1、Designation: G136 03 (Reapproved 2016)1Standard Practice forDetermination of Soluble Residual Contaminants inMaterials by Ultrasonic Extraction1This standard is issued under the fixed designation G136; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、 case of revision, the 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.1NOTEEditorial changes made throughout in May 2017.1. Scope1.1 This practice may be used to extract
3、 nonvolatile andsemivolatile residues from materials such as new and usedgloves, new and used wipes, component soft goods, and soforth. When used with proposed cleaning materials (wipes,gloves, and so forth), this practice may be used to determinethe potential of the proposed solvent or other fluids
4、 to extractcontaminants (plasticizers, residual detergents, brighteners,and so forth) and deposit them on the surface being cleaned.1.2 This practice is not suitable for the evaluation ofparticulate contamination.1.3 The values stated in SI units are to be regarded standard.No other units of measure
5、ment are included in this standard.1.4 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 limit
6、ations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization
7、TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE1235 Test Method for Gravimetric Determination of Non-volatile Residue (NVR) in Environmentally ControlledAreas for SpacecraftF324 Test Method for Nonvolatile Residue of Volati
8、leCleaning Solvents Using the Solvent Purity Meter (With-drawn 1987)3F331 Test Method for Nonvolatile Residue of Solvent Ex-tract from Aerospace Components (Using Flash Evapora-tor)3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 contaminant (contamination), nunwanted molecular
9、and particulate matter that could affect or degrade the perfor-mance of the components upon which they reside.3.1.2 contaminate, va process of contaminating.3.1.3 nonvolatile residue (NVR), nresidual molecular andparticulate matter remaining following the filtration and con-trolled evaporation of li
10、quid containing contaminants.3.1.4 particle (particulate contaminant), na piece of mat-ter in a solid state with observable length, width, and thickness.3.1.4.1 DiscussionThe size of a particle is usually definedby its greatest dimension and is specified in micrometres.3.1.5 molecular contaminant (n
11、on-particulatecontamination), nthe molecular contaminant may be in agaseous, liquid, or solid state.3.1.5.1 DiscussionA molecular contaminant may be uni-formly or nonuniformly distributed, or be in the form ofdroplets. Molecular contaminants account for most of theNVR.3.1.6 degas, vthe process of re
12、moving gases from a liquid.4. Summary of Practice4.1 A material, glove, hand wipe, and so forth, is placed ina container containing the test fluid. This container is thenplaced in an ultrasonic cleaning bath and treated for a givenperiod of time at the recommended temperature for the testfluid. This
13、 results in either a solution if the contaminant is1This practice is under the jurisdiction of ASTM Committee G04 on Compat-ibility and Sensitivity of Materials in Oxygen Enriched Atmospheres and is thedirect responsibility of Subcommittee G04.02 on Recommended Practices.Current edition approved May
14、 1, 2016. Published June 2016. Originallyapproved in 1995. Last previous edition approved in 2009 as G136 03(2009).DOI: 10.1520/G0136-03R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandardsvolume
15、 information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standa
16、rd was developed in accordance with internationally recognized principles 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.1soluble
17、 in the test fluid or an emulsion if the contaminant is notsoluble in the test fluid. The test fluid may then be analyzed fornonvolatile residue that was extracted from the test specimen.4.1.1 In the case of aqueous-based agents, the material maybe treated in accordance with Specification D1193 Type
18、 IIwater or Type II water containing an extracting agent.4.1.1.1 When Type II water is used, the water and materialmay be analyzed without further treatment. Typical methods ofanalysis may include weighing the material before and aftertreatment or more sophisticated analytical procedures such astota
19、l carbon (TC) or high-pressure liquid chromatography.4.1.1.2 When cleaning agents are used, the materials arerinsed with Type II water after the removal from the cleaningbath and then ultrasonically cleaned in reagent water to ensurethe removal of the extracting agent. Typical methods ofanalysis may
20、 include weighing the material before and aftercleaning or more sophisticated analytical procedures such asTC or high-pressure liquid chromatography.4.1.2 In the case of solvent-based agents, the weight of thematerial before and after cleaning may be determined or thesolvents may be analyzed using i
21、nfrared spectroscopy, gaschromatography, gas chromatography/mass spectroscopy, orthe NVR determined using Test Methods E1235, F324,orF331, as appropriate.5. Significance and Use5.1 This practice is suitable for the determination of extract-able substances that may be found in materials used in syste
22、msor components requiring a high level of cleanliness, such asoxygen systems. Soft goods, such as seals and valve seats, maybe tested as received. Gloves and wipes, or samples thereof, tobe used in cleaning operations may be evaluated prior to use toensure that the proposed extracting agent does not
23、 extract ordeposit chemicals, or both, on the surface to be cleaned.5.2 Wipes or other cleaning equipment may be tested afteruse to determine the amount of contaminant removed from asurface.NOTE 1The amount of material extracted may be dependent upon thefrequency and power density of the ultrasonic
24、unit.5.3 The extraction efficiency has been shown to vary withthe frequency and power density of the ultrasonic unit. Theunit, therefore, must be carefully evaluated to optimize theextraction conditions.6. Apparatus6.1 Ultrasonic Bath, with an operating frequency rangefrom 25 to 90 kHz, a typical po
25、wer range from 10 to 25 W/L,and a temperature-controlled bath capable of maintaining atemperature between ambient and 70C with an accuracy of62C is to be used.6.2 Parts Pans, stainless steel container with volumesbetween 1 and 4 L are to be used.6.3 A Bracket, to support the sample pans in the ultra
26、sonicbath is to be used.NOTE 2The bracket should be designed to hang in the ultrasonic bathwithout contact with the bottom.6.4 Balance, a minimum capacity of 50 g with an accuracyof 0.1 mg.7. Reagents7.1 Solventsthe following may be used: tetrachloroethyl-ene (perchloroethylene), trichloroethylene,
27、methylene chloride,and perfluorinated carbon fluids.NOTE 3Warning: Follow appropriate safe handling procedures whenusing the solvents approved for the use application. Many solvents withlow TLVs present hazards to personnel working with them as well as tothe systems being cleaned. The removal of the
28、se solvents from breathinggas systems must be assured. Many solvents are not considered to becompatible with oxygen and must be completely removed from materialsbefore their use in oxygen systems. The preferred solvent removal methodshall be determined by the user.7.2 Purity of WaterThe water used s
29、hall meet the require-ments of Specification D1193, Type II except that the require-ment for a maximum TC of 50 kg/L shall not be required.7.3 Purity of ReagentsReagent-grade chemicals shall beused in all tests. Unless otherwise indicated, all reagents shallconform to the specifications of the Commi
30、ttee on AnalyticalReagents of the American Chemical Society where suchspecifications are available. Other grades may be used, pro-vided it is first ascertained and that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination. Detergents to be us
31、ed shall be identified bythe manufacturer and name (registered trademark, if any).8. Procedure8.1 Sample Preparations:8.1.1 Prepare the sample for placement in the ultrasonicbath.8.1.1.1 To determine the amount of solvent-extractablematerial in a wiping cloth (new or used), cut out a test sectionapp
32、roximately 30 cm square, accurately measure and calculatethe area (S), in square centimetres, and determine the mass ofthe section in grams to the nearest tenth of a milligram (mg).Record the area and mass.8.1.1.2 If the residue is to be determined on used wipingcloths in an effort to assess the cle
33、anliness of a part or system,an extraction and a nonvolatile residue (NVR) or total carbon(TC) analysis shall be performed as described in 8.2 8.5 onan equivalent sample of unused cloth. Record this NVR as M2in mg/g or as M3 in mg/cm2or as TC in ppm/g or ppm/cm2.The NVR or TC value must be subtracte
34、d from that determinedfor the contaminated cloth.8.1.1.3 To determine the amount of extractable material in aglove to be used in a cleaning operation, cut several rectangularstrips from the fingers and palm areas of the glove, the areasthat would typically be exposed to the cleaning solvent,determin
35、e the mass in grams to the nearest tenth of a milligram,and record the mass (M1). Determine the dimensions of eachstrip in centimetres (cm) and record the total surface area of thestrips (S) in square centimetres.8.2 Parts Pan PreparationClean the stainless steel sampleparts pans. Conduct the extrac
36、tion procedure selected withouttest articles to verify the cleanliness of the parts pans. Use thesame volume of cleaning agent for the verification that will beG136 03 (2016)12used on the test articles. Determine the amount of NVR or TCfor the parts pan using the analysis procedure that will be used
37、on the actual test articles. Record the amount as the blank (B)for the parts pan and cleaning agent.8.3 Preliminary Procedure:8.3.1 If an extracting agent is being used that requiresdilution or special preparation, carefully follow the manufac-turers instructions. Use Type II water to prepare the aq
38、ueousextracting solutions or as the actual extracting agent.8.3.2 Place the support bracket in the ultrasonic bath, fillwith water to the level specified by the manufacturer, heat theultrasonic bath to the desired temperature, and degas the waterfor 10 min.8.3.3 Place the selected parts pan in the s
39、upport bracket inthe ultrasonic bath.8.4 Extraction Procedure:8.4.1 Place the material or part(s) to be extracted in thestainless steel parts pan.8.4.2 Pour a measured amount of the extracting agent intothe stainless steel parts pan sufficient to cover the parts. Coverthe parts pan with aluminum foi
40、l or a stainless steel lid, placethe parts pan and parts in the bracket in the ultrasonic bath,adjust the water level in the bath such that it is above theextracting agent level in the parts pan, and allow the extractingagent and bath temperature to equilibrate to the desiredtemperature.Alternativel
41、y, preheat the parts pan and extractingagent prior to the placement of the materials or parts into theparts pan. Then cover the parts pan with foil and place the partspan into the bracket in the bath and allow the extracting agentto equilibrate to the temperature of the bath.8.4.2.1 The ratio of ext
42、raction agent to parts surface areashall not exceed 1000 mL/0.1 m2; the preferred ratio is 500mL/0.1 m2.8.4.3 Subject the parts to the ultrasonic bath for 10 min.Perform the sampling procedure as soon as possible, with amaximum time limit of 120 min after turning off the ultrasonicbath.8.5 Sampling
43、Procedure for Solvent Extracted Parts:8.5.1 Remove the parts pan from the ultrasonic bath andremove the cover. Swirl the parts pan to thoroughly mix thesolvent.8.5.2 After swirling, quickly decant the solvent from theparts pan.8.5.3 Wash the parts pan and parts with a total of 500 mL offresh solvent
44、 in three roughly equal portions, combine with thesolvent from 8.5.2, and set aside as the sample for NVRanalysis.8.5.4 Determine the mass (M4) of the nonvolatile residue inmilligrams to the nearest tenth of a milligram using TestMethods E1235, F324,orF331. Ensure that the reported NVRis adjusted by
45、 subtracting the NVR of an equivalent volume of“blank” solvent.8.6 Sampling Procedure for Aqueous Extracted Materialsand Parts:8.6.1 Remove the parts pan from the ultrasonic bath andremove the cover. Swirl the parts pan to mix the extractingagent.8.6.2 After swirling, quickly decant the extracting a
46、gentfrom the parts pan.8.6.3 Wash the parts pan and parts with a total of 500 mL offresh Type II water in three roughly equal portions and discardunless Type II water was used as the extracting agent. If TypeII water was used as the extracting agent, combine the threeportions with the water from 8.6
47、.2, and set aside as the samplefor analysis. If a surface active compound was used, repeat theprocedures in 8.3 8.5 using Type II water and use the Type IIwater as the sample for analysis.8.6.4 Determine the NVR of the sample using TC or highpressure liquid chromatography (see 4.1.1.2).9. Report9.1
48、Report the following information:9.1.1 Identification of the part or material being cleaned(including tradename, part number, serial number, properchemical name,ASTM designation, lot number, batch number,and manufacturer).9.1.2 Cleaning reagent;9.1.3 Cleaning time;9.1.4 Cleaning temperature;9.1.5 Fr
49、equency of the ultrasonic bath, kHz;9.1.6 Power density of the ultrasonic bath, W/L;9.1.7 Volume of extracting agent used, mL;9.1.8 Mass (M1) of parts extracted, g;9.1.9 Mass (M2) of material extracted from unused wipes,mg/g, or (M3), mg/cm2, or TC in ppm/g or ppm/cm2;9.1.10 Mass (M4) of NVR determined using Test MethodsE1235, F324,orF331;9.1.11 Blank (B) for the parts pan and agent, mg; and,9.1.12 Surface area (S), cm2.10. Keywords10.1 contaminant; contamination; extraction; nonvolatileresidue; oxygen systems; total carbon (TC); ultrasonic extrac-tionG136
