Manual Sampling of Petroleum and Petroleum Products: Standard Practice For
Manual Sampling of Petroleum and Petroleum Products: Standard Practice For
This test method has been approved by the sponsoring committees and accepted by the Cooperating Societies in accordance with
established procedures. This method was issued as a joint ASTM-API standard in 1981.
This standard has been approved for use by agencies of the Department of Defense.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
1
D 4057
TABLE 1 Typical Sampling Procedures and Applicability
Application Type of Container Procedure
Liquids of more than (13.8 kPa) and not more than 101 kPa storage tanks, ship and barge tanks, tank cars, tank trucks bottle sampling
(14.7 psia) RVP
thief sampling
Liquids of 101 kPa (14.7 psia) RVP or less storage tanks with taps tap sampling
Bottom sampling of liquids of 13.8 kPa (2 psia) RVP or less storage tanks with taps tap sampling
Liquids of 101 kPa (14.7 psia) RVP or less pipes or lines pipeline sampling
Liquids of 13.8 kPa (2 psia) RVP or less storage tanks, ships, barges bottle sampling
Liquids of 13.8 kPa (2 psia) RVP or less free or open-discharge streams dipper sampling
Liquids of 13.8 kPa (2 psia) RVP or less drums, barrels, cans tube sampling
Bottom or thief sampling of liquids of 13.8 kPa (2 psia) RVP or less tank cars, storage tanks thief sampling
Liquids and semi-liquids of 13.8 kPa (2 psia) RVP or less free or open-discharge streams; open tanks or kettles with open dipper sampling
heads; tank cars, tank trucks, drums
Crude petroleum storage tanks, ship and barge, tanks, tank cars, tank trucks, automatic sampling
pipelines
thief sampling
bottle sampling
tap sampling
Industrial aromatic hydrocarbons storage tanks, ship and barge tanks bottle sampling
Waxes, solids bitumens, other soft solids barrels, cases, bags, cakes boring sampling
Petroleum coke; lumpy solids freight cars, conveyors, bags, barrels, boxes grab sampling
Greases, soft waxes, asphalts kettles, drums, cans, tubes grease sampling
Asphaltic materials storage tanks, tank cars, lines, packages ...
Emulsified asphalts storage tanks, tank cars, lines, packages ...
the Lines of an Operating Hydraulic Fluid Power System 3.1.1.3 bottom sample— a spot sample collected from the
(for Particulate Contamination Analysis) material at the bottom of the tank, container, or line at its
B93.44 Method for Extracting Fluid Samples from the lowest point.
Reservoir of an Operating Hydraulic Fluid Power System (a) Discussion—In practice, the term bottom sample has a
2.3 API Manual of Petroleum Measurement Standards:9 variety of meanings. As a result, it is recommended that the
Chapter 8.2 Automatic Sampling of Petroleum and Petro- exact sampling location (for example, 15 cm from the bottom)
leum Products should be specified when using this term.
Chapter 8.3 Standard Practice for Mixing and Handling of 3.1.1.4 bottom water sample—a spot sample of free water
Liquid Samples of Petroleum and Petroleum Products taken from beneath the petroleum contained in a ship or barge
Chapter 8.4 Standard Practice for the Sampling and Han- compartment or a storage tank.
dling of Fuels for Volatility Measurements 3.1.1.5 clearance sample— a spot sample taken with the
Chapter 9.3 Thermohydrometer Test Method for Density inlet opening of the sampling apparatus 10 cm (4 in.) (some
and API Gravity of Crude Petroleum and Liquid Petro- regulatory agencies require 15 cm (6 in.)) below the bottom of
leum Products the tank outlet.
Chapter 17.1 Guidelines for Marine Cargo Inspection (a) Discussion—This term is normally associated with small
Chapter 17.2 Measurement of Cargoes Aboard Marine Tank (159 m3 or 1000 Bbls or less) tanks, commonly referred to as
Vessels lease tanks.
Chapter 18.1 Measurement Procedures for Crude Oil Gath- 3.1.1.6 composite sample— a blend of spot samples mixed
ered from Small Tanks By Truck in proportion to the volumes of material from which the spot
Chapter 10, various sections, Sediment and Water Determi- samples were obtained.
nation
3.1.1.7 core sample— a sample of uniform cross sectional
3. Terminology area taken at a given height in a tank.
3.1.1.8 dipper sample— a sample obtained by placing a
3.1 Definitions of Terms Specific to This Standard:
dipper or other collecting vessel in the path of a free-flowing
3.1.1 Samples:
stream to collect a definite volume from the full cross section
3.1.1.1 all-levels sample—a sample obtained by submerg-
of the stream at regular time intervals for a constant time rate
ing a stoppered beaker or bottle to a point as near as possible
of flow or at time intervals varied in proportion to the flow rate.
to the draw-off level, then opening the sampler and raising it at
a rate such that it is approximately three-fourths full as it 3.1.1.9 drain sample— a sample obtained from the water
emerges from the liquid. draw-off valve on a storage tank.
3.1.1.2 boring sample— a sample of the material contained (a) Discussion—Occasionally, a drain sample may be the
in a barrel, case, bag, or cake that is obtained from the chips same as a bottom sample (for example, in the case of a tank
created by boring holes into the material with a ship auger. car).
3.1.1.10 floating roof sample—a spot sample taken just
below the surface to determine the density of the liquid on
9
Available from American Petroleum Institute, 1220 L St., NW, Washington, DC which the roof is floating.
20005. 3.1.1.11 flow proportional sample—a sample taken from a
2
D 4057
pipe such that the rate of sampling is proportional throughout 3.1.1.21 sampling—all the steps required to obtain a sample
the sampling period to the flow rate of the fluid in the pipe. that is representative of the contents of any pipe, tank, or other
3.1.1.12 grab sample— a sample obtained by collecting vessel and to place that sample in a container from which a
equal quantities from parts or packages of a shipment of loose representative test specimen can be taken for analysis.
solids such that the sample is representative of the entire 3.1.1.22 spot sample— a sample taken at a specific location
shipment. in a tank or from a flowing stream in a pipe at a specific time.
3.1.1.13 grease sample— a sample obtained by scooping or 3.1.1.23 surface sample— a spot sample skimmed from the
dipping a quantity of soft or semi-liquid material contained surface of a liquid in a tank.
from a package in a representative manner. 3.1.1.24 tank composite sample—a blend created from the
3.1.1.14 lower sample— a spot sample of liquid from the upper, middle, and lower samples from a single tank.
middle of the lower one-third of the tank’s content (a distance (a) Discussion—For a tank of uniform cross section, such as
of five-sixths of the depth liquid below the liquid’s surface). an upright cylindrical tank, the blend consists of equal parts of
See Fig. 1. the three samples. For a horizontal cylindrical tank, the blend
3.1.1.15 middle sample— a spot sample taken from the consists of three samples in the proportions shown in Table 2.
middle tank’s contents (a distance of one-half of the depth of 3.1.1.25 tap sample—a spot sample taken from a sample tap
liquid below the liquid’s surface). See Fig. 1. on the side of a tank. It may also be referred to as a tank-side
3.1.1.16 multiple tank composite sample—a mixture of sample.
individual samples or composites of samples that have been 3.1.1.26 top sample—a spot sample obtained 15 cm (6 in.)
obtained from several tanks or ship/barge compartments con- below the top surface of the liquid. See Fig. 1.
taining the same grade of material. 3.1.1.27 tube or thief sample—a sample obtained with a
(a) Discussion—The mixture is blended in proportion to the sampling tube or special thief, either as a core sample or spot
volume of material contained in the respective tanks or sample from a specific point in the tank or container.
compartments. 3.1.1.28 upper sample— a spot sample taken from the
3.1.1.17 outlet sample— a spot sample taken with the inlet middle of the upper one-third of the tank’s contents (a distance
opening of the sampling apparatus at the level of the bottom of of one-sixth of the liquid depth below the liquid’s surface). See
the tank outlet (fixed or floating). See Fig. 1. Fig. 1.
3.1.1.18 representative sample—a portion extracted from 3.1.2 Other Terms:
the total volume that contains the constituents in the same 3.1.2.1 automatic sampler—a device used to extract a
proportions that are present in that total volume. representative sample from the liquid flowing in a pipe.
3.1.1.19 running sample— a sample obtained by lowering a (a) Discussion—The automatic sampler generally consists
breaker or bottle to the level of the bottom of the outlet of a probe, a sample extractor, an associated controller, a flow
connection or swing line and returning it to the top of the oil at measuring device, and a sample receiver. For additional
a uniform rate such that the beaker or bottle is about three- information on an automatic sampler, see Practice D 4177.
fourths full when withdrawn from the oil. 3.1.2.2 dissolved water— water in solution in an oil.
3.1.1.20 sample—a portion extracted from a total volume 3.1.2.3 emulsion—an oil/water mixture that does not readily
that may or may not contain the constituents in the same separate.
proportions that are present in that total volume. 3.1.2.4 entrained water— water suspended in the oil.
(a) Discussion—Entrained water includes emulsions but
does not include dissolved water.
3.1.2.5 free water—the water that exists as a separate phase.
3.1.2.6 intermediate container—the vessel into which all or
part of the sample from a primary container/receiver is
transferred for transport, storage, or ease of handling.
3.1.2.7 primary sample receiver/receptacle—a container in
which a sample is initially collected.
100 80 50 20 3 4 3
90 75 50 20 3 4 3
NOTE 1—The location shown for the outlet sample applies only to tanks 80 70 50 20 2 5 3
with side outlets. It does not apply when the outlet comes from the floor 70 50 20 6 4
of the tank or turns down into a sump. Bottom sample location must be 60 50 20 5 5
specified. 50 40 20 4 6
40 20 10
NOTE 2—Samples should be obtained from within solid stand pipes as
30 15 10
the materials normally not representative of the material in the tank at that 20 10 10
point. 10 5 10
FIG. 1 Spot Sampling Locations
3
D 4057
(a) Discussion—Examples of primary sampler containers 6. Apparatus
include glass and plastic bottles, cans, core-type thief, and 6.1 Sample containers come in a variety of shapes, sizes,
fixed and portable sample receivers. and materials. To be able to select the right container for a
3.1.2.8 stand pipes— vertical sections of pipe or tubing given application one must have knowledge of the material to
extending from the gaging platform to near the bottom of tanks be sampled to ensure that there will be no interaction between
that are equipped with external or internal floating roofs. the sampled material and the container which would affect the
(a) Discussion—Stand pipes may also be found on ships and integrity of the other. Additional considerations in the selection
barges. of sample containers is the type of mixing required to remix the
3.1.2.9 test specimen— the representative sample taken contents before transferring the sample from the container and
from the primary or intermediate sample container for analysis. the type of laboratory analyses that are to be conducted on the
4. Summary of Practice sample. To facilitate the discussion on proper handling and
mixing of samples, sample containers are referred to as either
4.1 This practice provides procedures for manually obtain- primary or intermediate containers. Regardless of the type of
ing samples of petroleum and petroleum products of a liquid, sample container used, the sample container should be large
semi-liquid or solid state from tanks, pipelines, drums, barrels, enough to contain the required sample volume without exceed-
cans, tubes, bags, kettles and open-discharge streams. It ad- ing 80 % of the container capacity. The additional capacity is
dresses, in detail, the various factors which need to be required for thermal expansion of the sample and enhances
considered in obtaining a representative sample. These consid- sample mixing.
erations include the analytical tests to be conducted on the 6.2 General Container Design Considerations—Following
sample, the types of sample containers to be used and any are general design considerations for sample containers:
special instructions required for special materials to be
6.2.1 The bottom of the container should be sloped continu-
sampled. Test Method D 5854 can provide additional guidance.
ously downward to the outlet to ensure complete liquid
5. Significance and Use withdrawal.
5.1 Representative samples of petroleum and petroleum 6.2.2 There should be no internal pockets or dead spots.
products are required for the determination of chemical and 6.2.3 Internal surfaces should be designed to minimize
physical properties, which are used to establish standard corrosion, encrustation, and water/sediment clingage.
volumes, prices, and compliance with commercial and regula- 6.2.4 There should be an inspection cover/closure of suffi-
tory specifications. cient size to facilitate filling, inspection, and cleaning.
5.2 The following concepts must be considered when se- 6.2.5 The container should be designed to allow the prepa-
lecting a specific sampling procedure. ration of a homogeneous mixture of the sample while prevent-
5.2.1 Objective of Manual Sampling: ing the loss of any constituents which affect the representative-
5.2.1.1 The objective of manual sampling is to obtain a ness of the sample and the accuracy of the analytical tests.
small portion (spot sample) of material from a selected area 6.2.6 The container should be designed to allow the transfer
within a container that is representative of the material in the of samples from the container to the analytical apparatus while
area or, in the case of running or all-level samples, a sample maintaining their representative nature.
whose composition is representative of the total material in the 6.3 Bottles (Glass)—Clear glass bottles may be examined
container. A series of spot samples may be combined to create visually for cleanliness and allows visual inspection of the
a representative sample. sample for free water cloudiness, and solid impurities. Brown
5.2.2 Required Conditions for the Application of Manual glass bottles afford some protection to the samples when light
Sampling: may affect the test results.
5.2.2.1 Manual sampling may be applied under all condi- 6.4 Bottles (Plastic)—Plastic bottles made of suitable ma-
tions within the scope of this practice, provided that the proper terial may be used for the handling and storage of gas oil,
sampling procedures are followed. diesel oil, fuel oil, and lubricating oil. Bottles of this type
5.2.2.2 In many liquid manual sampling applications, the should not be used for gasoline, aviation jet fuel, kerosine,
material to be sampled contains a heavy component (such as crude oil, white spirit, medicinal white oil, and special boiling
free water) which tends to separate from the main component. point products unless testing indicates there is no problem with
In these cases, manual sampling is appropriate under the solubility, contamination, or loss of light components.
following conditions. 6.4.1 In no circumstances shall nonlinear (conventional)
(a) Sufficient time must have elapsed for the heavy compo- polyethylene containers be used to store samples of liquid
nent to adequately separate and settle. hydrocarbons. This is to avoid sample contamination or sample
(b) It must be possible to measure the level of the settled bottle failure. Used engine oil samples that may have been
component in order to stay well above that level when drawing subjected to fuel dilution should not be stored in plastic
representative samples, unless all or part of the heavy compo- containers.
nent will be included in the portion of the tank contents to be 6.4.2 Plastic bottles have an advantage in that they will not
identified. shatter like glass or corrode like metal containers.
(c) When one or more of these conditions cannot be met, 6.5 Cans—When cans are to be used, they must have seams
sampling is recommended and is accomplished by means of an that have been soldered on the exterior surfaces with a flux of
automatic sampling system (see Practice D 4177). rosin in a suitable solvent. Such a flux is easily removed with
4
D 4057
gasoline, whereas many others are very difficult to remove. 6.8.2 Manual and mechanical shaking of the sample con-
Minute traces of flux may contaminate the sample so that tainer are not recommended methods for mixing a sample for
results obtained on tests such as dielectric strength, oxidation sediment and water (S&W) analysis. Tests have shown it is
resistance, and sludge formation may be erroneous. Internal difficult to impart sufficient mixing energy to mix and maintain
epoxy lined cans may have residual contamination and precau- a homogeneous representative sample. Practice D 5854 con-
tions should be taken to ensure its removal. Practice D 4306 tains more detailed information.
should be used when taking samples for aviation fuels. 6.9 Other Equipment—A graduated cylinder or other mea-
6.6 Container Closures—Cork stoppers, or screw caps of suring device of suitable capacity is often required for deter-
plastic or metal may be used for glass bottles. Corks must be of mining sample quantity in many of the sampling procedures
good quality, clean, and free from holes and loose bits of cork. and for compositing samples.
Never use rubber stoppers. Prevent the sample from contacting 6.10 Sampling Devices—Sampling devices are described in
the cork by wrapping tin or aluminum foil around the cork detail under each of the specific sampling procedures. Sam-
before forcing it into the bottle. Screw caps providing a vapor pling devices shall be clean, dry, and free of all substances that
tight closure seal shall be used for cans. Screw caps must be might contaminate the material being sampled.
protected by a disk faced with material that will not deteriorate
7. Manual Sampling Considerations
and contaminate the sample. Containers used to take samples
that will be tested for density or gravity shall have screw caps. 7.1 The following factors must be considered in the devel-
6.7 Cleaning Procedure—Sample containers must be clean opment and application of manual sampling procedures:
and free from all substances which might contaminate the 7.1.1 Physical and Chemical Property Tests—The physical
material being sampled (such as water, dirt, lint, washing and chemical property tests to be performed on a sample will
compounds, naphtha and other solvents, soldering fluxes, dictate the sampling procedures, the sample quantity required,
acids, rust, and oil). Prior to further use, reusable containers and many of the sample handling requirements.
such as cans and bottles should be rinsed with a suitable 7.1.2 Sampling Sequence:
solvent. Use of sludge solvents to remove all traces of 7.1.2.1 Any disturbance of the material in a tank that is to be
sediments and sludge may be necessary. Following the solvent sampled may adversely affect the representative character of
wash, the container should be washed with a strong soap the sample(s). Therefore, the sampling operation should be
solution, rinsed thoroughly with tap water, and given a final conducted before innage gaging, the associated temperature
rinse using distilled water. Dry the container either by passing determination, and any other similar activity that could disturb
a current of clean warm air through the container or by placing the tank contents.
it in a hot dust-free cabinet at 40°C (104°F) or higher. When 7.1.2.2 To avoid contamination of the oil column during the
dry, stopper or cap the container immediately. Normally, it is sampling operation, the order of precedence for sampling
not necessary to wash new containers. should start from the top and work downward, according to the
following sampling sequence: surface, top, upper, middle,
6.7.1 Depending on service, receivers used in conjunction
lower, outlet, clearance, all-levels, bottom, and running
with automatic samplers may need to be washed with solvent
sample.
between uses. In most applications, it is not desirable or
7.1.3 Equipment Cleanliness—The sampling equipment
practical to wash these receivers using soap and water as
should be clean prior to commencing the sampling operation.
outlined above for cans and bottles. The cleanliness and
Any residual material left in a sampling device or sample
integrity of all sample containers/receivers must be verified
container from a previous sample or cleaning operation may
prior to use.
destroy the representative character of the sample. It is good
6.7.2 When sampling aviation fuel, Practice D 4306 should practice with light petroleum products to rinse the container
be consulted for recommended cleaning procedures for con- with the product to be sampled prior to drawing samples.
tainers that are to be used in tests for the determination of water 7.1.4 Compositing of Individual Samples:
separation, copper corrosion, electrical conductivity, thermal 7.1.4.1 If the sampling procedure requires that several
stability, lubricity, and trace metal content. different samples be obtained, physical property tests may be
6.8 Sample Mixing Systems—The sample container should performed on each sample or on a composite of the various
be compatible with the mixing system for remixing samples samples. When the respective tests are performed on individual
that have stratified to ensure that a representative sample is samples, which is the recommended procedure, the test results
available for transfer to an intermediate container or the are averaged generally.
analytical apparatus. This is especially critical when remixing 7.1.4.2 When a multiple tank composite sample is required,
crude, some black products, and condensates for sediment and such as on board ships and barges, a composite tank sample
water analysis to ensure a representative sample. The require- may be prepared from the samples from different tanks when
ments governing the amount of mixing and type of mixing they contain the same material. In order for such a composite
apparatus differ depending upon the petroleum or petroleum tank sample to be representative of the material contained in
product and the analytical test to be performed. Refer to the various tanks, the quantity from the individual samples
Practice D 5854 for more detailed information. used to prepare the composite tank sample must be propor-
6.8.1 When stratification is not a major concern, adequate tional to the volumes in the corresponding tanks. In most other
mixing may be obtained by such methods as shaking (manual compositing situations, equal volumes from the individual
or mechanical), or use of a shear mixer. samples must be used. The method of compositing should be
5
D 4057
documented and care taken to preserve the integrity of the static charge, nylon or polyester rope, cords, or clothing should
samples. It is recommended that a portion of each tank sample not be used.
be retained separately (not composited) for retesting if neces-
sary. 9. Special Instructions for Specific Materials
7.1.4.3 When compositing samples, exercise care to ensure 9.1 Crude Petroleum and Residual Fuel Oils:
sample integrity. Refer to Practice D 5854 for guidance on 9.1.1 Crude petroleum and residual fuel oils usually are
mixing and handling of samples. nonhomogeneous. Tank samples of crude oil and residual oils
7.1.4.4 Samples taken at specific levels, for example, upper- may not be representative for the following reasons:
middle-lower capping will require a small portion of the 9.1.1.1 The concentration of entrained water is higher near
sample to be poured out to create an ullage in the container the bottom. The running sample or the composite of the upper,
before capping. All other samples shall be capped immediately middle, and lower sample may not represent the concentration
and taken to the laboratory. of entrained water.
7.1.5 Sample Transfers—The number of intermediate trans- 9.1.1.2 The interface between oil and free water is difficult
fers from one container to another between the actual sampling to measure, especially in the presence of emulsion layers, or
operation and testing should be minimized. The loss of light sludge.
hydrocarbons as the result of splashing, loss of water due to 9.1.1.3 The determination of the volume of free water is
clingage, or contamination from external sources, or both, may difficult because the free water level may vary across the tank
distort test results, for example, density, sediment and water, bottom surface. The bottom is often covered by pools of free
product clarity. The more transfers between containers, the water or water emulsion impounded by layers of sludge or
greater the likelihood one or both of these problems may occur. wax.
See Practice D 5854 for additional information concerning the 9.1.2 Automatic sampling in accordance with Practice
handling and mixing of samples. D 4177 is recommended whenever samples of these materials
7.1.6 Sample Storage—Except when being transferred, are required for custody transfer measurements. However, tank
samples should be maintained in a closed container in order to samples may be used when agreed to by all parties to the
prevent loss of light components. Samples should be protected transaction.
during storage to prevent weathering or degradation from light, 9.2 Gasoline and Distillate Products— Gasoline and distil-
heat, or other potential detrimental conditions. late products are usually homogeneous, but they are often
7.1.7 Sample Handling—If a sample is not uniform (homo- shipped from tanks that have clearly separated water on the
geneous) and a portion of the sample must be transferred to bottom. Tank sampling, in accordance with the procedures
another container or test vessel, the sample must be thoroughly outlined in Section 13, is acceptable under the conditions
mixed in accordance with the type of material and appropriate covered in 5.2.2.
test method, in order to ensure the portion transferred is 9.3 Industrial Aromatic Hydrocarbons— For samples of
representative. Exercise care to ensure mixing does not alter industrial aromatic hydrocarbons (benzene, toluene, xylene,
the components within the sample, for example, loss of light and solvent naphthas), proceed in accordance with Sections
ends. See Practice D 5854 for more detailed instructions. 5.2.1, 6, and 10, and Sections 12.2-13, with particular emphasis
on the procedures pertaining to the precautions for care and
8. Special Precautions cleanliness. See Annex A1 for details.
8.1 This practice does not purport to cover all safety aspects 9.4 Lacquer Solvents and Diluents:
associated with sampling. However, it is presumed that the 9.4.1 When sampling bulk shipments of lacquer solvents
personnel performing sampling operations are adequately and diluents which are to be tested using Test D 268, observe
trained with regard to the safe application of the procedures the precautions and instructions described in 9.4.2 and 9.4.3.
contained herein for the specific sampling situation. 9.4.2 Tanks and Tank Cars—Obtain upper and lower
8.2 A degree of caution is required during all sampling samples (see Fig. 1) of not more than 1 L (qt) each by the thief
operations, but in particular when sampling certain products. or bottle spot sampling procedures outlined in 13.4. In the
Crude oil may contain varying amounts of hydrogen sulfide laboratory, prepare a composite sample of not less than 2 L/2
(sour crude), an extremely toxic gas. Annex A1 provides qts by mixing equal parts of the upper and lower samples.
precautionary statements that are applicable to the sampling 9.4.3 Barrels, Drums, and Cans—Obtain samples from the
and handling of many of these materials. number of containers per shipment as mutually agreed. In the
8.3 When taking samples from tanks suspected of contain- case of expensive solvents, which are purchased in small
ing flammable atmospheres, precautions should be taken to quantities, it is recommended that each container be sampled.
guard against ignitions from static electricity. Conductive Withdraw a portion from the center of each container to be
objects, such as gage tapes, sample containers, and thermom- sampled using the tube sampling procedure (see 9.4.3) or bottle
eters, should not be lowered into or suspended in a compart- sampling procedure (see 13.4.2, although a smaller bottle may
ment or tank that is being filled, or immediately after cessation be used). Prepare a composite sample of at least 1 L (1 qt) by
of pumping. Conductive material such as gage tape should mixing equal portions of not less than 500 mL (1 pt) from each
always be in contact with gage tube until immersed in the fluid. container sampled.
A waiting period (normally 30 min or more after filling 9.5 Asphaltic Materials—When sampling asphaltic materi-
cessation) will generally be required to permit dissipation of als that are to be tested using Test Method D 1856 or Test
the electrostatic charge. In order to reduce the potential for Method D 2172, obtain samples by the boring procedure in
6
D 4057
Section 17 or the grab procedure in Section 18. A sample of Method D 873, or equivalent methods, observe the precautions
sufficient size to yield at least 100 g (1⁄4 lb) of recovered and instructions that follow.
bitumen is required. About 1000 g (2 lb) of sheet asphalt 10.4.2 Precautions—Very small amounts (as low as
mixtures usually will be sufficient. If the largest lumps in the 0.001 %) of some materials, such as inhibitors, have a consid-
sample are 2.5 cm (1 in.), 2000 g (4 lb) will usually be erable effect upon oxidation stability tests. Avoid contamina-
required, and still larger samples if the mixture contains larger tion and exposure to light while taking and handling samples.
aggregates. To prevent undue agitation with air, which promotes oxidation,
9.6 Emulsified Asphalts—It is frequently necessary to test do not pour, shake, or stir samples to any greater extent than
samples in accordance with the requirements of Specification necessary. Never expose them to temperatures above those
D 977, and Test Methods D 244. Obtain samples from tanks, necessitated by atmospheric conditions.
tank cars, and tank trucks by the bottle sampling procedure 10.4.3 Sample Containers—Use only brown glass or
outlined in 13.4.2 using a bottle that has a 4-cm (11⁄2-in.) wrapped clear glass bottles as containers, since it is difficult to
diameter or larger mouth. Refer to Fig. 1 and Table 2 for make certain that cans are free of contaminants, such as rust
sampling locations. Use the dipper procedure in Section 15 to and soldering flux. Clean the bottles by the procedure de-
obtain samples for fill or discharge lines. Sample packages in scribed in 6.7. Rinse thoroughly with distilled water, dry, and
accordance with Table 3. If the material is solid or semisolid, protect the bottles from dust and dirt.
use the boring sampling procedure described in Section 17. 10.4.4 Sampling—A running sample obtained by the proce-
Obtain at least 4 L (1 gal) or 4.5 Kg (10 lbs) from each lot or dure in 13.5 is recommended because the sample is taken
shipment. Store the samples in clean, airtight containers at a directly in the bottle. This reduces the possibility of air
temperature of not less than 4°C (40°F) until the test. Use a absorption, loss of vapors, and contamination. Just before
glass or black iron container for emulsified asphalts of the RS-1 sampling, rinse the bottle with the product to be sampled.
type.
11. Special Instructions for Specific Applications
10. Special Instructions for Specific Tests 11.1 Marine Cargoes of Crude Oils:
10.1 General—Special sampling precautions and instruc- 11.1.1 Samples of ship or barge cargoes of crude petroleum
tions are required for some ASTM test methods and specifica- may be taken by mutual agreement by the following methods:
tions. Such instructions supplement the general procedures of 11.1.1.1 From the shore tanks before loading and both
this practice and supersede them if there is a conflict. before and after discharging as in Section 13.
10.2 Distillation of Petroleum Products— When obtaining 11.1.1.2 From the pipeline during discharging or loading.
samples of natural gasoline that are to be tested using Test Pipeline samples may be taken either manually or with an
Method D 86, the bottle sampling procedure described in automatic sampler. If the pipeline requires displacement or
13.4.2 is the preferred technique, with the exception that flushing, exercise care that the pipeline sample includes the
pre-cooled bottles and laboratory compositing is required. entire cargo and none of the displacement. Separate samples
Before obtaining the sample, pre-cool the bottle by immersing may be required to cover the effect of the line displacement on
it in the product, allowing it to fill, and discard the first filling. the prior or following transfer.
If the bottle procedure cannot be used, obtain the sample by the 11.1.1.3 From the ship’s or barge’s tanks after loading or
tap procedure and with the use of the cooling bath, as described before discharging. An all-levels sample, running sample,
in 13.6. Do not agitate the bottle while drawing the sample. upper-middle-lower sample, or spot samples at agreed levels
After obtaining the sample, close the bottle immediately with a may be used for sampling each cargo compartment of a ship or
tight-fitting stopper, and store it in an ice bath or refrigerator at barge.
a temperature of 0 to 4.5°C (32 to 40°F). 11.1.2 Ship and barge samples may be taken either through
10.3 Vapor Pressure—When sampling petroleum and petro- open hatches or by use of equipment designed for closed
leum products that are to be tested for vapor pressure, refer to systems.
Practice D 5842. 11.1.3 Normally, when loading a marine vessel, the shore
10.4 Oxidation Stability: tank sample or the pipeline sample taken from the loading line
10.4.1 When sampling products that are to be tested for is the custody transfer sample. However, ship’s/barge’s tank
oxidation stability in accordance with Test Method D 525, Test samples may also be tested for sediment and water (S&W) and
TABLE 3 Minimum Number of Packages to be Selected for
for other quality aspects, when required. The results of these
Sampling ship’s/barge’s tank sample tests, together with the shore tank
Packages Packages to be Packages Packages to be
sample tests, may be shown on the cargo certificate.
in Lot Sampled in Lot Sampled 11.1.4 When discharging a ship/barge, the pipeline sample
1 to 3 all 1332 to 1728 12 taken from a properly designed and operated automatic line
4 to 64 4 1729 to 2197 13 sampler, in the discharge line, should be the custody transfer
65 to 125 5 2198 to 2744 14 sample. Where no proper line sample is available, the ship’s/
126 to 216 6 2745 to 3375 15
217 to 343 7 3376 to 4096 16 barge’s tank sample can be the custody transfer sample except
344 to 512 8 4097 to 4913 17 where specifically exempted.
513 to 729 9 4914 to 5832 18 11.1.5 Samples of ship/barge cargoes of finished products
730 to 1000 10 5833 to 6859 19
1001 to 1331 11 6850 and greater 20 are taken from both shipping and receiving tanks and from the
pipeline, if required. In addition, the product in each of the
7
D 4057
ship/barge tanks should be sampled after the vessel is loaded or drained. When the actual sample is emptied into this container,
just before unloading. the sampling apparatus should be upended into the opening of
the sample container and should remain in this position until
NOTE 4—Refer to MPMS Chapter 17 for additional requirements
associated with sampling materials in marine vessels. the contents have been transferred so that no unsaturated air
will be entrained in the transfer of the sample.
11.2 Crude Oil Gathered By Truck—Refer to MPMS Chap-
12.2.4 When sampling nonvolatile liquid products, 13.8 kPa
ter 18.1 for additional sampling requirements when gathering
(2 psia) RVP or less, sampling apparatus shall be filled and
crude oil by tank truck.
allowed to drain before drawing the actual sample. If the actual
11.3 Tank Cars—Sample the material after the car has been
sample is to be transferred to another container, the sample
loaded or just before unloading.
container shall be rinsed with some of the product to be
11.4 Package Lots (Cans, Drums, Barrels, or Boxes)—Take
sampled and drained before it is filled with the actual sample.
samples from a sufficient number of the individual packages to
12.2.5 The transfer of crude oil samples from the sample
prepare a composite sample that will be representative of the
apparatus/receiver to the laboratory glassware in which they
entire lot or shipment. Select at random the individual pack-
will be analyzed requires special care to maintain their repre-
ages to be sampled. The number of random packages will
sentative nature. The number of transfers should be minimized.
depend on several practical considerations, such as (1) the
Mechanical means of mixing and transferring the samples in
tightness of the product specifications; (2) the sources and type
the sample receiver are recommended.
of the material and whether or not more than one production
batch may be represented in the load and (3) previous 12.3 Sample Handling:
experience with similar shipments, particularly with respect to 12.3.1 Volatile Samples—All volatile samples of petroleum
the uniformity of quality from package to package. In most and petroleum products shall be protected from evaporation.
cases, the number specified in Table 4 will be satisfactory. Transfer the product from the sampling apparatus to the sample
container immediately. Keep the container closed except when
12. Sampling Procedures (General) the material is being transferred. After delivery to the labora-
tory, volatile samples should be cooled before the containers
12.1 The standard sample procedures described in this
are opened.
practice are summarized in Table 1. Alternative sampling
procedures may be used if a mutually satisfactory agreement 12.3.2 Light Sensitive Samples—It is important that samples
has been reached by the parties involved. It is recommended sensitive to light, such as gasoline, be kept in the dark, if the
that such agreements be put in writing and signed by autho- testing is to include the determination of such properties as
rized officials. color, octane, tetraethyl lead and inhibitor contents, sludge
12.2 Precautions: forming characteristics, stability tests, or neutralization value.
12.2.1 Extreme care and good judgment are necessary to Brown glass bottles may be used. Wrap or cover clear glass
ensure that samples are obtained that represent the general bottles immediately.
characteristics and average condition of the material. Clean 12.3.3 Refined Materials—Protect highly refined products
hands are important. from moisture and dust by placing paper, plastic, or metal foil
12.2.2 Since many petroleum vapors are toxic and flam- over the stopper and the top of the container.
mable, avoid breathing them, igniting them from an open 12.3.4 Container Outage—Never fill a sample container
flame, burning embers, or a spark produced by static electricity. completely. Allow adequate room for expansion, taking into
All safety precautions specific to the material being sampled consideration the temperature of the liquid at the time of filling,
should be followed. and the probable maximum temperature to which the filled
12.2.3 When sampling relatively volatile products more container may be subjected. Adequate sample mixing is diffi-
than 13.8 kPa (2 psia) RVP, the sampling apparatus shall be cult if the container is more than 80 % full.
filled and allowed to drain before drawing the sample. If the 12.4 Sample Labeling—Label the container immediately
sample is to be transferred to another container, this container after a sample is obtained. Use waterproof and oil proof ink or
shall also be rinsed with some of the volatile product and then a pencil hard enough to dent the tag. Soft pencil and ordinary
ink markers are subject to obliteration from moisture, oil
smearing, and handling. Include the following information on
TABLE 4 Spot Sampling Requirements
the label:
NOTE 1—When samples are required at more than one location in the 12.4.1 Date and time (the period elapsed during continuous
tank, the samples shall be obtained beginning with the upper sample first sampling and the hour and minute of collection for dipper
and progressing sequentially to the lower sample. samples),
Required Samples 12.4.2 Name of the sampler,
Tank Capacity/Liquid Level
Upper Middle Lower 12.4.3 Name and number and owner of the vessel, car, or
Tank capacity less than or equal to 159 X container,
m3(1 000 bbls)
Tank capacity greater than 159 m3 X X X
12.4.4 Grade of material, and
(1 000 bbls) 12.4.5 Reference symbol or identification number.
Level # 3 m (10 ft) X 12.5 Sample Shipment—To prevent loss of liquid and va-
3 m (10 ft) < Level # 4.5 m (15 ft) X X
Level > 4.5 m (15 ft) X X X pors during shipment and to protect against moisture and dust,
cover the stoppers of glass bottles with plastic caps that have
8
D 4057
been swelled in water, wiped dry, placed over the tops of the 13.4.1.1 Application—The core thief spot sampling proce-
stoppered bottles, and allowed to shrink tightly in place. Before dure may be used for sampling liquids of 101 kPa (14.7 psia)
filling metal containers, inspect the lips and caps for dents, RVP or less in storage tanks, tank cars, tank trucks, ship, and
out-of-roundness, or other imperfections. Correct or discard the barge tanks.
cap or container, or both. After filling, screw the cap tightly and 13.4.1.2 Apparatus—A typical core-type thief is shown in
check for leaks. Appropriate governmental and carrier regula- Fig. 3. The thief shall be designed so that a sample can be
tions applying to the shipment of flammable liquids must be obtained within 2.0 to 2.5 cm (3⁄4 to 1 in.) of the bottom or at
observed. any other specific location within the tank or vessel. The size
of the core thief should be selected depending upon the volume
13. Tank Sampling of the sample required. The thief should be capable of
13.1 Samples should not be obtained from within solid penetrating the oil in the tank to the required level, mechani-
stand pipes as the material is normally not representative of the cally equipped to permit filling at any desired level, and
material in the tank at that point. Stand pipe samples should capable of being withdrawn without undue contamination of
only be taken from pipes with at least two rows of overlapping the contents. The thief may include the following features:
slots. See Fig. 2. (a) Uniform cross section and bottom closure,
13.2 When sampling crude oil tanks with diameters in (b) Extension rods for use in obtaining samples at levels
excess of 45 m (150 ft), additional samples should be taken corresponding with requirements for high connections or for
from any other available gaging hatches located around the samples to determine high settled sediment and water levels,
perimeter of the tank roof, safety requirements permitting. All (c) Sediment and water gage for determining the height of
the samples should be individually analyzed using the same sediment and water in the thief,
test method and the results should then be averaged arithmeti- (d) A clear cylinder that facilitates observing the gravity and
cally. temperature of the oil during a gravity test; it also should be
13.3 Composite Sample Preparation—A composite spot equipped with a windshield,
sample is a blend of spot samples mixed volumetrically (e) An opener to break the tension on the valve or slide at any
proportional for testing. Some tests may also be made on the desired level,
spot samples before blending and the results averaged. Spot (f) A thief cord marked so that the sample can be taken at any
samples from crude oil tanks are collected in the following depth in the vertical cross section of the tank,
ways:
13.3.1 Three-way—On tanks larger than 159 m3 (1000 bbls)
capacity, which contain in excess of 4.5 m (15 ft) of oil, equal
volume samples should be taken at the upper, middle, and
lower or outlet connection of the merchantable oil, in the order
named. This method may also be used on tanks up to and
including a capacity of 159 m3 (1000 bbls).
13.3.2 Two-way—On tanks smaller than 159 m3 (1000 bbls)
capacity, which contain in excess of 3 m (10 ft) and up to 4.5
m (15 ft) of oil, equal volume samples should be taken at the
upper and lower, or outlet connection of the merchantable oil,
in the order named. This method may also be used on tanks up
to and including a capacity of 159 m3 (1000 bbls).
13.4 Spot Sampling Methods—The requirements for spot
sampling are shown in Table 4. For sampling locations, see Fig.
1.
13.4.1 Core Thief Spot Sampling Procedure:
FIG. 2 Stand Pipe (with overlapping slots) FIG. 3 Core-Type Sampling Thief
9
D 4057
(g) A hook to hang the thief in the hatch vertically, and level (see Fig. 4A). Bottles of special dimensions are required
(h) Sample cocks for obtaining samples for determination of to fit a sampling cage. The use of sampling cage is generally
sediment and water spaced at the 10-cm (4-in.) and 20-cm preferred to that of a weighted sampling beaker for volatile
(8-in.) marker levels. products since loss of light ends is likely to occur when
(i) A graduated cylinder and sample container may also be transferring the sample from a weighted sampling beaker to
required for use with this procedure. another container.
13.4.1.3 Procedure: 13.4.2.3 Procedure:
(a) Inspect the thief, graduated cylinder, and sample con- (a) Inspect the sampling bottle or beaker, graduated cylinder,
tainer for cleanliness and use only clean, dry equipment. and sample container for cleanliness and use only clean, dry
(b) Obtain an estimate of the liquid level in the tank. Use an equipment.
automatic gage or obtain an outage measurement, if required. (b) Obtain an estimate of the liquid level in the tank. Use an
(c) Check the thief for proper operation. automatic gage or obtain an outage measurement if required.
(d) Open the bottom closure, and set the trip hook in the trip (c) Attach the weighted line to the sample bottle/beaker or
rod. place the bottle in a sampling cage, as applicable.
(e) Lower the thief to the required location. See Table 5. (d) Insert the cork in the sampling bottle or beaker.
(f) At the required location, close the bottom closure on the (e) Lower the sampling assembly to the required location.
thief with a sharp jerk of the line. See Table 5.
(g) Withdraw the thief. (f) At the required location, pull out the stopper with a sharp
(h) If only a middle sample is required, pour all of the jerk of the sampling line.
sample into the sample container. If samples are required at (g) Allow sufficient time for the bottle/beaker to completely
more than one location, measure out a specified amount of fill at the specific location.
sample with the graduated cylinder, and deposit it in the sample (h) Withdraw the sampling assembly.
container. (i) Verify the bottle/beaker is completely full. If not full,
NOTE 5—The amount of sample measured will depend upon the size of empty the bottle/beaker and repeat the procedure beginning
the thief and the tests to be performed but should be consistent for the with (d).
samples taken at different levels. (j) If only this spot sample is required for compositing will
(i) Discard the remainder of the sample from the sampling be accomplished elsewhere, pour all of the sample into the
thief as required. sample container or discard one-fourth of the sample, stopper
(j) Repeat steps (d) through (i) to obtain a sample(s) at the the bottle/beaker, and proceed to (n). If composited samples are
other sample location(s) required by Table 5 or to obtain required at more than one location, measure out a specific
additional sample volume, if only a middle sample is required. amount of sample with a graduated cylinder and deposit it in
(k) Install the lid on the sample container. the sample container.
(l) Label the sample container. NOTE 6—The amount of sample measured will depend upon the size of
(m) Return the sample container to the laboratory or other the bottle/beaker and the tests to be performed but should be consistent for
facility for mixing and testing. the samples taken at different levels.
13.4.2 Bottle/Beaker Spot Sampling: (k) Discard the remainder of the sample from the sampling
13.4.2.1 Application—The bottle or beaker spot sampling bottle/beaker as required.
procedure may be used for sampling liquids of 101 kPa (14.7 (l) Repeat (c) through (k) to obtain a sample(s) at the other
psia) RVP or less in storage tanks, tank cars, tank trucks, ship, sample location(s) required by Table 5 or to obtain additional
and barge tanks. Solids or semi-liquids that can be liquified by sample volume if only a middle sample is required.
heat may be sampled using this procedure, provided they are (m) Install the closure on the sample container.
true liquids at the time of sampling. (n) Disconnect the line from the bottle, or remove the sample
13.4.2.2 Apparatus—The bottle and beaker are shown in bottle from the sampling cage, as applicable.
Fig. 4. A graduated cylinder and possibly a sample container (o) Label the sample container.
are required for use with this procedure. The sampling cage (p) Return the sample container to the laboratory or other
shall be made of a metal or plastic suitably constructed to hold facility for mixing and testing.
the appropriate container. The combined apparatus shall be of 13.5 Running or All-Level Sampling:
such weight as to sink readily in the material to be sampled, 13.5.1 Application—The running and all levels sample
and provision shall be made to fill the container at any desired procedures are applicable for sampling liquids of 101 kPa (14.7
psia) RVP or less in tank cars, tank trucks, shore tanks, ship
TABLE 5 Weighted Sampling Bottle or Beaker tanks, and barge tanks. Solids or semi-liquids that can be
Diameter of Opening liquified by heat may be sampled by this procedure, provided
Material
cm in. they are true liquids at the time of sampling. A running/all-
Light lubricating oils, kerosines, gasolines, 2 ⁄
34 levels sample is not necessarily a representative sample be-
transparent gas oils, diesel fuels, distillates cause the tank volume may not be proportional to the depth and
Heavy lubricating oils, nontransparent gas oils 4 11⁄2 because the operator may not be able to raise the sampler at the
Light crude oils less than 43 cTs at 40°C 2 ⁄
34
Heavy crude and fuel oils 4 11⁄2 rate required for proportional filling. The rate of filling is
proportional to the square root of the depth of immersion.
10
D 4057
13.5.2 Apparatus—A suitable sampling bottle or beaker, as breather and balloon-roof type, spheroids, and so forth.
shown in Fig. 4A and B, equipped with notched cork or other (Samples may be taken from the drain cocks of gage glasses, if
restricted opening is required. Recommended opening diam- the tank is not equipped with sampling taps.)
eters for various applications are given in Table 5. 13.6.2 Apparatus:
13.5.3 Procedure: 13.6.2.1 Typical sample tap assembly is shown in Fig. 5.
13.5.3.1 Inspect the sampling bottle and sample container Each tap should be a minimum of 1.25 cm (1⁄2 in.) in diameter.
for cleanliness and use only clean, dry equipment. Taps 2.0 cm (3⁄4-in.) may be required for heavy, viscous liquids
13.5.3.2 Attach the weighted line to the sample bottle, or (for example, crude oil of .9465 density (18° API) or less). On
place the bottle in a sampling cage. tanks that are not equipped with floating roofs, each sample tap
13.5.3.3 If required to restrict the filling rate, insert a should extend into the tank a minimum of 10 cm (4 in.).
notched cork in the sampling bottle. Normally, a sample tap should be equipped with a delivery
13.5.3.4 At a uniform rate, lower the bottle assembly as near tube which permits the filling of the sample container from the
as possible to the level of the bottom of the outlet connection bottom.
or swing line inlet and, without hesitation, raise it such that the 13.6.2.2 For tanks having a side outlet, a tap for obtaining a
bottle is approximately three-fourths full when withdrawn from clearance sample may be located 2 cm (4 in.) below the bottom
the liquid. of the outlet connection. Other requirements for sample taps
13.5.3.5 Verify that a proper quantity of sample has been are outlined in Table 6.
obtained. If the bottle is more than three-fourths full, discard 13.6.2.3 Clean, dry glass bottles of convenient size and
the sample and repeat 13.5.3 and 13.5.4, adjusting the rate at strength to receive the samples are required.
which the bottle assembly is lowered and raised. Alternatively, 13.6.3 Procedure:
repeat 13.5.3 and 13.5.4 using a different notched cork. 13.6.3.1 Inspect the sample container(s) and graduated cyl-
13.5.3.6 Empty the contents of the bottle into the sample inder for cleanliness. If required, obtain clean equipment or
container, if necessary. clean the existing equipment with a suitable solvent, and rinse
13.5.3.7 If additional sample volume is required, repeat with the liquid to be sampled prior to proceeding to 13.6.3.2.
13.5.3.3-13.5.3.6. 13.6.3.2 Obtain an estimate of the liquid level in the tank.
13.5.3.8 Install the lid on the sample container. 13.6.3.3 If the material to be sampled is 101 kPa (14.7 psia)
13.5.3.9 Label the sample container. RVP or less, connect the delivery tube directly to the sample
13.5.3.10 Disconnect the line from the bottle, or remove the tap as required.
sample bottle from the sampling cage, as applicable. 13.6.3.4 Flush the sample tap and piping until they have
13.5.3.11 Return the sample container to the laboratory or been completely purged.
other facility for mixing and testing. 13.6.3.5 Collect the sample in a sample container or a
13.6 Tap Sampling: graduated cylinder in accordance with the requirements set
13.6.1 Application—The tap sampling procedure is appli- forth in Table 7. If samples are to be obtained from different
cable for sampling liquids of 101 kPa (14.7 psia) RVP or less taps, use a graduated cylinder to measure the appropriate
in tanks that are equipped with suitable sampling taps. This sample quantity. Otherwise, collect the sample directly in the
procedure is recommended for volatile stocks in tanks of the sample container. If a delivery tube is used, ensure the end of
11
D 4057
12
D 4057
13
D 4057
NOTE 1—Probes may be fitted with valves or plug cocks. The probe should be oriented horizontally.
FIG. 8 Probes for Spot Manual Samples
14.2.2 A short radius elbow or pipe bend. The end of the such that the velocity of liquid flowing through the probe is
probe should be chamfered on the inside diameter to give a approximately equal to the average linear velocity of the
sharp entrance edge (see Fig. 8B). stream flowing through the pipeline. Measure and record the
14.2.3 A closed-end tube with a round orifice spaced near rate of sample withdrawal as gallons per hour. Divert the
the closed end as shown in Fig. 8C. sample stream to the sampling container continuously or
14.3 Probe Location: intermittently to provide a quantity of sample that will be of
14.3.1 Since the fluid to be sampled may not always be sufficient size for analysis.
homogeneous, the location, position, and size of the sampling 14.4.2 In sampling crude petroleum and other petroleum
probe should be such as to minimize any separation of water products, samples of 250 mL (1⁄2pt) or more should be taken
and heavier particles that would make their concentration every hour or at increments less than an hour, as necessary. By
different in the gathered sample than in the main stream. mutual agreement, the sample period or sample size, or both,
14.3.2 The probe should always be in a horizontal plane to may be varied to accommodate the parcel size. It is important
prevent drain back of any part of the sample to the main that the size of the samples and the intervals between the
stream. sampling operations be uniform for a uniform flow rate. When
14.3.3 The sampling probe should preferably be located in a the main stream flow rate is variable, the sampling rate and
vertical run of pipe where such a vertical run can be provided. volume must be varied accordingly so that the flow is propor-
The probe may also be located in a horizontal run of pipe. The tional. In practice, this is difficult to accomplish manually.
flowing velocity must be high enough to provide adequate 14.4.3 Each sample of crude petroleum should be placed in
turbulent mixing (see Practice D 4177). a closed container, and at the end of the agreed upon time
14.3.4 Where adequate flowing velocity is not available, a period, the combined samples should be mixed and a compos-
suitable device for mixing the fluid flow should be installed ite sample taken for test purposes. Refer to 12.3 for mixing and
upstream of the sampling tap to reduce stratification to an handling. The sample container should be stored in a cool, dry
acceptable level. If flow has been vertical for a sufficient place; exposure to direct sunlight should be avoided.
distance, as in a platform riser, such a device may not be 14.4.4 Alternatively, line samples may be taken at regular
necessary even at low flow rates. Some effective methods for intervals and individually tested. The individual test results
obtaining adequate mixing are: a reduction in pipe size, a series may be arithmetically averaged, adjusting for variations in flow
of baffles, and orifice or perforated plate, or combination of any rate during the agreed upon time period.
of these methods. The design or sizing of the device is optional 14.4.5 Either composite or arithmetically averaged results
with the user, as long as the flowing stream is sufficiently well are acceptable by mutual agreement.
mixed to provide a representative sample from the probe. 14.4.6 With either procedure, always label each sample and
14.3.5 Sampling lines, used in conjunction with probes, deliver to the laboratory in the container in which it was
should be as short as is practical and should be cleared before collected.
any samples are taken.
14.3.6 When sampling semi-liquids, it may be necessary to 15. Dipper Sampling
heat the sample line, valves, and receiver to a temperature just 15.1 Application—The dipper sampling procedure is appli-
sufficient to keep the material liquid and to ensure accurate cable for sampling liquids of 13.8 kPa (2 psia) RVP or less and
sampling and mixing. semi-liquids where a free or open discharge stream exists, as in
14.3.7 To control the rate at which the sample is withdrawn, small filling and transfer pipelines, 5 cm (2 in.) in diameter or
the probe should be fitted with valves or plug cocks. less, and filling apparatus for barrels, packages, and cans.
14.4 Procedure: 15.2 Apparatus—Use a dipper with a flared bowl and a
14.4.1 Adjust the valve or plug cock from the sampling handle of conventional length made of a material such as
probe so that a steady stream is drawn from the probe. tinned steel that will not affect the product being tested. The
Whenever possible, the rate of sample withdrawal should be dipper should have a capacity suitable for the amount to be
14
D 4057
collected and must be protected from dust and dirt when not 16.3.1 Place the drum or barrel on its side with the bung up.
being used. Use a clean, dry sample container of the desired If the drum does not have a side bung, stand it upright and
size. sample from the top. If detection of water, rust, or other
15.3 Procedure—Insert the dipper in the free-flowing insoluble contaminants is desired, let the barrel or drum remain
stream so that a portion is collected from the full cross section in this position long enough to permit the contaminants to
of the stream. Take portions at time intervals chosen so that a settle. Remove the bung and place it beside the bung hole with
complete sample proportional to the pumped quantity is the oily side up. Close the upper end of the clean, dry sampling
collected. The gross amount of sample collected should be tube with the thumb, and lower the tube into the oil to a depth
approximately 0.1 percent, but not more than 150 L (40 gal) of of about 30 cm (1 ft). Remove the thumb, allowing oil to flow
the total quantity being sampled. Transfer the portions into the into the tube. Again, close the upper end with the thumb and
sample container as soon as they are collected. Keep the withdraw the tube. Rinse the tube with the oil by holding it
container closed, except when pouring a dipper portion into it. nearly horizontal and turning it so that the oil comes in contact
As soon as all portions of the sample have been collected, close with that part of the inside surface that will be immersed when
and label the sample container and deliver it to the laboratory. the sample is taken. Avoid handling any part of the tube that
will be immersed in the oil during the sampling operation.
16. Tube Sampling Discard the rinse oil and allow the tube to drain. Insert the tube
16.1 Application—The tube sampling procedure is appli- into the oil again, holding the thumb against the upper end. (If
cable for sampling liquids of 13.8 kPa (2 psia) RVP or less and an all-levels sample is desired, insert the tube with the upper
semi-liquids in drums, barrels, and cans. end open.) When the tube reaches the bottom, remove the
16.2 Apparatus—Either a glass or metal tube may be used, thumb and allow the tube to fill. Replace the thumb, withdraw
designed so that it will reach to within about 3 mm (1⁄8 in.) of the tube quickly, and transfer the contents to the sample
the bottom of the container. Capacity of the tube can vary from container. Do not allow the hands to come in contact with any
500 mL to 1 L (1 pt to 1 qt). A metal tube suitable for sampling part of the sample. Close the sample container; replace and
189 L (50-gal) drums is shown in Fig. 9. Two rings soldered to tighten the bung in the drum or barrel. Label the sample
opposite sides of the tube at the upper end are convenient for container and deliver it to the laboratory.
holding it by slipping two fingers through the rings, thus 16.3.2 Obtain samples from cans of 18.9 L (5 gal) capacity
leaving the thumb free to close the opening. Use clean, dry or larger in the same manner as for drums and barrels, using a
cans, or glass bottles for sample containers. tube of proportionately smaller dimensions. For cans of less
16.3 Procedure: than a 18.9-L (5-gal) capacity, use the entire contents as the
sample, selecting cans at random as indicated in Table 4 or in
accordance with the agreement between the purchaser and the
seller.
17. Boring Sampling
17.1 Application—The boring sampling procedure is appli-
cable for sampling waxes and soft solids in barrels, cases, bags,
and cakes when they cannot be melted and sampled as liquids.
17.2 Apparatus:
17.2.1 Use a ship auger 2 cm (3⁄4 in.) in diameter (preferred),
similar to that shown in Fig. 10, and of sufficient length to pass
through the material to be sampled.
17.2.2 Use clean, wide-mouth metal containers or glass jars
with covers for cover sample containers.
17.3 Procedure—Remove the heads or covers of barrels or
cases. Open bags and wrappings of cakes. Remove any dirt,
sticks, string, or other foreign substances from the surface of
the material. Bore three test holes through the body of the
material, one at the center, the other two halfway between the
center and the edge of the package on the right and left sides,
respectively. If any foreign matter is removed from the interior
of the material during the boring operation, include it as part of
the borings. Put the three sets of borings in individual sample
containers, label, and deliver them to the laboratory.
17.4 Laboratory Inspection—If there are any visible differ-
ences in the samples, examine and test each set of borings at
FIG. 9 Typical Drum or Barrel Sampler FIG. 10 Ship Auger for Boring Procedure
15
D 4057
the laboratory. Otherwise, combine the three sets of borings
into one sample. If subdivision of borings is desired, chill,
pulverize (if necessary), mix, and quarter the borings until
reduced to the desired amount.
18. Grab Sampling
18.1 Application—The grab sampling procedure is appli-
cable for sampling all lumpy solids in bins, bunkers, freight
cars, barrels, bags, boxes, and conveyors. It is particularly
FIG. 12 Location of Sampling Points from Exposed Surface for
applicable for the collection of green petroleum coke samples Rail Cars
from railroad cars and for the preparation of such samples for
laboratory analysis. Refer to Practice D 346 when other meth-
ods of shipping or handling are used. Petroleum coke may be on a hard, clean surface, free from cracks, and protected from
sampled while being loaded into railroad cars from piles or rain, snow, wind, and sun. Avoid contamination with cinders,
after being loaded into railroad cars from coking drums. sand, chips from the floor, or any other material. Protect the
18.2 Apparatus—A polyethylene pail of approximately 9.5 sample from loss or gain of moisture or dust. Mix and spread
L (10 qt) capacity shall be used as the sample container. Use a the sample in a circular layer, and divide it into quadrants.
stainless steel or aluminum No. 2 size scoop to fill the Combine two opposite quadrants to form a representative
container. reduced sample. If this sample is still too large for laboratory
18.3 Procedure—Lumpy solids are usually heterogeneous purposes, repeat the quartering operation. In this manner, the
and difficult to sample accurately. It is preferable to take sample will finally be reduced to a representative, suitable size
samples during the unloading of cars or during transit; obtain for laboratory purposes. Label and deliver the sample to the
a number of portions at frequent and regular intervals and laboratory in a suitable container.
combine them.
18.3.1 Sampling From Railroad Cars—Use one of the 19. Grease Sampling
following procedures: 19.1 Application—This method covers practices for obtain-
18.3.1.1 Cars Being Loaded from a Pile— Take a full scoop ing samples representative of production lots or shipments of
of sample at each of the five sampling points shown in Fig. 11, lubricating greases or of soft waxes or soft bitumens similar to
and deposit in a polyethylene pail. Cover the sample, and grease in consistency. This procedure is quite general because
deliver it to the laboratory. Each sampling point shall be a wide variety of conditions are often encountered, and the
located equidistant from the sides of the railroad car. procedure may have to be modified to meet individual speci-
18.3.1.2 After Direct Loading from Coking Drums—At any fications. Proceed in accordance with Sections 7 and 6,
five of the sampling points shown in Fig. 12, take a full scoop particularly those paragraphs pertaining to precautions, care
of coke from about 30 cm (1 ft) below the surface, and deposit and cleanliness, except where they conflict with instructions
it in a polyethylene pail. Cover the sample and deliver it to the given in this section.
laboratory. 19.2 Inspection:
18.3.2 Sampling From Conveyors—Take one scoop for 19.2.1 If the material is a lubricating grease and inspection
each 7 to 9 metric tons (8 to 10 short tons) of coke transported. is made at the manufacturing plant, take samples from finished
These samples may be handled separately or composited after shipping containers of each production batch or lot. Never take
all samples representing the lot have been taken. grease samples directly from grease kettles, cooling pans,
18.3.3 Sampling From Bags, Barrels, or Boxes: tanks, or processing equipment. Do not sample the grease until
18.3.3.1 Obtain portions from a number of packages se- it has cooled to a temperature not more than 9.4°C (15°F)
lected at random as shown in Table 3, or in accordance with the above that of the air surrounding the containers and until it has
agreement between the purchaser and seller. been in the finished containers for at least 12 h. When the
18.3.3.2 Carefully mix the grab sample and reduce it in size containers for a production batch of grease are of different
to a convenient laboratory sample by the quartering procedure sizes, treat the grease in each size of container as a separate lot.
described in Practice D 346. Perform the quartering operation When inspection is made at the place of delivery, obtain a
sample from each shipment. If a shipment consists of contain-
ers from more than one production batch (lot numbers), sample
each batch separately.
19.2.2 If the material being inspected is of grease-like
consistency, but is not actually a lubricating grease but some
mixture of heavy hydrocarbons, such as microcrystalline
waxes or soft bitumens, it is permissible to take samples from
pans, tanks, or other processing equipment, as well as from
containers of the finished product. The grease sampling method
shall be applicable to such stocks only if for some reason it is
FIG. 11 Location of Sampling Points at Different Levels for Rail not possible to apply heat and convert the material into a true
Cars liquid.
16
D 4057
19.3 Sample Size—Select containers at random from each kg (1 lb) can or suitable dipper. If any marked difference in the
lot or shipment to give the required quantity specified in Table grease from the various locations of an opened container is
8. found, take two separate samples of about 0.45 kg (1 lb) each,
19.4 Procedure: one from the top surface adjacent to the wall and the other from
19.4.1 Examine the opened containers to determine whether the center of the container, at least 15 cm (6 in.) below the top
the grease is homogeneous, comparing the grease nearest the surface. If any marked variations are noted between different
outer surfaces of the container with that in the center, at least containers of a lot or shipment, take separate samples of about
15 cm (6 in.) below the top surface, for texture and consistency. 0.45 (1 lb) from each container. When more than one sample of
When more than one container of a lot or shipment is opened, a batch or shipment is taken because of lack of uniformity, send
compare the grease in all open containers. them to the laboratory as separate samples.
19.4.2 If no marked difference in the grease is found, take 19.4.3 If more than one portion is required to represent a lot
one portion from the approximate center and at least 6.5 cm (3 or shipment of grease softer than 175 penetration (see Test
in.) below the surface of each opened container in sufficient Method D 217), prepare a composite sample by mixing equal
quantity to provide a composite sample of the desired quantity portions thoroughly. Use a large spoon or spatula and a clean
(see Table 8). Withdraw portions with a clean scoop, large container. Avoid vigorous mixing or working of air into the
spoon, or spatula, and place them in a clean container. Very grease. As grease samples become partially “worked” in being
soft, semi-fluid greases may be sampled by dipping with a 0.45 removed from containers, the procedure is not suitable for
obtaining samples of greases softer than 175 penetration on
TABLE 8 Size of Grease Samples which unworked penetration is to be determined. For greases
having a penetration of less than 175, cut samples from each
Container Lot or Shipment Minimum Sample
container with a knife in the form of blocks about 15 by 15 by
Tubes or packages, less All enough units for a 4.4
than 0.45 Kg (1 lb) Kg (2 lb) sample
5 cm (6 by 6 by 2 in.). If required, make unworked penetration
0.45 Kg (1 lb) cans All three cans tests on blocks as procured and other inspection tests on grease
2.3 or 4.6 Kg (5 or 10 lb) All one can cut from the blocks.
cans
Larger than 4.6 Kg (10 lb) less than 4536 Kg 1 to 1.4 Kg (2 to 3 lb)
(10 000 lb) from one or more
20. Keywords
containers 20.1 boring sampling; bottle/beaker sampling; core thief
Larger than 4.6 Kg (10 lb) 4536 to 22 680 Kg 1 to 2.3 Kg (2 to 5 lb)
(10 000 to 50 000 lb) from two or more spot sampling; dipper sampling; extended tube sampling; grab
containers sampling; grease sampling; marine custody transfer; sample
Larger than 4.6 Kg (10 lb) more than 22 680 Kg 1 to 2.3 Kg (2 to 5 lb) containers; sample handling; sample labeling; sample mixing;
(50 000 lb) from three or more
containers sample shipment; sampling; sampling cage; static sampling;
stand pipes; tap sampling; tube sampling
ANNEX
(Mandatory Information)
A1.1 The following substances may be used throughout the vapors and eliminate all sources of ignition, especially non-
course of this standard test method. The precautionary state- explosion proof electrical apparatus and heaters.
ments should be read prior to use of such substances. A1.1.2.4 Avoid prolonged breathing of vapors or spray mist.
A1.1.1 Benzene: A1.1.2.5 Avoid prolonged or repeated skin contact.
A1.1.1.1 Keep away from heat, sparks, and open flame. A1.1.3 Flammable Liquid (general):
A1.1.1.2 Keep container closed. A1.1.3.1 Keep away from heat, sparks, and open flame.
A1.1.1.3 Use with adequate ventilation. A1.1.3.2 Keep container closed.
A1.1.1.4 Use fume hood whenever possible. A1.1.3.3 Use only with adequate ventilation.
A1.1.1.5 Avoid build-up of vapors and eliminate all sources A1.1.3.4 Avoid prolonged breathing of vapor or spray mist.
of ignition, especially non-explosion proof electrical apparatus A1.1.3.5 Avoid prolonged or repeated contact with skin.
and heaters. A1.1.4 Gasoline (White):
A1.1.1.6 Avoid prolonged breathing of vapors or spray mist. A1.1.4.1 Harmful if absorbed through skin.
A1.1.1.7 Avoid contact with skin and eyes. Do not take A1.1.4.2 Keep away from heat, sparks, and open flame.
internally. A1.1.4.3 Keep container closed. Use with adequate ventila-
A1.1.2 Diluent (Naphtha): tion.
A1.1.2.1 Keep away from heat, sparks, and open flame. A1.1.4.4 Avoid build-up of vapors and eliminate all sources
A1.1.2.2 Keep container closed. of ignition especially non-explosion proof electrical apparatus
A1.1.2.3 Use with adequate ventilation. Avoid build-up of and heaters.
17
D 4057
A1.1.4.5 Avoid prolonged breathing of vapor or spray mist. A1.1.5.3 Keep container closed.
A1.1.4.6 Avoid prolonged or repeated skin contact. A1.1.5.4 Use with adequate ventilation. Avoid breathing of
A1.1.5 Toluene and Xylene: vapor or spray mist.
A1.1.5.1 Warning—Flammable. Vapor harmful.
A1.1.5.5 Avoid prolonged or repeated contact with skin.
A1.1.5.2 Keep away from heat, sparks, and open flame.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at
610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website (www.astm.org).
18