1、Designation: G 136 03 (Reapproved 2009)Standard Practice forDetermination of Soluble Residual Contaminants inMaterials by Ultrasonic Extraction1This standard is issued under the fixed designation G 136; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e 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.1. Scope1.1 This practice may be used to extract nonvolatile andsemivolatile residues from materia
3、ls 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 to extractcontaminants (plasticizers, residual de
4、tergents, 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 measurement are included in this standard.1.4 This stand
5、ard 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 limitations prior to use.2. Referenced Documents2.1 AS
6、TM Standards:2D 1193 Specification for Reagent WaterE 1235 Test Method for Gravimetric Determination of Non-volatile Residue (NVR) in Environmentally ControlledAreas for SpacecraftF 324 Test Method for Nonvolatile Residue of VolatileCleaning Solvents Using the Solvent Purity Meter3F 331 Test Method
7、for Nonvolatile Residue of SolventExtract from Aerospace Components (Using Flash Evapo-rator)3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 contaminant (contamination), nunwanted molecularand particulate matter that could affect or degrade the perfor-mance of the components u
8、pon 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 liquid containing contaminants.3.1.4 particle (particulate contaminant), na piece of mat-t
9、er 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 (non-particulate contamina-tion), nthe molecular contaminant may be in a gaseous,liquid, o
10、r 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 removing gases from aliquid.4. Summary of Practice4.1 A material, glove, hand wipe, and
11、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 results in either a solution if the contaminant issoluble in the test fluid or an emul
12、sion 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 D 1193 Type IIwater or Type II water co
13、ntaining 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 astotal carbon (TC) or high-pressu
14、re liquid chromatography.1This 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 April 1, 2009. Published Sept
15、ember 2009. Originallyapproved in 1995. Last previous edition approved in 2003 as G 136 03.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandardsvolume information, refer to the standards Document Sum
16、mary page onthe ASTM website.3Withdrawn1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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
17、cleaned in reagent water to ensurethe removal of the extracting agent. Typical methods ofanalysis may 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 wei
18、ght of thematerial before and after cleaning may be determined or thesolvents may be analyzed using infrared spectroscopy, gaschromatography, gas chromatography/mass spectroscopy, orthe NVR determined using Test Methods E 1235, F 324, orF 331, as appropriate.5. Significance and Use5.1 This practice
19、is suitable for the determination of extract-able substances that may be found in materials used in systemsor 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
20、in cleaning operations may be evaluated prior to use toensure that the proposed extracting agent does not 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
21、1The amount of material extracted may be dependent upon thefrequency and power density of the ultrasonic 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 con
22、ditions.6. Apparatus6.1 Ultrasonic Bath, with an operating frequency rangefrom 25 to 90 kHz, a typical power 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 cont
23、ainer with volumesbetween 1 and 4 L are to be used.6.3 A Bracket, to support the sample pans in the ultrasonicbath 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. Rea
24、gents7.1 Solventsthe following may be used: tetrachloroethyl-ene (perchloroethylene), trichloroethylene, 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
25、present hazards to personnel working with them as well as tothe systems being cleaned. The removal of these 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
26、. The preferred solvent removal methodshall be determined by the user.7.2 Purity of WaterThe water used shall meet the require-ments of Specification D 1193, 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 beu
27、sed in all tests. Unless otherwise indicated, all reagents shallconform to the specifications of the Committee 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 suffici
28、entlyhigh purity to permit its use without lessening the accuracy ofthe determination. Detergents to be used 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 dete
29、rmine the amount of solvent extractablematerial in a wiping cloth (new or used), cut out a test sectionapproximately 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 ar
30、ea and mass.8.1.1.2 If the residue is to be determined on used wipingcloths in an effort to assess the cleanliness 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 on anequivalent sample of unused cloth. Record
31、this NVR as M2 inmg/g or as M3 in mg/cm2or as TC in ppm/g or ppm/cm2. TheNVR or TC value must be subtracted from that determined forthe 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 fing
32、ers and palm areas of the glove, the areasthat would typically be exposed to the cleaning solvent,determine 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
33、square centimetres.8.2 Parts Pan PreparationClean the stainless steelsample parts pans. Conduct the extraction procedure selectedwithout test articles to verify the cleanliness of the parts pans.Use the same volume of cleaning agent for the verification thatwill be used on the test articles. Determi
34、ne the amount of NVRor TC for the parts pan using the analysis procedure that will beused 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 preparat
35、ion, carefully follow the manufac-turers instructions. Use Type II water to prepare the aqueousextracting 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 desi
36、red temperature, and degas the waterfor 10 min.G 136 03 (2009)28.3.3 Place the selected parts pan in the support 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 a
37、gent intothe stainless steel parts pan sufficient to cover the parts. Coverthe parts pan with aluminum foil or stainless steel lids, 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,
38、 and allow the extractingagent and bath temperature to equilibrate to the desiredtemperature. Alternatively, 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
39、 bath and allow the extracting agentto equilibrate to the temperature of the bath.8.4.2.1 Extraction agent to parts surface area ratio shall notexceed 1000 mL/0.1 m2; the preferred ratio is 500 mL/0.1 m2.8.4.3 Subject the parts to the ultrasonic bath for 10 min.Perform the sampling procedure as soon
40、 as possible, with amaximum time limit of 120 min after turning off the ultrasonicbath.8.5 Sampling 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
41、 solvent from theparts pan.8.5.3 Wash the parts pan and parts with a total of 500 mL offresh solvent 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 t
42、enth of a milligram using TestMethods E 1235, F 324, or F 331. Ensure that the reportedNVR is adjusted by subtracting the NVR of an equivalentvolume 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 co
43、ver. Swirl the parts pan to mix the extractingagent.8.6.2 After swirling, quickly decant the extracting agentfrom 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 a
44、gent. If TypeII water was used as the extracting agent, combine the threeportions with the water from 8.6.2, 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 D
45、etermine the NVR of the sample using G TC or highpressure liquid chromatography (see 4.1.1.2).9. Report9.1 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, b
46、atch number,and manufacturer).9.1.2 Cleaning reagent;9.1.3 Cleaning time;9.1.4 Cleaning temperature;9.1.5 Frequency 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
47、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 MethodsE 1235, F 324, or F 331;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; nonvol
48、atileresidue; oxygen systems; total carbon (TC); ultrasonicextractionAPPENDIX(Nonmandatory Information)X1. SELECTION OF ULTRASONIC BATHSX1.1 IntroductionThis appendix describes technical in-formation useful to the user in the selection of ultrasonic bathsfor aqueous extraction and cleaning applicati
49、ons. The follow-ing information was graciously provided by Blackstone Ultra-sonics4and is reprinted here with their permission.X1.2 Designing an immersible ultrasonic transducer systemrequires that several factors be taken into account. Each case isan individual. The following list will give the reader some ideaof the parameters that should be defined. Later, each will againbe considered as to its effect on the design of the system.X1.2.1 The Tank:X1.2.1.1 Volumecubic measure or gallons.X1.2.1.2 Shapelength, width and depth.X1.2.1.3 Internal Featuresheaters, ag
