1、Designation: D 3325 90 (Reapproved 2006)Standard Practice forPreservation of Waterborne Oil Samples1This standard is issued under the fixed designation D 3325; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、is 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,
4、 nonstandard simplifications are recom-mended that will minimize or eliminate consequent errors.NOTE 1Procedures for the analysis of oil spill samples are PracticesD 3326, D 3415, D 3650, and D 4489, and Test Methods D 3327, D 3328,and D 3414. A guide to the use of ASTM test methods for the analysis
5、 ofoil spill samples is found in Practice D 3415.1.3 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 re
6、gulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1129 Terminology Relating to WaterD 3326 Practice for Preparation of Samples for Identifica-tion of Waterborne OilsD 3327 Method for Analysis of Selected Elements inWarterborne Oils3D 3328 Test Methods for Comparison of W
7、aterborne Petro-leum Oils by Gas ChromatographyD 3414 Test Method for Comparison of Waterborne Petro-leum Oils by Infrared SpectroscopyD 3415 Practice for Identification of Waterborne OilsD 3650 Test Method for Comparison of Waterborne Petro-leum Oils By Fluorescence AnalysisD 4489 Practices for Sam
8、pling of Waterborne Oils3. Terminology3.1 DefinitionsFor definitions of terms used in this prac-tice, refer to Terminology D 1129.4. 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
9、 mixtures, emulsions, 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. S
10、ervices available for transpor-tation of samples are described.5. Apparatus5.1 Sample ContainersBorosilicate glass containers thathave been thoroughly cleaned are preferable. All glass contain-ers, new or used, must be thoroughly cleaned and washed priorto use. The cleaning steps consist of an initi
11、al wash with awarm aqueous detergent mixture followed by six hot tap waterrinses, two rinses with reagent water, a rinse with reagent-grade acetone, and a final rinse with a solvent such as pentane,hexane, cyclohexane, dichloromethane, or chloroform fol-lowed by drying in a clean oven at 105C or hot
12、ter for 30 min.If the glassware requires cleaning under field conditions, itshould 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,
13、the use ofpentane, hexane, 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
14、 many commercial plasticcontainers 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 Analy
15、sis forOrganic Substances in Water.Current edition approved Dec. 15, 2006. Published February 2007. Originallyapproved in 1974. Last previous edition approved in 2002 as D 3325 90 (2002)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at servic
16、eastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-
17、2959, United States.5.1.2 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 labo
18、ratory to 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-fluorocar
19、bon sheet, 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, sufficien
20、t to absorb 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 packagi
21、ng manufacturer.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 m
22、ay be used, 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. Sa
23、mpling7.1 Collect a representative sample in accordance withPractices D 4489.7.2 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.Nitro
24、gen or carbon 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
25、 States PostalService 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
26、, thedefinition 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
27、under the ICAO rules.NOTE 5For more information about the legal requirements for pack-aging and shipping petroleum oils and other hazardous materials, refer toU.S. Postal Service Publication 52, “Acceptance of Hazardous, Restricted,or Perishable Matter,” the Domestic Mail Manual, Part 124, “Nonmaila
28、bleMatterArticles and Substances; Special Mailing Rules,” and the pack-aging requirements listed in the Domestic Mail Manual, Part 121.9.2 Common carriers such as air express or air freight areoften employed for transportaiton of oil spill samples. Consultthe carrier for current packing and labellin
29、g requirements.9.3 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 thistable with the s
30、pecific sections of this practice to choose the4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole,
31、 Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Procedures for the Preservation of Waterborne Oil SamplesRecommendedOperationProcedure for EmergencyConditionsProcedures for Controlled Fieldor LaboratorySample c
32、ontainers Borosilicate glass jars for high boiling samples. Borosilicate glass 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 tapwa
33、ter and reagent water rinses. Rinse with acetone,chloroform, and oven dry.Closures 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 w
34、ith nitrogen or cabon dioxide. Store in dark inrefrigerator.Protection against 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, i
35、f possible, and label appropriately. Notifyrecipient.D 3325 90 (2006)2proper 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 lo
36、cation of selection changes to thispractice that have been incorporated since the last issue. Forthe convenience of the user, Committee D-19 has highlightedthose changes that may impact the use of this practice. Thissection may also include descriptions of the changes or reasonsfor the changes or bo
37、th.(1) Paragraph 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 tak
38、es no position 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 re
39、sponsibility.This 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 addres
40、sed to ASTM International 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 th
41、e address shown 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).D 3325 90 (2006)3
