1、Designation: D5761 96 (Reapproved 2017)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.1.7 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established
7、in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD
8、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 orglobules, or both, of one or more liquids in another liquid
9、.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 solid present.4. Summar
10、y 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 longer.4.2 Acalcium
11、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 when1This practice is under the jurisdiction of ASTM Committee D02 on Petrol
12、eumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.03 on Elemental Analysis.Current edition approved May 1, 2017. Published June 2017. Originallyapproved in 1995. Last previous edition approved in 2012 as D5761 96 (2012).DOI: 10.1520/D5761-96R17.2For refe
13、renced 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 United States Environmental ProtectionAgency (EPA), Wi
14、lliamJefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,http:/www.epa.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized pr
15、inciples on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1the original sample contains roughly equal volumes of organicand aqueous
16、 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 aresufficiently small in
17、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 prudent to retain a po
18、rtion of the sample in its original,multiphase form for some types of analyses.6. Interferences6.1 Not all samples 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.
19、6.2 Due to their physical composition, some samples are notsuitable for splitting and, as a result, cannot be emulsified 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
20、maynot be sufficient for splitting and, as a result, cannot beemulsified if some unemulsified sample must be retained.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-tain
21、ers must be marked to indicate that the sample integrity wasnot maintained during shipping/storage.7. Apparatus7.1 Funnel, Splitting2 L separatory funnel fitted with twin0.7 mm inside diameter glass discharge tubes as shown in Fig.1.47.2 High-Intensity Lamp.7.3 Polyethylene Transfer Pipet, 3.5 mL dr
22、aw.8. Reagents and Materials8.1 Aqueous EmulsifierPolyethylene glycol monoalkyester, also known as PEG400.58.2 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 th
23、ose described inPractices D4057 or D4177 and EPA/SW846. It is assumed forpurposes of this practice that the size 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, fo
24、r 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 volume of the total, and if there is asufficient sample available based on subsequent testingrequirements, then the sample is a candidate for the emulsifi-cation procedure.9.
25、3 (Optional.) If some unemulsified sample is to beretained, split the sample into two separate samples using 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
26、the whole sample. SeeAppendix X1 for an example worksheet on which to record theinformation.9.4.1 As a guide 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 h
27、eight shall be measured while lookingstraight and horizontally at the phase separation.9.4.2 Use a high-intensity 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 emulsifie
28、r forsamples which are greater than 60 % organic and the aqueousemulsifier for samples which are greater than 60 % water. 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 awar
29、e of alternative suppliers, please provide 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 andWitconate 605A,respec
30、tively) known to the committee at this 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
31、committee,1whichyou may attend.FIG. 1 Sample Splitter FunnelD5761 96 (2017)2the 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
32、to determine the grams ofemulsifier to add. (See the worksheet in Appendix X1.)NOTE 1An exact conversion of volume to mass 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
33、 at least 0.1 g.Using a plastic transfer pipet or similar device, add thecalculated quantity of the selected 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 approximately 1 g of th
34、e other surfactant.9.9 Mix the emulsified sample thoroughly by hand shakingfor 15 s immediately before each aliquot 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 heig
35、ht 3.0 cmAqueous phase height 7.5 cmPercent organic phase 29Percent aqueous phase 71Surfactant used Aqueous (H-31A)400 mL 0.025 = 10 g of aqueous surfactant added to the sample.11. Keywords11.1 emulsification; heterogeneous sample; multiphase;sample preparationAPPENDIX(Nonmandatory Information)X1. E
36、MULSIFICATION WORKSHEETX1.1 Fig. X1.1 is a sample emulsification worksheet.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 : Percent Organic :Percent A
37、queous : 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 : cmTotal Height : cm Total Heig
38、ht : 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 Organic Height : cmAqueous Height :
39、 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 :NOTE 1Sample Amount (mL) 0.025 = grams of surfactant to add (organic hei
40、ght)/(organic + aqueous height) 100 = % difference organic(aqueous height)/(organic + aqueous height) 100 = % difference aqueous.FIG. X1.1 Emulsification WorksheetD5761 96 (2017)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item me
41、ntionedin 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.This standard is subject to revision at any time by the responsible technical committe
42、e 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 International Headquarters. Your comments will receive careful consideration at a meeti
43、ng 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 shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO
44、 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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 96 (2017)4
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