ASTM D6596-00
(Practice)Standard Practice for Ampulization and Storage of Gasoline and Related Hydrocarbon Materials
Standard Practice for Ampulization and Storage of Gasoline and Related Hydrocarbon Materials
SCOPE
1.1 This practice covers a general guide for the ampulization and storage of gasoline and related hydrocarbon mixtures that are to be used as calibration standards or reference materials. This practice addresses materials, solutions, or mixtures, which may contain volatile components. This practice is not intended to address the ampulization of highly viscous liquids, materials that are solid at room temperature, or materials that have high percentages of dissolved gases that cannot be handled under reasonable cooling temperatures and at normal atmospheric pressure without losses of these volatile components.
1.2 This practice is applicable to automated ampule filling and sealing machines as well as to manual ampule filling devices, such as pipettes and hand-operated liquid dispensers.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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An American National Standard
Designation:D6596–00
Standard Practice for
Ampulization and Storage of Gasoline and Related
Hydrocarbon Materials
This standard is issued under the fixed designation D 6596; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope Evaluation of Interlaboratory Test Samples
2.3 Government Standard:
1.1 This practice covers a general guide for the ampuliza-
29 CFR 1910.1200 Hazard Communication
tion and storage of gasoline and related hydrocarbon mixtures
that are to be used as calibration standards or reference
3. Terminology
materials. This practice addresses materials, solutions, or
3.1 Definitions:
mixtures, which may contain volatile components. This prac-
3.1.1 accepted reference value (ARV)—a value that serves
tice is not intended to address the ampulization of highly
as an agreed-upon reference for comparison and that is derived
viscous liquids, materials that are solid at room temperature, or
as: (1) a theoretical or established value, based on scientific
materials that have high percentages of dissolved gases that
principles; (2) an assigned value, based on experimental work
cannot be handled under reasonable cooling temperatures and
of some national or international organization, such as the
at normal atmospheric pressure without losses of these volatile
National Institute of Standards and Technology (NIST); or (3)
components.
a consensus value, based on collaborative experimental work
1.2 This practice is applicable to automated ampule filling
under the auspices of a scientific or engineering group.
and sealing machines as well as to manual ampule filling
3.1.2 ampule—a glass vessel for the storage of liquid
devices, such as pipettes and hand-operated liquid dispensers.
materials, possessing a long narrow neck for the purpose of
1.3 This standard does not purport to address all of the
providing a flame-sealed closure.
safety concerns, if any, associated with its use. It is the
3.1.3 headspace—the unfilled capacity of an ampule that
responsibility of the user of this standard to establish appro-
allows for physical expansion due to temperature and pressure
priate safety and health practices and determine the applica-
changesofthefilledmaterialwhilemaintainingtheintegrityof
bility of regulatory limitations prior to use.
the package.
2. Referenced Documents 3.1.4 homogeneity—the uniformity of the characteristics of
the packaged material across the entire packaging run deter-
2.1 ASTM Standards:
mined for the purpose of demonstrating the suitability of the
D 6362 Practice for Certificates of Reference Fuels for
batch for its intended purpose.
Water Analysis
3.1.4.1 Discussion—There are two homogeneity testing
E 826 Practice for Testing Homogeneity of Materials for
cases; one in which the material is ampulized as a reference
Development of Reference Materials
4 material at the time of ampulization, and one in which the
2.2 ISO Standards:
material is not.
ISO Guide 30 Terms and Definitions Used in Connection
with Reference Materials
(1) reference material at time of ampulization—The material to be
ISO Guide 31 Contents of Certificates of Reference Mate- ampulized is a reference material that has accepted true or consensus
values. Ampulization of a reference material would require homoge-
rials
neity testing in order to assess the variability caused by the ampuliza-
ISO Guide 35 Certification of Reference Materials – Gen-
tion process on the true or consensus values for the reference material.
eral and Statistical Principles
(2) not a reference material at time of ampulization—Thematerialto
ISO/REMCO N280 Homogeneity Testing Procedure for the
be ampulized is not a reference material at the time of ampulization but
is intended to have characterization and assignment of true or consen-
sus values at some future date. Rigid homogeneity testing is not
This test method is under the jurisdiction of ASTM Committee D02 on
required on such a material at the time of ampulization since the true or
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
consensus values have not yet been determined. However, ampules
D02.04 on Hydrocarbon Analysis.
must be retained at the beginning, middle, and end of the ampulization
Current edition approved Dec. 10, 2000. Published February 2001.
Annual Book of ASTM Standards, Vol 05.04.
Annual Book of ASTM Standards, Vol 03.06.
4 th 5
Available from American National Standards Institute, 11 W 42nd Street, 13 Available from Superintendent of Documents, U.S. Government Printing
Floor, New York, NY 10017. Office, Washington, D.C. 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6596
process. It is recommended that qualitative testing be done on at least
5. Significance and Use
one sample from each of the beginning, middle, and end of the
5.1 Ampulization is desirable in order to minimize variabil-
ampulization process. The remaining ampules should then be retained
ity and maximize the integrity of calibration standards or RMs,
for future homogeneity testing to determine quantitative or consensus
or both, being used in calibration of analytical instruments and
values.
in validation of analytical test methods in round-robin or
3.1.5 reference material (RM)—a material or substance of
interlaboratory cross-check programs.This practice is intended
which one or more properties are sufficiently well established
tobeusedwhenthehighestdegreeofconfidenceinintegrityof
to enable the material to be used for the calibration of an
a material is desired.
apparatus, the assessment of a method, or the assignment of
5.2 This practice is intended to be used when it is desirable
values to similar materials.
to maintain the long term storage of gasoline and related liquid
3.1.6 shelf life—the period of time, under specified storage
hydrocarbon RMs, controls, or calibration standards for retain
conditions, for which the RM will possess the same properties
or repository purposes.
or true values, within established acceptance limits.
5.3 This practice may not be applicable to materials that
3.1.7 stability testing—tests required to demonstrate the
contain high percentages of dissolved gases, or to highly
chemical stability of the ampulized RM for the purpose of
viscous materials, due to the difficulty involved in transferring
determining the shelf life of the RM.
such materials without encountering losses of components or
ensuring sample homogeneity.
4. Summary of Practice
6. Procedure
4.1 The physical and chemical characteristics (for example,
volatility,reactivity,flammability,andsoforth)ofagasolineor
6.1 Manual Ampule Filling and Sealing:
related hydrocarbon mixture is first assessed to determine the
6.1.1 Apparatus—Devices used for manual filling of am-
appropriate procedures for sample handling, sample transfer,
pules include glass pipettes as well as other types of commer-
and ampulization. Then a uniform quantity of gasoline or
cially available hand-operated, mechanical, liquid-dispensing
hydrocarbon mixture is dispensed into suitably sized glass
devices.
ampules (purged with an inert gas), and the ampules are
6.1.2 Storage of Bulk Material—Bulk gasoline and similar
flame-sealed with a torch.Anumber of ampules from through-
liquid hydrocarbon materials must be adequately sealed and
out the filling and sealing process are selected and tested by
stored to prevent loss of volatile components prior to ampuli-
appropriate test methods to determine homogeneity across the
zation. Refrigerated storage in sealed metal drums, barrels, or
lot. Additional ampules are retained for later testing to deter-
amber glass containers is recommended.
mine stability and shelf life.
6.1.3 Compatibility of Materials/Sources of Contamination:
4.2 This practice addresses the common difficulties associ-
6.1.3.1 MaterialsthatcomeincontactwiththebulkRMand
ated with the ampulization and storage of gasoline and similar
its vapors during dispensing must be compatible with the
liquid hydrocarbon materials, which may contain volatile
gasoline or hydrocarbon material. Glass pipettes are recom-
components. The process of ampulization, whether performed
mended. Plastic or rubber materials containing phthalates or
using manual or automated equipment, involves the same
other types of plasticizers must be avoided.
fundamental issues, namely, assessment of the characteristics
6.1.3.2 Any part of the dispensing device that comes in
of the material to be ampulized, sources of contamination,
contact with the material, including glass pipettes, hand dis-
sampling of the bulk container, volume dispensing accuracy,
pensers, and any necessary connection hardware, must be
inert atmosphere blanketing, flame sealing, sequential ampule
cleaned prior to packaging a different material. Recommended
labeling, packaging homogeneity sampling, and homogeneity
cleaning procedures involve soaking parts in soapy water,
testing. Failure to adequately consider any of the above issues
rinsing with clean water, followed by methanol or other
may negatively impact the quality, consistency, and value of
suitable solvent, followed by drying under a stream of clean
the ampulized material as an RM.
nitrogen.
4.3 Confidence in the homogeneity of the ampulized prod-
6.1.4 Assessment of Material to Be Ampulized:
uct can only be established through homogeneity testing,
6.1.4.1 Volatility—Prior to packaging, materials containing
which involves the sampling, analysis, and statistical treatment
highly volatile components must be cooled sufficiently to
of data from randomly selected ampules obtained from the
minimize volatile losses during ampulization. Failure to suffi-
beginning, middle, and end of the ampulized lot. Determina-
ciently cool the material also may result in difficulty in
tion of ampulization homogeneity requires that the order in obtaining effective ampule sealing. The material must not be
which the ampules have been filled and sealed be maintained.
cooled to temperatures below which the composition of the
Homogeneity testing reveals the variability of the product
RM would be affected (for example, producing precipitation or
introduced during the ampulization process. Homogeneity
solidification). Gasoline may be cooled to –20°C without
results must be within acceptable limits of the ARV or
incurring compositional changes. The bulk material must be
consensus value for the RM.
kept cold during the filling process.
4.4 Ampulization does not necessarily guarantee sample 6.1.4.2 Reactivity—Consideration should be given to the
stability or indefinite shelf life of the RM. Initial homogeneity chemical reactivity of the RM being packaged. Gasoline
data establish reference values for future tests of sample samples containing olefins and diolefins should be packaged
stability and determination of shelf life. under an inert atmosphere blanket of nitrogen, argon, or other
D6596
suitable gas. Ampules should be flushed with inert gas imme- container that is at a temperature of approximately –20°C.This
diately prior to dispensing of the gasoline. Use of amber glass may be achieved by using crushed dry ice.
ampules will minimize photo-oxidation.
6.1.6.7 The ampules should be sealed as soon as possible
6.1.4.3 Odors—Odorous materials such as gasoline should afterfillingtoavoidlossofvolatilecomponents.Ifampulesare
bepackagedinawell-ventilatedarea.Thebulkmaterialshould being manually sealed, a two person operation, in which one
be kept adequately sealed during the ampulization process to person dispenses the material and a second person seals the
minimize loss of volatiles. ampules, is suggested.
6.1.4.4 Flammability—Ampule sealing requires use of a 6.1.6.8 Periodically inspect filled and sealed ampules to
flame hot enough to melt glass. Care must be taken in ensure that the fill volume is maintained throughout the
ampulization of highly flammable materials since ampule packaging run.
contents could ignite. Ampules must be kept cold through the
6.1.7 Ampule Sealing:
sealing step. However, care should be taken to avoid, as much
6.1.7.1 Ampules may be flame-sealed by hand, using a
as possible, condensation of water inside the ampule. Ampu-
suitable torch. The flame used must be hot enough to quickly
lization is best carried out when the room humidity is low.
soften the neck of the ampule. Propane/air or natural gas/air
6.1.5 Sampling of the Bulk Container:
flames are sufficient for most applications. Hydrogen/oxygen
6.1.5.1 After bringing the bulk container temperature down flames may be required for sealing large, thick-walled glass
to the working temperature, withdraw a minimum of three ampules.
samples from each bulk container, using clean manual pipettes.
6.1.7.2 The ampule should be kept cold through the sealing
Immediately dispense the material into crimp top chromatog-
process.
raphy vials, seal, and label. These samples will be designated
6.1.7.3 To facilitate sealing, the torch should be mounted on
as representative of the bulk material and will be used to
a stand on a bench top such that both hands can be free to
establish reference values for the homogeneity testing.
perform the actual sealing process.
6.1.5.2 Some vial closures are not suitable for hydrocarbon
6.1.7.4 Wearing gloves, hold the ampule by the bottom in
analyses, such as uncoated silicone rubber. Only TFE-
one hand and by the neck tip in the other. Alternatively, large
fluorocarbon-coated closures should be used. In addition, the
tongs may be used to hold the neck in order to minimize the
vials should be analyzed as soon as is practical, since no
risk. The ampule neck is placed into the flame, constantly
crimped vial is completely leak free.
rotating to ensure uniform heating of the glass. Focus the flame
6.1.6 Adjusting Dispensing Volume:
midway between the open end and the breakmark on the
6.1.6.1 Typically, it is more important to provide a mini- ampule. The flame should never contact the contents of the
mum dispensed volume in the ampule rather than to provide an ampule or the direct open end of the ampule. (Warning—For
accurately determined volume of RM. The minimum dispens- safety reasons, if the material being ampulized is flammable, it
ing volume for packaging the RM must be known ahead of is recommended that the volume being ampulized be mini-
time. mized.)
6.1.6.2 Introduce an inert atmosphere into the ampule by 6.1.7.5 After several seconds of exposure to the flame, the
purg
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