ASTM D4296-24

Standard Practice for Sampling Pitch

SIGNIFICANCE AND USE
5.1 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.  
5.2 Samples may be taken for either of the following two purposes:  
5.2.1 To represent as nearly as possible an average of the bulk of the materials sampled, or  
5.2.2 To ascertain the maximum variation in characteristics which the material possesses.  
5.3 A good sampling plan has the following characteristics:  
5.3.1 It protects the consumer against the acceptance of a bad batch of material.  
5.3.2 It protects the producer against the rejection of a good batch of material.  
5.3.3 It gives long-range protection to the consumer.  
5.3.4 It encourages the producer to keep his process in control.  
5.3.5 It minimizes the cost of sampling, inspection of testing, and administration.  
5.3.6 It provides information concerning the quality of the product.  
5.4 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 The values stated in SI units are to be regarded as standard. The values in parentheses are for information only.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in Section 12.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 29-Feb-2024
• ICS: 91.100.50 - Binders. Sealing materials
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material

Relations

• Replaces: ASTM D4296-18 - Standard Practice for Sampling Pitch
• Effective Date: 01-Mar-2024
• Referred By: ASTM D2319/D2319M-20 - Standard Test Method for Softening Point of Pitch (Cube-in-Air Method)
• Effective Date: 01-Mar-2024
• Referred By: ASTM D2764-20 - Standard Test Method for Dimethylformamide-Insoluble (DMF-I) Content of Tar and Pitch
• Effective Date: 01-Mar-2024
• Referred By: ASTM D71-94(2019) - Standard Test Method for Relative Density of Solid Pitch and Asphalt (Displacement Method)
• Effective Date: 01-Mar-2024
• Referred By: ASTM D4715-98(2022)e1 - Standard Test Method for Coking Value of Tar and Pitch (Alcan)
• Effective Date: 01-Mar-2024
• Referred By: ASTM D4892-14(2019)e1 - Standard Test Method for Density of Solid Pitch (Helium Pycnometer Method)
• Effective Date: 01-Mar-2024
• Referred By: ASTM D4616-23 - Standard Test Method for Microscopical Analysis by Reflected Light and Determination of Mesophase in a Pitch
• Effective Date: 01-Mar-2024
• Referred By: ASTM D7280-20 - Standard Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch by Stainless Steel Crucible Filtration
• Effective Date: 01-Mar-2024
• Referred By: ASTM D2320-98(2022)e1 - Standard Test Method for Density (Relative Density) of Solid Pitch (Pycnometer Method)
• Effective Date: 01-Mar-2024
• Referred By: ASTM D4312-20 - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)
• Effective Date: 01-Mar-2024
• Referred By: ASTM D2415-20 - Standard Test Method for Ash in Coal Tar and Pitch
• Effective Date: 01-Mar-2024
• Referred By: ASTM D4072-23 - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch
• Effective Date: 01-Mar-2024
• Referred By: ASTM D3104-14a(2018) - Standard Test Method for Softening Point of Pitches (Mettler Softening Point Method)
• Effective Date: 01-Mar-2024
• Referred By: ASTM D3461-18 - Standard Test Method for Softening Point of Asphalt and Pitch (Mettler Cup-and-Ball Method)
• Effective Date: 01-Mar-2024
• Referred By: ASTM D2318-20 - Standard Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch
• Effective Date: 01-Mar-2024

Overview

ASTM D4296-24: Standard Practice for Sampling Pitch delivers comprehensive procedures for obtaining representative samples of pitch at all key points in its lifecycle - including manufacture, storage, and delivery. Developed by ASTM, this standard ensures that pitch samples accurately reflect the material’s properties, assisting both producers and consumers in making informed decisions on quality and consistency.

The significance of proper sampling is paramount, as the results of subsequent analyses rely on the accuracy and integrity of the initial sample. ASTM D4296-24 covers both liquid and solid forms of pitch and defines sampling procedures suited to various container types and handling situations.

Key Topics

• Sampling Objectives:

  • To obtain samples that represent an average or determine the variability of the bulk material.
  • To enable quality control and process management for both producer and consumer.

• Integrity of Sampling:

  • Emphasizes the need for carefully designed sampling plans tailored to pitch form and container type.
  • Details measures to prevent sample contamination or changes that could affect validity.

• Sampling Equipment and Methods:

  • Specifies tools such as shovels, thief samplers, sample valves, scoops, and riffles for both liquid and solid pitches.
  • Outlines how to select and use appropriate sample containers for preserving sample integrity.
  • Provides specific guidance for collecting increments to form gross and composite samples.

• Sample Documentation:

  • Requires properly marked containers and detailed sample identification, including data such as sampling date, method, location, batch, and equipment used.

• Safety and Environmental Practice:

  • Advises users of the need to follow appropriate safety, health, and environmental practices during sampling.
  • Recommends protective equipment and proper procedures for handling hot pitch or hazardous environments.

Applications

ASTM D4296-24 is crucial across industries where pitch is a key material component, supporting:

• Petroleum and Chemicals:
  Facilitates quality control in refineries and chemical plants producing or using pitch products.

• Manufacturing and Processing:
  Enables producers to implement consistent quality assurance measures for pitch used in products like electrodes, roofing, and paving.

• Logistics and Storage:
  Provides guidelines for on-site and in-transit sampling to validate the condition and quality of pitch delivered or stored.

• Laboratory Testing:
  Ensures laboratories receive representative pitch samples, leading to valid analytical results and compliance with buyer specifications.

• Regulatory Compliance:
  Assists organizations in meeting international trade, safety, and quality requirements for sampling and analysis of pitch products.

Related Standards

For a robust pitch quality management system, consider these related ASTM and international standards:

• ASTM D4175: Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants (referenced within D4296 for consistent terminology).
• Industry guidelines on sampling petroleum products and petrochemical feedstocks.
• International standards developed in alignment with WTO TBT principles, ensuring global acceptance and harmonization.

Practical Value

Implementing ASTM D4296-24 drastically reduces the risk of incorrect analytical results due to faulty sampling, which can lead to costly errors, product rejection, or acceptance of substandard material. By adhering to this standard, organizations ensure efficient, precise, and credible pitch sampling that supports product quality, consumer protection, and regulatory due diligence.

Keywords: pitch sampling, ASTM D4296-24, sampling practice, pitch quality, composite sample, petroleum standards, material testing, industrial pitch, sampling procedures, representative sample.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4296 − 24
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* portions of gross samples from different lots together in mass
fraction proportioned to the consignment.
1.1 This practice covers procedures for sampling pitch at
3.1.4 gross sample, n—in pitch, the original, uncrushed
points of manufacture, storage, and delivery.
representative portion taken from a shipment of pitch.
1.2 The values stated in SI units are to be regarded as
3.1.5 increment, n—a portion of a material to be combined
standard. The values in parentheses are for information only.
with other portions of the same material to provide a larger
1.3 This standard does not purport to address all of the
sample which will represent the whole material.
safety concerns, if any, associated with its use. It is the
3.1.6 representative sample, n—a portion extracted from a
responsibility of the user of this standard to establish appro-
total volume that may or may not contain the constituents in the
priate safety, health, and environmental practices and deter-
same proportions are present in the total volume.
mine the applicability of regulatory limitations prior to use.
Specific warning statements are given in Section 12.
3.1.7 sample, n—a part taken as representative of a whole
1.4 This international standard was developed in accor-
material.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Summary of Practice
Development of International Standards, Guides and Recom-
4.1 Samples of liquid pitches are taken from process lines,
mendations issued by the World Trade Organization Technical
storage, and shipment containers in increments required to
Barriers to Trade (TBT) Committee.
prepare a representative sample for testing.
2. Referenced Documents 4.2 Samples of solid pitches are taken from loading
2 systems, storage, and shipment containers in increments re-
2.1 ASTM Standards:
quired to prepare a representative sample for testing.
D4175 Terminology Relating to Petroleum Products, Liquid
Fuels, and Lubricants
5. Significance and Use
3. Terminology
5.1 Sampling is as important as testing. If the sampling is
improperly done, the sample of the material will be in error,
3.1 Definitions:
and the analysis will not represent the true properties of the
3.1.1 For definitions of terms used in this practice, refer to
material, and it may be impossible or impracticable to take
Terminology D4175.
another sample; whereas, if the sample is properly taken and
3.1.2 bulk sample, n—the reduced and divided representa-
the analysis is in error, another analysis can readily be made of
tive portion of the gross sample as prepared for shipment to and
the original sample.
received by a laboratory to be prepared for analysis.
5.2 Samples may be taken for either of the following two
3.1.3 composite sample, n—in pitch, a sample, representa-
purposes:
tive of an entire consignment of pitch, generated by mixing
5.2.1 To represent as nearly as possible an average of the
bulk of the materials sampled, or
5.2.2 To ascertain the maximum variation in characteristics
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum
which the material possesses.
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-
mittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
5.3 A good sampling plan has the following characteristics:
Current edition approved March 1, 2024. Published April 2024. Originally
5.3.1 It protects the consumer against the acceptance of a
approved in 1983. Last previous edition approved in 2018 as D4296 – 18. DOI:
10.1520/D4296-24.
bad batch of material.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.3.2 It protects the producer against the rejection of a good
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
batch of material.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 5.3.3 It gives long-range protection to the consumer.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4296 − 24
5.3.4 It encourages the producer to keep his process in conveyer belts, and so forth, the gross sample shall consist of
control. not less than 25 nor more than 50 increments of approximately
5.3.5 It minimizes the cost of sampling, inspection of equal quantity.
testing, and administration.
5.3.6 It provides information concerning the quality of the
10. Protection and Preservation of Samples
product.
10.1 Sample containers shall be new or reusable containers
5.4 Sampling Integrity—When one takes a sample, one is
which can be thoroughly cleaned with a solvent and wiped dry
attempting to represent a batch or lot of material with that with a clean dry cloth.
sample. Different forms of pitch, and pitch in different types of
10.2 Care shall be taken to prevent the sample from becom-
containers, need to have different sampling plans and appro-
ing contaminated. Immediately after filling, hot liquid sample
priate sampling equipment. Each sampling plan should be
containers shall be positively covered, but not tightly sealed.
designed so that it accomplishes its objective, which is to
Containers of solid materials shall be tightly and positively
ascertain the characteristics or quality of a batch or lot of
sealed.
material.
10.3 While sampling during inclement weather, attention
shall be paid to prevent water from dropping into the hot liquid
6. Selection of Samples
sample or samples of solid materials.
6.1 Pitches shall be sampled by the producer at the point of
10.4 Immediately after filling and sealing, the sampling
manufacture or storage, and at such time as to allow the tests
containers shall be properly marked for identification with a
controlling acceptance or rejection of quality, as specified by
suitable pencil on the container itself, not on the lid.
the consumer, to be made in advance of a shipment.
6.2 Samples of pitches shall be taken by the consumer from
11. Apparatus
the shipment containers immediately upon delivery and receipt
11.1 Sampling Equipment for Liquid Materials:
and tests controlling acceptance or rejection of quality, as
11.1.1 If so equipped, pipe lines and storage tanks may be
described by the consumer’s specifications, shall be made as
sampled from valves installed in the lines or up the side of the
soon as possible.
tanks. A typical tank valve is shown in Fig. 1, and suitable line
7. Size of Samples
valves are illustrated in Fig. 2 and Fig. 3.
11.1.2 For sampling tank trucks, a pipe connection with
7.1 The sample size of liquid materials shall be as follows:
attached sample valve similar to the one shown in Fig. 2 may
7.1.1 From process lines, 1 L (1 qt).
be inserted between the outlet pipe and unloading line.
7.1.2 From bulk storage, 1 L (1 qt) or 1 L aliquot of com-
posite sample.
7.1.3 From bulk shipment containers, 1 L (1 qt) or 1 L
aliquot of composite sample.
7.1.4 From barrels or drums, 0.5 L (1 pt) or 0.5 L aliquot of
composite sample.
7.2 The sample size of solid materials shall be as follows:
7.2.1 From storage area, 4 L (1 gal) or 4 L aliquot of
composite sample.
7.2.2 From bulk shipment containers, 4 L (1 gal) aliquot of
composite sample.
7.2.3 From barrels or drums, 0.5 L (1 pt) or 0.5 L aliquot of
composite sample.
8. Collection of Gross Sample
8.1 A collection of gross sample represents a lot or batch of
material and is composed of a number of increments.
8.1.1 Collect the increments regularly and systematically, so
that the entire quantity of pitch sampled will be represented
proportionately in the gross sample, and with such frequency
that a gross sample of the required amount will be collected.
9. Size of Increments
9.1 To collect samples, use a shovel or specially designed
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, FIG. 1 Typical Submerged Sampling Device
D4296 − 24
FIG. 2 In-Line Sampling Device
FIG. 3 Pipeline Sampler
11.1.3 A weighted sample bottle similar to those shown in
Fig. 4 and Fig. 5, or a “thief sampler” as shown in Fig. 6, or a
D4296 − 24
FIG. 4 Weighted Sampling Can
“dip sampler” similar to that shown in Fig. 7, may be used to 11.3.2 Containers for formed pitches or crushed solid pitch
sample production and storage tanks, tank cars, and tank
shall be triple-seal friction-top cans, sealable plastic or paper
trucks. cartons with inert inside coating, plastic sacks placed in other
11.1.4 A “tube” or “thief” sampler may be used to sample
containers suitable for handling, or substantial strength paper
materials in drums or barrels.
bag which can be stapled closed.
11.2 Sampling Equipment for Solid Materials:
11.4 Mixing Equipment for Solid Materials:
11.2.1 Samples from loading systems may be taken with a
11.4.1 Section of clean canvas or plastic sheet of sufficient
shovel, metal or plastic scoop, or metal can.
size to contain a large bulk sample which is to be reduced by
11.2.2 A shovel may be used to sample storage bins, pitch
mixing and quartering.
piles, pitch bays, hopper cars, and dump trucks.
11.4.2 A “riffle” as shown in Fig. 9 may be used for
11.2.3 A sampling spear as shown in Fig. 8 may be used to
reducing gross samples to smaller sizes for testing.
sample materials in drums, barrels, bags, and silos.
11.4.3 A “shovel” may be used to reduce gross samples to
11.3 Sampling Containers:
smaller sizes by mixing and quartering as shown in Fig. 10.
11.3.1 Containers for liquid materials shall be wide-mouth
cans with line screw caps or triple-seal friction-top cans. 11.5 Mixing Equipment for Liquid Materials:
D4296 − 24
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
11.5.1 Sample sizes of 4 L (1 gal) or less can be mixed by 12.4 It is recommended that no fewer than two persons be
thorough stirring with a metal rod or wide blade metal paddle. present when samples are taken from hot bulk vessels such as
11.5.2 A heavy duty electric stirrer is recommended for storage tanks, tank cars, and tank trucks.
sample volumes over 4 L (1 gal) to 20 L (5 gal) in size.
13. Sampling Liquid Pitch
12. Hazards
13.1 The following three sampling methods are recom-
mended for sampling vertical tanks not capable of being
12.1 The sampler shall wear protective clothing, goggles,
agitated:
and rubber or heat-resistant gloves to protect oneself from
13.1.1 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
12.2 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
the second in the middle of the tank; and the third in the bottom
avoid inhalation of pitch vapors or dust. It is recommended that
third of the tank, but no lower than 1.1 m (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
12.3 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- 13.1.2 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 − 24
13.1.3.1 The essential feature of the method is to drop the
stoppered bottle into the material to the desired depth, and then
pull the stopper by means of an attached chain. When the
material fills the bottle, lift out of the liquid and empty into a
clean container. Drain the bottle as completely as possible,
re-insert the stopper, lower into the material to the next
sampling depth.
13.1.3.2 Normally, there is not enough undrained residue
from the first sample to affect the properties of the next sample
taken from a different level. However, if substantial material
difference is suspected at various levels of the material, discard
the first of successive samples to rinse the bottle and then
return the bottle to the same level for another sample.
13.1.3.3 The three samples may be tested separately for
consistency to detect stratification or they may be combined,
thoroughly mixed, and a 1 L to 4 L ( ⁄4 gal to 1 gal) aliquot of
the composite taken for determining the average characteristics
of the material.
NOTE 1—This type sampler is lowered into the tank with bottom valve 13.2 Sampling Bulk Storage Tanks Equipped with Mechani-
open (there is no top closure). When the desired depth is reached, the
cal Agitators or Recirculating Pumps—When the tank is
lowering chain is given a snap tug which closes the bottom valve. The
equipped with operating mechanical agitators or recirculating
sampler is then withdrawn from the tank and the contents transferred to
pumping systems which are performing adequate mixing of the
the sample container. This sampler may be used for repetitive sampling in
tank contents, take a single sample by any of the methods
the same tank.
FIG. 6 Thief Sampler described in 13.1.1, 13.1.2, or 13.1.3 to use for test purposes.
13.3 Sampling Tank Cars and Tank Trucks:
13.3.1 Samples of hot liquid materials may be taken by the
dip method using a clean wide-mouth or friction-top can in a
suitable
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4296 − 18 D4296 − 24
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*
1.1 This practice covers procedures for sampling pitch at points of manufacture, storage, and delivery.
1.2 The values stated in SI units are to be regarded as standard. The values in parentheses are for information only.
1.3 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. Specific warning statements are given in Section 1112.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
3. Terminology
3.1 Definitions of Terms Specific to This Standard:Definitions:
3.1.1 For definitions of terms used in this practice, refer to Terminology D4175.
3.1.2 bulk sample, n—a large sample, either from one place or made up of several incremental samples of the same material.the
reduced and divided representative portion of the gross sample as prepared for shipment to and received by a laboratory to be
prepared for analysis.
3.1.3 composite sample, n—in pitch, a thoroughly mixed gross sample.sample, representative of an entire consignment of pitch,
generated by mixing portions of gross samples from different lots together in mass fraction proportioned to the consignment.
3.1.4 gross sample, n—a largein pitch, sample made up of several portions (increments) of a mass of material.the original,
uncrushed representative portion taken from a shipment of pitch.
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Dec. 1, 2018March 1, 2024. Published December 2018April 2024. Originally approved in 1983. Last previous edition approved in 20152018
ɛ1
as D4296 – 83 (2015)D4296 – 18. . DOI: 10.1520/D4296-18.10.1520/D4296-24.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4296 − 24
3.1.5 increment, n—a portion of a material to be combined with other portions of the same material to provide a larger sample
which will represent the whole material.
3.1.6 representative sample, n—a part of a homogeneous material, or a part of the composited and mixed portions of a material,
which carries all the true properties and physical characteristics of the whole material.portion extracted from a total volume that
may or may not contain the constituents in the same proportions are present in the total volume.
3.1.7 sample, n—a part taken as representative of a whole material.
4. Summary of Practice
4.1 Samples of liquid pitches are taken from process lines, storage, and shipment containers in increments required to prepare a
representative sample for testing.
4.2 Samples of solid pitches are taken from loading systems, storage, and shipment containers in increments required to prepare
a representative sample for testing.
5. Significance and Use
5.1 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.
5.2 Samples may be taken for either of the following two purposes:
5.2.1 To represent as nearly as possible an average of the bulk of the materials sampled, or
5.2.2 To ascertain the maximum variation in characteristics which the material possesses.
5.3 A good sampling plan has the following characteristics:
5.3.1 It protects the consumer against the acceptance of a bad batch of material.
5.3.2 It protects the producer against the rejection of a good batch of material.
5.3.3 It gives long-range protection to the consumer.
5.3.4 It encourages the producer to keep his process in control.
5.3.5 It minimizes the cost of sampling, inspection of testing, and administration.
5.3.6 It provides information concerning the quality of the product.
5.4 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.
6. Selection of Samples
6.1 Pitches shall be sampled by the producer at the point of manufacture or storage, and at such time as to allow the tests
controlling acceptance or rejection of quality, as specified by the consumer, to be made in advance of a shipment.
6.2 Samples of pitches shall be taken by the consumer from the shipment containers immediately upon delivery and receipt and
tests controlling acceptance or rejection of quality, as described by the consumer’s specifications, shall be made as soon as possible.
D4296 − 24
7. Size of Samples
7.1 The sample size of liquid materials shall be as follows:
7.1.1 From process lines, 1 L (1 qt).
7.1.2 From bulk storage, 1 L (1 qt) or 1 L aliquot of composite sample.
7.1.3 From bulk shipment containers, 1 L (1 qt) or 1 L aliquot of composite sample.
7.1.4 From barrels or drums, 0.5 L (1 pt) or 0.5 L aliquot of composite sample.
7.2 The sample size of solid materials shall be as follows:
7.2.1 From storage area, 4 L (1 gal) or 4 L aliquot of composite sample.
7.2.2 From bulk shipment containers, 4 L (1 gal) aliquot of composite sample.
7.2.3 From barrels or drums, 0.5 L (1 pt) or 0.5 L aliquot of composite sample.
8. Collection of Gross Sample
8.1 A collection of gross sample represents a lot or batch of material and is composed of a number of increments.
8.1.1 Collect the increments regularly and systematically, so that the entire quantity of pitch sampled will be represented
proportionately in the gross sample, and with such frequency that a gross sample of the required amount will be collected.
9. Size of Increments
9.1 To collect samples, use a shovel or specially designed tool or mechanical means for taking equal portions or increments. 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.
10. Protection and Preservation of Samples
10.1 Sample containers shall be new or reusable containers which can be thoroughly cleaned with a solvent and wiped dry with
a clean dry cloth.
10.2 Care shall be taken to prevent the sample from becoming 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.
10.3 While sampling during inclement weather, attention shall be paid to prevent water from dropping into the hot liquid sample
or samples of solid materials.
10.4 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.
11. Apparatus
11.1 Sampling Equipment for Liquid Materials:
11.1.1 If so equipped, pipe lines and storage tanks may be sampled from valves installed in the lines or up the side of the tanks.
A typical tank valve is shown in Fig. 1, and suitable line valves are illustrated in Fig. 2 and Fig. 3.
11.1.2 For sampling tank trucks, a pipe connection with attached sample valve similar to the one shown in Fig. 2 may be inserted
between the outlet pipe and unloading line.
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FIG. 1 Typical Submerged Sampling Device
11.1.3 A weighted sample bottle similar to those shown in Fig. 4 and Fig. 5, or a “thief sampler” as shown in Fig. 6, or a “dip
sampler” similar to that shown in Fig. 7, may be used to sample production and storage tanks, tank cars, and tank trucks.
11.1.4 A “tube” or “thief” sampler may be used to sample materials in drums or barrels.
11.2 Sampling Equipment for Solid Materials:
11.2.1 Samples from loading systems may be taken with a shovel, metal or plastic scoop, or metal can.
11.2.2 A shovel may be used to sample storage bins, pitch piles, pitch bays, hopper cars, and dump trucks.
11.2.3 A sampling spear as shown in Fig. 8 may be used to sample materials in drums, barrels, bags, and silos.
11.3 Sampling Containers:
11.3.1 Containers for liquid materials shall be wide-mouth cans with line screw caps or triple-seal friction-top cans.
11.3.2 Containers for formed pitches or crushed solid pitch shall be triple-seal friction-top cans, sealable plastic or paper cartons
with inert inside coating, plastic sacks placed in other containers suitable for handling, or substantial strength paper bag which can
be stapled closed.
11.4 Mixing Equipment for Solid Materials:
11.4.1 Section of clean canvas or plastic sheet of sufficient size to contain a large bulk sample which is to be reduced by mixing
and quartering.
11.4.2 A “riffle” as shown in Fig. 9 may be used for reducing gross samples to smaller sizes for testing.
11.4.3 A “shovel” may be used to reduce gross samples to smaller sizes by mixing and quartering as shown in Fig. 10.
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FIG. 2 In-Line Sampling Device
FIG. 3 Pipeline Sampler
11.5 Mixing Equipment for Liquid Materials:
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FIG. 4 Weighted Sampling Can
11.5.1 Sample sizes of 4 L (1 gal) or less can be mixed by thorough stirring with a metal rod or wide blade metal paddle.
11.5.2 A heavy duty electric stirrer is recommended for sample volumes over 4 L (1 gal) to 20 L (5 gal) in size.
12. Hazards
12.1 The sampler shall wear protective clothing, goggles, and rubber or heat-resistant gloves to protect oneself from accidental
contact with hot liquid pitch.
12.2 For prolonged exposure to the presence of pitch vapors or pitch dust, a suitable respirator mask should be worn to avoid
inhalation of pitch vapors or dust. It is recommended that an appropriate barrier cream be applied to exposed areas of the skin.
12.3 Sampling from rail cars shall be avoided when there is a possibility of shunting operations taking place. It is recommended
that flags be placed on both ends of the car to prevent accidental movement during sampling.
12.4 It is recommended that no fewer than two persons be present when samples are taken from hot bulk vessels such as storage
tanks, tank cars, and tank trucks.
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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
13. Sampling Liquid Pitch
13.1 The following three sampling methods are recommended for sampling vertical tanks not capable of being agitated:
13.1.1 Sample-Valve Method—Locate valves, with easy and safe access provided, on the side of the tank with the first in the top
third of the tank, but no higher than 1 m (3 ft) from the top; the second in the middle of the tank; and the third in the bottom third
of the tank, but no lower than 1.1 m (3 ⁄2 ft) from the bottom. A recommended design of the sample valve is shown in Fig. 1. Draw
a minimum of 4 L (1 gal) of the product from each sample valve for test or composite.
13.1.2 Thief Sampling Method—Take samples at the top, middle and lower sections of the tank by lowering a thief sampler into
the material. A satisfactory type with instructions for use is shown in Fig. 6. The samples may be tested separately or combined
and mixed thoroughly for a composite analysis.
13.1.3 Weighted Sample Bottle Method—Take samples at the top, middle, and lower sections of the tank by lowering the bottle
into the material. Two types of weighted sampling bottles are illustrated in Fig. 4 and Fig. 5.
13.1.3.1 The essential feature of the method is to drop the stoppered bottle into the material to the desired depth, and then pull
the stopper by means of an attached chain. When the material fills the bottle, lift out of the liquid and empty into a clean container.
Drain the bottle as completely as possible, re-insert the stopper, lower into the material to the next sampling depth.
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NOTE 1—This type sampler is lowered into the tank with bottom valve open (there is no top closure). When the desired depth is reached, the lowering
chain is given a snap tug which closes the bottom valve. The sampler is then withdrawn from the tank and the contents transferred to the sample container.
This sampler may be used for repetitive sampling in the same tank.
FIG. 6 Thief Sampler
NOTE 1—Sampler with can secured in place is rapidly lowered into tank to desired depth and allowed to fill with sample. The sampler is then withdrawn
from the tank and the contents transferred to the sample container. A clean container must be used to take each sample.
FIG. 7 Dip Sampler
13.1.3.2 Normally, there is not enough undrained residue from the first sample to affect the properties of the next sample taken
from a different level. However, if substantial material difference is suspected at various levels of t
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