)
6.7.3 Choose a sterile sample bottle HNO to pH < 2 13 days (hard plastic)
containing Na2S2O3 if the water being Total 100 P. G HNO3 to pH 2 38 days (glass)
sampled contains residual chlorine, has 13 days (hard plastic)
been chlorinated, or contains any free or Nitrogen:
Ammonia 400 P. G Cool. 4°C 24 hours4
combined available oxidizing agent H2SO4 to pH < 2
intended to sterilize it. If such sterilizing Kjeldahl 500 P. G Cool, 4°C 7 days
agents are not present, the thiosulfate Total H2SO4 to pH < 2
may be omitted. In cases where Nitrate 100 P. G Cool, 4°C 24 hours4
thiosulfate interferes with subsequent H2SO4 to pH < 2
Nitrite 50 P. G Cool, 4°C 24 hours4
examination, such as examination for NTA 50 P. G Cool, 4°C 24 hours
sulfatereducing bacteria, etc., omit the Oil and grease 1000 G only Cool, 4°C 24 hours
use of thiosulfate in the sample bottle H2SO4 to pH < 2 or HCl
even if such sterilizing agents are Organic carbon 25 P. G Cool, 4°C 24 hours
H2SO4 to pH < 2
present. In this case, if such sterilizing pH 25 P. G Cool, 4°C Determine on site 6 hours4
agents are present, the examination must Phenolics 500 G only Cool, 4°C 24 hours
be performed as soon as possible. H3PO4 to pH < 4
1. O g CUSO4/I
6.7.4 Remove the stopper from the Phosphorous:
sample bottle. Grasp the stopper by the Orthophosphate, dissolved 50 P. G Filter on site 24 hours4
dust cover so as not to contaminate it by Cool, 4°C
touching it; do not lay it down. Hold the Hydrolyzable 50 P, G Cool. 4°C 24 hours4
Total 50 P, G Cool, 4°C 7 Days
bottle by the bottom to avoid touching H2SO4 to pH < 2
the neck. Do not rinse the bottle with the Total, dissolved 50 P, G Filter on site 24 hours'
sample. Quickly hold the bottle under the Cool, 4°C
flowing water to be sampled until it is Residue:
Filterable 100 PG Cool, 4°C 7 days
about three-fourths full to permit mixing Nonfilterable 100 PG Cool, 4°C 7 days
by shaking prior to testing. Replace the Total 100 PG Cool, 4°C 7 days
stopper and promptly crimp the metal Volatile 100 PG Cool, 4°C 7 days
dust cover in place over the neck of the Settleable matter 1000 PG None required 24 hours
bottle. Take care that the stopper and Selenium 50 PG HNO3 to pH < 2 6 months
Silica 50 P only Cool, 4°C 7 days
bottle neck are not touched during this Specific conductance 100 PG Cool, 4°C 24 hours5
operation and that no dust blows into the Sulfate 50 PG Cool, 4°C 7 days
bottle, insofar as possible. Sulfide 500 P.G 2 mL zinc acetate 24 hours
Sulfite 50 PG Determine on site No holding
Temperature 1000 PG Determine on site No holding
7. PRESERVATION OF SAMPLES Treshold odor 200 G only Cool, 4°C 24 hours
Turbidity 100 P.G Cool, 4°C 7 days
1 More specific instructions for preservation and sampling are found with each procedure as detailed in the
7.1 Add chemical preservatives to appropriate reference.
2 Plastic or glass.
samples for chemical, physical, or 3 If samples cannot be returned to the laboratory in less than 6 hours and holding time exceeds this limit, the
radiological examination only as final reported data should indicate the actual holding time.
specified in Table 1. Quick freezing has 4 Mercuric chloride may be used as an alternate preservative at a concentration of 40 mIJL, especially if a
longer holding time is required. However, the use of mercuric chloride is discouraged whenever possible.
been found to be beneficial in preserving 5 If the sample is stabilized by cooling. it should be warmed to 25°C for reading, or temperature correction
some organic constituents. Note any made and results reported at 25°C.
preservatives added on the label. 6 It has been shown that samples properly preser, ed may be held for extended periods beyond the
recommended holding time.

594
T 264
7.2 Samples for bacteriological
examination require refrigeration if they
cannot be processed within 1 hour after
collection.
7.3 If the sample is to be examined
within 1 hour of collection, store it in a
cool place without icing.
7.4 If the sample is held more than 1
hour before examination, store it in a
refrigerator or ice chest at a temperature
of not more than 4°C. The interval
between collection and examination of
the sample must in no case be more than
12 hours, or 6 hours if the sample is
suspected to contain large numbers of
organisms. Field examination procedures
should be considered for longer periods.
7.5 If the sample is transported, ship it in
an insulated, iced container to maintain
the temperature between 0 and 4°C to
allow it to be examined within 12 hours
of collection.
7.6 If the conditions in Section 7.4 or 7.5
cannot be met, note the actual conditions
on the examination report.
8. TIME INTERVAL BETWEEN
COLLECTION AND ANALYSIS
OF SAMPLES
8.1 In general, allow as short a time as
possible to elapse between the collection
of a sample and its analysis. Under some
conditions, analysis in the field is
necessary to secure reliable results. The
actual time that may be allowed to
intervene between the collection and
analysis of a sample varies with the type
of examination to be conducted, the
character of the sample, and the time
interval allowable for applying corrective
treatment.
METHODS OF SAMPLING AND TESTING
8.2 On the statement of an analysis,
specify the length of time elapsed
between collection and analysis of the
sample.
8.3 Make the determination of dissolved
gases, such as oxygen, hydrogen sulfide,
and carbon dioxide at the source, except
that in some cases such constituents may
be fixed and determined later as specified
in the specific test methods.
8.4 When sampling for radioactivity
determinations, note the exact time of
sample collection. If short-lived activity
is of interest, analysis should be made as
rapidly as practical to minimize loss of
activity by radioactive decay. If only
long-lived activity is of interest,
measurement of the radioactivity
sometimes can be simplified by allowing
sufficient time before analysis for the
decay of the short-lived radionuclides.
9. LABELING AND TRANSPORTA-
TION OF SAMPLES
9.1 Provide space for the following
information on an etched area of the
bottle, a gummed label, or a cardboard or
linen tag securely affixed to the
container:
Sample number,
Date and time of sampling, Source of
sample,
Point of sampling (designated in
sufficient detail to enable anyone to
collect a second sample from the
identical spot rom which the first sample
was taken),
Temperature and rate of flow of the
fluid in the equipment from which the
sample as taken,
Temperature of sample,
Type and quantity of preservative
added,
Results of field tests made on the
sample,
Signature of sampler.
9.2 Fix the stoppers closing the sample
containers in place by wire, tape, or cord
to prevent leakage in transit. The sample
containers shall be of such size that when
filled with the desired amount of sample,
space roughly equivalent to 1 percent of
the volumetric capacity of the containers
will be available for expansion of the
liquid. Exceptions to this are for those
constituents noted in Section 8.3.
9.3 The sample shipping container shall
be a case (wood preferred) having a
separate compartment for each sample
container. Line the compartment around
each sample container with corrugated
paper, felt, or similar material; or hold
the sample containers in place with
spring clips, sawdust, excelsior, foamed
plastic, or similar material. Use insulated
containers for quick-frozen samples,
usually shipped with solid carbon dioxide
to maintain the sample in frozen
condition.
9.4 Print the addresses of consignee and
consignor plainly upon two sides of the
outer container, or attach firmly thereon
by cards or labels. Attach warning and
descriptive labels to the outer container
such as "Fragile," "Liquid," "Glass,"
"Handle With Care," "This Side Up,"
etc., when applicable. In cold weather,
attach the label "Keep from Freezing" to
the outer container, except for those
samples which are intentionally frozen.
595