ASTM D4296-83(1999)
(Practice)Standard Practice for Sampling Pitch
Standard Practice for Sampling Pitch
SCOPE
1.1 This practice covers procedures for sampling pitch at points of manufacture, storage, and delivery.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 10.
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An American National Standard
Designation:D4296–83 (Reapproved 1999)
Standard Practice for
Sampling Pitch
This standard is issued under the fixed designation D 4296; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Significance and Use
1.1 This practice covers procedures for sampling pitch at 4.1 Sampling is as important as testing. If the sampling is
points of manufacture, storage, and delivery. improperly done, the sample of the material will be in error,
1.2 This standard does not purport to address all of the and the analysis will not represent the true properties of the
safety concerns, if any, associated with its use. It is the material, and it may be impossible or impracticable to take
responsibility of the user of this standard to establish appro- another sample; whereas, if the sample is properly taken and
priate safety and health practices and determine the applica- the analysis is in error, another analysis can readily be made of
bility of regulatory limitations prior to use. Specific hazard the original sample.
statements are given in Section 11. 4.2 Samples may be taken for either of the following two
purposes:
2. Terminology
4.2.1 To represent as nearly as possible an average of the
2.1 Definitions: bulk of the materials sampled, or
2.1.1 bulk sample—a large sample, either from one place or
4.2.2 To ascertain the maximum variation in characteristics
made up of several incremental samples of the same material. which the material possesses.
2.1.2 composite sample—a thoroughly mixed gross sample.
4.3 A good sampling plan has the following characteristics:
2.1.3 gross sample—a large sample made up of several 4.3.1 It protects the consumer against the acceptance of a
portions (increments) of a mass of material.
bad batch of material.
2.1.4 increment—a portion of a material to be combined 4.3.2 It protects the producer against the rejection of a good
with other portions of the same material to provide a larger
batch of material.
sample which will represent the whole material. 4.3.3 It gives long-range protection to the consumer.
2.1.5 representative sample—a part of a homogeneous ma-
4.3.4 It encourages the producer to keep his process in
terial, or a part of the composited and mixed portions of a
control.
material, which carries all the true properties and physical 4.3.5 It minimizes the cost of sampling, inspection of
characteristics of the whole material.
testing, and administration.
2.1.6 sample—a part taken as representative of a whole 4.3.6 It provides information concerning the quality of the
material.
product.
4.4 Sampling Integrity:
3. Summary of Practice
4.4.1 When one takes a sample, one is attempting to
3.1 Samples of liquid pitches are taken from process lines,
represent a batch or lot of material with that sample. Different
storage, and shipment containers in increments required to
forms of pitch, and pitch in different types of containers, need
prepare a representative sample for testing.
to have different sampling plans and appropriate sampling
3.2 Samples of solid pitches are taken from loading sys-
equipment. Each sampling plan should be designed so that it
tems, storage, and shipment containers in increments required
accomplishes its objective, which is to ascertain the character-
to prepare a representative sample for testing.
istics or quality of a batch or lot of material.
5. Selection of Samples
This practice is under the jurisdiction of ASTM Committee D-2 on Petroleum
5.1 Pitches shall be sampled by the producer at the point of
ProductsandLubricantsandisthedirectresponsibilityofSubcommitteeD02.05.OF
manufacture or storage, and at such time as to allow the tests
on Industrial Pitches.
controlling acceptance or rejection of quality, as specified by
Current edition approved Oct. 28, 1983. Published February 1984.Originally
e1
published as D 4296 - 83. Last previous edition D 4296- 83 (1994) . the consumer, to be made in advance of a shipment.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4296
5.2 Samples of pitches shall be taken by the consumer from 10.1.1 If so equipped, pipe lines and storage tanks may be
the shipment containers immediately upon delivery and receipt sampled from valves installed in the lines or up the side of the
and tests controlling acceptance or rejection of quality, as tanks.Atypical tank valve is shown in Fig. 1, and suitable line
described by the consumer’s specifications, shall be made as valves are illustrated in Fig. 2 and Fig. 3.
soon as possible. 10.1.2 For sampling tank trucks, a pipe connection with
attached sample valve similar to the one shown in Fig. 2 may
6. Size of Samples
be inserted between the outlet pipe and unloading line.
6.1 The sample size of liquid materials shall be as follows:
10.1.3 A weighted sample bottle similar to those shown in
6.1.1 From process lines, 1 L (1 qt). Fig. 4 and Fig. 5, or a “thief sampler” as shown in Fig. 6, or a
6.1.2 From bulk storage, 1 L (1 qt) or 1-L aliquot of
“dip sampler” similar to that shown in Fig. 7, may be used to
composite sample. sample production and storage tanks, tank cars, and tank
6.1.3 From bulk shipment containers, 1 L (1 qt) or 1-L
trucks.
aliquot of composite sample. 10.1.4 A “tube” or “thief” sampler may be used to sample
6.1.4 From barrels or drums, 0.5 L(1 pt) or 0.5-Laliquot of
materials in drums or barrels.
composite sample. 10.2 Sampling Equipment for Solid Materials:
6.2 The sample size of solid materials shall be as follows: 10.2.1 Samples from loading systems may be taken with a
6.2.1 From storage area, 4 L (1 gal) or 4-L aliquot of shovel, metal or plastic scoop, or metal can.
composite sample. 10.2.2 A shovel may be used to sample storage bins, pitch
6.2.2 From bulk shipment containers, 4 L (1 gal) aliquot of
piles, pitch bays, hopper cars, and dump trucks.
composite sample. 10.2.3 A sampling spear as shown in Fig. 8 may be used to
6.2.3 From barrels or drums, 0.5-L(1 pt) or 0.5-Laliquot of
sample materials in drums, barrels, bags, and silos.
composite sample. 10.3 Sampling Containers:
10.3.1 Containers for liquid materials shall be wide-mouth
7. Collection of Gross Sample
cans with line screw caps or triple-seal friction-top cans.
7.1 Acollection of gross sample represents a lot or batch of
10.3.2 Containers for formed pitches or crushed solid pitch
material and is composed of a number of increments.
shall be triple-seal friction-top cans, sealable plastic or paper
7.1.1 Collect the increments regularly and systematically, so
cartons with inert inside coating, plastic sacks placed in other
that the entire quantity of pitch sampled will be represented
containers suitable for handling, or substantial strength paper
proportionately in the gross sample, and with such frequency
bag which can be stapled closed.
that a gross sample of the required amount will be collected.
10.4 Mixing Equipment for Solid Materials:
10.4.1 Section of clean canvas or plastic sheet of sufficient
8. Size of Increments
size to contain a large bulk sample which is to be reduced by
8.1 To collect samples, use a shovel or specially designed
mixing and quartering.
tool or mechanical means for taking equal portions or incre-
10.4.2 A “riffle” as shown in Fig. 9 may be used for
ments. When samples are collected from the surface of loaded
reducing gross samples to smaller sizes for testing.
shipments, the gross sample shall consist of nine increments of
10.4.3 A “shovel” may be used to reduce gross samples to
approximately equal quantity. When sampling from piles,
smaller sizes by mixing and quartering as shown in Fig. 10.
conveyer belts, etc, the gross sample shall consist of not less
10.5 Mixing Equipment for Liquid Materials:
than 25 nor more than 50 increments of approximately equal
quantity.
9. Protection and Preservation of Samples
9.1 Sample containers shall be new or reusable containers
which can be thoroughly cleaned with a solvent and wiped dry
with a clean dry cloth.
9.2 Care shall be taken to prevent the sample from becom-
ing contaminated. Immediately after filling, hot liquid sample
containers shall be positively covered, but not tightly sealed.
Containers of solid materials shall be tightly and positively
sealed.
9.3 While sampling during inclement weather, attention
shall be paid to prevent water from dropping into the hot liquid
sample or samples of solid materials.
9.4 Immediately after filling and sealing, the sampling
containers shall be properly marked for identification with a
suitable pencil on the container itself, not on the lid.
10. Apparatus
10.1 Sampling Equipment for Liquid Materials: FIG. 1 Typical Submerged Sampling Device
D4296
FIG. 2 In-Line Sampling Device
FIG. 3 Pipeline Sampler
10.5.1 Sample sizes of 4 L (1 gal) or less can be mixed by 10.5.2 A heavy duty electric stirrer is recommended for
thorough stirring with a metal rod or wide blade metal paddle. sample volumes over 4 L (1 gal) to 20 L (5 gal) in size.
D4296
FIG. 4 Weighted Sampling Can
11. Hazards 12. Sampling Liquid Pitch
11.1 The sampler shall wear protective clothing, goggles,
12.1 The following three sampling methods are recom-
and rubber or heat-resistant gloves to protect oneself from
mended for sampling vertical tanks not capable of being
accidental contact with hot liquid pitch.
agitated:
11.2 For prolonged exposure to the presence of pitch vapors
12.1.1 Sample-Valve Method—Locate valves, with easy and
or pitch dust, a suitable respirator mask should be worn to
safe access provided, on the side of the tank with the first in the
avoidinhalationofpitchvaporsordust.Itisrecommendedthat
top third of the tank, but no higher than 1 m (3 ft) from the top;
an appropriate barrier cream be applied to exposed areas of the
thesecondinthemiddleofthetank;andthethirdinthebottom
skin.
third of the tank, but no lower than 1.1 m (3 ⁄2 ft) from the
11.3 Sampling from rail cars shall be avoided when there is
bottom. A recommended design of the sample valve is shown
a possibility of shunting operations taking place. It is recom-
in Fig. 1. Draw a minimum of 4 L (1 gal) of the product from
mended that flags be placed on both ends of the car to prevent
each sample valve for test or composite.
accidental movement during sampling.
12.1.2 Thief Sampling Method—Take samples at the top,
11.4 It is recommended that not less than two persons be
middle and lower sections of the tank by lowering a thief
present when samples are taken from hot bulk vessels such as
storage tanks, tank cars, and tank trucks. sampler into the material. A satisfactory type with instructions
D4296
NOTE 1—This type sampler is lowered into the tank with the stopper in place. When the desired depth is reached, the stopper is removed by means
of the attached wire, cord, or chain and the container allowed to fill. Complete filling is indicated by the cessation of bubbles of air from the can at the
surface of the liquid. The sampler is then withdrawn from the tank and the contents poured into the clean sampler container. A clean can (bottle) must
be used for each sample taken.
FIG. 5 Throw-Away Container Sampler
for use is shown in Fig. 6. The samples may be tested 12.1.3.3 The three samples may be tested separately for
separately or combined and mixed thoroughly for a composite consistency to detect stratification or they may be combined,
analysis. thoroughly mixed, anda1to4-L( ⁄4 to 1-gal) aliquot of the
12.1.3 Weighted Sample Bottle Method—Take samples at composite taken for determining the average characteristics of
the top, middle, and lower sections of the tank by lowering the the material.
bottle into the material. Two types of weighted sampling 12.2 Sampling Bulk Storage Tanks Equipped with Mechani-
bottles are illustrated in Fig. 4 and Fig. 5. cal Agitators or Recirculating Pumps—When the tank is
12.1.3.1 The essential feature of the method is to drop the equipped with operating mechanical agitators or recirculating
stoppered bottle into the material to the desired depth, and then pumping systems which are performing adequate mixing of the
pull the stopper by means of an attached chain. When the tank contents, take a single sample by any of the methods
material fills the bottle, lift out of the liquid and empty into a described in 12.1.1, 12.1.2, or 12.1.3 to use for test purposes.
clean container. Drain the bottle as completely as possible, 12.3 Sampling Tank Cars and Tank Trucks:
re-insert the stopper, lower into the material to the next 12.3.1 Samples of hot liquid materials may be taken by the
sampling depth. dip method using a clean wide-mouth or friction-top can in a
12.1.3.2 Normally, there is not enough undrained residue suitable holder or firmly attached to a metal rod. One such dip
from the first sample to affect the properties of the next sample apparatus is shown in Fig. 7. Quickly lower the dip sample
taken from a different level. However, if substantial material about 0.3 m (1 ft) below the surface of the liquid and carefully
difference is suspected at various levels of the material, discard remove. Use a clean container to take each sample, and then
the first of successive samples to rinse the bottle and then transfer the material sampled to another clean container for
return the bottle to the same level for another sample. retention and testing.
D4296
discharge side of the pump, or in a completely filled line in
which gravity creates the material’s flow.
12.3.3.1 A suitable in-line sampling pipe is shown in Fig. 2
and Fig. 3. Turn the opening of the sampling pipe to face the
flow of the liquid. Provide the pipe with a valve or plug cock
and discharge into a sample receiver. Before the sample is
taken, draw 4 L (1 gal) of the material from the pipe valve and
discard.
12.3.3.2 Take samples of 1 L(1 qt) at such frequency during
the loading or unloading to providea4to8-L(1to 2-gal)
composite of the material. At the completion of the loading or
unloading, thoroughly mix the collected sample and take a 0.5
to 4-L ( ⁄8 to 1-gal) portion for testing.
12.4 Sampling from Drums or Barrels:
12.4.1 High-softening point pitches poured into drums for
storage and shipment will solidify at ambient temperatures and
sampling should be made in accordance with the procedure in
12.5.
12.4.2 Some
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