1、Designation: D5761 96 (Reapproved 2012)Standard Practice forEmulsification/Suspension of Multiphase Fluid WasteMaterials1This standard is issued under the fixed designation D5761; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 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 the generation of a single-phasesuspension or emulsion from multiphase samples which are
3、primarily 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 whole. The sample may reform multip
4、le 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 This practice assumes that a repre
5、sentative sample ofnot more than 1 L 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, associated with its use. It is therespon
6、sibility 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:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Autom
7、atic 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 liquids in another liquid.3.2 Definitions of T
8、erms 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 solid present.4. Summary of Practice4.1 An e
9、mulsifier 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 longer.4.2 A calcium sulfonate emulsifier
10、 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 of organicand aqueous material.5. Signifi
11、cance 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 aresufficiently small in size to be suspended
12、 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. It1This practice is under the jurisdiction of ASTM
13、Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.03 onElemental Analysis.Current edition approved April 15, 2012. Published May 2012. Originallyapproved in 1995. Last previous edition approved in 2006 as D576196(2006).DOI: 10.1520/D5761-96R12.2Fo
14、r referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from the Environmental Protection Agency, 401 M Stree
15、t, SW,Washington, DC 20460.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.may be prudent to retain a portion of the sample in its original,multiphase form for some types of analyses.6. Interferences6.1 Not all samples can be emulsif
16、ied, 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 emulsified if anone
17、mulsified 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 retained.6.4 Erroneo
18、us 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. Apparatus7.1 Funnel, Splitt
19、ing2-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 Organic Emulsifi
20、erCalcium 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 D4057 or D4177 and EPA/SW846. It is assumed forpurposes of this practice that the size of the sample
21、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 at least 10 % by
22、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 using thesplitter fun
23、nel 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 guide to classifying
24、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-intensity lamp to ba
25、cklight 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 than 60 % water. Fo
26、rthe 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 worksheet in Appendix
27、X1.)4The 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 provide this information to ASTMInternational Headquarters. Your comments will receive
28、 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 time is Witco Corp., 3200 Brookfield,Houston, TX 77045-2817. If you are aware of
29、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 Sample Splitter FunnelD5761 96 (2012)2NOTE 1An exact conversion of volume to mass
30、is not necessary forthis 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 selected emulsifier to
31、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 aliquot is removed.1
32、0. 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 (H-31A)400 mL 3 0.02
33、5 = 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.D5761 96 (2012)3ASTM International takes no positio
34、n 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.
35、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 addressed to ASTM I
36、nternational 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 sho
37、wn 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
38、-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/).Sample Number : Sample Number :Sample Amount : mL Sample Amount : mLOrganic Height : cm Organic Height
39、: 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 :Sample Number : Sample Number :Sample Amount : mL Sa
40、mple Amount : mLOrganic Height : cm Organic 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 :S
41、ample 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 : Percent Organic :Percent Aqueous : Percent Aqueous :Surfactant : Surfactant :Surfactant Amount : g Sur
42、factant 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 WorksheetD5761 96 (2012)4
