-------
of the T-handle swivel. The closure system of the sampler consists of
a sharply taped neoprene stopper attached to a 0.95-cm (3/8-in.) O.D.
rod, usually PVC. The upper end of the stopper rod is connected to
the swivel of the aluminum T-handle. The sharply tapered neoprene
stopper can be fabricated according to specifications by plastic products
manufacturers at an extremely high price, or it can be made in-house by
grinding down the inexpensive stopper with a shop grinder as described in
Note 1 of Appendix B.
Two types of Coliwasa samplers are made, namely plastic or glass.
The plastic type consists of translucent plastic (usually PVC) sampling
tube. The glass Coliwasa uses borosilicate glass plumbing pipe as the
sampling tube and Teflon plastic stopper rod.
The complete list of parts for constructing the two types of Coliwasa
samplers is given in Appendix B. The suppliers and approximate costs of
the parts as well as the directions for fabricating the commercially
unavailable parts are also given.
1.
3.
4.
7.
Uses
The sampler is assembled as shown in Figure 1 and as follows:
Attach the swivel to the T-handle with the 3.18 cm(l% in.) long
bolt and secure with the 0.48 cm(3/16 in.) National Coarse(NC)
washer and lock nut.
Attach the neoprene stopper to one end of the stopper rod and
secure with the 0.95 cm(3/8 in.) washer and lock nut.
Install the stopper and stopper rod assembly in the sampling tube.
Secure the locking block sleeve on the block with glue or screws.
This block can also be fashioned by shaping a solid plastic rod
on a lathe to the required dimensions.
Position the locking block on top of the sampling tube such that
the sleeveless portion of the block fits inside the tube, the
sleeve sits against the top end of the tube, and the upper end of
the stopper rod slips through the center hole of the block.
Attach the upper end of the stopper rod to the swivel of the
T-handle. ;
Place the sampler in the close position and adjust the tension on
the stopper by screwing the T-handle in or out.
The plastic Coliwasa is used to sample most containerized liquid
wastes except wastes that contain ketones, nitrobenzene, dimethylforamide,
mesityl oxide, and tetrahydrofuran. '
-------
The glass Coliwasa is used to sample all other containerized liquid
wastes that cannot be sampled with the plastic Coliwasa except strong
alkali and hydrofluoric acid solutions.
Procedure for Use
1. Choose the plastic or glass Coliwasa for the liquid waste to be
sampled and assemble the sampler as shown in Figure 1.
2. Make sure that the sampler is clean (see Section 5).
3. Check to make sure the sampler is functioning properly. Adjust
the locking mechanism if necessary to make sure the neoprene
rubber stopper provides a tight closure.
4. Wear necessary protective clothing and gear and observe required
sampling precautions (see Section 6).
5. Put the sampler in the open position by placing the stopper rod
handle in the T-position and pushing the rod down until the handle
sits against the sampler's locking block.
6. Slowly lower the sampler into the liquid waste. (Lower the sampler
at a rate that permits the levels of the liquid inside and outside
the sampler tube to be about the same. If the level of the liquid
in the sampler tube is lower than that outside the sampler, the
sampling rate is too fast and will result in a nonrepresentative
sample).
7. When the sampler stopper hits the bottom of the waste container,
push the sampler tube downward against the stopper to close the
sampler. Lock the sampler in the close position by turning the T
handle until it is upright and one end rests tightly on the locking
block. \
8. Slowly withdraw the sampler from the waste container with one hand
while wiping the sampler tube with a disposable cloth or rag with
the other hand.
9. Carefully discharge the sample into a suitable sample container
(see Section 6) by slowly opening the sampler. This is done by
slowly pulling the lower end of the T handle away from the locking
block while the lower end of the sampler is positioned in a sample
container.
10. Cap the sample container; attach label and seal; record in field
log book; and complete sample analysis request sheet and chain of
custody record.
-------
11. Unscrew the T handle of the sampler and disengage the locking
block. Clean sampler on site (see Section 5) or store the con-
taminated parts of the sampler in a plastic storage tube for
subsequent cleaning. Store used rags in plastic bags for
subsequent disposal.
12. Deliver the sample to the laboratory for analysis (see Section 6).
SOLID WASTE SAMPLERS
A number of tools are available for sampling solid substances. The
most suitable of these for sampling hazardous solid wastes are the grain
sampler, sampling trier, and the trowel or scoop.
Grain Sampler
The grain sampler (Figure 2) consists of two slotted telescoping
tubes, usually made of brass or stainless steel. The outer tube has a
conical, pointed tip on one end that permits the sampler to penetrate the
material being sampled. The sampler is opened and closed by rotating the
inner tube. Grain samplers are generally 61 to 100 cm (24 to 40 in.)
long by 1.27 to 2.54 cm (% to 1 in.) in diameter, and they are commercially
available at laboratory supply houses.
Uses—
The grain sampler is used for sampling powdered or granular wastes
or materials in bags, fiberdrums, sacks or similar containers. This
sampler is most useful when the solids are no greater than 0.6 cm (h in.)
in diameter.
Procedure for Use—
1. While the sampler is in the close position, insert it into the
granular or powdered material or waste being sampled from a point
near a top edge or corner, through the center, and to a point
diagonally opposite the point of entry.5
2. Rotate the inner tube of the sampler into the open position.
3. Wiggle the sampler a few times to allow materials to enter the
open slots.
4. Place the sampler in the close position and withdraw from the
material being sampled.
5. Place the sampler in a horizontal position with the slots facing
upward.
6. Rotate and slide out the outer tube from the inner tube.
-------
7. Transfer the collected sample in the inner tube into a suitable
sample container (see Section 6).
8. Collect two or more core samples at different points (see Section
6), and combine the samples in the same container.
9. Cap the sample container; attach label and seal; record in field
log book; and complete sample analysis request sheet and chain
of custody record. I
10. Clean (see Section 5) or store the sampler in plastic bag for
subsequent cleaning.
11. Deliver the sample to the laboratory for analysis (see Section 6).
61-100 cm, !-
(24-40")
1.27-2.54 cm (%-!")
Figure 2. Grain sampler.
10
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61-100 cm,
(24-40")
X
\
1.27-2.54 cm (%-!")
Figure 3. Sampling trier.
Sampling trier
A typical sampling trier (Figure 3) is a long tube with a slot that
extends almost its entire length. The tip and edges of the tube slot are
sharpened to allow the trier to cut a core of the material to be sampled
when rotated after insertion into the, material. Sampling triers are
usually made of stainless steel with wooden handles. They are about 61
to 100 cm (24 to 40 in.) long and 1.27 to 2.54 cm (% to 1 in.) in diameter.
They can be purchased readily from laboratory supply houses.
Uses—
The use of the trier is similar to that of the grain sampler dis-
cussed above. It is preferred over the grain sampler when the powdered or
11
-------
granular material to be sampled is moist or sticky.
In addition, the sampling trier can be used to obtain soft or loosened
soil samples up to a depth of 61 cm(24 in.) as outlined below.
Procedure for Use—
1. Insert the trier into the|waste material at a 0 to 45° angle from
horizontal. This orientation minimizes the spillage of sample
from the sampler. Extraction of samples might require tilting of
the containers.
2. Rotate the trier once or twice to cut a core of material.
[
3. Slowly withdraw the trierj making sure that the slot is facing
upward.
4. Transfer the sample into a suitable container (see Section 6) with
the aid of a spatula and/or brush.
i
5. Repeat the sampling at different points (see Section 6). Two or
more times and combine the samples in the same sample container.
6. Cap the sample container; attach the label and seal; record in
field log book; and complete sample analysis request sheet and
chain of custody record.
j
7. Wipe the sampler clean, or store it in a plastic bag for subsequent
cleaning.
8. Deliver the sample to the laboratory for analysis (see Section 6).
Trowel or Scoop
A garden-variety trowel looks like a small shovel (Figure 4). The
blade is usually about 1 by 13 cm(3 by 5 in.) with a sharp tip. A labor-
atory scoop is similar to the trowel, but the blade is usually more curved
and has a closed upper end to permit the containment of material. Scoops
come in different sizes and makes. Stainless steel or polypropylene scoops
with 7 by 15-cm(2 3/4 by 6-in.) blades are preferred. A trowel can be
bought from hardware stores; the scoop can be bought from laboratory supply
houses.
Uses— i
An ordinary zinc-plated gar|den trowel can be used in some cases for
sampling dry granular or powderejd materials in bins or other shallow con-
tainers. The laboratory scoop, however, is a superior choice. It is
usually made of materials less subject to corrosion or chemical reactions,
thus lessening the probability o£ sample contamination.
12
-------
The trowel or scoop can also be used in collecting top surface soil ,
samples.
Procedure for Use—
1. At regular intervals (see Section 6), take small, equal portions of
sample from the surface or near the surface of the material to be
sampled.
2. Combine the samples in a suitable container (see Section 6).
3. Cap the container; attach the label and seal; record in field log
book; and complete sample analysis request sheet and chain of
custody record.
4. Deliver the sample to the laboratory for analysis (see Section 6).
SOIL SAMPLERS
There is a variety of soil samplers used. For taking soil core
samples, the scoop, sample trier, soil auger, and Veihmeyer sampler can be
used. These samplers are commercially available and relatively inexpensive.
Scoop or Trowel
See the preceding section on solid waste samplers for the description
of a scoop or trowel (Figure 4).
Figure 4. Trowel or scoop with calibrations.
13
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Uses—
The scoop is used to collect; soil samples up to 8 cm(3 in.) deep.
It is simple to use, but identical mass sample units for a composite sample
are difficult to collect with this sampler. The procedure for use of the
scoop is outlined in the preceding section on solid waste samplers.
Sampling Trier j
j
See the preceding section on solid waste samplers for the description
of a sampling trier (Figure 3).
Uses— |
This sampler can be used to [collect soil samples at a depth greater
than 8 cm(3 in.)« The sampling depth is determined by the hardness and
types of soil being sampled. This sampler can be difficult to use in
stony, dry, very heavy, or sandy soil. The collected sample tends to be
slightly compacted, but this method permits observation of the core sample
before removal.
Procedure for Use—
Procedure for use of the sampling trier can be found in the section
on solid waste samplers. !
Soil Auger
This tool consists of a hard metal central shaft and sharpened spiral
blades (Figure 5). When the tool is rotated clockwise by its wooden
T handle, it cuts the soil as it moves forward and discharges most of the
loose soil upward. The cutting diameter is about 5 cm(2 in.). The length
is about 1 m(40 in.), with graduations every 15.2 cm(6 in.). The length
can be increased up to 2 m(80 in.). This tool can be bought from stores
and, in some cases, from laboratory supply houses.
|
Uses—
The auger is particularly useful in collecting soil samples at depths
greater than 8 cm(3 in.). This sampler destroys the structure of cohesive
soil and does not distinguish between samples collected near the surface
or toward the bottom. It is not recommended, therefore, when an undis-
turbed soil sample is desired.
Procedure for Use—
1. Select the sampling point (see Section 6) and remove unnecessary
rocks, twigs, and other nonj-soi'l materials.
14
-------
2. Install the sampler's wooden T handle in its socket.
3. Bore a hole through the middle of an aluminum pie pan large enough to
allow the blades of the auger to pass through. The pan will be used
to catch the sample brought to the surface by the auger.
4. Spot the pan against the selected sampling point.
5. Start augering through the hole in the pan until the desired sampling
depth is reached.
6. Back off the auger and transfer the sample collected in the catch pan
and the sample adhering to the auger to a suitable container (see
Section 6). Spoon out the rest of the loosened sample with a sampling
trier.
7. Repeat the sampling at different sampling points (see Section 6), and
combine the samples in the same container as in step 6.
8. Cap the sample container; attach label and seal; record in field log
book; and complete sample analysis request sheet and chain of cus-
tody record.
9. Brush off and wipe the sampler clean, or store it in a plastic bag
for subsequent cleaning.
10. Deliver the sample to the laboratory for analysis (see Section ,6).
101.6 cm (40")
5o08 cm (2")
Figure 5. Soil auger.
15
-------
A. Drive hammer
B. Head
C. Tube
D. Point
Standard point
\ /
Constricted point
Bulge point
Special point
Point types
Puller jack and grip
Figure 6. Veihmeyer sampler
16
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Veihmeyer Soil Sampler
This sampler was developed by Professor F.J. Veihmeyer of the Univer-
sity of California in Davis.' The parts of a basic sampler and the corres-
ponding costs are given in Table 1, and the basic sampler is shown in
Figure 6.
TABLE 1. BASIC PARTS AND COSTS OF A VEIHMEYER SOIL SAMPLER
Parta
Costc
Tube, 1.5 m (5 ft.)
Tube, 3m (10 ft.)
Tip, type A, general use
Drive head
Drop hammer, 6.8 kg (15 Ib.)
Puller jack and gripc
Total
$ 50.40
84.75
25.80
29.05
71.85
161.90
$ 433.75
a Only one of each part is needed. They are manufactured by
Hansen Machine Works, 334 N. 12th Street, Sacramento, CA
95815.
b Based on August 1, 1977, price list.
c Recommended for deep soil sampling.
The tube is chromium-molybdenum steel and comes in various standard
lengths from 0.91 to 4.9 m(3 to 16 ft.) and calibrated every 30.48 cm(12
in.). Longer tubes can be obtained on special order. Different points
(Figure 6) are also available for different types of soil and sampling.
Each point is shaped to penetrate specific types of soil without pushing
the soil ahead of it, thus preventing the core from compacting in the tube.
The standard point is adequate for most general sampling purposes. The
inside taper of each point is designed to keep the sample from being
sucked out of the tube as it is pulled from the ground. The drive head
protects the top of the tube from deforming when the tube is driven into
the ground with the drive hammer. The hammer doubles as a drive weight
and handle when pulling the sampler from the ground. When the sampler tube
cannot be pulled easily from the ground, a special puller jack and grip
17
-------
are also available. Specificatiojis for the various parts of the Veihmeyer
sampler are given as follows: j
I
Points Chrome-molly steel, heat-treated. Includes a
standard polint for general use, a constricted
point for deep sampling in heavy clay (keeps
core from hieing sucked out of the tube) , a
bulge point for shallow sampling in heavy clay,
and a special point for dry sand. (See Figure
6D). i
Drive hammer
Tubes
Head
Puller jack
Grip
. Standard weight is 6.8 kg (15 lb.). (See Figure 6A)
. Chrome-molljy steel. Maximum length is 4.9 m
(16 ft.). i(See Figure 6C) .
. Chrome-molly steel, heat-treated. (See Figure 6B).
. Cast aluminum frame with steel roller assembly
and handle.!
i
. Chrome-molljy steel, heat-treated.
Uses—
The Veihmeyer sampler is recommended for core sampling of most types
of soil. It may not be applicablfe to sampling stony, rocky, or very wet
soil. !
Procedure for Use—
i
1. Assemble the sampler by screwing in the tip and the drive head on
the sampling tube. |
2. Insert the tapered handle (drive guide) of the drive hammer through
the drive head.
3. Place the sampler in a perpendicular position on the soil to be
sampled. i
i
4. With the left hand holding {the tube, drive the sampler into the
ground to the desired sampling depth by pounding the drive head
with the drive hammer. Do hot drive the tube further than the
tip of the hammer's drive gjjide.
i
5. Record the length of the tube that penetrated the ground.
6. Remove the drive hammer and!fit the keyhole-like opening on the flat
side of the hammer onto the1drive head. In this position, the ham-
mer serves as a handle for the sampler.
18
-------
I
7. Rotate the sampler at least two revolutions to shear off the sample
at the bottom.
Lower the sampler handle (hammer) until it just clears the two ear-
like protrusions on the drive head and rotate about 90°.
Withdraw the sampler from the ground by pulling the handle (hammer)
upwards. When the sampler cannot be withdrawn by hand, as in deep
soil sampling, use the puller jack and grip.
Dislodge the hammer from the sampler; turn the sampler tube upside
down; tap the head gently against the hammer; and carefully recover
the sample from the tube. The .sample should slip out easily.
Store the core sample, preferably, in a rigid, transparent, or trans-
lucent plastic tube when observation of soil layers is to be made.
The use of the tube will keep the sample relatively undisturbed. In
other cases, use a 1000-or 2000-ml (1-qt. or %-gal) sample container
(see Section 6) to store the sample.
12. Collect additional core samples at different points (see Section 6).
8.
9.
10.
11.
13.
Label the samples; affix the seals; record in the field log book;
complete analysis request sheet and chain of custody record; and
deliver the samples to the laboratory for analysis (see Section 6)
Waste Pile Sampler
A waste pile sampler (Figure 7) is essentially a large sampling trier.
It is commercially available, but it can be easily fabricated from sheet
metal plastic pipe. A polyvinyl chloride plumbing pipe 1.52 m(5 ft ) long
by 3.2 cm(lJz; in.) I.D. by 0.32 cm(l/8 in.) wall thickness is adequate. The
pipe is sawed lengthwise (about 60/40 split) until the last 10 cm(4 in.)
The narrower piece is sawn off and hence forms a slot in the pipe. The
edges of the slot and the tip of the pipe are sharpened to permit the
sampler to cut into the waste material being sampled. The unsplit length
of the pipe serves as the handle. The plastic pipe can 'be purchased from
hardware stores.
Uses—
The waste pile sampler is used for sampling wastes in large heaps with
cross-sectional diameters greater than 1 m(39. 4 in.). It can also be used
for sampling granular or powdered wastes or materials in large bins, barges,
or silos where the grain sampler or sampling trier is not long enough.
This sampler does not collect representative samples when the diameters of
the solid particles are greater than half the diameter of the tube.
Procedure for Use—
19
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1. Insert the sampler into the waste material being sampled at 0 to 45°
from horizontal. !
2. Rotate the sampler two or three times in order to cut a core of the
material. |
3. Slowly withdraw the sampler, making sure that the slot is facing
upward. ;
4. Transfer the sample into ajsuitable container (see Section 6) with
the aid of a spatula and/or brush.
i
5. Repeat the sampling at different sampling points (see Section 6) two
or more times and combine the samples in the same sample container in
step 4.
6. Cap the container; attach label and seal; record in field log book;
and complete sample analysis request sheet and chain of custody
record.
7. Wipe the sampler clean or store it in a plastic bag for subsequent
cleaning.
8. Deliver the sample to 'the laboratory for analysis (see Section 6).
1
122-183 bm
(48-72"!)
•it
5.08-7o62 cm
(2-3") I.D.
Pond Sampler
Figure 7. Waste pile sampler.
The pond sampler (Figure 8)1 consists of an adjustable clamp attached
to the end of a two or three piepe telescoping aluminum tube that serves
as the handle. The clamp is used to secure a sampling beaker. The sampler
is not commercially available, but it is easily and inexpensively fabri-
20
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cated. The tubes can be readily purchased from most hardware or swimming
pool supply stores. The adjustable clamp and sampling beaker can be
obtained from most laboratory supply houses. The materials required to
fabricate the sampler are given in Table 2.
-Varigrip clamp
-/A
Bolt hole
Beaker, polyprop-
ylene, 250 ml
(1 qt)
Pole, telescoping, aluminum, heavy
duty, 250-450 cm (96-180")
Figure 8. Pond sampler.
TABLE 2. BASIC PARTS AND APPROXIMATE COSTS OF A POND SAMPLER
Quantity
Item
Supplier
Approximate
Cost-
1
4
4
Clamp, adjustable, 6.4 to
8.9 cm(2% to 3% in.) for
250-to 600-ml(% to 1%-pt.)
beakers
Tube, aluminum, heavy duty,
telescoping extends 2.5 to
4.5 m(8 to 15 ft.) with
joint cam locking mechanism.
Pole diameters 2.54 cm(l in.)
I.D. and 3.18 cm(l% in.) I.D.
Beaker, polypropylene,
250-ml(% pt.)
Bolts, 6.35 by 0.64 cm(2%.by
Vin.) NC
Nuts, 0.64 cm(% in.) NC
. Total
Laboratory supply
houses
Olympic Swimming
Pool Co. 807 Buena
Vista Street, Alameda,
Calif. 94501 or other
general swimming pool
supply houses.
Laboratory supply
houses.
Hardware stores
Hardware stores
$7.00
16.24
1.00
.20
.20
$24.64
21
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Uses—
The pond sampler is used toi collect liquid waste samples from disposal
ponds, pits, lagoons, and similar reservoirs. Grab samples can be obtained
at distances as far as 3.5 m(.ll% ft ) from the edge of the ponds. The
tubular aluminum handle may bow when sampling very viscous liquids if
sampling is not done slowly.
Procedure for Use—
1. Assemble the pond sampler.' Make sure that the sampling beaker and
the bolts and nuts that sepure the clamp to the pole are tightened
properly. |
I
2. With proper protective garment and gear (.see Section 6), take grab
samples from the pond at different distances and depths (see Section
6). :
3. Combine the samples in one suitable container (see Section 6).
I
4. Cap the container; label and affix the seal; record in field log
book; and complete sample analysis request sheet and chain of
custody record.
5. Dismantle the sampler; wipe the parts with terry towels or rags and
store them in plastic bags for subsequent cleaning. Store used
towels or rags in garbage bags for subsequent disposal.
6. Deliver the sample to the laboratory for analysis (.see Section 6).
Weighted Bottle Sampler
This sampler (Figure 9) consists of a bottle, usually glass, a weight
sinker, a bottle stopper, and a line that is used to open the bottle and to
lower and raise the sampler during sampling. There are a few variations
of this sampler, as illustrated in the ASTM Methods D 2708 and E 3009.
The ASTM sampler, which uses a metallic bottle basket that also serves as
weight sinker, is preferred. The weighted bottle sampler can either be
fabricated or purchased.
Uses—
The weighted bottle sampler)can be used to sample liquids in storage
tanks, wells, sumps, or other containers that cannot be adequately sampled
with a Coliwasa. The sampler cannot be used to collect liquids that are
incompatible or that react chemically with the weight sinker and line.
Procedure for use—
1. Assemble the weighted bottle sampler as shown in Figure 9.
22
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Using protective sampling equipment, in turn, lower the sampler to
proper depths to collect the following samples:
a) upper sample - middle of upper third of tank contents.
b) middle sample - middle of tank contents.
c) lower sample - near bottom of tank contents.
Pull out the bottle stopper with a sharp jerk of the sampler line.
Allow the bottle to fill completely, as evidence by the cessation of
air bubbles.
Raise the sampler and retrieve and cap the bottle. Wipe off the out-
side of the bottle with a terry towel or rag. The bottle can serve
as the sample container.
Label each of the three samples collected; affix seal; fill out sample
analysis request sheet and chain of custody record; record in the
field log book.
Clean onsite or store contaminated sampler in a plastic bag for sub-
sequent cleaning.
Deliver the sample to the laboratory for analysis (see Section 6).
Instruct the laboratory to perform analysis on each sample or a
composite of the samples.
Washer
Pin
Eyelet
Cork
Washer
Nut
1000-ml (1-quart) weighted
bottle catcher
Figure 9. Weighted bottle sampler.
23
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SECTION 5
PREPARATION FOR SAMPLING
GENERAL CONSIDERATIONS
Adequate preparation for sampling is necessary to perform proper sam-
pling of any hazardous waste. A checklist of items required for field
sampling helps to ensure proper preparation. Such a checklist is given in
Appendix C. The appendix lists the [minimal equipment, accessories, and
supplies necessary to sample any type of solid or liquid waste. When the
type of waste to be sampled is known beforehand, the list can be narrowed
down to the actual pieces of equipment to be used.
When sample analyses are to be performed in the field, such as for pH,
flammability, or explosivity, then t:he necessary apparatus for such tests
should also be included in the preparation for sampling.
CLEANING AND STORAGE OF SAMPLER j
All samplers must be clean before use. Used samplers must be washed
with warm detergent solution (i.e., [Liquinox or Alconox), rinsed several
times with tap water, rinsed with distilled water, drained of excess water,
and air dried or dried with a stream of warm, dry air or wiped dry. For
samplers that have been used to sample petroleum products and oil residues,
it may be necessary first to wipe the samplers with absorbent cloth to
eliminate the residues. The equipment is then rinsed with an organic sol-
vent such as petroleum naphtha or trichloroethane, followed by washing with
the detergent solution and rinsing with water. A necessary piece of equip-
ment for cleaning the tube of a Colxwasa is a bottle brush that fits tight-
ly the inside diameter of the tube, j The brush is connected to a ;rod of
sufficient length to allow for reaching the entire length of the sampler
tube. Using this ramrod and fiber-ifeinforced paper towels, the Coliwasa
tube may be quickly cleaned.
Improper cleaning of sampling equipment will cause cross contamination
of samples. Such contamination is of particular importance in samples
taken for legal or regulatory purposes. Also, contamination becomes im-
portant when sampling wastes from different production sources within the
same time frame. A detailed study of cross contamination as a function of
cleaning procedures has not been carried out. A recommended policy is that
if samples are to be taken for legal or regulatory purposes, or if analysis
is to be performed on samples expected to contain low-level (low ppm range)
24
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concentrations of hazardous components, that a fresh, unused sampler be
used. The Coliwasa in particular was designed to be semidisposable. Parts
of the device that become contaminated during sampling (i.e., the tube, the
stopper rod, and the stopper mechanism) may be discarded at little expense.
In addition, or these parts may later be disassembled, secured, and returned
to the laboratory for thorough decontamination and reused.
If the cleaning process has the potential for producing toxic fumes,
ensure adequate ventilation. If the washings are hazardous, store them
in closed waste containers and dispose of them properly in approved dis-
posal sites. Locations of these sites close to one's area may be obtained
by calling the agency in the State responsible for the regulation of hazard-
ous wastes. Store the clean samplers in a clean and protected area. Poly-
ethylene plastic tubes or bags are usually adequate for storing the samplers.
25
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SECTION 6
i
SAMPLING PROCEDURES
PURPOSES AND GENERAL CONSIDERATIONS
i
Sampling of hazardous wastes i is conducted for different purposes. In
most instances, it is performed to determine compliance with existing regu-
lations promulgated by the different regulatory agencies. In some cases,
it is conducted to obtain data for purposes of classifying, treating, reco-
vering, recycling, or determining!compatibility characteristics of the
wastes. Sampling is also conducted as an important part of research activ-
ities.
In general, sampling of hazardous wastes requires the collection of
adequate sized, representative samples of the body of wastes. Sampling
situations vary widely and therefore no universal sampling procedure can be
recommended. Rather, several procedures are outlined for sampling different
types of wastes in various states|and containers.
i
i
These procedures require a plan of action to maximize safety of sam-
pling personnel, minimize sampling time and cost, reduce errors in sampling,
and protect the integrity of the samples after sampling. The following
steps are essential in this plan of action:
1. Research background information about the waste.
2. Determine what should be sampled.
3. Select the proper sampler.
4. Select the proper sample container and closure.
5. Design an adequate sampling plan that includes the following:
a) Choice of the proper sampling point.
b) Determination of the number of samples to be taken.
c) Determination of the volumes of samples to be taken.
6. Observe proper sampling precautions.
7. Handle samples properly. |
8. Identify samples and protect them from tampering.
9. Record all sample information in a field notebook.
10. Fill out chain of custody record.
11. Fill out the sample analysis r'equest sheet.
12. Deliver or ship the samples to the laboratory for analysis.
26
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BACKGROUND INFORMATION ABOUT THE WASTE
Accurate background information about the waste to be sampled is very
important in planning any sampling activity. The information is used to
determine the types of protective sampling equipment to be used, sampling
precautions to be observed, as well as the types of samplers, sample con-
tainers, container closures, and preservatives (when needed) required.
Generally, the information about the waste determines the kind of sampling
scheme to be used.
Most often, the information about the waste is incomplete. In these
instances, as much information as possible must be obtained by examining
any documentation pertaining to the wastes, such as the hauler's manifest
(Figure 10). When documentation is not available, information may be
obtained from the generator, hauler, disposer, or processor. The informa-
tion obtained is checked for hazardous properties against references such
as the Dangerous Properties of Industrial Materials,10 the Merck Index,3
the Condensed Chemical Dictionary,H Toxic and Hazardous Industrial Chemi-
cals Safety Manual for Handling and Disposal with Toxicity and Hazardous
Data,1^ or other chemical references.
SELECTION OF SAMPLER
Hazardous wastes are usually complex, multiphase mixtures of liquids,
semisolids, sludges, or solids.1 The liquid and semisolid mixtures vary
greatly in viscosity, corrosivity, volatility, explosivity, and flamma-
bility. The solid wastes can range from powders to granules to big lumps.
The wastes are contained' in drums, barrels, sacks, bins, vacuum trucks,
ponds, and other containers. No single type of sampler can therefore be
used to collect representative samples of all types of wastes. Table 3
lists most waste types and the corresponding recommended samplers to be
used.
SELECTION OF SAMPLE CONTAINER, CONTAINER CLOSURE, AND CLOSURE LINING
Containers
The most important factors to consider when choosing containers for
hazardous waste samples are compatibility, resistance to breakage, and
volume. Containers must not melt, rupture, or leak as a result of chemical
reactions with constituents of waste samples. Thus, it is important to
have some idea of the components of the waste. The containers must have
adequate wall thickness to withstand handling during sample collection and
transport to the laboratory. Containers with wide mouths are desirable to
facilitate transfer of samples from samplers to containers. Also, the
containers must be large enough to contain the required volume of samplers
or the entire volume of a sample contained in samplers.
Plastic and glass containers are generally used for collection and
storage of hazardous waste samples. Commonly available plastic containers
27
-------
are made of high-density or linear polyethylene (LPE), conventional poly-
ethylene, polypropylene, polycarbonate, teflon FEP (fluorinated ethylene
propylene), polyvinyl chloride (PVC), or polymethylpentene. Teflon FEP is
the most inert plastic, but LPE offers the best combination of chemical
resistance and low cost. ' |
Glass containers are relatively inert to most 'chemicals and can be
used to collect and store almostiall hazardous waste samples except those
that contain strong alkali and hydrofluoric acid. Soda glass bottles are
the cheapest and most readily available. Borosilicate such as Pyrex and
Corex glass containers are also commercially available, but they are ex-
pensive and not always readily obtainable. Glass containers are breakable
and much heavier than plastic containers.
RrviMrf D*««mMr 1f74
CALIFORNIA LIQUID WASTE HAULER RECORD
STATE WATER RESOURCES CONTROL BOARD
009-000928
STATE JDEPAHTM
PRODUCER Of* WASTI 0*** be. fitted by producer* |
I H
(*..*T •• T"*l I <=«•« "">•
P'kk i*a Addta**: '
(•UMB>H| (•TH»T) (CITT)
|
wttUhPradurwIWMfiB' ____ _ 1 1 1 1 1
(Examples: metal pitting, equipment cleaning, oil drilling — coon NO.
wettewater treatment, pickling bath, petroleum refining)
OC9Cn!PTK>N OF WAXTE (MiMCtefUMbvpraduQcri |
Ch««k type •* wMtni
3 O AtKelir* eelutlBn 7. G Chemlca* toilet westee 2. D Cannery watt*
OotrteriSoeetrvl 1 1 1 1
C*m*«Aentt; i "*"*" "™*
t««*m oin; Hydf Khlor k acM. Urn*, caustic wd*. Concentration:
»ft«n«)!K%, *oh«nia (Ititl. mMala (tin). Upper Lower % ; ppm
«teanwa (U«J, cvanUe)
n n
3,
3,
___—_———_ — =, ( _
4.
»,
«^
ruiwtMut rr«pente« or wactai
OH D n«ne D toxic D flammable D eorrotlv* D explosive
_„ __ __ barrels __ i
Rwlfc Vclwme? _ Q eel U ton* U {42 gal.) D otner.. ^ A j.v,
rhyHe^Sut., O wild D liquid O ilud0e D otn.f_T___T_
j
The MMt« H deeef ib*d to th« beet of my ability and It wee de*Iye*ed to • IleertMd liquid wane heoter (if
*a*ltca^ai; j
1 tantfV (•* d«cl»r«) vnd *r penalty of perjury '
th*t lhaj fMeoaln« to tn*e arx) correct. 1
*1«H*TUH« Of AUTHOMIIBa ABBHT «NO TTTt«
HAULER OF WASTE (Mu« t» f iUed by hauler) |
1 1 1. 1
COOK HO.
a am
Plf.li lip; TIm«: nom
State IJqilMWKTt Mt»'-''« H-gl«r-t!nn No. (if applicable) :.,., __9 . ......
l«h Mn r Mo. of Lflarf- nr Trip.- „ Unit No.
(•PCCIFY)
facilitv named below and w« accepted.
1 certify (or declare) under penalty of perjury
lieMATURB O^ *OTHOBII«O AO««T AND TITt.*
DISPOSER- OF WASTE (Mutt be filled by dhpOMrt 1
Nem*{pr- 1 1 1 1
The hauler above delivered the described watte to thl« dlipoial facilitv and ft was an acceptable
local restrictions.
Handling Method(t):
D recovery
n trurm.ot (u^clfvl- __ 1 1 1
D dltpoeel (specify}: D Pond D epreeding D landfill D injection well . . .
1 certify (or declare) under penalty of perjury
that the foregoing Is true and correct.
The site operator shell submit a legible copy of each completed Record to the S tat e'O apartment of
FOR INFORMATION RILATEDTO SPILLS OB OTHER EMERGENCIES INVOLVING
HAZARDOUS WASTE OR OTHER MATERIALS CALL (BOO) 424-93OO.
O.O.T. Proper Shipping Name)
Figure 10. Example of waste manifest
28
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TABLE 3. SAMPLERS RECOMMENDED FOR VARIOUS TYPES OF WASTE
Waste type
Recommended
sampler•
Limitations
Liquids, sludges, Coliwasa
and slurries in
drums, vacuum a) Plastic
trucks, barrels,
and similar
containers , x „..
b) Glass
Liquids and
sludges in ponds,
pits, or lagoons
Powdered or gran-
ular solids in
bags, drums,
barrels, and
similar con-
tainers
Dry wastes in
shallow contain-
ers and surface
soil
Pond
a) Grain
sampler
b) Sampling
trier
Trowel or
scoop
Not for containers 1.5 m(5 ft ) deep.
Not for wastes containing ketones,
nitrobenzene, dimethylformamide,
mesityl oxide, or tetrahydrofuran^'^.
Not for wastes containing hydro-
fluoric acid and concentrated alkali
solutions.
Cannot be used to collect samples
beyond 3.5 m(11.5 ft ). Dip and
retrieve sampler slowly to avoid
bending the tubular aluminum handle.
Limited application for sampling moist
and sticky solids with a diameter
0.6 cm(h in.).
May incur difficulty in retaining core
sample of very dry granular materials
during sampling.
Not applicable to sampling deeper than
8 cm(3 in.). Difficult to obtain
reproducible mass of samples.
Waste piles
Soil deeper
than 8 cm(3 in.)
Wastes in
storage .tanks
Waste pile
sampler
a) Soil auger
b) Veihmeyer
sampler
Weighted
bottle sampler
Not applicable to sampling solid
wastes with dimensions greater than
half the diameter of the sampling tube.
Does not collect undisturbed core
sample.
Difficult to use on stony, rocky, or
very wet soil.
May be difficult to use on very
viscous liquids.
29
-------
Wide-mouth 1000-and 2000-ml(l qt-and %-gal.) glass bottles are recom-
mended for waste samples containing petroleum distillates, chlorinated
hydrocarbons, pesticides, and pettoleum residues that are mostly incom-
patible with plastic containers. JFor all other types of samples, 1000-and
2000-ml(l-qt and %-gal.) wide-mouth LPE bottles are recommended.
i
Container Closures and Closure Linings
The containers must have tight, screw-type lids. Plastic bottles are
usually provided with screw caps made of the same material as the bottles.
No cap liners are usually required. Glass containers usually come with
glass or rigid plastic screw caps such as Bakelite. The plastic caps are
popularly provided with waxed paper liners. Other liner materials are
polyethylene, polypropylene, neoprene, and Teflon FEP plastics. For con-
taining hazardous waste samples requiring petroleum distillates, chlori-
nated hydrocarbons, pesticides, and petroleum residue analyses. Bakelite
caps with Teflon liners are recommended to be used with glass bottles.
Teflon liners may be purchased from plastic specialty supply houses (e.g.,
Scientific Specialties Service, Inc., P.O. Box 352, Randallstown, Md.
21133). [
Table 4 shows most types of wastes and the corresponding sampling
containers and closures recommended.
i
SAMPLING PLAN
The sampling plan should be •sjrell formulated before any actual sampling
is attempted. The plan must be consistent with the objectives of the
sampling. It must include the selected point(s) of sampling and the in-
tended number, volumes, and types! (i.e., composite, grab, etc.) of samples
to be taken. These requirements are discussed below.
POINT OF SAMPLING
A representative sample is crucial to the sampling plan. This sample
depends on proper selection of sampling points in the bulk of the waste.
Hazardous wastes are usually multiphase mixtures and are contained and
stored in containers of different sizes and shapes. No single sampling
point can be specified for all types of containers. Table 5 lists most
types of containers used for hazardous wastes and the corresponding
recommended sampling pqints. j
NUMBER OF SAMPLES
The number of samples to be taken primarily depends on the information
desired. Table 6 lists the recommended number of samples to be collected
consistent with the information sought and the types of wastes to be
sampled. In hazardous waste management, the properties and the average
concentrations of the hazardous components are usually desired. In this
30
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TABLE 4. SAMPLE CONTAINERS AND CLOSURES RECOMMENDED FOR
VARIOUS TYPES OF WASTE
Waste type
item
Re commende d
container
Recommended
closure
Oil wastes except
pesticides, HC,
chlorinated HC, and
photosensitive
wastes
Linear polyethylene (LPE)
bottles,3 1000-and 2000-
ml(l-qt. and %-gal.),
wide mouth
LPE caps
Pesticides, HC,
and chlorinated
HC
Glass bottles,b wide-
mouth, 1000-and 2000-ml
(1-qt. and %-gal.).
Bakelite caps
with Teflon
liner0
Photosensitive
wastes
Amber LPE or brown
glassd bottles, wide-
mouth, 1000-and 200-ml
(1-qt. and %-gal.)
LPE caps for
the LPE bottles;
Bakelite caps
with Teflon
liner for the
glass bottles
aNalgene, Cat. Nos. 2104-0032 and 2120-0005, or equivalent.
bScientific Products, Cat. Nos. 87519-32 and B7519-64, or equivalent.
Available from Scientific Specialities, P.O. Box 352, Randallstown,
Md.
Scientific Products, Cat. Nos. B7528-050 and 7528-2L, or equivalent.
31
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TABLE 5. SAMPLING POINTS RECOMMENDED FOR MOST .WASTE CONTAINERS
Container type
Sampling point
Drum, bung on one end
Drum, bung on side
Barrel, fiberdrum,
buckets, sacks, bags
Vacuum truck and
similar containers
Pond, pit, lagoons
Waste pile
Storage tank
Soil
Withdraw sample through the bung opening.
Lay drum on side with bung up. Withdraw
sample through the bung opening.
I
Withdraw samples through the top of barrels,
fiberdrums, buckets, and similar containers.
Withdraw samples through fill openings of
bags land sacks. Withdraw samples through
the center of the containers and to different
point's diagonally opposite the point of entry.
Withdraw sample through open hatch. Sample
all other hatches.
Divide surface area into an imaginary grid.a
Take [three samples, if possible: one sample
near [the surface, one sample at mid-depth or
at center, and one sample at the bottom.
Repeat the sampling at each grid over the
entire pond or site.
I
Withdraw samples through at least three
different points near the top of pile to
points diagonally opposite the point of
entry.
Sample from the top through the sampling hole.
Divide the surface area into an imaginary
grid.3 Sample each grid.
aThe number of grid is determined by the desired number of samples
to be collected, which when combined should give a representative
sample of the wastes.
32
-------
respect, collecting one representative sample of a given waste is usually
adequate. This sample can either be collected from a single sampling point
with a composite sampler, or several samples can be collected from various
sampling points and combine into one composite sample.
When gathering evidence for possible legal actions, multiple samples
of a waste are usually collected. Three identical samples are desirable:
one sample is given to the company or organization responsible for the
waste, the second sample is submitted to the laboratory for analysis, and
the third sample is. kept in storage for possible use as a referee sample.
Subdividing a waste sample is not recommended unless it is homogeneous.
VOLUME OF SAMPLES
Sufficient volume of a sample, representative of the main body of the
waste, must be collected. This sample must be adequate in size for all
needs, including laboratory analysis, splitting with other organizations
involved, etc. In collecting liquid waste samples in drums, vacuum trucks,
or similar containers, the volume collected in the Coliwasa usually deter-
mines the volume of the sample. This volume can range from 200 to 1800
(h pt. to 1.9 qt.). In most cases, 1000 ml(l qt.) of a sample is usually
sufficient. Hazardous wastes usually contain high concentrations of the
hazardous components, and only a small aliquot of the sample is used for
analysis.
SAMPLING PRECAUTIONS AND PROTECTIVE GEAR
Proper safety precautions must always be observed when sampling ha-
zardous wastes. In all cases, a person collecting a sample must be aware
that the waste can be a strong sensitizer and can be corrosive, flammable,
explosive, toxic, and capable of releasing extremely poisonous gases.13
The background information obtained about the waste should be helpful in
deciding the extent of sampling safety precautions to be observed and in
choosing protective equipment to be used.
For full protection, the person collecting the sample must use a self-
contained breathing apparatus, protective clothing, hard hat, neoprene
rubber gloves, goggles, and rubber boots.
A self-contained breathing apparatus consists of an air-tight face
mask and a supply of air in a pressure tank equipped with a pressure
regulator. Protective clothing consists of long-sleeved neoprene rubber
coat and pants, or long-sleeved coverall and oil-and-acid proof apron. In
hot weather, the coverall-apron combination might be preferred. Table 7
lists the uses and commercial availability of respiratory protective equip-
ment. All equipment except the respirator must be properly washed and
cleaned between uses (see Section 5).
33
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TABLE 6. NUMBER OF SABLES TO BE COLLECTED
Case
No.
Information
desired
Waste
type
Container type
Number of samples
to be collected
1 Average
concentration
2 Average
concentration
3 Average
concentration
4 Average
concentration
5 Average
concentration
6 Concentration
range
7 Concentration
range
8 Concentration
range
9 Concentration
range
10 Concentration
range
11 Average
concentration
for legal
evidence
Liquid Drum, vacuum truck,
and similar
containers
Liquid Pond, pit, lagoon
Bag5 drum, bin
Solid
(powder
or gran-
ular)
Waste
pile
Soil
Liquid Drum, vacuum truck,
tank
storage
Liquid Ponds, pit, lagoon
Solid
(powder
or gran-
ular)
Waste
pile
Soil
All
types
Bag, drum, bin
All; containers
1 Collected with
Coliwasa
1 Composite sample of
several samples
collected at differ-
ent, sampling points
or levels
Same as Case #2
Same as Case #2
1 Composite sample of
several samples
collected at differ-
ent sampling areas
3 to 10 separate sam-
ples, each from a
different depth of
the liquid
3 to 20 separate sam-
ples from different
sampling points and
depths
3 to 5 samples from
different sampling
points
Same as Case #8
3 to 20 separate sam-
ples from different
sampling areas
3 Identical samples or
1 composite sample
divided into 3
identical samples if
homogeneous
12
13
Average
concentration
Average
concentration
Liquid
Liquid
Storage tank
Stotage tank
Same as Case #2
Same as Case #6
34
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TABLE 7. RESPIRATORY PROTECTIVE DEVICES RECOMMENDED
FOR VARIOUS HAZARDS
Type of hazard
Recommended respiratory device
Oxygen deficiency
Gaseous contaminant
immediately dangerous
to life
Gaseous contaminant
not immediately
dangerous to life
Particulate contaminant
Combination of gaseous and
particulate contaminants
immediately dangerous to
life
Combination of gaseous
and particulate contaminants
not immediately
dangerous to life
Self-contained breathing apparatus,
hose mask with blower
Self-contained breathing apparatus,
hose mask with blower,
gas mask
Air-line respirator,
hose mask without blower,
chemical-cartridge respirator
Dust, mist, or fume respirator,
:air-line respirator,
:abrasive-blasting respirator
.Self-contained breathing apparatus,
hose mask with blower,
gas mask with special filter
Air-line respirator,
hose mask without blower,
chemical-cartridge respirator
with special filter
Source: Reference 14.
35
-------
The self-contained breathing Apparatus may not be required in all
sampling situations. In some case|s, gas-masks or chemical cartridge-type
respirators with filters will suffice. Table 7 may be used to select the
proper protective respiratory devijce.
For added protection in sampling, a second person with a radio-
telephone and first-aid kit must be present to render any necessary
help or call for assistance. '
SAMPLING PROCEDURES
t
The following procedures are [recommended for sampling different types
of hazardous wastes in various containers.
Sampling a Drum
_
Drums containing liquid wastes can be under pressure or vacuum. A
bulging drum usually indicates tha|t it is under high pressure and should
not be sampled until the pressure ,can be safely relieved. A heavily
corroded or rusted drum can readily rupture and spill its contents when
disturbed; it should only be sampljed with extreme caution. Opening the
bung of a drum can produce a spark that might detonate an explosive gas
mixture in the drum. This situation is difficult to predict and must be
taken into consideration every time a drum is opened. The need for full
protective sampling equipment cannot be overemphasized when sampling a
drum. ''
i
s
1. Position the drum so that the 'bung is up (drums with the bung on the
end should be positioned upright; drums with bungs on the side should
be laid on its side, with the [bungs up).
i
2. Allow the contents of the drum to settle.
i
3. Slowly loosen the bung with a Ibung wrench, allowing any gas pressure
to release.
4. Remove the bung and collect a [sample through the bung hole with a
Coliwasa, as directed in Section 4.
5. When there is more than one drum of waste at a site, segregate and
sample the drums according to waste types, using a table of random
numbers as outlined in Appendix D.
Sampling a Vacuum Truck
Sampling a vacuum truck requires the person collecting the sample to
climb onto the truck and walk along a narrow catwalk. In some trucks, it
requires climbing access rungs to the tank hatch. These situations pre-
sent accessability problems to the sample collector, who most usually
36
-------
wear full protective sampling gear. Preferably, two persons should
perform the sampling: One person should do the actual sampling and the
other should hand the sampling device, stand ready with the sample con-
tainer, and help deal with any problems. The sample collector should
position himself to collect samples only after the truck driver has
opened the tank hatch. The tank is usually under pressure or vacuum.
The driver should open the hatch slowly to release pressure or to break
the vacuum.
1. Let the truck driver open the tank hatch.
2. Using protective sampling gear, assume a stable stance on the, tank
catwalk or access rung to the hatch.
3. Collect a sample through the hatch opening with a Coliwasa, as
directed in Section 4.
4. If the tank truck is not horizontal, take one additional sample each
from the rear and front clean out hatches and combine all three
samples in one sample container.
5. When necessary, carefully take sediment sample from the tank through
the drain spigot.
Sampling a Barrel, Fiberdrum, Can, Bags, or Sacks Containing Powder
or Granular Waste
The proper protective respirator (see Table 7), in addition to the
other protective gear, must be worn when sampling dry powdered or granu-
lar wastes in these containers. These wastes tend to generate airborne
particles when the containers are disturbed. The containers must be
opened slowly. The barrels, fiberdrums, and cans must be positioned
upright. If possible, sample sacks or bags in the position you find
them, since standing them upright might rupture the bags or sacks.
1. Collect a composite sample from the container with a grain sampler
or sampler trier, as directed in Section 4.
2. When there is more than one container of waste at a site, segregate
and sample the containers according to a table of random numbers, as
outlined in Appendix D.
Sampling a Pond
Storage or evaporation ponds for hazardous wastes vary greatly in
size from a few to a hundred meters. It is difficult to collect repre-
sentative samples from the large ponds without incurring huge expense
and assuming excessive risks. Any samples desired beyond 3.5m(llig ft)
from the bank may require the use of a boat, which is very risky, or
the use of a crane or a helicopter, which is very expensive. The
37
-------
information sought must be weighed against the risk and expense of col-
lecting the samples. The pond sampler described in Section 4 can be used
to collect samples as far as 3.5 m(llJg ft.) from the bank.
i
1. Collect a composite sample with pond sampler, as directed in Section
4.
Sampling Soil
I
The techniques of soil sampling are numerous. The procedures out-
lined below are adopted from ASTM [methods.15 The procedures are consist-
ent with the hazardous waste management objective of collecting soil
samples which is usually to deternjiine the amount of hazardous material
deposited on a particular area ofiland or to determine the leaching rate
of the material and/or determine the residue level on the soil. Elaborate
statistically designed patterns have been designed for sampling soils. If
one of these patterns is to be used, a good statistics book may have to be
consulted. In^the following procedures, soil samples are taken in a grid
pattern over the entire site to ensure a uniform coverage.
1. Divide the area into an imaginary grid (see Table 5).
2. Sample each grid and combine the samples into one.
I
3. To sample up to 8 cm(3 in.) deep, collect samples with a scoop, as
directed in Section 4. ,
4. To sample beyond 8 cm(3 in.) deep, collect samples with a soil auger
or Veihmeyer soil sampler, as directed in Section 4.
Sampling a Waste Pile
Waste piles can range from small heaps to a large aggregates of
wastes. The wastes are predominantly solid and can be a mixture of powders,
granules, and chunks as large as or greater than 2.54 cm(l in.) average
diameter. A number of core samples have to be taken at different angles
and composited to obtain a sample jthat, on analysis, will give average
values for the hazardous components in the waste pile.
1. Determine the sampling points (see Table 5).
2. Collect a composite sample with a waste pile sampler according to the
directions in Section 4.
Sampling a Storage Tank
The collection of liquid samples in storage tanks is extremely dis-
cussed in the ASTM methods. The procedure used here is adopted from one
of those methods.16
38
-------
Sampling a storage tank requires a great deal of manual dexterity.
Usually it requires climbing to the top of the tank through a narrow
vertical or spiral stairway while wearing protective sampling equipment
and carry sampling paraphernalia. At least two persons must always per-
form the sampling: One should collect the actual samples and the other
should stand back, usually at the head of the stairway, and observe, ready
to assist or call for help. The sample collectors must be accompanied by
a representative of the company, who must open the sampling hole, usually
on the tank roof.
1. Collect one sample each from the upper, middle, and lower sections of
the tank contents with a weighted bottle sampler, as outlined in
Section 4.
2. Combine the samples one container and submit it as a composite sample.
SAMPLE HANDLING
After a sample is transferred into the proper sample container, the
container must be tightly capped as quickly as possible to prevent the
loss of volatile components and to exclude possible oxidation from the air.
The use of a preservative or additive is not recommended. However,
if only one or two components of a waste are of interest, and if these
components are known to rapidly degrade or deteriorate chemically or bio-
chemically, the sample may be refrigerated at 4 to 6°C.(39.2 to 42.8°F.)
or treated with preservatives according to Section 8.
To split or withdraw an aliquot of a sample, considerable mixing,
homogenization, or quartering is required to ensure that representative
or identical portions are obtained. When transferring a sample aliquot,
open the container as briefly as possible.
IDENTIFICATION OF SAMPLE
Each sample must be labeled and sealed properly immediately after
collection.
Sample Labels
Sample labels (Figure 11) are necessary to prevent misidentification
of samples. Gummed paper labels or tags are adequate. The label must
include at least the following information:
Name of collector.
Date and time of collection.
Place of collection.
Collector's sample number, which uniquely identifies the sample.
39
-------
OFFICIAL SAMPLE LABEL
Collector
Collector's Sample No.
Place of Collection
Date Sampled_
Time Sampled_
Field Information
Figure 11. Example; of official sample label.
OFFICIAL SAMPLE SEAL
State of California
Department of Health Services
Collected by_
Date Collected__
Place Collected
(signature)
Public Health Division
Hazardous Materials Laboratory
Collector's Sample No._
Time Collected
Figure 12. Example of official sample seal
40
-------
Sample Seals
Sample seals are used to preserve the integrity of the sample from the
time it is collected until it is opened in the laboratory. Gummed paper
seals can be used as official sample seals. The paper seal must carry
information such as:
Collector's name
Date and time of sampling
Collector's sample number. (This number must be identical with the
number on the sample label). i
The seal must be attached in such a way that it is necessary to break
it in order to open the sample container. An example of a sample seal is
shown in Figure 12. '
FIELD LOG BOOK
All information pertinent to a field survey and/or sampling must be
recorded in a log book. This must be a bound book, preferabley with con-
secutively numbered pages that are 21.6 by 27.9 cm(8% by 11 in.). Entries
in the log book must include at least the following:
Purpose of sampling (e.g., surveillance, etc.)
Location of sampling (e.g., hauler, disposal site, etc.) and address
Name and address of field contact
Producer of waste and address
Type of process (if known) producing waste
Type of waste (e.g., sludge, wastewater, etc.)
Declared waste components and concentrations
Number and volume of sample taken
Description of sampling point ;
Date and time of collection
Collector's sample identification number(s)
Sample distribution (e.g., laboratory, hauler, etc.)
References such as maps or photographs of the sampling site
Field observations
Any field measurements made such as pH, flammability, explositivity,
etc.
Sampling situations vary widely. No general rule can be given as to
the extent of information that must be entered in the log book. A good
41
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1
rule, however, is to record sufficient information so that someone can
reconstruct the sampling situation without reliance on the collector's
memory. ;
The log book must be protected and kept in a safe place.
CHAIN OF CUSTODY RECORD
To establish the documentation necessary to trace sample possession
from the time of collection, a chain of custody record must be filled out
and accompany every sample. This record becomes especially important when
the sample is to be introduced as evidence in a court litigation. An
example of a chain of custody record is illustrated in Figure 13.
The record must contain the jfollowing minimum information:
Collector's sample number
Signature of collector
Date and time of collection
Place and address of collection
Waste type
Signatures of persons involved in the chain of possession
Inclusive dates of possession
SAMPLE ANALYSIS REQUEST SHEET
The sample analysis request sheet (Figure 14) is intended to accom-
pany the sample on delivery to the laboratory. The field portion of this
form must be completed by the person collecting the sample and should
include most of the pertinent information noted in the log book. The
laboratory portion of this form is intended to be completed by laboratory
personnel and to include: j
Name of person receiving the,sample
Laboratory sample number \
Date of sample receipt !
Sample allocation |
Analyses to be performed
SAMPLE DELIVERY TO THE LABORATORY
Preferably, the sample must be delivered in person to the laboratory
for ana3.ysis as soon as practicable—usually the same day as the sampling.
Consult Section 8 when.sample preservation is required. The sample must
42
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California Department of Health
Hazardous Materials Laboratory
Collector's Sample No.
CHAIN OF CUSTODY RECORD
Hazardous Materials
Location of Sampling: Producer Hauler Disposal Site
Other: .
Company's Name
Address
Telephone ( )
number street
Collector's Name
Date Sampled
city
signature
state zip
Telephone ( )
Time Sampled_
Type of Process Producing Waste_
Waste Type Code Other
Field Information
hours
Sample Allocation:
1.
2.
3.
Chi
1.
2.
3.
name of organization
name of organization
.n of Possession
signature
signature
signature
name of organization
title
title
title
inclusive dates
inclusive dates
inclusive dates
Figure 13. Example of chain of custody record
43
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PRIORITY California Department of Health Services
(explain) Hazardous Materials Laboratory
HAZARDOUS MATERIALS SAMPLE ANALYSIS REQUEST
PART I; FIELD SECTION
Collector Date Sampled Time hours
Location of Sampling ; ,
name of [company, disposal site, etc.
Addres s
number street city state . , zip
Telephone ( ) Company Contact
HML NO. COLLECTOR'S TYPE OF
(Lab only) SAMPLE NO. SAMPLE* FIELD INFORMATION**
Analysis Requested_
Special Handling and/or Storage_
PART II: LABORATORY SECTION
Received by Title Date_
Sample Allocation: __HML LBL LABL SRL Date_
Analysis Required _________
*Indicate whether sample is sludge, soil, etc.;**Use back of page for
additional information.
Figure 14. Example of hazardous waste sample analysis request sheet
44
-------
be accompanied by the chain of custody record and by a sample analysis.
request sheet (Figure 14). The sample must be delivered to the person'
in the laboratory authorized to receive samples (often referred to as
the sample custodian).
SHIPPING OF SAMPLES
When a sample is shipped to the laboratory, it must be packaged in a
proper shipping container to avoid leakage and/or breakage. A cardboard
box that will provide at least 10 cm(4 in.) of tight packing around the
sample container must be used. Acceptable packing materials include saw-
dust, crumpled newspapers, vermiculite, polyurethane chips, etc. Other
samples that require refrigeration must be packed with reusable plastic
packs or cans of frozen freezing gels in molded polyurethane boxes with
sturdy fiberboard protective case. The boxes must be taped closed with
masking tape or fiber plastic tape. '
All packages must be accompanied by a sample analysis sheet and chain
of custody record. Complete address of the sender and the receiving lab-
oratory must legibly appear on each package. .When sent by mail, register
the package with return receipt requested. When sent by common carrier,
obtain a copy of the bill of lading. Post office receipts,and bill.of
lading copies may be used as part of the chain of custody documentation.^
45
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SECTION 7
i
[
RECEIPT AND LOGGING OF SAMPLE
Field samples are delivered to the laboratory either personally or
through a public carrier. In the!laboratory, a sample custodian should
be assigned to receive the samples,. Upon receipt of a sample, the custo-
dian should inspect the condition!of the sample and the sample seal,
reconcile the information on the sample label and seal against that on the
chain of custody record, assign a laboratory number, log in the sample in
the laboratory log book, and store the sample in a secured sample storage
room or cabinet until assigned to]an analyst for analysis.
SAMPLE INSPECTION
i
The sample custodian should inspect the sample for any leakage from
the container. A-leaky containericontaining multiphase sample should
not be accepted for analysis. This sample will no longer be a represen-
tative sample. If the sample is Contained in a plastic bottle and the
walls show any bulging or collapsing, the custodian should note that the
sample is under pressure or releasing gases, respectively. A sample
under pressure should be treated with caution. It can be explosive or
release extremely poisonous gasesi The custodian should examine whether
the sample seal is intact or broken, since broken seal may mean sample
tampering and would make analysis;results inadmissible in court as evi-
dence. Discrepancies between the!information on the sample label and seal
and that on the chain of custody record and the sample analysis request
sheet should be resolved before the sample is assigned for analysis. This
effort might require communication with the sample collector. Results of
the inspection should be noted oni the sample analysis request sheet and
on the laboratory sample log bookl
I
ASSIGNMENT OF LABORATORY NUMBER
Incoming samples usually carry the inspector's or collector's identi-
fication numbers. To further identify these samples, the laboratory
should assign its own identification numbers, which normally are given
consecutively. Each sample should be marked with the assigned laboratory
number. This number is correspondingly recorded on a laboratory sample
log book along with the information describing the sample. The sample
information is copied from the sample analysis request sheet and cross-
checked against that on the sampl^ label.
46
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ASSIGNMENT OF SAMPLE FOR ANALYSIS
In most cases, the laboratory supervisor assigns the sample for ana-
lysis. The supervisor should review the information on the sample analysis
request sheet, which now includes inspection notes recorded by the labora-
tory sample custodian. The supervisor should then decide what analyses
are to be performed. The sample may have to be split with other labora-
tories to obtain tne necessary information about the sample. The super-
visor should decide on the sample allocation and delineate the types of
analyses to be performed on each allocation. In his own laboratory, the
supervisor should assign the sample analysis to at least one chemist, who
is to be responsible for the care and : custody of the sample once it is
handed to him. He should be prepared to testify that the sample was in
his possession or secured in the laboratory at all times from the moment
it was received from the custodian until the analyses were performed.
The receiving chemist should record in his laboratory notebook the
identifying information about the sample, the date of receipt, and other
pertinent information. .This record should also include the subsequent
analytical data and calculations.
47
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SECTION 8
PRESERVATION AND STORAGE OF SAMPLES
Ideally, hazardous waste samples should be analyzed immediately after
collection for maximum reliability of the analytical results. Hazardous
wastes are such complex mixtures :that it is difficult to exactly predict
the physical, biological, and chemical changes that occur in the samples
with time. After collection of samples, pH may change significantly in a
matter of minutes; sulfides and cyanides may be oxidized or-evolve as
gases; and hexavalent chromium may slowly be reduced to the trivalent
state. Certain cations may be partly lost as a result of adsorption to
the walls of the sample containers. Growth of microorganisms may also
cause changes to certain constituents of the sample. Volatile compounds
may be rapidly lost.
In a number of cases, the above changes may be slowed down or pre-
vented by refrigeration at 4 to 6°C, or by the addition of preservatives.
However, these treatments mostly apply to one or two components or pro-
perties. Refrigeration may deter the evolution of volatile components and
acid gases such as hydrogen sulfides and hydrogen cyanides, but it also
introduces the uncertainty that some salts may precipitate at lower temper-
ature. On warming to room temperature for analysis, the precipitates may
not redissolve, thus incurring error in determining the actual concentra-
tions of dissolved sample constituents. Addition or preservatives may,
retard biochemical changes, whereas other additives may convert some
constituents to stable hydroxides, salts, or compounds. Unknown in these
treatments, however, is the possible conversion of other compounds to other
forms (such as the products of nitration, sulfonation, oxidation, etc., of
organic components). In subsequent analyses, the results may not reflect
the original identity of the components.
Thus, both advantages and disadvantages are associated with the refri-
geration and/or addition of preservatives or additives to waste samples.
These methods of preservation or stabilization are not recommended for
hazardous waste samples unless only one or two components or properties
are to be analyzed.
Standard methods books 18,19 have compilations of useful preservatives
for various constitutents. Table 8 is excerpted from these lists and shows
only the preservation methods that may be used for hazardous wastes.
48
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TABLE 8. METHODS OF PRESERVATION FOR HAZARDOUS WASTES
Waste constituent
to be preserved
Acidity
Alkalinity
Ammonia
Arsenic
Chlorine
Chromium (VI)
Cyanides
Fluoride
Metals :
1) dissolved
2) suspended
3) Total
Mercury
1) dissolved
2) Total
PH
Phenolics
Residue, volatile
Selenium
Specific
conductance
Sulfide
Sulfide
Zinc
Preservation method
Cool to 4° C
Cool to 4° C
Add 1 ml cone. H2S04/&
Add 6 ml cone. HN03/ &
Cool to 4° C
Add 6 ml cone. H2S04/&
Add 2.5 ml of 50% NaOH/£ ;
cool to 4° C
Cool to 4° C
Filter on site; add 5 ml
cone. HN03/&
Filter on site
Add 5 ml cone. HN03/&
Filter; add 5 ml cone. HN03/£
Add 5 ml cone. HN03/&
Determine on site; cool to 4 C
Add H3P04 to pH 4 and 1 g.
CuS04/& ; refrigerate at 4° C
Cool to 4° C
Add 5 ml cone. HN03/£
Cool to 4° C
Add 2 ml of 2N Zn(AC)2/£
Cool to 4° C
Add 4 ml cone. HC1/&
Storage time
24 hr
24 hr
24 hr
6 months
24 hr
24 hr
24 hr
7 days
6 months
6 months
6 months
38 days
38 days
6 hr
24 hr
7 days
6 months
24 hr
24 hr
24 hr
—
aSource: References18»19'and
20
49
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REFERENCES
[
1. Stephens, R. D. 1976. Hazardous Sampling; Residual Management by Land
Disposal. Proceedings of the Hazardous Waste Research Symposium,
University of Arizona, Tucson, Ariz.
2. Eichenberger, B., J. R. Edwards, K. Y. Chen, and R. D. Stephens. 1977.
A Case Study of Hazardous Wastes Input Into Class I Landfills. U.S.
Environmental Protection Agency, Cincinnati, Ohio.
I
3. Merck Index, An Encyclopedia! of Chemicals and Drugs. 1968. 9th Ed.
Merck & Co., Rahway. j
4. Chemical Resistance of Excelpn R-4000. 1977. Thermoplastic Process,
Inc., Stirling, N.J. i
5. Sampling Procedure for Animal Feed. Official Methods of Analysis of
the Association of Official Analytical Chemists. 1975. 12th Ed.
Washington, D.C., p. 129. i
6. Guidelines on Sampling and Statistical Methodologies for Ambient Pesti-
cide Monitoring. 1974. Federal Working Group on Pest Management, U.S.
Environmental Protection Agency, Washington, D.C., p. III-5.
i
7. Veihmeyer, F. J. 1929. An Improved Soil-Sampling Tube. Soil Science
217(2): 147-152. \
I
8. American Society for Testing and Materials. 1975. ASTM D270. ASTM
Standards. The Society, Philadelphia, Pa.
9. American Society for Testing' and Materials. 1973. ASTM E 300. ASTM
Standards. The Society, Philadelphia, Pa.
10. Sax, I. N. 1968. Dangerous Properties of Industrial Materials. 3rd
Ed. Van Nostrand Reinhold Co!. New York, N.Y.
11. Condensed Chemical Dictionary. 1977. 8th Ed. Van Nostrand Reinhold
Co., New (York, N.Y. j
12. Toxic and Hazardous Industrial Chemicals Safety Manual for Handling
and Disposal With Toxicity and Hazardous Data. 1976. International
Technical Information Institute, Tokyo, Japan.
13. Dunlap, J. 1972. Industrial Waste Law (AB 596), State of California.
50
-------
14. Bureau of Labor Standards. Respiratory Protective Equipment.
Bulletin 226. Safety in Industry; Environmental and Chemical
Hazards, No. 3. U.S. Department of Labor, Washington, B.C.
15. American Society for Testing and Materials. ASTM D1452, D1586 and
D3550. ASTM Standards. The Society, Philadelphia, Pa.
16. American Society for Testing and Materials. ASTM D270 and E 300
ASTM Standards. The Society, Philadelphia, Pa.
17. Compliance Monitoring Procedures. 1974. EPA 330/1-74-/002. U.S.
Environmental Protection Agency, Denver, Colo.
18. Manual of Methods for Chemical Analysis of Water and Wastewater.
1974. EPA-625/6-74-003. U.S. Environmental Protection Agency,
Washing ton, D.C.
19. Standard Methods for Examination of Water and Wastewater. 1975. 14th
Ed. American Public Health Association, New York, N.Y.
20. Collection, Storage,. Transportation, and Pretreatment of Water and
Wastewater Samples. 1971. California Department of Health Services,
Berkeley, Ca.
51
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APPENDICES
i
APPENDIX A. DEVELOPMENT OF THE COMPOSITE LIQUID WASTE SAMPLER (COLIWASA)
I
Early in the development of the California waste management program,
the needs were recognized for accurate information about waste composition
and adequate equipment and procedures for sampling and analysis.
I
In 1975, the California Department of Health Services engaged in a
cooperative study with the University of Southern California (Environmental
Engineering Department) under U.S. Environmental Protection Agency's spon-
sorship to collect and analyze a large number of hazardous waste samples
at a number of Class I disposal sitjss in Los Angeles County. In the prep-
aration of this study, the Department of Health Services personnel designed
and constructed a simple tube samplbr suitable for use in liquid and sludge
wastes. The objective of the sampler design was to obtain samples represent-
ative of complex, heterogeneous wastes contained in vacuum trucks and drums.
In preliminary testing, the prototype design shown in Figure A-l appeared to
give good representative samples. At this time, the sampling device was
named the composite liquid waste sampler, or Coliwasa for short.
Requirements for Hazardous Waste Sampling Procedures and Equipment
Approximately 24 of these devices were constructed for use in the Los
Angeles County sampling program. During a 2-week period in 1975, 400 samples
of hazardous wastes were taken from vacuum trucks and drums. The wastes
represented an extremely wide variety of chemical compositions and physical
characteristics. The experience given by this sampling program emphasized
the following important requirements of hazardous waste sampling procedures
and equipment:
1) Sampling equipment must be of simple design to facilitate easy cleaning
or to allow discard if necessarly to prevent sample cross contamination.
Many wastes, because of their chemical composition and/or physical nature,
so fouled sampling equipment that it required discarding or extensive
cleaning. Extensive cleaning produces a significant volume of cleaning
waste that must be properly disposed. Equipment that has complicated
valves, levers, and other fittings would never survive many hazardous
wastes.
2) Equipment must be light weight :and leak p'roof. Sampling personnel are
required to climb and move about on tank trucks and other dangerous areas
while holding sampling equipment. Once the sampler is filled with its
52
-------
charge of hazardous waste, it must not discharge until properly inside
a sample receptacle. Thus, a positive locking mechanism is needed.
3) Several types of sampling equipment must be available, for no one de-
sign or material meets all hazardous waste sampling requirements.
4) Sampling requires a minimum of two persons equipped with the proper
and complete complement of safety equipment. Even at a well-run waste
disposal site using an approved manifest system, surprises occur. A
waste sample collector never knows for sure what he will find when a
vacuum truck or barrel is opened.
V
183 cm (72")
152 cm (60")
\
Rod, WC, 0.95 cm (3/8") O.D.
Pipe, WC, 4.13 cm (1 5/8") I.D.,
4.78 cm (1 7/8") O.D.
•Stopper, neoprene, #9
-Nut and washer, stainless steel,
0.95 cm (3/8")
Figure 1. Coliwasa, Model 1.
Sampler Selection
A review of the literature was conducted to investigate the availabil-
ity of commercial equipment that would better suit the sampling require-
ments than the Coliwasa. The guidelines used in the selections were
commercial availability, cost, simplicity in design, chemical inertness,
and adaptability for use in composite sampling of liquid hazardous wastes.
Preliminary tests were performed.on a number of candidate liquid
samplers. The tests included physical inspections of the sampling mechan-
isms for ease of operation and applicability. Water was the initial test
•liquid. The test water was placed in a fabricated tank made out of a
53
-------
122-cm(4-ft) tall by 15.2-cm(6-in.) I.D. glass cylinder. Each sampler
under test was lowered slowly into the tank to determine whether the check
valve or closing device or sampling orifice would allow the sample to flow
in the sampler. The sampler was then withdrawn and tested for leakage and
ease of transfer of the collected sample.
None of the commercially available samplers was found to be satis-
factory. The Coliwasa designed by the Department of Health Services
appeared to be the most promising.
First Coliwasa Model
The early design of the Coliwasa (Model 1; Figure A-l) consisted of
1.52-m(5-ft.) by 4.13-cm(l 5/8-in.) I.D., opaque PVC pipe as the sampling
tube and a ne.oprene stopper attached to one end of a 0.95-cm(3/8~in.) O.D.
PVC rod as the closing mechanism., To collect a sample with this sampler,
the stopper is pushed out about 5 cm(2 in.) from the bottom end of the
sampling tube. Then the sampler is lowered straight down through the body
of liquid waste to be sampled to the bottom of the waste container. The
liquid in the tube is trapped by plugging the bottom of the tube with the
stopper by pulling up the stopper'rod with one hand and holding the tube
with the other hand. j
This early design of the Coliwasa, albeit functional, was deficient in
a number of aspects. First, it was difficult to put the sampler in the
close position. The stopper did not easily line up with the bottom opening
of the sampling tube. Several manipulations of the stopper rod were usually
required to effect closure. This difficulty tended to disturb the bottom
layer of the waste being sampled and undoubtedly contributed to the col-
lection of nonrepresentative samples.
Second, the sampler was not equipped with a mechanism that positively
and independently locked it closed. Closure was maintained by using one
hand to hold the sampling tube and the other hand to maintain a. constant
upward pressure on the upper end |of the stopper rod to keep the stopper
tightly seated against the bottom opening of the sampler. In some samp-
ling instances, this method of closure was not always practical. When
sampling waste containers as deep; as the length of the sampler, the opera-
tor could not withdraw the sampler without freeing the hand that maintains
the closing pressure on the stopper rod. Thus, the snug contact between
the neoprene stopper and the inner opening of the sampling tube was the
only force that locked the sampler closed. The weight of the sample con-
tained in the sampling tube has in some cases pushed out the stopper,
resulting in lost samples and exposure of the sample collector to unneces-
sary hazards.
Third, samples contained in the sampler were difficult to transfer
into sample containers at regulated rates, and caused some samples to be
lost from splashings.
54
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Attempts were made to improve the first model of the Coliwasa. These
efforts led to fabrication of the other models shown in Figures A-2 through'
A-5, and finally to the recommended version as shown in Figure 1 of the text.
Models 2 and 3
The improvement in the second model of the Coliwasa (Figure A-2) con-
sisted of making diametrical slits, 5 cm(2 in.) deep by 2 cm(0.79 in.) wide, '
and indentations 90° from the slits at the top of the sampler tube. The
slits accommodate the T-handle of the stopper rod in the open position, which
allows the stopper to extend down about 5 cm(2 in.) below the bottom of the
sampler. The indentations serve as support for the T-handle when the sam-
pler is placed in the close position. When this improved Coliwasa was tested
the neoprene stopper still did not readily line up with the bottom opening
of the sampling tube. Several twisting manipulations of the stopper rod
were required to bring the sampler into the close position. This problem
was remedied by installing three stainless steel guide wires (18 gauge) on
the stopper, with the upper wire ends secured to the stopper rod, as shown
in Figure A-3. This version (Model 3) of the sampler was again tested. The
sampler was found functional and relatively easy to operate. It can be dis-
assembled and reassembled for cleaning in about 2 minutes. It can be built
for less than $10.00. The closing tension on the stopper of this sampler,
however, is not easily adjusted while sampling. This drawback might incur
some sample loss.
l\
152 cm (60"
\/
\f
OPEN
1 J
1 \
(61")
EXPA
/
' j
f — '
>— N
X
//
r
/
NDEI
) \
1.91 cm'
O.D,
N/
^_
*
riEW
t
/
X
OF
(3/4")
rod
!}•
i
i
It
1
Ij
1
i
u
<
<
TOP OF SAMPLER
CLOSE
Figure A-2. Coliwasa, Model 2.
0.95 cm (3/8") O.D.
rod, PVC
4.13 cm (1 5/8")
I.D. pipe, PVC
Stopper, neoprene,
#9, with PVC nut
and washer
55
-------
Q
•
O
en
S
o
O
o
o
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Model 4
Further investigation into improving the design of the Coliwasa re-
sulted in Model 4(Figure A-4). In this;version, the locking mechanism of
the sampler consisted of a threaded PVC plug that rides on a short threaded
0.95~cm(3/8-in.) O.D. metal rod. The metal rod is coupled with the PVC
stopper1 rod. To sample, the plug is screwed out about 5 cm and then the
stopper rod is pushed downward to open the sampler. The sampler is lowered
slowly into the liquid. Upon reaching the bottom of the container, the
stopper rod is pulled up to close the sampler. The PVC plug is screwed in
until tight to secure the stopper in the close position. This design of
the Coliwasa is simple, functional, and provides the person collecting the
sample with control over the tightness of the stopper against the bottom
of the sampler. It is, likewise, easily disassembled and reassembled for
cleaning. This sampler, however, is slow to operate, the PVC plug does not
screw in and out fast enough. This drawback tends to expose the sample col-
lector to the liquid waste during sampling longer than is perhaps necessary.
Model 5
Another model of the Coliwasa was fabricated using a closing principle
similar to a float valve (Figure A-5). This sampler was fabricated from a
1.52-m(5-ft) by 5.1-cm(2-in.) I.D. plastic pipe. At the bottom end is a
plastic reducer fitting (5.1-cm(2-in.) to 3.18-cm(1.5-in.) I.D.)- A manu-
ally operated neoprene rubber plug attached to a rod is used as the closing
device. When sampling, the rubber plug is raised about 5 cm(2-in.) above
its seat, and the sampler is slowly lowered into the liquid.' On reaching
the bottom of the container, the sampler is closed by slowly lowering the
plug back to its seat. The sampler is withdrawn and the sample is dischar-
ged into a sample container. Tests performed on this sampler showed no
leakage of collected samples. This sampler was also found to be the easiest
to disassemble and reassemble for cleaning. However, the annular clearance
between the outside diameter of the stopper and the inside diameter of the
sampling tube was too narrow. The sampler tended to stir the liquid mixture
on filling, which could incur the collection of nonrepresentative sample.
In addition, the sampler tended to exclude large particles in the wastes.
Increasing the tube/stopper annular clearance did not seem practical because
it conversely reduced the opening of the reducer fitting of the sampling
tube.
Final Design
A much improved and recommended model of the Coliwasa is shown in Fig-
ure 1 of the text. This model features three main improvements over the
previous models. The first improvement consists of the use of a positive,
quick engaging closing and locking mechanism. This mechanism consists of a
short-length, channeled aluminum bar that is attached to the sampler's
stopper rod by an adjustable swivel. The aluminum bar serves both as a
T-handle and lock for the sampler's closure system. When the sampler is in
the open position, the handle is placed in the T-position and pushed
down agains the locking block. This manipulation pushes out the
57
-------
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neoprene stopper and opens the sampling tube. In the close position, the
handle is rotated until one leg of the T is squarely perpendicular against
the locking block. This tightly seats the neoprene stopper against the
bottom opening of the sampling tube and positively locks the sampler in the
close position. The closure tension can be adjusted by shortening or length-
ening the stopper rod by slightly screwing it in or out of the T handle
swivel. In discharging a collected sample, the T handle is slowly brought
into the T-position. This facilitates the opening of the sampler at a con-
trollable rate and permits the transfer of the sample into a sample container
at a regulated rate, thus minimizing splashing or loss of sample.
The second improvement made is the use of a sharply tapered neoprene
stopper. The sharp taper of the stopper eliminates the use of guide wires
and facilitates the proper seating of the stopper against the opening of the
sampling tube on closure. This stopper can be fabricated to specfications by
plastic products manufacturers at an extremely high price, or it can be made
by simply grinding down the inexpensive,and commercially available neoprene
stopper to the desired taper with a shop grinder (Note 1 in Appendix B).
The third improvement is the use of translucent PVC and glass pipes
as the sampling tubes. These tubes permit the observation of the phases of
the liquid waste sample collected in the sampler. The glass sampling tube
is usually used with a Teflon stopper rod. Each tube is used for different
purposes, as described in Section 4 of the text.
The improved model of the Coliwasa was tested in the field and in the
laboratory and found to be the most practical and capable of collecting
representative samples of multiphase liquid wastes samples.
Laboratory Tests
In the laboratory, the testing was conducted using test liquid mixtures
in a 122-cm (4-ft) tall by 15.2-cm(6-in.) I.D. glass cylindrical tank. The
glass tank was ideal for the tests because it permitted observation and
measurement of the relative heights of the liquid phases.
A two-phase liquid^mixture consisting of about 13.9 liters of water
and 3.29 liters of waste oil was sampled with the Coliwasa. The sample
was emptied into a 1000-ml (1.056 qt) graduated cylinder. The relative
volumes of the liquids were determined and given in Table A-l.
The results indicate that the Coliwasa is capable of obtaining a repre-
sentative sample of a two-phase liquid mixture.
59
-------
TABLE A-l.
Relative Volumes of Liquids in the Two-Phase Mixture
Item
Oil
Water
% by height of
phases in tank
% by volume collected
19
22
81
78
A three-phase mixture was sampled next. The mixture was prepared by
combining waste oil, water, and trichloroethylene (TCE) in the test tank.
The TCE extracted some of the waste oil and foamy emulsions formed at the
oil/water and the water/TCE interfaces. However, three distinct phases
were still obtained. Just like tihe previous experiment, the starting
heights of the liquid phases for :each trial were measured. The mixture
was sampled with the Coliwasa. The samples were each discharged into
1000-ml (1.056 qt) graduated cylinders and the relative volumes of the
liquid phases were determined (Table A-2).
TABLE A-2.
Relative Volumes of Liquids in the Three-Phase Mixture
Item
Oil
Aqueous
TCE
Trial I:
% by height of
phases in tank
% by volume collected
Trial II:
% by height of
phases in tank
% by volume collected
Average:
% by height of
phases in tank
% by volume collected
9.3
10 i. 2
i
8.8
9.8
77.4
79.6
75.0
79.0
76.0
79.0
14.7
10.8
15.0
10.7
15.0
11.0
60
-------
1
The results indicate that the Coliwasa is capable of collecting a
representative sample of a three-phase mixture within 5% accuracy. The
greatest nonrepresentative error, as anticipated, occured at the bottom
phase because the samplers rubber stopper prevents sampling of the last
2.54 cm(l in.) to the bottom of the container. This error decreases as
the bottom phase increases in volume as compared to the upper phases.
With less viscous and completely immiscible test liquids, the representa-
tiveness of the sample collected approaches unity.
Field Tests
The field tests consisted of sampling liquid wastes in drums and in
vacuum trucks. Drums of unknown liquid wastes are sampled at a hazardous
waste (Class I) disposal site in California. The sampler, which has a
4.8-cm (1 7/8-in.) O.D., easily cleared through the drum's bung holes.
Sampling was relatively fast. From the time a drum was opened, a
sample was collected and transferred into a container in less than 5
minutes. While a sample was in the sampler, no leakage was detected,
indicating a positive seal by the sampler's closing mechanism. On the
transfer of sample to a container, no splashings were observed, showing
that the sampler's content can be discharged at a regulated rate.
A drum containing a two-phase liquid waste mixture was also sampled.
Replicate samples were obtained, and each was placed in separate contain-
ers. The ratios of the liquid phases in each of the samples were deter-
mined and found to be approximately the same, indicating that reproducible
samples can be collected with the sampler.
Incoming vacuum trucks carrying liquid wastes to the disposal site
were sampled next with the Coliwasa. Again, the sampler was found to be
functional and very easy to use. Collection of samples was very fast,
minimizing the exposure of the sample collector to hazardous fumes and
other emissions from the wastes. Only one vacuum truck with a narrow hatch
opening and a total depth of about 163 cm(5.3 ft) was not successfully
sampled. The sampling tube of the Coliwasa is only 152 cm(5 ft) long.
A longer sampling tube (i.e.,183 cm(6 ft) long) could have remedied
the problem.
61
-------
APPENDIX B. PARTS FOR CONSTRUCTING THE COLIWASA
Item
Supplier
Approximate
Cost3
Sample tube, PVC plastic, trans-
lucent, 4.13 cm(l 5/8 in.) I.D. X
1.52 m(5 ft) long X 0.4 cm(5/32 in.)
Sample tube, glass borosilicate,
4.13 cm(l 5/8 in.) I.D. X 1.52 m
(5 ft) long, Code 72-1602.
Stopper, rubber, neoprene, #9,
modified as described in footnote'."
Stopper rod, PVC, 0.95 cm(3/8 in.)
O.D. X 1.67 m(5h ft) long. |
Stopper rod, Teflon, 0.95 cm(3/8 in.)
O.D. X 1.67 m(5% ft) long.
Locking block without sleeve, PVC|,
3.8 cm(l% in.) O.D. X 10.2 cm(4 ifr.)
long with l.ll-cm(7/16 in.) hole ;
drilled through center.
Sleeve, PVC, 4.13 cm(l 5/8 in.) ll.D.
X 6.35 (2% in.) long.
T-handle, aluminum, 18 cm(7 in.)long
X 2.86 cm(l 1/8 in.) wide with 1.27
cm(% in.) wide channel.
Swivel, aluminum bar, 1.27 cm(% ih.)
square X 3.8 cm(l% in.)long with i
3/8 National Coarse (NC) inside
thread to attach stopper rod.
Nut, PVC, 3/8 in. NC thread
Washer, PVC, 3/8 in.
Nut, SS, 3/8 in., NC
Washer, SS, 3/8 in.
Bolt, 3.12 cm(l h in.)long X 3/16; in.
Nut, 3/16 in., NC
Washer, lock 3/16 in.
Plastic supply houses $ 4.00 each
Corning Glass Works,
Corning, N.Y. '
Laboratory supply
$18.00 each
$ 6.00/0.45
kg(lb)
Plastic supply houses $ 5.00/6.1 m
(20 ft)
Plastic supply houses $30.00/3.05 m
(10 ft)
Fabricate. Rods avail-
able at plastic supply
houses. Can be bought
in 30.48 cm(l ft)length
Fabricate from stock of $ .80/30.48
4.13 cm(l 5/8 in.) I.D. cm(ft)
PVC pipe. Available at
plastic supply houses
Fabricate. Aluminum bar $3.00/1.83
stock available at hard- m(6 ft)
ware stores.
Fabricate. Aluminum bar $ 3.00/1.83
stock available at hard- m(6 ft)
ware stores.
Plastic supply houses $ .03 each
Plastic supply houses $ .03 each
Hardware stores $ .10 each
Hardware stores $ .10 each
Hardware stores $ .10 each
Hardware stores $ .03 each
Hardware stores $ .03 each
1977 prices
62
-------
I
Shape the stopper into a cone as follows: Bore a 0.95-cm(3/8-in.)
diameter center hole through the stopper. Insert a short piece of
0.95-cm(3/8~in.) O.D. handle through the hole until the end of the
handle is flush against the bottom (smaller diameter) surface of
the stopper. Carefully and uniformly turn the stopper into a cone
against a grinding wheel. This is done by turning the stopper with
the handle and grinding it down conically from about 0.5 cm(3/16 in.)
of the top (larger diameter) surface to the edge of the 0.95-cm(3/8-in.)
hole on the bottom surface.
APPENDIX C. CHECKLIST OF ITEMS REQUIRED IN THE FIELD SAMPLING OF HAZARDOUS
WASTES.
Quantity
Item
Use
Supplier
Approximate
Cost
Coliwasa,
plastic
type
(Section 4)
Coliwasa,
glass type
(Section 4)
Soil samp-
ler j auger
(Section 4)
Grain
sampler
(Section 4)
Scoop,
stainless
steel blade
(Section 4)
Fabricate^ Parts
can be purchased
from hardware
stores (see
Section 4)
To sample liquid Fabricate^ Parts $ 16.00
wastes, except
ketones, nitro-
benzene, dimethyl-
foramide, tetra-
hydrofuran and
pesticides
To sample liquid Fabricate; Glass $ 25.00
waste with pesticides, tube available from
and other wastes that Corning Glass Co.
cannot be sampled with Corning, K.Y. 14830
plastic Coliwasa ex- (see Section 4)
cept strong alkali and
hydrofluoric acid
solution
To sample contaminated Weyco Distributor $ 70.00
soil, dried ponds, etc. 1417 Heskett Way
Sacramento,Calif.
95825
To sample powdered
or granular wastes
Laboratory supply $ 50.00
houses
To sample top soil or Cole-Parmer
shallow layers of solid Instruments
wastes Chicago, 111.
$ 25.00
63
-------
APPENDIX C (continued).
Quantity Item
Use
Supplier
Approximate
Cost
Veihmeyer
soil samp-
ler
(Section 4)
Pond samp-
ler
(Section 4)
To collect soil core
samples
To sample ponds, pits,
etc. I
Trier,
single slot
(Section 4)
Waste pile
sampler
(Section 4)
To sample granular
and powdered material
in piles, sacks,
fiberdrums, etc.
To sample waste piles
1000-,2000- To contain solid and
ml(l-qt,2-qt) liquid samples except
linear pesticides and chlor-
polyethylene inated\hydrocarbons
i
Coverall, Protective garment
long- i
sleeved,
cotton
Suit,
neoprene
rubber, long"-
sleeved
Protective garment
Hansen Machine, $ 200.00
334 N. 125h St.,
Sacramento,Calif.
95815
Fabricate (see $ 9.00
Section 4).Clamps
available at
Cole-Parmer
Instrument
3060 Gibraltar Ave.
Costa Mesa,Calif.
92626
Telescoping handle $ 16.24
available at
swimming pool
supply houses
Curtin-Matheson
Scientific
470 Valley Drive
P.O.Box 386
Brisbane,Calif.
94005
Fabricate. PVC
pipe available at
hardware stores
(see Section 4)
Laboratory supply
houses
$ 25.00
$ 3.00
11.OO/
pkg.6
1
pair
Gloves, neo- Protective garment
prene rubber
Clothing stores $ 14.00
MSA,Catalog #33496 $ 210.00
Laboratory supply $ 4.20
houses
64
-------
I
APPENDIX C (continued).
Quantity
Item
Use
Supplier
Approximate
Cost
12
each
Self-contained For use in atmospheres MSA,Catalog
breathing deficient in oxygen #461704,
apparatus or otherwise immedi- Model 401 or
ately dangerous to equivalent
life.
Respirator,
chemical
cartridge
type
Cartridges for
respirator
For use in atmospheres Comfo 11 Respir-
not immediately ator, MSA,Catalog
dangerous to life #460968
or equivalent
For use in atmospheres CMC Cartridge,MSA
not immediately Cat.#459317 & GMD
dangerous to life Cartridge, MSA
Cat.#459318 or
equivalent
1
pair
1
1
Goggles
Portable
eyewash
Fire extin
quisher
Hard hat
Gas mask
18.9-liter
(5-gal) water
in cubitainer
or equivalent
with spigot
Teflon liners
for Bakelite
caps
Eye protection
For emergency
eyewash
Fire suppression
Head protection
For use in contami-
nated atmospheres
immediately dangerous
to life
For miscellaneous
washing purposes
To provide inert cap
liners
Sample labels, To document sample
seals, sample
analysis re-
quest sheets,
chain of
custody
records
65
MSA,Cat.#79179 or
equivalent
Laboratory supply
houses
Scientific Products
S1365-1 or equiva-
lent
MSA, Cat.#454740 or
equivalent
MSA, Cat.#448983 or
equivalent
Laboratory supply
houses
Scientific Special-
ties, P.O.Box 352
Randallstown, Md.
21133 or other
suppliers
Design using infor-
mation from Section
6
$580.00
$ 9.00
$ 5.00
$ 5.00
$ 4.00
$ 60.00
$ 5.00
$ 70.00
$ 5.50
$ 9.00
-------
APPENDIX C (continued).
Quantity Item
1
1
1
6
12
4
1
1
1
1
Field log book
(Section 6)
Weighted bottom
sampler
(Section 4)
Disposable
towels or
rags
Large poly-
ethylene bags
Polyethylene
bags
Waterproof
pens
Technical
grade
trichloro-
ethylene
Apron, oil
and acid
proof
Face mask
18.9 liter
(5-gal)
can
Usje
To keep isample records
To sample storage
tanks or similar
containers
To clean sampling
equipment
To store' waste papers ,
rags, etc.
To store sample
containers
i
To complete records
and labels
To clean samplers
Protective garment
Protective garment
i
To store used
cleaning solvent
'
Supplier Approximate
Cost
Office supply
stores
Fabricate (see
Section 4 and
Figure 9)
Terry towels or
$ 2.00
$ 25.00
$ 4.00/
equivalent . Avail- pkg .
able at chemical
supply houses
Plastic supply
houses
Plastic supply
houses
Stationery stores
Chemical supply
stores
McMaster-Carr Co.
P.O.Box 4355
Chicago, 111.
MSA
400 Penn Center
Blvd.
Pittsburg, Pa.
15235
Hardware stores
$ 11. OO/
pkg/ 100
$ 4.00/
pkg/100
$ 3.00
$ 22. OO/
gal.
$ 9.00
$ 4.00
$ 5.00
66
-------
APPENDIX D. RANDOM SAMPLING
Random Numbers
03
97
16
12
55
16
84
63
33
57
18
26
23
52
37
70
56
99
16
31
47
74
76
56
59
22
42
01
21
60
18
62
42
36
85
29
62
49
08
16
43
24
62
85
56
77
17
63
12
86
07
38
40
28
94
17
18
57
15
93
73
67
27
99
35
94
53
78
34
32
92
97
64
19
35
12
37
22
04
32
86
62
66
26
64
39
31
59
29
44
46
75
74
95
12
13
35
77
72
43
36
42
56
96
38
49
57
16
78
09
44
84
82
50
83
40
96
88
33
50
96
81
50
96
54
54
24
95
64
47
17
16
97
92
39
33
83
42
27
27
47
14
26
68
82
43
55
55
56
27
16
07
77
26
50
20
50
95
14
89
36
57
71
,27
46
54
06
67
07
96
58
44
77
11
,08
38
87
:45
,34
87
61
20
07
31
22
82
88
19
82
54
09
99
81
97
30
26
75
72
09
19
46
42
32
05
31
17
77
98
52
49
79
83
07
00
42
13
97
16
45
20
98
53
90
03
62
37
04
10
42
17
83
11
45
56
34
89
12
64
59
15
63
32
79
72
43
93
74
50
07
46
86
46
32
76
07
51
25
36
34
37
71
37
78
93
09
23
47
71
44
09
19
32
14
31
96
03
93
16
68
00
62
32
53
15
90
78
67
75
38
62
62
24
08
38
88
74
47
00
49
49
HOW TO USE THE TABLE OF RANDOM NUMBERS:
1. Based on available information, segregate the containers (i.e., drums,
sacks, etc.) according to waste types.
2. Number the containers containing the same waste types consecutively,
starting from 01.
3. Decide on how many samples you wish to take. This number is usually
determined by the objective of the sampling. For regular surveil-
lance sampling, the collection of one or two samples is usually
adequate. In this case, random sampling is not necessary. But for
regulatory or research purposes, more samples (such as one sample for
every group of five containers) taken at random will generate more
statistically valid data. Hence if there were 20 drums containing
the same type of waste, 5 drums have to be sampled.
4. Using the set of random numbers above, choose any number as a starting.
point.
5. From this number, go down the column, then to the next column to the
right, or go in any predetermined direction until you have selected
five numbers between 01 and 20, with no repetitions. Larger numbers
are ineligible.
Example: If you were to choose 19 as the starting point on column
four, the next eligible numbers as you go down this
column are 12 and 04. So far you have chosen only three
67
-------
eligible numbers. [Proceed to the next column to the right.
Going down and starting from the top of this column, the
next eligible numbers are 12 and 13. But 12 is already
chosen. Proceeding to the sixth column, the next eligible
number is 16. Your five random numbers, therefore, are
19, 12, 04, 13 and 16. Thus the drums with corresponding
numbers have to be| sampled.
APPENDIX E. SYSTEMATIC ERRORS USING THE COLIWASA
j
Certain systematic errors may occur in the determination of relative
phase composition of waste when using the Coliwasa. This error, in which
certain phases are disproportionately represented, results from the use
of a straight-sided sample tube tfci sample a container (tank truck) with
a circular cross section. On the* basis of a two-phase system, error is
at a minimum when the phase interface is at the tank center and at a
maximum when the interface is neajr the bottom or top of the tank. These
errors do not occur when sampling! a drum or other container when sampling
is done down the axis of the container (cylinder).
i
Errors in relative phase composition encountered in sampling the
typical cylindrical vacuum truck may be estimated using Table E-l. Num-
bers given in the table are representative values calculated from the
equations given below, which relajte the geometry of the sample tube to
the geometry of the tank truck. |
% A (tank) t= (9-Sin 9)
j 2ir
% A(sample) = 1-Cos % 9
' 2
Vacuum truck
Sample tube
68
-------
TABLE E-l. SAMPLE VOLUME CORRECTION FACTORS WHEN
SAMPLING CYLINDRICAL TANKS WITH"COLIWASA
% A in sample
% A in tank
Correction
10
20
30
40
50
60
70
80
90
100
5.20
14.2
25.2
37.4
50
62.6
74.8
85 . 8
94.8
100
+ 4.80
+ 5.8
+ 4.8
+ 2.6
0
- 2.6
- 4.8
- 5.8
- 4.8
0
69
-------
I
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-600/2-80-018
2.
3. RECIPIENT'S ACCESSION-NO.
4. TITLE AND SUBTITLE
Samplers and Sampling Procedures fori Hazardous
Waste Streams !
5. REPORT DATE
January 1980 (Issuing Date)
6. PERFORMING ORGANIZATION CODE
7< AUTHOR|mil R. deVera, Bart P. Simmons, Robert D.
Stephens and David L. Storm. [
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Hazardous Materials Laboratory [
California Department of HealthjServices
2151 Berkeley Way
Berkeley, CA 94704 j
10. PROGRAM ELEMENT NO.
C73D1C, SOS #1, Task 32
11. CONTRACT/GRANT NO.
R 804692010
12, SPONSORING AGENCY NAME AND ADDRESS \ (Jin . , UtL
Municipal Environmental Research Laboratory—
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268 I
13. TYPE OF REPORT AND PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
EPA/600/14
15. SUPPLEMENTARY NOTES
Richard A. Carries, Project Officer (513/684-7871)
16. ABSTRACT
The goal of this project was to develop simple but effective sampling equipment
and procedures for collecting, handling, storing, and recording samples of hazardous
wastes. The report describes a variety! of sampling devices designed to meet the needs
of those who regulate and manage hazardous wastes. Particular emphasis is given to
the development of a composite liquid waste sampler, the Coliwasa. This simple device
is designed for use on liquid and semi-jliquid wastes in a variety of containers, tanks,
and ponds. Devices for sampling solids and soils are also described.
In addition to the sampling devices, the report describes procedures for develop-
ment of a sampling plan, sample handling, safety precautions, proper recordkeeping
and chain of custody, and sample containment, preservation, and transport. Also
discussed are certain limitations and potential sources of error that exist in the
sampling equipment and the procedures. ! The statistics of sampling are covered
briefly, and additional references in tihis area are given.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSAT1 Field/Group
Samplers
Lagoons (ponds)—waste disposal
Hazardous materials
Representative sampling
Composite sampling
Sampling plans
Sampling procedures
Hazardous waste
Composite liquid waste
sampler
68C
18. DISTRIBUTION STATEMENT
Release unlimited
19. SECURITY CLASS (ThisReport)
unclassified
21. NO. OF PAGES
78
20. SECURITY CLASS (Thispage)
unclassified
22. PRICE
EPA Form 2220-1 (9-73)
70
* U.S. GOVERNMENT PRINTING OFFICE: 1960-657-165/0005
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