1、Designation: G 136 03Standard 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 the case of revision
2、, 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 may be used to extract nonvolatile andsemivolatile residues from materials such as new an
3、d 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 detergents, brighte
4、ners,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 standard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use.
5、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 1193 Specification for Reagent WaterE 1235 Test Method for Gravimetric Deter
6、mination of Non-volatile Residue (NVR) in Environmentally ControlledAreas for SpacecraftF 324 Test Method for Nonvolatile Residue of VolatileCleaning Solvents Using the Solvent Purity MeterF 331 Test Method for Nonvolatile Residue of HalogenatedSolvent Extract from Aerospace Components Using RotaryF
7、lash Evaporator3. 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 upon which they reside.3.1.2 contaminate, va process of contaminating.3.1.3 non
8、volatile 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-ter in a solid state with observable length, width, and thickness.3.1.4.1 Discu
9、ssionThe 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, or solid state.3.1.5.1 DiscussionA molecular contaminant may be uni-formly or n
10、onuniformly 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 so forth, is placed ina container containing the test fluid. This container is
11、 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 emulsion if the contaminant is notsoluble in the test fluid. The test fluid may th
12、en 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 containing an extracting agent.4.1.1.1 When Type II water is used, the water and
13、 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-pressure liquid chromatography.4.1.1.2 When cleaning agents are used, the materials
14、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 of1This practice is under the jurisdiction of ASTM Committee G-4 on Compat-ibility and Sensitivity of Materials in Oxyge
15、n-Enriched Atmospheres and is thedirect responsibility of Subcommittee G04.02 on Recommended Practices.Current edition approved Sept. 10, 2003. Published December 2003. Originallyapproved in 1995. Last previous edition approved in 1996 as G 136 96.2For referenced ASTM standards, visit the ASTM websi
16、te, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandardsvolume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States
17、.analysis 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 weight of thematerial before and after cleaning may be determined or thesolvents may be ana
18、lyzed 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 is suitable for the determination of extract-able substances that may be found in materi
19、als 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 in cleaning operations may be evaluated prior to use toensure that the proposed extracti
20、ng 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 1The amount of material extracted may be dependent upon thefrequency and power density o
21、f 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 conditions.6. Apparatus6.1 Ultrasonic Bath, with an operating frequency rangefrom 25 to 90
22、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 container with volumesbetween 1 and 4 L are to be used.6.3 A Bracket, to support the sample
23、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. Reagents7.1 Solventsthe following may be used: tetrachloroethyl-ene (perchloroethylene), tr
24、ichloroethylene, 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. T
25、he 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. The preferred solvent removal methodshall be determined by the user.7.2 Purity of Wate
26、rThe 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 beused in all tests. Unless otherwise indicated, all reagents shallconform to the specifica
27、tions 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 sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination. D
28、etergents 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 determine the amount of solvent extractablematerial in a wiping cloth (new or used), cut out
29、 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 area and mass.8.1.1.2 If the residue is to be determined on used wipingcloths in an effort
30、 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 this NVR as M2 inmg/g or as M3 in mg/cm2or as TC in ppm/g or ppm/cm2. TheNVR or TC value
31、 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 fingers and palm areas of the glove, the areasthat would typically be exposed to the cleanin
32、g 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 square centimetres.8.2 Parts Pan PreparationClean the stainless steelsample parts pans.
33、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. Determine the amount of NVRor TC for the parts pan using the analysis procedure that will beuse
34、d 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
35、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 desired temperature, and degas the waterfor 10 min.8.3.3 Place the selected parts pan in the
36、 support bracket inthe ultrasonic bath.8.4 Extraction Procedure:G1360328.4.1 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 alu
37、minum 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, and allow the extractingagent and bath temperature to equilibrate to the desiredtemperature. Alt
38、ernatively, 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 Extract
39、ion 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 as possible, with amaximum time limit of 120 min after turning off the ultrasonicbath.8.5 Sampli
40、ng 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 solv
41、ent 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 E 1235, F 324, or F 331. Ensure that the reportedNVR is adj
42、usted 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 cover. Swirl the parts pan to mix the extractingagent.8.6.2 After swirling, quickly decant the extr
43、acting 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 agent. If TypeII water was used as the extracting agent, combine the threeportions with the water
44、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 Determine the NVR of the sample using G TC or highpressure liquid chromatography (see 4.1.1.2).9.
45、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, batch number,and manufacturer).9.1.2 Cleaning reagent;9.1.3 Cleaning time;9.1.4 Cleaning temperatu
46、re;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 extracted from unused wipes,mg/g, or (M3), mg/cm2, or TC in ppm/g or ppm/cm2;9.1.10 Mass (M4) of
47、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; nonvolatileresidue; oxygen systems; total carbon (TC); ultrasonicextractionAPPENDIX(Nonmandatory Inform
48、ation)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 applications. The follow-ing information was graciously provided by Blackstone Ultra-sonics3and is reprint
49、ed 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, agitators, linings, sub-mersible pumps, Etc.X1.2.1.4 Cleaning Zoneparts placement and racking.3Black
