1、Designation: D3325 90 (Reapproved 2013)Standard Practice forPreservation of Waterborne Oil Samples1This standard is issued under the fixed designation D3325; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This practice covers the preservation of waterborne oilsamples from the time of collection to the time of analysis.Information is
3、provided to ensure sample integrity and to avoidcontamination and to minimize microbial degradation.1.2 The practice is for controlled field or laboratory condi-tions and specifies thorough preparation of equipment andprecise operation. Where these details must be compromised ina field emergency, no
4、nstandard simplifications are recom-mended that will minimize or eliminate consequent errors.NOTE 1Procedures for the analysis of oil spill samples are PracticesD3326, D3415, D3650, and D4489, and Test Methods D3327, D3328, andD3414. A guide to the use of ASTM test methods for the analysis of oilspi
5、ll samples is found in Practice D3415.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with 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 li
6、mitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD3326 Practice for Preparation of Samples for Identificationof Waterborne OilsD3327 Method for Analysis of Selected Elements in Wart-erborne Oils3D3328 Test Methods for Comparison of Waterborne Petro
7、-leum Oils by Gas ChromatographyD3414 Test Method for Comparison of Waterborne Petro-leum Oils by Infrared SpectroscopyD3415 Practice for Identification of Waterborne OilsD3650 Test Method for Comparison of Waterborne Petro-leum Oils By Fluorescence AnalysisD4489 Practices for Sampling of Waterborne
8、 Oils3. Terminology3.1 DefinitionsFor definitions of terms used in thispractice, refer to Terminology D1129.4. Summary of Practice4.1 Special types of sample containers and shipping con-tainers are recommended. Samples may be of several types: tarballs, collected oil, oil-water mixtures, emulsions,
9、and oil andwater on collecting devices such as silanized glass cloth,TFE-fluorocarbon polymer, or other materials. Instructions aregiven for the care of samples to minimize changes due toautoxidation and microbial attack between the time of sam-pling and the time of analysis. Services available for
10、transpor-tation of samples are described.5. Apparatus5.1 Sample ContainersBorosilicate glass containers thathave been thoroughly cleaned are preferable. All glasscontainers, new or used, must be thoroughly cleaned andwashed prior to use. The cleaning steps consist of an initialwash with a warm aqueo
11、us detergent mixture followed by sixhot tap water rinses, two rinses with reagent water, a rinse withreagent-grade acetone, and a final rinse with a solvent such aspentane, hexane, cyclohexane, dichloromethane, or chloroformfollowed by drying in a clean oven at 105C or hotter for 30min. If the glass
12、ware requires cleaning under field conditions,it should be washed with warm aqueous detergent followed byextensive water rinsing. A solvent rinse with acetone should bemade, if possible, followed by lengthy air drying to removeresidual solvent. (WarningFor safety reasons, the use ofpentane, hexane,
13、or cylcohexane is recommended over use ofdichloromethane or carbon tetrachloride. )NOTE 2Hot reagent water rinses are advisable where hot tap watermight reintroduce contamination.5.1.1 Plastic containers are not acceptable since volatilehydrocarbons diffuse readily through many commercial plasticcon
14、tainers or may be absorbed into the plastic. In addition, theplasticizer may dissolve in the sample causing misleadingresults.1This practice is under the jurisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.06 on Methods for Analysis forOrganic Substances i
15、n Water.Current edition approved Feb. 15, 2013. Published March 2013. Originallyapproved in 1974. Last previous edition approved in 2002 as D3325 90 (2006).DOI: 10.1520/D3325-90R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.or
16、g. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. Unit
17、ed States15.1.2 Metal containers usually should be avoided becausethe nickel and vanadium determinations could be invalidatedby introduction of metal from the can.5.1.3 When field expedients must be employed, an emptycontainer of each type used should be included in the shipmentto the laboratory to
18、be used as a blank to measure inadvertentcontamination.5.2 ClosuresProper choice of closures is critical to avoidcontamination and to preserve sample. Use caps withaluminum-coated or TFE-fluorocarbon-coated cardboard in-serts. Aluminum foil sheet should not be used. Inserts ofTFE-fluorocarbon sheet,
19、 however, are acceptable.5.3 Refrigerator, explosion-proof at about 4 to 5C.5.4 Shipping ContainersSturdy cartons or wooden boxesshould be used. These should be sufficiently large so thesample containers are adequately surrounded by absorbentpacking material, such as vermiculite, sufficient to absor
20、b theentire contents should breakage occur and be lined with agrease proof plastic bag.NOTE 3After Dec. 31, 1990, packagings used for shipment ofdangerous goods such as oil must be tested for compliance with UNPerformance Packaging Standards and certified by a marking applied bythe packaging manufac
21、turer.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Soci-ety.4Other grades may be used
22、, provided it is first ascertainedthat the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.6.2 Acetone.6.3 N-hexane, Mixed Hexanes, Cyclohexane, Pentane,Dichloromethane, or Chloroform, spectroquality or equivalenthigh purity.7. Sampling7.1
23、Collect a representative sample in accordance withPractices D4489.7.2 Sample containers should be carefully prepared asdescribed in 5.1.8. Preservation of Samples8.1 Protection Against AutoxidationTreat the sample con-tainer to displace air and store in a dark area in a refrigerator.Nitrogen or carb
24、on dioxide can be used as inert gases todisplace air.8.2 Protection Against Microbial AttackMaintain refrig-eration (4 to 5C) once samples are received in the laboratory.9. Shipment of Samples9.1 The shipping of oil samples is regulated by bothDepartment of Transportation (DOT) and United States Pos
25、talService regulations.NOTE 4As of Sept. 18, 1988, the U.S. Postal Service regulations wereamended to reflect implementation of the International Civil AviationOrganization (ICAO) Technical Instructions for the Safe Transport ofDangerous Goods by Air. Under these international regulations, thedefini
26、tion of flammable liquid is different from the U.S. DOT definition.Under ICAO rules, a Flammable LiquidClass 3 is defined as a liquidhaving a flashpoint of 141F (60.5C) or less. In addition, the limitedquantity provisions for flammable liquids under U.S. DOT regulations arenot applicable under the I
27、CAO rules.NOTE 5For more information about the legal requirements forpackaging and shipping petroleum oils and other hazardous materials,refer to U.S. Postal Service Publication 52, “Acceptance of Hazardous,Restricted, or Perishable Matter,” the Domestic Mail Manual, Part 124,“Nonmailable MatterArti
28、cles and Substances; Special Mailing Rules,”and the packaging requirements listed in the Domestic Mail Manual, Part121.9.2 Common carriers such as air express or air freight areoften employed for transportaiton of oil spill samples. Consultthe carrier for current packing and labelling requirements.9
29、.3 It is good practice to notify the receiving laboratory ofshipment arrangements.10. Procedure10.1 The prescribed standard procedures for controlled fieldor laboratory conditions and recommended modification foremergency conditions are summarized in Table 1. Use this4Reagent Chemicals, American Che
30、mical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. P
31、harmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Procedures for the Preservation of Waterborne Oil SamplesRecommendedOperationProcedure for EmergencyConditionsProcedures for Controlled Fieldor LaboratorySample containers Borosilicate glass jars for high boiling samples. Borosilicate glass
32、jars for high boiling samples.Cleaning containers Wash with warm aqueous detergent followed bywater rinsing. Rinse with acetone, if available,followed by air drying.Wash with warm aqueous detergent followed with hot tapwater and reagent water rinses. Rinse with acetone,chloroform, and oven dry.Closu
33、res TFE-fluorocarbon sheet or TFE-fluorocarbon oraluminum-coated cardboard inserts.TFE-fluorocarbon sheet or TFE-fluorocarbon oraluminum-coated cardboard inserts.Protection against autoxidation Store in dark. Remove air with nitrogen or cabon dioxide. Store in dark inrefrigerator.Protection against
34、microbial attack Refrigerate to 4 to 5C, if possible. Samples should be stored in laboratory refrigerator at about4to5C.Shipment of samples Pack in ice, if possible, and label appropriately.Notify recipient.Pack in ice, if possible, and label appropriately. Notifyrecipient.D3325 90 (2013)2table with
35、 the specific sections of this practice to choose theproper measures for preservation of the specific waterborneoils under consideration.11. Keywords11.1 identification; oil spill; preservation; sample; shipment;storage; waterborne oilSUMMARY OF CHANGESThis section identifies the location of selecti
36、on changes to this practice that have been incorporated since thelast issue. For the convenience of the user, Committee D-19 has highlighted those changes that may impact theuse of this practice. This section may also include descriptions of the changes or reasons for the changes or both.(1) Paragra
37、ph 5.1 includes the addition of alternative solventsfor cleaning sample containers.(2) Note 3, Note 4, and Note 5 contain information on changesto shipping regulations and references useful for determiningcurrent regulations in effect by the date of this revision.ASTM International takes no position
38、 respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.T
39、his standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM In
40、ternational Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address show
41、n below.This standard is copyrighted by ASTM International, 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 aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D3325 90 (2013)3
