ASTM D4296-83(2004)
(Practice)Standard Practice for Sampling Pitch
Standard Practice for Sampling Pitch
SIGNIFICANCE AND USE
Sampling is as important as testing. If the sampling is improperly done, the sample of the material will be in error, and the analysis will not represent the true properties of the material, and it may be impossible or impracticable to take another sample; whereas, if the sample is properly taken and the analysis is in error, another analysis can readily be made of the original sample.
Samples may be taken for either of the following two purposes:
4.2.1 To represent as nearly as possible an average of the bulk of the materials sampled, or
4.2.2 To ascertain the maximum variation in characteristics which the material possesses.
A good sampling plan has the following characteristics:
4.3.1 It protects the consumer against the acceptance of a bad batch of material.
4.3.2 It protects the producer against the rejection of a good batch of material.
4.3.3 It gives long-range protection to the consumer.
4.3.4 It encourages the producer to keep his process in control.
4.3.5 It minimizes the cost of sampling, inspection of testing, and administration.
4.3.6 It provides information concerning the quality of the product.
Sampling Integrity—When one takes a sample, one is attempting to represent a batch or lot of material with that sample. Different forms of pitch, and pitch in different types of containers, need to have different sampling plans and appropriate sampling equipment. Each sampling plan should be designed so that it accomplishes its objective, which is to ascertain the characteristics or quality of a batch or lot of material.
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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4296–83 (Reapproved 2004)
Standard Practice for
Sampling Pitch
This standard is issued under the fixed designation D4296; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3.2 Samples of solid pitches are taken from loading sys-
tems, storage, and shipment containers in increments required
1.1 This practice covers procedures for sampling pitch at
to prepare a representative sample for testing.
points of manufacture, storage, and delivery.
1.2 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 Sampling is as important as testing. If the sampling is
responsibility of the user of this standard to establish appro-
improperly done, the sample of the material will be in error,
priate safety and health practices and determine the applica-
and the analysis will not represent the true properties of the
bility of regulatory limitations prior to use. Specific warning
material, and it may be impossible or impracticable to take
statements are given in Section 11.
another sample; whereas, if the sample is properly taken and
2. Terminology the analysis is in error, another analysis can readily be made of
the original sample.
2.1 Definitions:
4.2 Samples may be taken for either of the following two
2.1.1 bulk sample—a large sample, either from one place or
purposes:
made up of several incremental samples of the same material.
4.2.1 To represent as nearly as possible an average of the
2.1.2 composite sample—a thoroughly mixed gross sample.
bulk of the materials sampled, or
2.1.3 gross sample—a large sample made up of several
4.2.2 To ascertain the maximum variation in characteristics
portions (increments) of a mass of material.
which the material possesses.
2.1.4 increment—a portion of a material to be combined
4.3 A good sampling plan has the following characteristics:
with other portions of the same material to provide a larger
4.3.1 It protects the consumer against the acceptance of a
sample which will represent the whole material.
bad batch of material.
2.1.5 representative sample—a part of a homogeneous ma-
4.3.2 It protects the producer against the rejection of a good
terial, or a part of the composited and mixed portions of a
batch of material.
material, which carries all the true properties and physical
4.3.3 It gives long-range protection to the consumer.
characteristics of the whole material.
4.3.4 It encourages the producer to keep his process in
2.1.6 sample—a part taken as representative of a whole
control.
material.
4.3.5 It minimizes the cost of sampling, inspection of
3. Summary of Practice testing, and administration.
4.3.6 It provides information concerning the quality of the
3.1 Samples of liquid pitches are taken from process lines,
product.
storage, and shipment containers in increments required to
4.4 Sampling Integrity—When one takes a sample, one is
prepare a representative sample for testing.
attempting to represent a batch or lot of material with that
sample. Different forms of pitch, and pitch in different types of
containers, need to have different sampling plans and appro-
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum
Products and Lubricants and is the direct responsibility of Subcommittee D02.05 on
priate sampling equipment. Each sampling plan should be
Properties of Fuels, Petroleum Coke and Carbon Material.
designed so that it accomplishes its objective, which is to
Current edition approved Nov. 1, 2004. Published November 2004. Originally
ascertain the characteristics or quality of a batch or lot of
approved in 1983. Last previous edition approved in 1999 as D4296 – 83 (1999).
DOI: 10.1520/D4296-83R04. material.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4296–83 (2004)
5. Selection of Samples 9.4 Immediately after filling and sealing, the sampling
containers shall be properly marked for identification with a
5.1 Pitches shall be sampled by the producer at the point of
suitable pencil on the container itself, not on the lid.
manufacture or storage, and at such time as to allow the tests
controlling acceptance or rejection of quality, as specified by
10. Apparatus
the consumer, to be made in advance of a shipment.
10.1 Sampling Equipment for Liquid Materials:
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,ora
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-
ments. When samples are collected from the surface of loaded
shipments, the gross sample shall consist of nine increments of
approximately equal quantity. When sampling from piles,
conveyer belts, and so forth, the gross sample shall consist of
not less 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. FIG. 1 Typical Submerged Sampling Device
D4296–83 (2004)
FIG. 2 In-Line Sampling Device
FIG. 3 Pipeline Sampler
10.4.2 A “riffle” as shown in Fig. 9 may be used for 10.4.3 A “shovel” may be used to reduce gross samples to
reducing gross samples to smaller sizes for testing. smaller sizes by mixing and quartering as shown in Fig. 10.
D4296–83 (2004)
FIG. 4 Weighted Sampling Can
10.5 Mixing Equipment for Liquid Materials: 11.4 It is recommended that no fewer than two persons be
10.5.1 Sample sizes of 4 L (1 gal) or less can be mixed by present when samples are taken from hot bulk vessels such as
thorough stirring with a metal rod or wide blade metal paddle. storage tanks, tank cars, and tank trucks.
10.5.2 A heavy duty electric stirrer is recommended for
12. Sampling Liquid Pitch
sample volumes over 4 L (1 gal) to 20 L (5 gal) in size.
12.1 The following three sampling methods are recom-
11. Hazards
mended for sampling vertical tanks not capable of being
11.1 The sampler shall wear protective clothing, goggles, agitated:
and rubber or heat-resistant gloves to protect oneself from 12.1.1 Sample-Valve Method—Locate valves, with easy and
accidental contact with hot liquid pitch. safe access provided, on the side of the tank with the first in the
11.2 For prolonged exposure to the presence of pitch vapors top third of the tank, but no higher than 1 m (3 ft) from the top;
or pitch dust, a suitable respirator mask should be worn to thesecondinthemiddleofthetank;andthethirdinthebottom
avoidinhalationofpitchvaporsordust.Itisrecommendedthat third of the tank, but no lower than 1.1m(3 ⁄2 ft) from the
an appropriate barrier cream be applied to exposed areas of the bottom. A recommended design of the sample valve is shown
skin. in Fig. 1. Draw a minimum of 4 L (1 gal) of the product from
11.3 Sampling from rail cars shall be avoided when there is each sample valve for test or composite.
a possibility of shunting operations taking place. It is recom- 12.1.2 Thief Sampling Method—Take samples at the top,
mended that flags be placed on both ends of the car to prevent middle and lower sections of the tank by lowering a thief
accidental movement during sampling. sampler into the material. A satisfactory type with instructions
D4296–83 (2004)
NOTE—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
theattachedwire,cord,orchainandthecontainerallowedtofill.Completefillingisindicatedbythecessationofbubblesofairfromthecanatthesurface
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.
D4296–83 (2004)
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 shou
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