1、Designation: D 5761 96 (Reapproved 2006)An American National StandardStandard Practice forEmulsification/Suspension of Multiphase Fluid WasteMaterials1This standard is issued under the fixed designation D 5761; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers the generation of a single-phasesuspension or emulsion f
3、rom multiphase samples which areprimarily liquid in order to facilitate sample preparation,transfer, and analysis.1.2 This practice is designed to keep a multiphase fluidsample in an emulsified/suspended state long enough to take asingle, composite sample that is representative of the sample asa who
4、le. The sample may reform multiple layers after standing.1.3 The emulsion/suspension generated by following thispractice can be used only for analytical procedures designedfor the total sample and procedures not significantly affected bythe emulsifier or the presence of an emulsion/suspension.1.4 Th
5、is practice assumes that a representative sample ofnot more than one litre has been obtained.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns, if any, as
6、sociated 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 limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 4057 Practice for Manual Sampling of Petroleum andPet
7、roleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products2.2 EPA Standard:SW846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods33. Terminology3.1 Definitions:3.1.1 emulsion, na suspension of fine particles or glob-ules, or both, of one or more liquid
8、s in another liquid.3.2 Definitions of Terms Specific to This Standard:3.2.1 multiphase fluid waste material, na substance ormixture of chemicals that is no longer useful for its originalpurpose that visibly involves a solid and at least one liquidphase or more than one liquid phase without any soli
9、d present.4. Summary of Practice4.1 An emulsifier is added and mixed well with a sample ofmultiphase fluid waste material, to produce a uniform mixturesuitable for subsequent aliquoting. A satisfactory homogeniza-tion has been attained when the sample appears to remain as asingle phase for 30 s or l
10、onger.4.2 A calcium sulfonate emulsifier is used when the originalsample is primarily organic in nature; a polyethylene glycolmonoalky ester is used when the original sample is primarilyaqueous in nature. A blend of the two emulsifiers is used whenthe original sample contains roughly equal volumes o
11、f organicand aqueous material.5. Significance and Use5.1 This practice is intended as a solution to the difficulty ofobtaining reproducible test results from heterogeneoussamples.5.2 This practice works best with multilayered liquids, butcan also be applied to samples with solid particles that aresu
12、fficiently small in size to be suspended in an emulsion.5.3 The emulsified/suspended sample can be used for allbulk property testing such as microwave digestion/inductivelycoupled argon plasma (ICAP), ion chromatography, heat ofcombustion, ash content, water, nonvolatile residue, and pH. Itmay be pr
13、udent to retain a portion of the sample in its original,multiphase form for some types of analyses.1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.03 onElemental Analysis.Current edition approved
14、May 1, 2006. Published June 2006. Originallyapproved in 1995. Last previous edition approved in 2001 as D 5761 96 (2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refe
15、r to the standards Document Summary page onthe ASTM website.3Available from the Environmental Protection Agency, 401 M Street, SW,Washington, DC 20460.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Interferences6.1 Not all sample
16、s can be emulsified, due to varyingchemical reactions with the surfactants. If the emulsion is notstable for at least 30 s after shaking, it may not be suitable fortesting as an emulsion.6.2 Due to their physical composition, some samples are notsuitable for splitting and, as a result, cannot be emu
17、lsified if anonemulsified retain is required. For example, excessiveamounts of solids and semisolids or tars do not permit splitting.6.3 In some instances, the amount of sample submitted maynot be sufficient for splitting and, as a result, cannot beemulsified if some unemulsified sample must be reta
18、ined.6.4 Erroneous results can be obtained if precautions are nottaken to avoid the loss of volatile material. Do not opencontainers unnecessarily. Results for samples from leaky con-tainers must be marked to indicate that the sample integrity wasnot maintained during shipping/storage.7. Apparatus7.
19、1 Funnel, Splitting2-L separatory funnel fitted withtwin 0.7-mm inside diameter glass discharge tubes as shown inFig. 1.47.2 High-Intensity Lamp.7.3 Polyethylene Transfer Pipet, 3.5-mL draw.8. Reagents and Materials8.1 Aqueous EmulsifierPolyethylene glycol monoalky es-ter, also known as PEG400.58.2
20、Organic EmulsifierCalcium sulfonate (60 % weight)in heavy aromatic naphtha.59. Procedure9.1 Representative samples are to be provided to the labo-ratory using standard techniques such as those described inPractices D 4057 or D 4177 and EPA/SW846. It is assumed forpurposes of this practice that the s
21、ize of the sample in thelaboratory is one litre or less. Adjustments in procedure will benecessary for larger volumes.9.2 Vigorously shake multiphase samples by hand, or bymechanical means, for up to 30 s. If within 1 min after shaking,the sample appears to separate and each of the layers consistsof
22、 at least 10 % by volume of the total, and if there is asufficient sample available based on subsequent testing require-ments, then the sample is a candidate for the emulsificationprocedure.9.3 (Optional.) If some unemulsified sample is to be re-tained, split the sample into two separate samples usi
23、ng thesplitter funnel shown in Fig. 1.9.4 Tentatively classify any liquid phase, using informationknown about the sample, as organic or aqueous and determinetheir volume percentages relative to the whole sample. SeeAppendix X1 for an example worksheet on which to record theinformation.9.4.1 As a gui
24、de to classifying a sample in a clear glass jar,measure phase height from the inside bottom of the jar, notfrom the bench top, using a ruler held up to the outer verticalside of the jar. Phase height shall be measured while lookingstraight and horizontally at the phase separation.9.4.2 Use a high-in
25、tensity lamp to backlight the sample andprovide better definition of phases. Short duration applicationof the lamp will not heat the sample.9.5 Select an emulsifier. Select the organic emulsifier forsamples which are greater than 60 % organic and the aqueousemulsifier for samples which are greater t
26、han 60 % water. Forthe multiphase samples where the organic layer is between 40to 60 %, use an equal mixture of the emulsifiers (equalvolumetric proportions).9.6 Estimate the total volume of sample in millilitres.Multiply this number by 0.025 to determine the grams ofemulsifier to add. (See the work
27、sheet in Appendix X1.)NOTE 1An exact conversion of volume to mass is not necessary for4The sole source of supply of the apparatus known to the committee at this timeis Universal Instrument Co., 315 W. Colfax, Palatine, IL 60067 (Part No. F-4001).If you are aware of alternative suppliers, please prov
28、ide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.5The sole source of supply of the emulsifier (Witconol H31 and Witconate 605A,respectively) known to the committee at this
29、 time is Witco Corp., 3200 Brookfield,Houston, TX 77045-2817. If you are aware of alternative suppliers, please providethis information to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.FIG. 1
30、Sample Splitter FunnelD 5761 96 (2006)2this practice. The amount of surfactant added has been developedassuming this conversion. Record the information.9.7 Place the sample on a balance reading to at least 0.1 g.Using a plastic transfer pipet or similar device, add thecalculated quantity of the sele
31、cted emulsifier to the sample.Shake as vigorously as possible until a milky homogeneousdispersion is formed.9.8 If the emulsion does not stay together for at least 60 s,add approximately1goftheother surfactant.9.9 Mix the emulsified sample thoroughly by hand shakingfor 15 s immediately before each a
32、liquot is removed.10. Calculation10.1 The following is an example of the determination ofthe amount of surfactant required:Sample amount in container 400 mL (10.5 cm height)Organic phase height 3.0 cmAqueous phase height 7.5 cmPercent organic phase 29Percent aqueous phase 71Surfactant used Aqueous (
33、H-31A)400 mL 3 0.025 = 10 g of aqueous surfactant added to the sample.11. Keywords11.1 emulsification; heterogeneous sample; multiphase;sample preparationAPPENDIX(Nonmandatory Information)X1. EMULSIFICATION WORKSHEETX1.1 Fig. X1.1 is a sample emulsification worksheet.D 5761 96 (2006)3ASTM Internatio
34、nal takes 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
35、 own responsibility.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
36、 addressed 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
37、, at the 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 610-832-9
38、585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).Sample Number : Sample Number :Sample Amount : mL Sample Amount : mLOrganic Height : cm Organic Height : cmAqueous Height : cm Aqueous Height : cmTotal Height : cm Total Height : cmPercent Organic
39、 : Percent Organic :Percent Aqueous : Percent Aqueous :Surfactant : Surfactant :Surfactant Amount : g Surfactant Amount : gAnalyst : Analyst :Date : Date :Sample Number : Sample Number :Sample Amount : mL Sample Amount : mLOrganic Height : cm Organic Height : cmAqueous Height : cm Aqueous Height : c
40、mTotal Height : cm Total Height : cmPercent Organic : Percent Organic :Percent Aqueous : Percent Aqueous :Surfactant : Surfactant :Surfactant Amount : g Surfactant Amount : gAnalyst : Analyst :Date : Date :Sample Number : Sample Number :Sample Amount : mL Sample Amount : mLOrganic Height : cm Organi
41、c Height : cmAqueous Height : cm Aqueous Height : cmTotal Height : cm Total Height : cmPercent Organic : Percent Organic :Percent Aqueous : Percent Aqueous :Surfactant : Surfactant :Surfactant Amount : g Surfactant Amount : gAnalyst : Analyst :Date : Date :NOTESample Amount (mL) 3 0.025 = grams of surfactant to add (organic height)/(organic + aqueous height) 3 100 = % difference organic(aqueous height)/(organic + aqueous height) 3 100 = % difference aqueous.FIG. X1.1 Emulsification WorksheetD 5761 96 (2006)4
