ASTM G136-03(2009)
(Practice)Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction
Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction
SIGNIFICANCE AND USE
This practice is suitable for the determination of extractable substances that may be found in materials used in systems or components requiring a high level of cleanliness, such as oxygen systems. Soft goods, such as seals and valve seats, may be tested as received. Gloves and wipes, or samples thereof, to be used in cleaning operations may be evaluated prior to use to ensure that the proposed extracting agent does not extract or deposit chemicals, or both, on the surface to be cleaned.
Wipes or other cleaning equipment may be tested after use to determine the amount of contaminant removed from a surface.
Note 1—The amount of material extracted may be dependent upon the frequency and power density of the ultrasonic unit.
The extraction efficiency has been shown to vary with the frequency and power density of the ultrasonic unit. The unit, therefore, must be carefully evaluated to optimize the extraction conditions.
SCOPE
1.1 This practice may be used to extract nonvolatile and semivolatile residues from materials such as new and used gloves, new and used wipes, component soft goods, and so forth. When used with proposed cleaning materials (wipes, gloves, and so forth), this practice may be used to determine the potential of the proposed solvent or other fluids to extract contaminants (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 of particulate 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 standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: G136 − 03(Reapproved 2009)
Standard Practice for
Determination of Soluble Residual Contaminants in
Materials by Ultrasonic Extraction
This standard is issued under the fixed designation G136; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This practice may be used to extract nonvolatile and 3.1 Definitions of Terms Specific to This Standard:
semivolatile residues from materials such as new and used 3.1.1 contaminant (contamination), n—unwantedmolecular
gloves, new and used wipes, component soft goods, and so and particulate matter that could affect or degrade the perfor-
forth. When used with proposed cleaning materials (wipes, mance of the components upon which they reside.
gloves, and so forth), this practice may be used to determine
3.1.2 contaminate, v—a process of contaminating.
the potential of the proposed solvent or other fluids to extract
3.1.3 nonvolatile residue (NVR), n—residual molecular and
contaminants (plasticizers, residual detergents, brighteners,
particulate matter remaining following the filtration and con-
and so forth.) and deposit them on the surface being cleaned.
trolled evaporation of liquid containing contaminants.
1.2 This practice is not suitable for the evaluation of
3.1.4 particle (particulate contaminant), n—a piece of mat-
particulate contamination.
terinasolidstatewithobservablelength,width,andthickness.
1.3 ThevaluesstatedinSIunitsaretoberegardedstandard.
3.1.4.1 Discussion—The size of a particle is usually defined
No other units of measurement are included in this standard.
by its greatest dimension and is specified in micrometres.
1.4 This standard does not purport to address all of the
3.1.5 molecular contaminant (non-particulate
safety concerns, if any, associated with its use. It is the
contamination), n—the molecular contaminant may be in a
responsibility of the user of this standard to establish appro-
gaseous, liquid, or solid state.
priate safety and health practices and determine the applica-
3.1.5.1 Discussion—A molecular contaminant may be uni-
bility of regulatory limitations prior to use.
formly or nonuniformly distributed, or be in the form of
droplets. Molecular contaminants account for most of the
2. Referenced Documents
NVR.
2.1 ASTM Standards:
3.1.6 degas, v—theprocessofremovinggasesfromaliquid.
D1193Specification for Reagent Water
E1235Test Method for Gravimetric Determination of Non-
4. Summary of Practice
volatile Residue (NVR) in Environmentally Controlled
4.1 Amaterial, glove, hand wipe, and so forth, is placed in
Areas for Spacecraft
a container containing the test fluid. This container is then
F324Test Method for Nonvolatile Residue of Volatile
placed in an ultrasonic cleaning bath and treated for a given
Cleaning Solvents Using the Solvent Purity Meter (With-
3 period of time at the recommended temperature for the test
drawn 1987)
fluid. This results in either a solution if the contaminant is
F331Test Method for Nonvolatile Residue of Solvent Ex-
solubleinthetestfluidoranemulsionifthecontaminantisnot
tract fromAerospace Components (Using Flash Evapora-
solubleinthetestfluid.Thetestfluidmaythenbeanalyzedfor
tor)
nonvolatile residue that was extracted from the test specimen.
4.1.1 In the case of aqueous-based agents, the material may
This practice is under the jurisdiction of ASTM Committee G04 on Compat-
be treated in accordance with Specification D1193 Type II
ibility and Sensitivity of Materials in Oxygen Enriched Atmospheres and is the
direct responsibility of Subcommittee G04.02 on Recommended Practices.
water or Type II water containing an extracting agent.
Current edition approved April 1, 2009. Published September 2009. Originally
4.1.1.1 When Type II water is used, the water and material
approved in 1995. Last previous edition approved in 2003 as G136–03. DOI:
maybeanalyzedwithoutfurthertreatment.Typicalmethodsof
10.1520/G0136-03R09.
analysis may include weighing the material before and after
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
treatment or more sophisticated analytical procedures such as
Standardsvolume information, refer to the standard’s Document Summary page on
total carbon (TC) or high-pressure liquid chromatography.
the ASTM website.
3 4.1.1.2 When cleaning agents are used, the materials are
The last approved version of this historical standard is referenced on
www.astm.org. rinsed with Type II water after the removal from the cleaning
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
G136 − 03 (2009)
shall be determined by the user.
bath and then ultrasonically cleaned in reagent water to ensure
the removal of the extracting agent. Typical methods of
7.2 Purity of Water—The water used shall meet the require-
analysis may include weighing the material before and after
ments of Specification D1193, Type II except that the require-
cleaning or more sophisticated analytical procedures such as
ment for a maximum TC of 50 kg/L shall not be required.
TC or high-pressure liquid chromatography.
7.3 Purity of Reagents—Reagent grade chemicals shall be
4.1.2 In the case of solvent-based agents, the weight of the
used in all tests. Unless otherwise indicated, all reagents shall
material before and after cleaning may be determined or the
conform to the specifications of the Committee on Analytical
solvents may be analyzed using infrared spectroscopy, gas
Reagents of the American Chemical Society where such
chromatography, gas chromatography/mass spectroscopy, or
specifications are available. Other grades may be used, pro-
the NVR determined using Test Methods E1235, F324,or
videditisfirstascertainedandthatthereagentisofsufficiently
F331, as appropriate.
high purity to permit its use without lessening the accuracy of
the determination. Detergents to be used shall be identified by
5. Significance and Use
the manufacturer and name (registered trademark, if any).
5.1 Thispracticeissuitableforthedeterminationofextract-
ablesubstancesthatmaybefoundinmaterialsusedinsystems
8. Procedure
or components requiring a high level of cleanliness, such as
8.1 Sample Preparations:
oxygensystems.Softgoods,suchassealsandvalveseats,may
8.1.1 Prepare the sample for placement in the ultrasonic
be tested as received. Gloves and wipes, or samples thereof, to
bath.
beusedincleaningoperationsmaybeevaluatedpriortouseto
8.1.1.1 To determine the amount of solvent extractable
ensure that the proposed extracting agent does not extract or
material in a wiping cloth (new or used), cut out a test section
deposit chemicals, or both, on the surface to be cleaned.
approximately 30 cm square, accurately measure and calculate
5.2 Wipes or other cleaning equipment may be tested after
the area (S), in square centimetres, and determine the mass of
use to determine the amount of contaminant removed from a
the section in grams to the nearest tenth of a milligram (mg).
surface.
Record the area and mass.
NOTE 1—The amount of material extracted may be dependent upon the
8.1.1.2 If the residue is to be determined on used wiping
frequency and power density of the ultrasonic unit.
cloths in an effort to assess the cleanliness of a part or system,
5.3 The extraction efficiency has been shown to vary with an extraction and a nonvolatile residue (NVR) or total carbon
the frequency and power density of the ultrasonic unit. The (TC) analysis shall be performed as described in 8.2 – 8.5 on
unit, therefore, must be carefully evaluated to optimize the an equivalent sample of unused cloth. Record this NVR as M2
2 2
extraction conditions.
in mg/g or as M3 in mg/cm or as TC in ppm/g or ppm/cm .
TheNVRorTCvaluemustbesubtractedfromthatdetermined
6. Apparatus
for the contaminated cloth.
8.1.1.3 Todeterminetheamountofextractablematerialina
6.1 Ultrasonic Bath, with an operating frequency range
glovetobeusedinacleaningoperation,cutseveralrectangular
from 25 to 90 kHz, a typical power range from 10 to 25 W/L,
strips from the fingers and palm areas of the glove, the areas
and a temperature controlled bath capable of maintaining a
that would typically be exposed to the cleaning solvent,
temperature between ambient and 70°C with an accuracy of
determinethemassingramstothenearesttenthofamilligram,
62°C is to be used.
and record the mass (M1). Determine the dimensions of each
6.2 Parts Pans, stainless steel container with volumes
stripincentimetres(cm)andrecordthetotalsurfaceareaofthe
between 1 and 4 L are to be used.
strips (S) in square centimetres.
6.3 A Bracket, to support the sample pans in the ultrasonic
8.2 Parts Pan Preparation—Cleanthestainlesssteelsample
bath is to be used.
parts pans. Conduct the extraction procedure selected without
NOTE 2—The bracket should be designed to hang in the ultrasonic bath
test articles to verify the cleanliness of the parts pans. Use the
without contact with the bottom.
same volume of cleaning agent for the verification that will be
6.4 Balance, a minimum capacity of 50 g with an accuracy
used on the test articles. Determine the amount of NVR or TC
of 0.1 mg.
for the parts pan using the analysis procedure that will be used
on the actual test articles. Record the amount as the blank (B)
7. Reagents
for the parts pan and cleaning agent.
7.1 Solvents—the following may be used: tetrachloroethyl-
8.3 Preliminary Procedure:
ene(perchloroethylene),trichloroethylene,methylenechloride,
8.3.1 If an extracting agent is being used that requires
and perfluorinated carbon fluids.
dilution or special preparation, carefully follow the manufac-
turer’s instructions. Use Type II water to prepare the aqueous
NOTE3—Warning:Followappropriatesafe-handlingprocedureswhen
using the solvents approved for the use application. Many solvents with
extracting solutions or as the actual extracting agent.
low TLVs present hazards to personnel working with them as well as to
8.3.2 Place the support bracket in the ultrasonic bath, fill
the systems being cleaned. The removal of these solvents from breathing
with water to the level specified by the manufacturer, heat the
gas systems must be assured. Many solvents are not considered to be
ultrasonic bath to the desired temperature, and degas the water
compatible with oxygen and must be completely removed from materials
beforetheiruseinoxygensystems.Thepreferredsolventremovalmethod for 10 min.
G136 − 03 (2009)
8.3.3 Place the selected parts pan in the support bracket in 8.6.1 Remove the parts pan from the ultrasonic bath and
the ultrasonic bath. remove the cover. Swirl the parts pan to mix the extracting
agent.
8.4 Extraction Procedure:
8.6.2 After swirling, quickly decant the extracting agent
8.4.1 Place the material or part(s) to be extracted in the
from the parts pan.
stainless steel parts pan.
8.6.3 Washthepartspanandpartswithatotalof500mLof
8.4.2 Pour a measured amount of the extracting agent into
freshType II water in three roughly equal portions and discard
the stainless steel parts pan sufficient to cover the parts. Cover
unless Type II water was used as the extracting agent. If Type
the parts pan with aluminum foil or stainless steel lids, place
II water was used as the extracting agent, combine the three
the parts pan and parts in the bracket in the ultrasonic bath,
portions with the water from 8.6.2, and set aside as the sample
adjust the water level in the bath such that it is above the
for analysis. If a surface active compound was used, repeat the
extractingagentlevelinthepartspan,andallowtheextracting
proceduresin8.3–8.5usingTypeIIwaterandusetheTypeII
agent and bath temperature to equilibrate to the desired
water as the sample for analysis.
temperature.Alternatively,preheatthepartspanandextracting
8.6.4 DeterminetheNVRofthesampleusingGTCorhigh
agent prior to the placement of the materials or parts into the
pressure liquid chromatography (see 4.1.1.2).
partspan.Thencoverthepartspanwithfoilandplacetheparts
pan into the bracket in the bath and allow the extracting agent
9. Report
to equilibrate to the temperature of the bath.
8.4.2.1 Extraction agent to parts surface area ratio shall not
9.1 Report the following information:
2 2
exceed 1000 mL/0.1 m ; the preferred ratio is 500 mL/0.1 m .
9.1.1 Identification of the part or material being cleaned
8.4.3 Subject the parts to the ultrasonic bath for 10 min.
(including tradename, part number, serial number, proper
Perform the sampling procedure as soon as possible, with a
chemical name,ASTM designation, lot number, batch number,
maximumtimelimitof120minafterturningofftheultrasonic
and manufacturer).
bath.
9.1.2 Cleaning reagent;
9.1.3 Cleaning time;
8.5 Sampling Procedure for Solvent Extracted Parts:
9.1.4 Cleaning temperature;
8.5.1 Remove the parts pan from the ultrasonic bath and
9.1.5 Frequency of the ultrasonic bath, kHz;
remove the cover. Swirl the parts pan to thoroughly mix the
9.1.6 Power density of the ultrasonic bath, W/L;
solvent.
9.1.7 Volume of extracting agent used, mL;
8.5.2 After swirling, quickly decant the solvent from the
9.1.8 Mass (M1) of parts extracted, g;
parts pan.
9.1.9 Mass (M2) of material extracted from unused wipes,
8.5.3 Washthepartspanandpartswithatotalof500mLof
2 2
mg/g, or (M3), mg/cm , or TC in ppm/g or ppm/cm ;
freshsolventinthreeroughlyequalportions,combinewiththe
9.1.10 Mass (M4) of NVR determined using Test Methods
solvent from 8.5.2, and set aside as the sample for NVR
E1235, F324,or F331;
analysis.
9.1.11 Blank (B) for the parts pan and agent, mg; and,
8.5.4 Determinethemass(M4)ofthenonvolatileresiduein
milligrams to the nearest tenth of a milligram using Test 9.1.12 Surface area (S), cm .
Methods E1235, F324,or F331. Ensure that the reported NVR
is adjusted by subtracting the NVR of an equivalent volume of 10. Keywords
“blank” solvent.
10.1 contaminant; contamination; extraction; nonvolatile
8.6 Sampling Procedure for Aqueous Extracted Materials residue; oxygen systems; total carbon (TC); ultrasonic extrac-
and Parts: tion
APPENDIX
(Nonmandatory Information)
X1. SELECTION OF ULTRASONIC BATHS
X1.1 Introduction—This appendix describes technical in- X1.2 Designing an immersible ultrasonic transducer system
formation useful to the user in the selection of ultrasonic baths requiresthatseveralfactorsbetakenintoaccount.Eachcaseis
for aqueous extraction and cleaning applications. The follow- anindividual.Thefollowinglistwillgivethereadersomeidea
ing infor
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:G136–03 Designation:G136–03 (Reapproved 2009)
Standard Practice for
Determination of Soluble Residual Contaminants in
Materials by Ultrasonic Extraction
This standard is issued under the fixed designation G 136; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice may be used to extract nonvolatile and semivolatile residues from materials such as new and used gloves, new
and used wipes, component soft goods, and so forth. When used with proposed cleaning materials (wipes, gloves, and so forth),
this practice may be used to determine the potential of the proposed solvent or other fluids to extract contaminants (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 of particulate contamination.
1.3The values stated in SI units are standard.
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 standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
E 1235 Test Method for Gravimetric Determination of Nonvolatile Residue (NVR) in Environmentally Controlled Areas for
Spacecraft
F 324 Test Method for Nonvolatile Residue of Volatile Cleaning Solvents Using the Solvent Purity Meter
F 331 Test Method for Nonvolatile Residue of Halogenated Solvent Extract fromAerospace Components Using Rotary (Using
Flash Evaporator)
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 contaminant (contamination), n—unwanted molecular and particulate matter that could affect or degrade the performance
of the components upon which they reside.
3.1.2 contaminate, v—a process of contaminating.
3.1.3 nonvolatile residue (NVR), n—residual molecular and particulate matter remaining following the filtration and controlled
evaporation of liquid containing contaminants.
3.1.4 particle (particulate contaminant), n—a piece of matter in a solid state with observable length, width, and thickness.
3.1.4.1 Discussion—The size of a particle is usually defined by its greatest dimension and is specified in micrometres.
3.1.5 molecular contaminant (non-particulate contamination), n—the molecular contaminant may be in a gaseous, liquid, or
solid state.
3.1.5.1 Discussion—A molecular contaminant may be uniformly or nonuniformly distributed, or be in the form of droplets.
Molecular contaminants account for most of the NVR.
3.1.6 degas, v—the process of removing gases from a liquid.
4. Summary of Practice
4.1 A material, glove, hand wipe, and so forth, is placed in a container containing the test fluid. This container is then placed
This practice is under the jurisdiction of ASTM Committee G04 on Compatibility and Sensitivity of Materials in Oxygen Enriched Atmospheres and is the direct
responsibility of Subcommittee G04.02 on Recommended Practices.
Current edition approved Sept. 10, 2003. Published December 2003. Originally approved in 1995. Last previous edition approved in 1996 as G136–96.
Current edition approved April 1, 2009. Published September 2009. Originally approved in 1995. Last previous edition approved in 2003 as G 136 – 03.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standardsvolume information, refer to the standard’s Document Summary page on the ASTM website.
Withdrawn
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
G136–03 (2009)
in an ultrasonic cleaning bath and treated for a given period of time at the recommended temperature for the test fluid.This results
in either a solution if the contaminant is soluble in the test fluid or an emulsion if the contaminant is not soluble in the test fluid.
The test fluid may then be analyzed for nonvolatile residue that was extracted from the test specimen.
4.1.1 In the case of aqueous-based agents, the material may be treated in accordance with Specification D 1193 Type II water
or Type II water containing an extracting agent.
4.1.1.1 When Type II water is used, the water and material may be analyzed without further treatment. Typical methods of
analysis may include weighing the material before and after treatment or more sophisticated analytical procedures such as total
carbon (TC) or high-pressure liquid chromatography.
4.1.1.2 When cleaning agents are used, the materials are rinsed withType II water after the removal from the cleaning bath and
then ultrasonically cleaned in reagent water to ensure the removal of the extracting agent.Typical methods of analysis may include
weighing the material before and after cleaning or more sophisticated analytical procedures such as TC or high-pressure liquid
chromatography.
4.1.2 In the case of solvent-based agents, the weight of the material before and after cleaning may be determined or the solvents
may be analyzed using infrared spectroscopy, gas chromatography, gas chromatography/mass spectroscopy, or the NVR
determined using Test Methods E 1235, F 324, or F 331, F324, or F331, as appropriate.
5. Significance and Use
5.1 This practice is suitable for the determination of extractable substances that may be found in materials used in systems or
components requiring a high level of cleanliness, such as oxygen systems. Soft goods, such as seals and valve seats, may be tested
as received. Gloves and wipes, or samples thereof, to be used in cleaning operations may be evaluated prior to use to ensure that
the proposed extracting agent does not extract or deposit chemicals, or both, on the surface to be cleaned.
5.2 Wipesorothercleaningequipmentmaybetestedafterusetodeterminetheamountofcontaminantremovedfromasurface.
NOTE 1—The amount of material extracted may be dependent upon the frequency and power density of the ultrasonic unit.
5.3 The extraction efficiency has been shown to vary with the frequency and power density of the ultrasonic unit. The unit,
therefore, must be carefully evaluated to optimize the extraction conditions.
6. Apparatus
6.1 Ultrasonic Bath, with an operating frequency range from 25 to 90 kHz, a typical power range from 10 to 25 W/L, and a
temperature controlled bath capable of maintaining a temperature between ambient and 70°C with an accuracy of 62°C is to be
used.
6.2 Parts Pans, stainless steel container with volumes between 1 and 4 L are to be used.
6.3 A Bracket, to support the sample pans in the ultrasonic bath is to be used.
NOTE 2—The bracket should be designed to hang in the ultrasonic bath without contact with the bottom.
6.4 Balance, a minimum capacity of 50 g with an accuracy of 0.1 mg.
7. Reagents
7.1 Solvents—the following may be used: tetrachloroethylene (perchloroethylene), trichloroethylene, methylene chloride, and
perfluorinated carbon fluids.
NOTE 3—Warning: Follow appropriate safe-handling procedures when using the solvents approved for the use application. Many solvents with low
TLVs present hazards to personnel working with them as well as to the systems being cleaned. The removal of these solvents from breathing gas systems
must be assured. Many solvents are not considered to be compatible with oxygen and must be completely removed from materials before their use in
oxygen systems. The preferred solvent removal method shall be determined by the user.
7.2 Purity of Water—The water used shall meet the requirements of Specification D 1193, Type II except that the requirement
for a maximum TC of 50 kg/L shall not be required.
7.3 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, all reagents shall
conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are available. Other grades may be used, provided it is first ascertained and that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination. Detergents to be used shall be identified by the
manufacturer and name (registered trademark, if any).
8. Procedure
8.1 Sample Preparations:
8.1.1 Prepare the sample for placement in the ultrasonic bath.
8.1.1.1 To determine the amount of solvent extractable material in a wiping cloth (new or used), cut out a test section
approximately 30 cm square, accurately measure and calculate the area (S), in square centimetres, and determine the mass of the
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 wiping cloths 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 an
G136–03 (2009)
2 2
equivalentsampleofunusedcloth.RecordthisNVRasM2inmg/gorasM3inmg/cm orasTCinppm/gorppm/cm .TheNVR
or TC value must be subtracted from that determined for the contaminated cloth.
8.1.1.3 To determine the amount of extractable material in a glove to be used in a cleaning operation, cut several rectangular
strips from the fingers and palm areas of the glove, the areas that 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 each strip in
centimetres (cm) and record the total surface area of the strips (S) in square centimetres.
8.2 Parts Pan Preparation—Clean the stainless steel sample parts pans. Conduct the extraction procedure selected without test
articles to verify the cleanliness of the parts pans. Use the same volume of cleaning agent for the verification that will be used on
the test articles. Determine the amount of NVR orTC for the parts pan using the analysis procedure that will be used 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 requires dilution or special preparation, carefully follow the manufacturer’s
instructions. Use Type II water to prepare the aqueous extracting solutions or as the actual extracting agent.
8.3.2 Place the support bracket in the ultrasonic bath, fill with water to the level specified by the manufacturer, heat the
ultrasonic bath to the desired temperature, and degas the water for 10 min.
8.3.3 Place the selected parts pan in the support bracket in the ultrasonic bath.
8.4 Extraction Procedure:
8.4.1 Place the material or part(s) to be extracted in the stainless steel parts pan.
8.4.2 Pour a measured amount of the extracting agent into the stainless steel parts pan sufficient to cover the parts. Cover the
parts pan with aluminum foil or stainless steel lids, place the parts pan and parts in the bracket in the ultrasonic bath, adjust the
water level in the bath such that it is above the extracting agent level in the parts pan, and allow the extracting agent and bath
temperature to equilibrate to the desired temperature. Alternatively, preheat the parts pan and extracting agent prior to the
placement of the materials or parts into the parts pan. Then cover the parts pan with foil and place the parts pan into the bracket
in the bath and allow the extracting agent to equilibrate to the temperature of the bath.
2 2
8.4.2.1 Extraction agent to parts surface area ratio shall not exceed 1000 mL/0.1 m ; the preferred ratio is 500 mL/0.1 m .
8.4.3 Subject the parts to the ultrasonic bath for 10 min. Perform the sampling procedure as soon as possible, with a maximum
time limit of 120 min after turning off the ultrasonic bath.
8.5 Sampling Procedure for Solvent Extracted Parts:
8.5.1 Remove the parts pan from the ultrasonic bath and remove the cover. Swirl the parts pan to thoroughly mix the solvent.
8.5.2 After swirling, quickly decant the solvent from the parts pan.
8.5.3 Wash the parts pan and parts with a total of 500 mL of fresh solvent in three roughly equal portions, combine with the
solvent from 8.5.2, and set aside as the sample for NVR analysis.
8.5.4 Determine the mass (M4) of the nonvolatile residue in milligrams to the nearest tenth of a milligram using Test Methods
E 1235, F 324, or F 331, F324, or F331. Ensure that the reported NVR is adjusted by subtracting the NVR of an equivalent volume
of “blank” solvent.
8.6 Sampling Procedure for Aqueous Extracted Materials and Parts:
8.6.1 Remove the parts pan from the ultrasonic bath and remove the cover. Swirl the parts pan to mix the extracting agent.
8.6.2 After swirling, quickly decant the extracting agent from the parts pan.
8.6.3 Wash the parts pan and parts with a total of 500 mL of fresh Type II water in three roughly equal portions and discard
unlessType II water was used as the extracting agent. IfType II water was used as the extracting agent, combine the three portions
with the water from 8.6.2, and set aside as the sample for analysis. If a surface active compound was used, repeat the procedures
in 8.3-8.5 using Type II water and use the Type II water as the sample for analysis.
8.6.4 Determine the NVR of the sample using G TC or high pressure liquid chromatography (see 4.1.1.2).
9. Report
9.1 Report the following information:
9.1.1 Identification of the part or material being cleaned (including tradename, part number, serial number, proper chemical
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 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;
2 2
9.1.9 Mass (M2) of material extracted from unused wipes, mg/g, or (M3), mg/cm , or TC in ppm/g or ppm/cm ;
9.1.10 Mass (M4) of NVR determined using Test Methods E 1235, F 324, or F 331, F32
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