ASTM D6596-00(2011)
(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
SIGNIFICANCE AND USE
Ampulization is desirable in order to minimize variability and maximize the integrity of calibration standards or RMs, or both, being used in calibration of analytical instruments and in validation of analytical test methods in round-robin or interlaboratory cross-check programs. This practice is intended to be used when the highest degree of confidence in integrity of a material is desired.
This practice is intended to be used when it is desirable to maintain the long term storage of gasoline and related liquid hydrocarbon RMs, controls, or calibration standards for retain or repository purposes.
This practice may not be applicable to materials that contain high percentages of dissolved gases, or to highly viscous materials, due to the difficulty involved in transferring such materials without encountering losses of components or ensuring sample homogeneity.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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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Standards Content (Sample)
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Designation: D6596 − 00(Reapproved 2011)
Standard Practice for
Ampulization and Storage of Gasoline and Related
Hydrocarbon Materials
This standard is issued under the fixed designation D6596; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.2 ISO Standards:
ISO Guide 30Terms and Definitions Used in Connection
1.1 This practice covers a general guide for the ampuliza-
with Reference Materials
tion and storage of gasoline and related hydrocarbon mixtures
ISO Guide 31Contents of Certificates of Reference Materi-
that are to be used as calibration standards or reference
als
materials. This practice addresses materials, solutions, or
ISOGuide35CertificationofReferenceMaterials–General
mixtures, which may contain volatile components. This prac-
and Statistical Principles
tice is not intended to address the ampulization of highly
ISO/REMCO N280Homogeneity Testing Procedure for the
viscousliquids,materialsthataresolidatroomtemperature,or
Evaluation of Interlaboratory Test Samples
materials that have high percentages of dissolved gases that
2.3 Government Standard:
cannot be handled under reasonable cooling temperatures and
29 CFR 1910.1200Hazard Communication
at normal atmospheric pressure without losses of these volatile
components.
3. Terminology
1.2 This practice is applicable to automated ampule filling
3.1 Definitions:
and sealing machines as well as to manual ampule filling
3.1.1 accepted reference value (ARV)—a value that serves
devices, such as pipettes and hand-operated liquid dispensers.
asanagreed-uponreferenceforcomparisonandthatisderived
1.3 The values stated in SI units are to be regarded as
as: (1) a theoretical or established value, based on scientific
standard. No other units of measurement are included in this
principles; (2) an assigned value, based on experimental work
standard.
of some national or international organization, such as the
National Institute of Standards and Technology (NIST); or (3)
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the a consensus value, based on collaborative experimental work
responsibility of the user of this standard to establish appro- under the auspices of a scientific or engineering group.
priate safety and health practices and determine the applica-
3.1.2 ampule—a glass vessel for the storage of liquid
bility of regulatory limitations prior to use.
materials, possessing a long narrow neck for the purpose of
providing a flame-sealed closure.
2. Referenced Documents
3.1.3 headspace—the unfilled capacity of an ampule that
2.1 ASTM Standards:
allows for physical expansion due to temperature and pressure
D6362Practice for Certificates of Reference Materials for
changesofthefilledmaterialwhilemaintainingtheintegrityof
Water Analysis
the package.
E826Practice for Testing Homogeneity of a Metal Lot or
3.1.4 homogeneity—the uniformity of the characteristics of
Batch in Solid Form by Spark Atomic Emission Spec-
the packaged material across the entire packaging run deter-
trometry
mined for the purpose of demonstrating the suitability of the
batch for its intended purpose.
3.1.4.1 Discussion—There are two homogeneity testing
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum
cases; one in which the material is ampulized as a reference
ProductsandLubricantsandisthedirectresponsibilityofSubcommitteeD02.04.0A
material at the time of ampulization, and one in which the
on Preparation of Standard Hydrocarbon Blends.
Current edition approved May 1, 2011. Published May 2011. Originally
approved in 2000. Last previous edition approved in 2005 as D6596–00 (2005).
DOI: 10.1520/D6596-00R11. Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4th Floor, New York, NY 10036, http://www.ansi.org.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6596 − 00 (2011)
material is not. may negatively impact the quality, consistency, and value of
(1) reference material at time of ampulization—The the ampulized material as an RM.
material to be ampulized is a reference material that has
4.3 Confidence in the homogeneity of the ampulized prod-
accepted true or consensus values. Ampulization of a refer-
uct can only be established through homogeneity testing,
ence material would require homogeneity testing in order to
whichinvolvesthesampling,analysis,andstatisticaltreatment
assess the variability caused by the ampulization process on
of data from randomly selected ampules obtained from the
the true or consensus values for the reference material.
beginning, middle, and end of the ampulized lot. Determina-
(2) not a reference material at time of ampulization—The
tion of ampulization homogeneity requires that the order in
material to be ampulized is not a reference material at the
which the ampules have been filled and sealed be maintained.
timeofampulizationbutisintendedtohavecharacterization
Homogeneity testing reveals the variability of the product
and assignment of true or consensus values at some future
introduced during the ampulization process. Homogeneity
date. Rigid homogeneity testing is not required on such a
results must be within acceptable limits of the ARV or
material at the time of ampulization since the true or
consensus value for the RM.
consensus values have not yet been determined. However,
4.4 Ampulization does not necessarily guarantee sample
ampules must be retained at the beginning, middle, and end
stability or indefinite shelf life of the RM. Initial homogeneity
of the ampulization process. It is recommended that quali-
data establish reference values for future tests of sample
tativetestingbedoneonatleastonesamplefromeachofthe
stability and determination of shelf life.
beginning,middle,andendoftheampulizationprocess.The
remaining ampules should then be retained for future homo-
5. Significance and Use
geneity testing to determine quantitative or consensus val-
5.1 Ampulization is desirable in order to minimize variabil-
ues.
ityandmaximizetheintegrityofcalibrationstandardsorRMs,
3.1.5 reference material (RM)—a material or substance of
or both, being used in calibration of analytical instruments and
which one or more properties are sufficiently well established
in validation of analytical test methods in round-robin or
to enable the material to be used for the calibration of an
interlaboratorycross-checkprograms.Thispracticeisintended
apparatus, the assessment of a method, or the assignment of
tobeusedwhenthehighestdegreeofconfidenceinintegrityof
values to similar materials.
a material is desired.
3.1.6 shelf life—the period of time, under specified storage
5.2 This practice is intended to be used when it is desirable
conditions, for which the RM will possess the same properties
tomaintainthelongtermstorageofgasolineandrelatedliquid
or true values, within established acceptance limits.
hydrocarbon RMs, controls, or calibration standards for retain
3.1.7 stability testing—tests required to demonstrate the
or repository purposes.
chemical stability of the ampulized RM for the purpose of
5.3 This practice may not be applicable to materials that
determining the shelf life of the RM.
contain high percentages of dissolved gases, or to highly
viscous materials, due to the difficulty involved in transferring
4. Summary of Practice
such materials without encountering losses of components or
4.1 The physical and chemical characteristics (for example,
ensuring sample homogeneity.
volatility,reactivity,flammability,andsoforth)ofagasolineor
related hydrocarbon mixture is first assessed to determine the
6. Procedure
appropriate procedures for sample handling, sample transfer,
6.1 Manual Ampule Filling and Sealing:
and ampulization. Then a uniform quantity of gasoline or
6.1.1 Apparatus—Devices used for manual filling of am-
hydrocarbon mixture is dispensed into suitably sized glass
pules include glass pipettes as well as other types of commer-
ampules (purged with an inert gas), and the ampules are
cially available hand-operated, mechanical, liquid-dispensing
flame-sealed with a torch.Anumber of ampules from through-
devices.
out the filling and sealing process are selected and tested by
6.1.2 Storage of Bulk Material—Bulk gasoline and similar
appropriate test methods to determine homogeneity across the
liquid hydrocarbon materials must be adequately sealed and
lot. Additional ampules are retained for later testing to deter-
stored to prevent loss of volatile components prior to ampuli-
mine stability and shelf life.
zation. Refrigerated storage in sealed metal drums, barrels, or
4.2 This practice addresses the common difficulties associ- amber glass containers is recommended.
ated with the ampulization and storage of gasoline and similar 6.1.3 Compatibility of Materials/Sources of Contamination:
liquid hydrocarbon materials, which may contain volatile 6.1.3.1 MaterialsthatcomeincontactwiththebulkRMand
components. The process of ampulization, whether performed its vapors during dispensing must be compatible with the
using manual or automated equipment, involves the same gasoline or hydrocarbon material. Glass pipettes are recom-
fundamental issues, namely, assessment of the characteristics mended. Plastic or rubber materials containing phthalates or
of the material to be ampulized, sources of contamination, other types of plasticizers must be avoided.
sampling of the bulk container, volume dispensing accuracy, 6.1.3.2 Any part of the dispensing device that comes in
inert atmosphere blanketing, flame sealing, sequential ampule contact with the material, including glass pipettes, hand dis-
labeling, packaging homogeneity sampling, and homogeneity pensers, and any necessary connection hardware, must be
testing. Failure to adequately consider any of the above issues cleaned prior to packaging a different material. Recommended
D6596 − 00 (2011)
cleaning procedures involve soaking parts in soapy water, 6.1.6.3 If using graduated pipettes, introduce a sufficient
rinsing with clean water, followed by methanol or other volume of material to the ampule to meet the minimum
suitable solvent, followed by drying under a stream of clean dispensing volume requirements for packaging the RM. Note
nitrogen. that the final dispensed volume at room temperature will be
affected by the bulk material temperature at the time of
6.1.4 Assessment of Material to Be Ampulized:
dispensing. Therefore, for consistent volume dispensing, the
6.1.4.1 Volatility—Prior to packaging, materials containing
temperature of the bulk material must be known and must be
highly volatile components must be cooled sufficiently to
kept constant during the entire dispensing process.
minimize volatile losses during ampulization. Failure to suffi-
6.1.6.4 If other types of nongraduated, manual, filling de-
ciently cool the material also may result in difficulty in
vices are being used, they must be calibrated. Using Class A
obtaining effective ampule sealing. The material must not be
glassware or pipettes, measure into an ampule a volume of
cooled to temperatures below which the composition of the
room temperature water equal to the volume of RM to be
RMwouldbeaffected(forexample,producingprecipitationor
dispensed. Mark the level on the ampule.
solidification). Gasoline may be cooled to –20°C without
6.1.6.5 Make adjustments to the manual dispensing device
incurring compositional changes. The bulk material must be
until 50 consecutive ampules are consistently filled to the
kept cold during the filling process.
predetermined mark on the ampule.
6.1.4.2 Reactivity—Consideration should be given to the
6.1.6.6 Once volume dispensing adjustments have been
chemical reactivity of the RM being packaged. Gasoline
completed,beginfillingampulesfromthebulksupply,keeping
samples containing olefins and diolefins should be packaged
the filled ampules cold by placing them immediately into a
under an inert atmosphere blanket of nitrogen, argon, or other
containerthatisatatemperatureofapproximately–20°C.This
suitable gas. Ampules should be flushed with inert gas imme-
may be achieved by using crushed dry ice.
diately prior to dispensing of the gasoline. Use of amber glass
6.1.6.7 The ampules should be sealed as soon as possible
ampules will minimize photo-oxidation.
afterfillingtoavoidlossofvolatilecomponents.Ifampulesare
6.1.4.3 Odors—Odorous materials such as gasoline should
being manually sealed, a two person operation, in which one
bepackagedinawell-ventilatedarea.Thebulkmaterialshould
person dispenses the material and a second person seals the
be kept adequately sealed during the ampulization process to
ampules, is suggested.
minimize loss of volatiles.
6.1.6.8 Periodically inspect filled and sealed ampules to
6.1.4.4 Flammability—Ampule sealing requires use of a
ensure that the fill volume is maintained throughout the
flame hot enough to melt glass. Care must be taken in
packaging run.
ampulization of highly flammable materials since ampule
6.1.7 Ampule Sealing:
contents could ignite. Ampules must be kept cold through the
6.1.7.1 Ampules may be flame-sealed by hand, using a
sealing step. However, care should be taken to avoid, as much
suitable torch. The flame used must be hot enough to quickly
as possible, condensation of water inside the ampule. Ampu-
soften the neck of the ampule. Propane/air or natural gas/air
lization is best carried out when the room humidity is low.
flames are sufficient for most applications. Hydrogen/oxygen
6.1.5 Sampling of the Bulk Container:
flames may be required for sealing large, thick-walled glass
6.1.5.1 After bringing the bulk container temperature down
ampules.
to the working temperature, withdraw a minimum of three
6.1.7.2 The ampule should be kept cold through the sealing
samplesfromeachbulkcontainer,usingcleanmanualpipettes.
process.
Immediately dispense the material into crimp top chromatog-
6.1.7.3 Tofacilitatesealing,thetorchshouldbemountedon
raphy vials, seal, and label. These samples will be designated
a stand on a bench top such th
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