Astmd1265 1547
Astmd1265 1547
Astmd1265 1547
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D1265 − 23
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U.S. 49 CFR Transportation6 5.2 Equipment described by this practice may be suitable
2.3 Other Publications: for transportation of LPG samples, subject to applicable
API RP 2003 Protection Against Ignitions Arising Out of transportation regulations.
Static, Lightning, and Stray Currents
6. General Information
3. Terminology 6.1 Considerable effort is required to obtain a representative
3.1 Definitions: sample, especially if the material being sampled is a mixture of
3.1.1 For definitions of terms used in this practice, refer to liquefied petroleum gases. Consider the following factors:
Terminology D4175. 6.1.1 Obtain samples of the liquid phase only.
3.1.2 high pressure sample cylinder, n—a container used for 6.1.2 When it is definitely known that the material being
storage and transportation of a sample obtained at pressures sampled is composed predominantly of only one liquefied
above atmospheric pressure. petroleum gas, a liquid sample may be taken from any part of
3.1.3 liquefied petroleum gas (LP Gas, LPG), n—a narrow the vessel.
boiling range mixture of hydrocarbons consisting of propane, 6.1.3 When the material being sampled has been mixed or
propylene, butanes and butylenes, individually or in specified circulated until it is homogeneous, a liquid sample may be
combinations, with limited amounts of other hydrocarbons taken from any part of the vessel.
(such as ethane) and may contain naturally occurring, 6.1.4 Because of wide variations in the construction details
petroleum-derived, non-hydrocarbons. of containers for liquefied petroleum gases, it is difficult to
3.1.4 maximum fill volume (reduced fill volume), n—the specify a uniform method for obtaining representative samples
volume of a container that may be safely occupied by the liquid of heterogeneous mixtures. If it is not practicable to homog-
sample, usually expressed as a percentage of the total capacity. enize a mixture to ensure uniformity, obtain liquid samples by
3.1.4.1 Discussion—Some regulatory agencies use the ex- a procedure which has been agreed upon by the contracting
pressions “maximum fill density” and “reduced fill density.” parties.
3.1.5 outage tube (internal), n—a “cut to length” tube 6.1.5 Directions for sampling cannot be made explicit
placed inside the cylinder used as a way to remove excess enough to cover all cases. They must be supplemented by
liquid sample from the cylinder via manual evacuation after the judgment, skill, and sampling experience. Extreme care and
sample cylinder assembly is removed from the sample point. good judgment are necessary to ensure samples which repre-
sent the general character and average condition of the mate-
3.1.6 outaging, n—practice of removing a portion of liquid
rial. Because of the hazards involved, liquefied petroleum
contents from a conventional sampling cylinder after filling to
gases should be sampled by, or under the supervision of,
provide expansion room.
persons familiar with the necessary safety precautions.
3.1.7 ullage (outage), n—in LPG sampling, the volume in a 6.1.6 Control hydrocarbon vapors vented during sampling
container after filling that remains as vapor phase above the to ensure compliance with applicable safety and environmental
liquid contents to allow for thermal expansion of the liquid. regulations. Do not vent near ignition sources.
3.1.8 upright, adj—the vertical orientation of the cylinder 6.1.7 This standard is applicable to flow-through double-
where the outage tube end is at the top. ended cylinders with two valves. It is not applicable to
single-ended (single valve) cylinders or larger LPG sample
4. Summary of Practice containers such as those utilized for barbecue grills and/or
4.1 A liquid sample of LPG is transferred from the source forklift cylinders. Additional pertinent information for these
into a high pressure sample container by purging the container applications can be found in Practice D6849.
and filling it with liquid, then providing a minimum 20 % 6.1.8 Elimination of potential static charge accumulation
ullage by venting liquid, so that 80 % or less of the liquid and discharge is critical for safety. Provisions for grounding/
volume remains. bonding shall be in place for the sample station and sample
NOTE 2—When sampling under very cold conditions, where there is a
cylinders. Having continuous electrical contact to dissipate
significant difference between original sample temperature and sample charge is required, including the transfer lines. Non-conductive
temperature in a laboratory or shipping situation, an ullage volume greater materials cannot be utilized unless special grounding provi-
than 20 % may be required to safely account for the significant expansion sions are applied. More information on static charge accumu-
of LPG with a large rise in temperature. lation and grounding/bonding can be obtained from API RP
2003.
5. Significance and Use
5.1 Samples of liquefied petroleum gases are examined by 7. Interferences
various test methods to determine physical and chemical
characteristics and conformance with specifications. 7.1 Certain properties of interest can be affected by the
material making up the sampling system and sample cylinder
assembly. Two examples of analytes commonly associated
6
with adsorption (and desorption) at lower concentrations (for
Available from U.S. Government Printing Office Superintendent of Documents,
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, https:// example, <100 ppm by mass) are active sulfur compounds and
www.ecfr.gov/. water. Without the use of properly treated equipment, there is
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potential for lower response from analytes than actually present regulations. See 49 CFR 180.209 for information on requalification
in the sample due to adsorption (or, in the case of desorption, requirements for cylinders.
higher response). NOTE 6—This standard is not applicable to single valve cylinders or
larger LPG sample containers such as those utilized for barbecue grills
7.2 Adsorption and desorption can result from physical and/or forklift cylinders.
attraction or chemical attraction.7 Due to adsorption, tubing
8.1.1 The sample container should be fitted with an internal
and cylinder components exposed to a sample may need
outage (ullage) tube to permit release of a minimum 20 % of
surface treatment (that is, with an inert surface material) in
the container capacity as a liquid. The end of the container
order to collect a representative sample to be analyzed for the
fitted with the outage (ullage) tube shall be clearly marked.
property of interest.
Typical sample containers are shown in Figs. 1 and 2.
7.3 Tubing that is rough on the inside results in a larger 8.1.2 The use of sample containers without internal outage
surface area than expected. In order to reduce the surface area, (ullage) tubes may be prohibited at some locations. Where
the tubing needs to be smooth. Additionally, a surface treat- sample containers without internal outage (ullage) tubes are
ment on the internal wall is needed to reduce the potential for acceptable, alternative purging and venting procedures to
polar molecules to adsorb. For stainless steel tubing and obtain a minimum 20 % ullage in the container, as described in
cylinders (which have a high potential for adsorption of polar 11.2.1, are required.
molecules), this may be achieved by electropolishing and fused
8.1.3 Leak checks are to be performed prior to first use, after
silica coating.
any maintenance, and at the very least annually by pressurizing
7.3.1 This inerting treatment aids in reducing the potential
the cylinder to a minimum of 2758 kPa (400 psig) with inert
for adsorption of the analyte of interest.
gas, followed by immersing the cylinder fittings in a bucket of
7.3.2 Samples to be tested for the presence of corrosive
water.
compounds or sulfur compounds should be taken in containers
made inert to such compounds and equipped with valves 8.1.4 Regulatory and/or local site compliance may require
compatible with chemical, pressure, and temperature require- sample cylinder assemblies to incorporate a pressure relief
ments; otherwise, determinations of mercaptans and hydrogen device. The two common types of pressure relief devices are
sulfide, for example, can be misleading. Internal surfaces of the spring relief valve and the rupture disc.
sample containers, valves, outage tubes, and associated lines 8.1.4.1 The spring relief valve (also known as a “poppet
and fittings may be surface coated to reduce bare metal valve”) is a reclosing device. It is designed to open at a preset
surfaces reacting with trace reactive components. pressure, where a minimal amount of sample material is
released to the immediate vicinity until the pressure drops to a
NOTE 3—Adsorption is not passivation. With adsorption, molecules are level when the valve re-seats (recloses).
both adsorbing and desorbing. Since each individual action can occur at
any time, there is potential for an analysis to see less or more of an analyte 8.1.4.2 The rupture disc is a non-reclosing device. This is
than actually present in the sample. Passivation is a permanent or often called a burst disc. It contains a bulged disc that is
long-term surface treatment that minimizes adsorption of polar com- designed to burst or fail when a specified pressure range is
pounds. reached. The disk is destroyed in the process of relieving
8. Apparatus pressure, and the entire contents of the sample cylinder will be
released to the immediate vicinity.
8.1 High Pressure Sample Cylinder—Use corrosion resis-
8.1.4.3 The user is cautioned to understand the hazards
tant metal sample containers certified by the authority having
associated with the type of relief device being used. Both
jurisdiction for pressure vessels with adequate pressure rating
release sample material when a design pressure is reached.
for the product being sampled. Suitable materials include
However, a rupture disc releases all contents of the cylinder,
stainless steel, Monel, and possibly other materials. Protective
thereby creating potentially more risk of exposure or larger
internal coatings or surface treatments to render the internal
incident if an ignition source is encountered. While a spring
surface inert are acceptable. The size of the container depends
relief device does not release the entire content, if activated to
upon the amount of sample required for the laboratory tests to
release some pressure, the sample has been compromised and
be made. If the container is to be transported, it shall also
should be discarded just as if the cylinder had leaked (refer to
conform to specifications published in transportation legisla-
15.1).
tion such as U.S. 49 CFR or Canadian Transportation of
Dangerous Goods Regulations, and their supplements, 8.2 Sample Transfer Line made of stainless steel or other
reissues, or similar regulations in other jurisdictions. compatible metal hose, impervious to the product being
NOTE 4—It has been common practice to refer to LPG sample sampled, is required. The line can include a flexible hose made
containers as “sample bombs.” Use of this term is discouraged because of of material that is compatible with the chemical, pressure, and
obvious misunderstanding by many people. Alternate names such as temperature encountered during use. The most satisfactory line
“pressurized sample container” or “high pressure sample cylinder” are is one equipped with two valves on the sample-container end,
recommended. Fig. 1, a sampling valve, A, and a vent valve, B.
NOTE 5—DOT 3E cylinders are exempt from requalification in some
jurisdictions. Other cylinders may need to be requalified according to local 8.3 Sample System—Consists of sampling line, cylinder, and
vent valve. Electrical continuity should be established and
7
Waters, T., Industrial Sampling Systems, Reliable Design & Maintenance for maintained across the sample system to decrease risk of static
Process Analyzers, Swagelok Company, 2013. discharge while sampling.
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10.3.1 With the container in an upright position (Fig. 1) and Method D1838). For these transfers, the user needs to consider
its Valve D (outlet) at the top, close Valve B (vent) and Valve the physical properties of the sample and ensure the transfer
C (inlet) and open Valve A (sampling). Open Valve C (inlet) setup maintains the sample’s integrity.
and partly fill the container with sample by slowly opening the 11.2.1 For these transfers, connect cylinders together by a
Valve D (outlet). Close the Valve A (sampling) and allow part suitable system/apparatus, with proper grounding and bonding
of the sample to escape in the vapor phase through Valve D of the system to prevent static discharge (Fig. 3). The empty
(outlet). Close Valve D (outlet) and release the remainder of the secondary cylinder (for example, corrosion cylinder, LPG
sample in the liquid phase by opening Valve B (vent). Repeat
vapor pressure apparatus, etc.) shall be clean and free of any
the purging operation at least three times.
residues (including moisture) or any solvents that could con-
11. Transfer of Sample taminate the sample.
11.1 Position the sample container securely in an upright 11.2.2 Cylinder A may need to be pressurized to maintain
position with Valve D (outlet) at the top (Fig. 1) and both sample integrity and ensure transfer of liquid sample amount
Valves C and D closed. required for testing to the secondary cylinder. Cylinders and
11.1.1 Close Valve B (vent), open Valve A (sampling), open associated equipment for transfer should be maintained at the
Valve C (inlet), and fill container with the sample. Close Valve same temperature to aid in preventing flashing of liquid to
C (inlet) and the valve at the product source. Open Valve B vapor.
(vent). After the pressure is fully reduced, disconnect sample 11.2.3 After confirming proper ullage by procedure or by
container from the transfer line. Discard the sample if a leak weight, ensure homogeneity with mixing by repeated inverting
develops or if either valve is opened during subsequent and uprighting cylinder position several times before transfer-
handling of the sample container before performing the outage ring sample. Ensure all valves are closed to begin. Workers
(ullage) operations outlined in Section 12. should also ground and bond themselves when performing the
11.2 The transfer of a sample from one container to another transfer. 6.1.8 contains additional information on grounding/
is sometimes desired for a test method (for example, Test bonding.
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11.2.4 Cylinder A contains the sample to be transferred to legislation such as U.S. 49 CFR, Canadian Transportation of Dangerous
secondary cylinder (empty, but might be pressurized with inert Goods Regulations, and IATA regulations limit the percent fill of
containers used for shipping LPG and may quote this requirement as a
or noble gas, depending on application). Once electrical reduced fill density or maximum fill density (normally 80 % maximum
continuity is confirmed across all components of the system, liquid fill at 15 °C). A lower percent fill (lower fill density) may be
open Valve C (cylinder A outlet), then open Valve B (secondary required if sampling at lower temperatures.
cylinder inlet). Allow needed amount of sample to pass from NOTE 8—Extreme low temperature sampling. LPG has a larger coeffi-
Cylinder A to secondary cylinder. Once sample amount has cient of thermal expansion than gasoline or distillate fuels. Sampling at
extremely low ambient temperatures or from cryogenic sources may
been transferred, close Valve B (secondary cylinder inlet), then require additional precautions to prevent sample cylinders from becoming
close Valve C (cylinder A outlet). Ensure proper ullage was liquid full (liquid locked, hydraulically locked) from warming the sample
maintained. The secondary cylinder can be either a double- to high ambient temperature.
ended cylinder assembly (for example, LPG Corrosion Cylin- 12.1.1.2 Where immediate venting is not possible, for
der) or single-ended cylinder assembly (for example, LPG example inside hazardous locations or with toxic materials
Vapor Pressure Cylinder). (especially H2S), provisions shall be made to prevent tempera-
11.2.4.1 When transferring samples in a laboratory ture increase prior to venting in a safe location, transfer to a
(cylinder-to-cylinder), due to the limited amount of sample larger cylinder or immediate analysis or other disposition in
material in Cylinder A, purges of the secondary cylinder are accordance with the authority having jurisdiction. It is the
typically not an option due to loss of material needed for responsibility of the user to establish safe procedures for use in
testing. Confirm that sample amount is transferred before permitted facilities that are regulated by site permits or
testing. equivalent, separate from transportation regulations.
12. Sample Outage (Ullage) NOTE 9—Improperly venting LPG vapor to establish the minimum
20 % outage will result in large changes in composition of the remaining
12.1 Immediately after obtaining the sample, place the liquid due to fractional distillation. It is important that only liquid be
container in an upright position with the outage (ullage) tube at vented from the cylinder, and that venting be stopped at the first indication
the top. of vapor. Use of proper liquid venting technique will result in only very
12.1.1 Open Valve D (outlet) slightly. Allow excess liquid to small changes in composition to the remaining liquid which will not affect
escape and close the valve at the first sign of vapor, as indicated product specification results required for compliance with Specification
D1835.
by the first “sputtering” and change in flow behavior of the NOTE 10—It is important to understand that the ullage tube alone does
vented liquid. If no liquid escapes, discard the sample and refill not create the proper vapor phase. It is a tool to assist, along with other
the container. protocols to achieve the desired ullage.
12.1.1.1 The cylinder shall not be stored/transported beyond 12.2 For sampling containers without an internal ullage
80 % of its capacity with sample. Liquid sample shall be tube, the procedure in 11.2.1 may be used.
vented out to the required “reduced fill density” (typically 12.2.1 One acceptable alternative procedure to use is weigh-
80 % or less) prior to transport. ing the sample container immediately after filling, and creating
NOTE 7—Consult the authority having jurisdiction for LPG cylinder the ullage before analysis. The procedure is to completely fill
ullage requirements for transport of LPG sample cylinders. Transportation the sample container using slight overflow indication to ensure
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complete filling. Without warming the sample, immediately 13.2.7 The system is typically set to bypass mode after
weigh the container plus sample on a balance, and record gross sampling is complete.
weight. Carefully drain off liquid from the bottom of the 13.3 Expansion Chamber (Displacement Vessel) Sample
vertically oriented container in an environmentally approved Station:
manner. Then weigh the vented container, and using the tare 13.3.1 Often referred to as an expansion chamber design, it
weight of the container, estimate the ullage of the sample in the is more of a displacement vessel to create the required ullage.
container. Repeat the venting and weighing procedures to This system contains another cylinder as part of the system.
obtain 22 % 6 2 % ullage of the sample. When utilizing this The size of this second cylinder shall be sized to provide the
procedure, it is important that the scale used for weighing is required ullage amount. The size should take into consideration
calibrated and working properly. both the volume of the sample cylinder and the volume of
certain pieces of tubing in the system.
13. Closed-Loop Sample Stations 13.3.2 The expansion chamber sample station is appropriate
13.1 It is often desired to keep the entire collection process when the sample material is not compatible with the sight glass
as a closed-loop system. material, rendering the sight glass station unusable.
13.1.1 There are multiple designs employed as closed-loop 13.3.3 For this design, position the valve according to the
systems, with two common designs being the Sight Glass cylinder as referenced in Section 10.
Sample Station and the Expansion Chamber Sample Station. 13.3.4 When the cylinder is purged, position the valve
Closed-loop sample stations can be of standard design but are according to the procedural step to start the purge and liquid
often designed locally, with both intended to allow for the safe begins flowing through the system and can be observed with a
collection of a representative sample from a given sample flow indicator.
point. 13.3.5 Once purging is complete, the cylinder is essentially
13.1.1.1 Each sample station shall have explicit written filled liquid full, meaning it has no ullage after filling.
directions to describe all steps required to safely collect a 13.3.6 Procedural steps are then followed to position valves
representative sample. If possible, the directions should be to allow for displacement and expansion of liquid material to
affixed to a plate on the mounting panel for the sample station. create a vapor space in the sample cylinder for the required
13.1.2 Closed-loop systems are typically designed to allow ullage.
for purging, filling, and creating the proper ullage via proce- 13.3.7 Once the proper ullage is reached, close the valves on
dural steps. the cylinder. Vent the rest of the system to flare or other
13.1.3 They typically include a bypass line to keep material designated safe location to remove material and pressure from
flowing to/from the sample point to the return point. As this the lines before disconnecting.
constant flow keeps the sample lines purged, this reduces the 13.3.8 The system is typically set to bypass mode after
amount of purging needed to the tubing/connections that are sampling is complete.
not part of the sample line directed to the bypass line and the NOTE 11—When the term “expansion room” is used, this is synony-
sample cylinder. This can reduce the amount of time required mous with ullage, as it refers to the vapor space to allow for thermal
for purging. expansion. When “expansion chamber” is used, this refers to a vessel that
is part of a certain closed-loop sample station design.
13.2 Sight Glass Sample Station:
13.2.1 For this design, the cylinder is connected in the 14. Checking for Leaks
upright position, and the material is purged through the
cylinder as referenced in Section 10. 14.1 After eliminating the excess liquid sample so that only
13.2.2 The valving is usually lined up with the stream on 80 % or less of the liquid sample remains, if leaks are
bypass. When the cylinder is purged, the valve can be suspected, immerse in a water bath and check the sample
positioned according to the procedural step to start the purge cylinder for leaks. If a leak is detected at any time during the
and liquid begins flowing through the system and can be sampling operation, discard the sample. Repair or replace the
observed with a flow indicator, which can also be part of the leaky container before obtaining another sample. Alternate
sight glass. procedures such as use of soap/water leak detection fluid, leak
13.2.3 The sight glass becomes completely filled during the detection instruments or recording of total cylinder weights
purging and sampling steps. may also be used to detect leaks.
13.2.4 Once purging is complete, the cylinder is essentially 14.1.1 Leak checks are to be performed prior to first use,
filled liquid full, meaning it has no ullage after filling. after any maintenance, and at a minimum annually by pressur-
13.2.5 Procedural steps are then followed to position valves izing the cylinder to a minimum of 2758 kPa (400 psig) with
to allow for venting part of the liquid to flare or approved safe inert gas, followed by immersing the cylinder fittings in a
location until the liquid level in the sight glass drops to the container of water.
location of the bottom of the ullage tube in the cylinder. This
results in creating the proper ullage. 15. Care of Samples and Sample Containers
13.2.6 Once the proper ullage is reached, close the valves on 15.1 Place samples in a cool location as soon as possible.
the cylinder. Vent the rest of the system to flare or other Keep them there until all tests have been completed. Discard
designated safe location to remove material and pressure from any samples in containers which develop leaks. Protect the
the lines before disconnecting. valves on the sample container, either by packing the container
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in a crate in an approved manner or by using a protective cap, 16. Keywords
so that accidental unseating of the valve or tampering with it is 16.1 liquefied petroleum gases; LPG; sampling
avoided.
15.2 When shipping cylinders that contain LPG materials
within the U.S., metal pressure relief devices are required per
U.S. 49 CFR. Cylinders must be plugged on each end for
shipping.
SUMMARY OF CHANGES
Subcommittee D02.H0 has identified the location of selected changes to this standard since the last issue
(D1265 – 22) that may impact the use of this standard. (Approved March 1, 2023.)
(1) Updated Section 1. (7) Updated Figs. 1 and 2, and added Fig. 3.
(2) Updated U.S. 49 CFR and associated footnote, and added (8) Revised Section 10.
Practice D6849 and API RP 2003 (Section 2). (9) Added to and updated Section 11.
(3) Added terms to Terminology Subsection 3.1. (10) Updated Section 12.
(4) Updated 4.1. (11) Added Section 13.
(5) Updated and added additional subsections to Section 6. (12) Updated Section 14.
(6) Added Interferences Section 7. (13) Added 15.2 to Section 15.
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