1、Designation: D6596 00 (Reapproved 2011)Standard Practice forAmpulization and Storage of Gasoline and RelatedHydrocarbon Materials1This standard is issued under the fixed designation D6596; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers a general guide for the ampuliza-tion and storage of gasoline and related hydro
3、carbon mixturesthat are to be used as calibration standards or referencematerials. This practice addresses materials, solutions, ormixtures, which may contain volatile components. This prac-tice is not intended to address the ampulization of highlyviscous liquids, materials that are solid at room te
4、mperature, ormaterials that have high percentages of dissolved gases thatcannot be handled under reasonable cooling temperatures andat normal atmospheric pressure without losses of these volatilecomponents.1.2 This practice is applicable to automated ampule fillingand sealing machines as well as to
5、manual ampule fillingdevices, such as pipettes and hand-operated liquid dispensers.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated w
6、ith its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D6362 Practice for Certificates of Reference Materials forWater A
7、nalysisE826 Practice for Testing Homogeneity of a Metal Lot orBatch in Solid Form by Spark Atomic Emission Spectrom-etry2.2 ISO Standards:3ISO Guide 30 Terms and Definitions Used in Connectionwith Reference MaterialsISO Guide 31 Contents of Certificates of Reference Mate-rialsISO Guide 35 Certificat
8、ion of Reference Materials Gen-eral and Statistical PrinciplesISO/REMCO N280 Homogeneity Testing Procedure for theEvaluation of Interlaboratory Test Samples2.3 Government Standard:429 CFR 1910.1200 Hazard Communication3. Terminology3.1 Definitions:3.1.1 accepted reference value (ARV)a value that ser
9、vesas an agreed-upon reference for comparison and that is derivedas: (1) a theoretical or established value, based on scientificprinciples; (2) an assigned value, based on experimental workof some national or international organization, such as theNational Institute of Standards and Technology (NIST
10、); or (3)a consensus value, based on collaborative experimental workunder the auspices of a scientific or engineering group.3.1.2 ampulea glass vessel for the storage of liquidmaterials, possessing a long narrow neck for the purpose ofproviding a flame-sealed closure.3.1.3 headspacethe unfilled capa
11、city of an ampule thatallows for physical expansion due to temperature and pressurechanges of the filled material while maintaining the integrity ofthe package.3.1.4 homogeneitythe uniformity of the characteristics ofthe packaged material across the entire packaging run deter-mined for the purpose o
12、f demonstrating the suitability of thebatch for its intended purpose.3.1.4.1 DiscussionThere are two homogeneity testingcases; one in which the material is ampulized as a referencematerial at the time of ampulization, and one in which thematerial is not.(1) reference material at time of ampulization
13、The material to beampulized is a reference material that has accepted true or consensus1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.04.0Aon Preparation of Standard Hydrocarbon Blends.Current ed
14、ition approved May 1, 2011. Published May 2011. Originallyapproved in 2000. Last previous edition approved in 2005 as D659600 (2005).DOI: 10.1520/D6596-00R11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of A
15、STMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Available from U.S. Government Printing Office Superintendent of Documents,
16、732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.values. Ampulization of a reference material would require homoge-neity testing in order to assess
17、 the variability caused by the ampuliza-tion process on the true or consensus values for the reference material.(2) not a reference material at time of ampulizationThe material tobe ampulized is not a reference material at the time of ampulization butis intended to have characterization and assignme
18、nt of true or consen-sus values at some future date. Rigid homogeneity testing is notrequired on such a material at the time of ampulization since the true orconsensus values have not yet been determined. However, ampulesmust be retained at the beginning, middle, and end of the ampulizationprocess.
19、It is recommended that qualitative testing be done on at leastone sample from each of the beginning, middle, and end of theampulization process. The remaining ampules should then be retainedfor future homogeneity testing to determine quantitative or consensusvalues.3.1.5 reference material (RM)a mat
20、erial or substance ofwhich one or more properties are sufficiently well establishedto enable the material to be used for the calibration of anapparatus, the assessment of a method, or the assignment ofvalues to similar materials.3.1.6 shelf lifethe period of time, under specified storageconditions,
21、for which the RM will possess the same propertiesor true values, within established acceptance limits.3.1.7 stability testingtests required to demonstrate thechemical stability of the ampulized RM for the purpose ofdetermining the shelf life of the RM.4. Summary of Practice4.1 The physical and chemi
22、cal characteristics (for example,volatility, reactivity, flammability, and so forth) of a gasoline orrelated hydrocarbon mixture is first assessed to determine theappropriate procedures for sample handling, sample transfer,and ampulization. Then a uniform quantity of gasoline orhydrocarbon mixture i
23、s dispensed into suitably sized glassampules (purged with an inert gas), and the ampules areflame-sealed with a torch. A number of ampules from through-out the filling and sealing process are selected and tested byappropriate test methods to determine homogeneity across thelot. Additional ampules ar
24、e retained for later testing to deter-mine stability and shelf life.4.2 This practice addresses the common difficulties associ-ated with the ampulization and storage of gasoline and similarliquid hydrocarbon materials, which may contain volatilecomponents. The process of ampulization, whether perfor
25、medusing manual or automated equipment, involves the samefundamental issues, namely, assessment of the characteristicsof the material to be ampulized, sources of contamination,sampling of the bulk container, volume dispensing accuracy,inert atmosphere blanketing, flame sealing, sequential ampulelabe
26、ling, packaging homogeneity sampling, and homogeneitytesting. Failure to adequately consider any of the above issuesmay negatively impact the quality, consistency, and value ofthe ampulized material as an RM.4.3 Confidence in the homogeneity of the ampulized prod-uct can only be established through
27、homogeneity testing,which involves the sampling, analysis, and statistical treatmentof data from randomly selected ampules obtained from thebeginning, middle, and end of the ampulized lot. Determina-tion of ampulization homogeneity requires that the order inwhich the ampules have been filled and sea
28、led be maintained.Homogeneity testing reveals the variability of the productintroduced during the ampulization process. Homogeneityresults must be within acceptable limits of the ARV orconsensus value for the RM.4.4 Ampulization does not necessarily guarantee samplestability or indefinite shelf life
29、 of the RM. Initial homogeneitydata establish reference values for future tests of samplestability and determination of shelf life.5. Significance and Use5.1 Ampulization is desirable in order to minimize variabil-ity and maximize the integrity of calibration standards or RMs,or both, being used in
30、calibration of analytical instruments andin validation of analytical test methods in round-robin orinterlaboratory cross-check programs. This practice is intendedto be used when the highest degree of confidence in integrity ofa material is desired.5.2 This practice is intended to be used when it is
31、desirableto maintain the long term storage of gasoline and related liquidhydrocarbon RMs, controls, or calibration standards for retainor repository purposes.5.3 This practice may not be applicable to materials thatcontain high percentages of dissolved gases, or to highlyviscous materials, due to th
32、e difficulty involved in transferringsuch materials without encountering losses of components orensuring sample homogeneity.6. Procedure6.1 Manual Ampule Filling and Sealing:6.1.1 ApparatusDevices used for manual filling of am-pules include glass pipettes as well as other types of commer-cially avai
33、lable hand-operated, mechanical, liquid-dispensingdevices.6.1.2 Storage of Bulk MaterialBulk gasoline and similarliquid hydrocarbon materials must be adequately sealed andstored to prevent loss of volatile components prior to ampuli-zation. Refrigerated storage in sealed metal drums, barrels, orambe
34、r glass containers is recommended.6.1.3 Compatibility of Materials/Sources of Contamination:6.1.3.1 Materials that come in contact with the bulk RM andits vapors during dispensing must be compatible with thegasoline or hydrocarbon material. Glass pipettes are recom-mended. Plastic or rubber material
35、s containing phthalates orother types of plasticizers must be avoided.6.1.3.2 Any part of the dispensing device that comes incontact with the material, including glass pipettes, hand dis-pensers, and any necessary connection hardware, must becleaned prior to packaging a different material. Recommend
36、edcleaning procedures involve soaking parts in soapy water,rinsing with clean water, followed by methanol or othersuitable solvent, followed by drying under a stream of cleannitrogen.6.1.4 Assessment of Material to Be Ampulized:6.1.4.1 VolatilityPrior to packaging, materials containinghighly volatil
37、e components must be cooled sufficiently tominimize volatile losses during ampulization. Failure to suffi-ciently cool the material also may result in difficulty inobtaining effective ampule sealing. The material must not becooled to temperatures below which the composition of theD6596 00 (2011)2RM
38、would be affected (for example, producing precipitation orsolidification). Gasoline may be cooled to 20C withoutincurring compositional changes. The bulk material must bekept cold during the filling process.6.1.4.2 ReactivityConsideration should be given to thechemical reactivity of the RM being pac
39、kaged. Gasolinesamples containing olefins and diolefins should be packagedunder an inert atmosphere blanket of nitrogen, argon, or othersuitable gas. Ampules should be flushed with inert gas imme-diately prior to dispensing of the gasoline. Use of amber glassampules will minimize photo-oxidation.6.1
40、.4.3 OdorsOdorous materials such as gasoline shouldbe packaged in a well-ventilated area. The bulk material shouldbe kept adequately sealed during the ampulization process tominimize loss of volatiles.6.1.4.4 FlammabilityAmpule sealing requires use of aflame hot enough to melt glass. Care must be ta
41、ken inampulization of highly flammable materials since ampulecontents could ignite. Ampules must be kept cold through thesealing step. However, care should be taken to avoid, as muchas possible, condensation of water inside the ampule. Ampu-lization is best carried out when the room humidity is low.
42、6.1.5 Sampling of the Bulk Container:6.1.5.1 After bringing the bulk container temperature downto the working temperature, withdraw a minimum of threesamples from each bulk container, using clean manual pipettes.Immediately dispense the material into crimp top chromatog-raphy vials, seal, and label.
43、 These samples will be designatedas representative of the bulk material and will be used toestablish reference values for the homogeneity testing.6.1.5.2 Some vial closures are not suitable for hydrocarbonanalyses, such as uncoated silicone rubber. Only TFE-fluorocarbon-coated closures should be use
44、d. In addition, thevials should be analyzed as soon as is practical, since nocrimped vial is completely leak free.6.1.6 Adjusting Dispensing Volume:6.1.6.1 Typically, it is more important to provide a mini-mum dispensed volume in the ampule rather than to provide anaccurately determined volume of RM
45、. The minimum dispens-ing volume for packaging the RM must be known ahead oftime.6.1.6.2 Introduce an inert atmosphere into the ampule bypurging the ampule for a few seconds with nitrogen or otherinert gas immediately prior to filling. A disposable glassdropper connected to a gas source using rubber
46、 tubing providesa convenient way of purging the ampule.6.1.6.3 If using graduated pipettes, introduce a sufficientvolume of material to the ampule to meet the minimumdispensing volume requirements for packaging the RM. Notethat the final dispensed volume at room temperature will beaffected by the bu
47、lk material temperature at the time ofdispensing. Therefore, for consistent volume dispensing, thetemperature of the bulk material must be known and must bekept constant during the entire dispensing process.6.1.6.4 If other types of nongraduated, manual, filling de-vices are being used, they must be
48、 calibrated. Using Class Aglassware or pipettes, measure into an ampule a volume ofroom temperature water equal to the volume of RM to bedispensed. Mark the level on the ampule.6.1.6.5 Make adjustments to the manual dispensing deviceuntil 50 consecutive ampules are consistently filled to thepredeter
49、mined mark on the ampule.6.1.6.6 Once volume dispensing adjustments have beencompleted, begin filling ampules from the bulk supply, keepingthe filled ampules cold by placing them immediately into acontainer that is at a temperature of approximately 20C. Thismay be achieved by using crushed dry ice.6.1.6.7 The ampules should be sealed as soon as possibleafter filling to avoid loss of volatile components. If ampules arebeing manually sealed, a two person operation, in which oneperson dispenses the material and a second person seals theampules, is suggested.6.1.6
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