ASTM G136-96
(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
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 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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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: G 136 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.3 nonvolatile residue (NVR), n—residual molecular and
particulate matter remaining following the filtration and con-
1.1 This practice may be used to extract nonvolatile and
trolled evaporation of liquid containing contaminants.
semivolatile residues from materials such as new and used
3.1.4 particle (particulate contaminant), n—a piece of mat-
gloves, new and used wipes, component soft goods, and so
ter in a solid state with observable length, width, and thickness.
forth. When used with proposed cleaning materials (wipes,
3.1.4.1 Discussion—The size of a particle is usually defined
gloves, and so forth), this practice may be used to determine
by its greatest dimension and is specified in micrometres.
the potential of the proposed solvent or other fluids to extract
3.1.5 molecular contaminant (non-particulate contamina-
contaminants (plasticizers, residual detergents, brighteners,
tion), n—the molecular contaminant may be in a gaseous,
and so forth.) and deposit them on the surface being cleaned.
liquid, or solid state.
1.2 This practice is not suitable for the evaluation of
3.1.5.1 Discussion—A molecular contaminant may be uni-
particulate contamination.
formly or nonuniformly distributed, or be in the form of
1.3 The values stated in SI units are standard.
droplets. Molecular contaminants account for most of the
1.4 This standard does not purport to address all of the
NVR.
safety concerns, if any, associated with its use. It is the
3.1.6 degas, v—the process of removing gases from a
responsibility of the user of this standard to establish appro-
liquid.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Practice
2. Referenced Documents 4.1 A material, glove, hand wipe, and so forth, is placed in
a container containing the test fluid. This container is then
2.1 ASTM Standards:
placed in an ultrasonic cleaning bath and treated for a given
D 1193 Specification for Reagent Water
period of time at the recommended temperature for the test
E 1235 Test Method for Gravimetric Determination of Non-
fluid. This results in either a solution if the contaminant is
volatile Residue (NVR) in Environmentally Controlled
soluble in the test fluid or an emulsion if the contaminant is not
Areas for Spacecraft
soluble in the test fluid. The test fluid may then be analyzed for
F 324 Test Method for Nonvolatile Residue of Volatile
nonvolatile residue that was extracted from the test specimen.
Cleaning Solvents Using the Solvent Purity Meter
4.1.1 In the case of aqueous-based agents, the material may
F 331 Test Method for Nonvolatile Residue of Halogenated
be treated in accordance with Specification D 1193 Type II
Solvent Extract from Aerospace Components Using Rotary
water or Type II water containing an extracting agent.
Flash Evaporator
4.1.1.1 When Type II water is used, the water and material
3. Terminology
may be analyzed without further treatment. Typical methods of
analysis may include weighing the material before and after
3.1 Definitions of Terms Specific to This Standard:
treatment or more sophisticated analytical procedures such as
3.1.1 contaminant (contamination), n—unwanted molecular
total carbon (TC) or high-pressure liquid chromatography.
and particulate matter that could affect or degrade the perfor-
4.1.1.2 When cleaning agents are used, the materials are
mance of the components upon which they reside.
rinsed with Type II water after the removal from the cleaning
3.1.2 contaminate, v—a process of contaminating.
bath and then ultrasonically cleaned in reagent water to ensure
the removal of the extracting agent. Typical methods of
This practice is under the jurisdiction of ASTM Committee G-4 on Compat-
analysis may include weighing the material before and after
ibility and Sensitivity of Materials in Oxygen-Enriched Atmospheres and is the
cleaning or more sophisticated analytical procedures such as
direct responsibility of Subcommittee G04.02 on Recommended Practices.
Current edition approved March 10, 1996. Published August 1996. Originally
TC or high-pressure liquid chromatography.
published as G 136 – 95. Last previous edition G 136 – 95.
4.1.2 In the case of solvent-based agents, the weight of the
Annual Book of ASTM Standards, Vol 11.01.
3 material before and after cleaning may be determined or the
Annual Book of ASTM Standards, Vol 15.03.
solvents may be analyzed using infrared spectroscopy, gas
Discontinued; see 1986 Annual Book of ASTM Standards, Vol 10.05.
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
G 136
chromatography, gas chromatography/mass spectroscopy, or high purity to permit its use without lessening the accuracy of
the NVR determined using Test Methods E 1235, F 324, or the determination. Detergents to be used shall be identified by
F 331, as appropriate. the manufacturer and name (registered trademark, if any).
8. Procedure
5. Significance and Use
8.1 Sample Preparations:
5.1 This practice is suitable for the determination of extract-
8.1.1 Prepare the sample for placement in the ultrasonic
able substances that may be found in materials used in systems
bath.
or components requiring a high level of cleanliness, such as
8.1.1.1 To determine the amount of solvent extractable
oxygen systems. Soft goods, such as seals and valve seats, may
material in a wiping cloth (new or used), cut out a test section
be tested as received. Gloves and wipes, or samples thereof, to
approximately 30 cm square, accurately measure and calculate
be used in cleaning operations may be evaluated prior to use to
the area (S), in square centimetres, and determine the mass of
ensure that the proposed extracting agent does not extract or
the section in grams to the nearest tenth of a milligram (mg).
deposit chemicals, or both, on the surface to be cleaned.
Record the area and mass.
5.2 Wipes or other cleaning equipment may be tested after
8.1.1.2 If the residue is to be determined on used wiping
use to determine the amount of contaminant removed from a
cloths in an effort to assess the cleanliness of a part or system,
surface.
an extraction and a nonvolatile residue (NVR) or total carbon
NOTE 1—The amount of material extracted may be dependent upon the
(TC) analysis shall be performed as described in 8.2-8.5 on an
frequency and power density of the ultrasonic unit.
equivalent sample of unused cloth. Record this NVR as M2 in
2 2
5.3 The extraction efficiency has been shown to vary with
mg/g or as M3 in mg/cm or as TC in ppm/g or ppm/cm . The
the frequency and power density of the ultrasonic unit. The
NVR or TC value must be subtracted from that determined for
unit, therefore, must be carefully evaluated to optimize the
the contaminated cloth.
extraction conditions.
8.1.1.3 To determine the amount of extractable material in a
glove to be used in a cleaning operation, cut several rectangular
6. Apparatus
strips from the fingers and palm areas of the glove, the areas
6.1 Ultrasonic Bath, with an operating frequency range that would typically be exposed to the cleaning solvent,
determine the mass in grams to the nearest tenth of a milligram,
from 25 to 90 kHz, a typical power range from 10 to 25 W/L,
and a temperature controlled bath capable of maintaining a and record the mass (M1). Determine the dimensions of each
strip in centimetres (cm) and record the total surface area of the
temperature between ambient and 70°C with an accuracy of
62°C is to be used. strips (S) in square centimetres.
8.2 Parts Pan Preparation—Clean the stainless steel
6.2 Parts Pans, stainless steel container with volumes
between 1 and 4 L are to be used. sample parts pans. Conduct the extraction procedure selected
without test articles to verify the cleanliness of the parts pans.
6.3 A Bracket, to support the sample pans in the ultrasonic
Use the same volume of cleaning agent for the verification that
bath is to be used.
will be used on the test articles. Determine the amount of NVR
NOTE 2—The bracket should be designed to hang in the ultrasonic bath
or TC for the parts pan using the analysis procedure that will be
without contact with the bottom.
used on the actual test articles. Record the amount as the blank
6.4 Balance, a minimum capacity of 50 g with an accuracy
(B) for the parts pan and cleaning agent.
of 0.1 mg.
8.3 Preliminary Procedure:
8.3.1 If an extracting agent is being used that requires
7. Reagents
dilution or special preparation, carefully follow the manufac-
7.1 Solvents—the following may be used: tetrachloroethyl-
turer’s instructions. Use Type II water to prepare the aqueous
ene (perchloroethylene), trichloroethylene, methylene chloride,
extracting solutions or as the actual extracting agent.
and perfluorinated carbon fluids.
8.3.2 Place the support bracket in the ultrasonic bath, fill
with water to the level specified by the manufacturer, heat the
NOTE 3—Warning: Follow appropriate safe handling procedures when
ultrasonic bath to the desired temperature, and degas the water
using solvents such as tetrachloroethylene (perchloroethylene), trichloro-
ethylene, methylene chloride that have relative low threshold limit values. for 10 min.
Many solvents are not considered to be compatible with oxygen and must
8.3.3 Place the selected parts pan in the support bracket in
be completely removed from materials prior to use in oxygen systems. The
the ultrasonic bath.
preferred method of removal shall be determined by the user.
8.4 Extraction Procedure:
7.2 Purity of Water—The water used shall meet the require-
8.4.1 Place the material or part(s) to be extracted in the
ments of Specification D 1193, Type II except that the require- stainless steel parts pan.
ment for a maximum TC of 50 kg/L shall not be required. 8.4.2 Pour a measured amount of the extracting agent into
7.3 Purity of Reagents—Reagent grade chemicals shall be the stainless steel parts pan sufficient to cover the parts. Cover
used in all tests. Unless otherwise indicated, all reagents shall the parts pan with aluminum foil or stainless steel lids, place
conform to the specifications of the Committee on Analytical the parts pan and parts in the bracket in the ultrasonic bath,
Reagents of the American Chemical Society where such adjust the water level in the bath such that it is above the
specifications are available. Other grades may be used, pro- extracting agent level in the parts pan, and allow the extracting
vided it is first ascertained and that the reagent is of sufficiently agent and bath temperature to equilibrate to the desired
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
G 136
temperature. Alternatively, preheat the parts pan and extracting unless Type II water was used as the extracting agent. If Type
agent prior to the placement of the materials or parts into the II water was used as the extracting agent, combine the three
parts pan. Then cover the parts pan with foil and place the parts portions with the water from 8.6.2, and set aside as the sample
pan into the bracket in the bath and allow the extracting agent for analysis. If a surface active compound was used, repeat the
to equilibrate to the temperature of the bath. procedures in 8.3-8.5 using Type II water and use the Type II
8.4.2.1 Extraction agent to parts surface area ratio shall not water as the sample for analysis.
2 2
exceed 1000 mL/0.1 m ; the preferred ratio is 500 mL/0.1 m .
8.6.4 Determine the NVR of the sample using G TC or high
8.4.3 Subject the parts to the ultrasonic bath for 10 min.
pressure liquid chromatography (see 4.1.1.2).
Perform the sampling procedure as soon as possible, with a
maximum time limit of 120 min after turning off the ultrasonic 9. Report
bath.
9.1 Report the following information:
8.5 Sampling Procedure for Solvent Extracted Parts:
9.1.1 Identification of the part or material being cleaned
8.5.1 Remove the parts pan from the ultrasonic bath and
(including tradename, part number, serial number, proper
remove the cover. Swirl the parts pan to thoroughly mix the
chemical name, ASTM designation, lot number, batch number,
solvent.
and manufacturer).
8.5.2 After swirling, quickly decant the solvent from the
9.1.2 Cleaning reagent;
parts pan.
9.1.3 Cleaning time;
8.5.3 Wash the parts pan and parts with a total of 500 mL of
9.1.4 Cleaning temperature;
fresh solvent in three roughly equal portions, combine with the
solvent from 8.5.2, and set aside as the sample for NVR 9.1.5 Frequency of the ultrasonic bath, kHz;
analysis. 9.1.6 Power density of the ultrasonic bath, W/L;
8.5.4 Determine the mass (M4) of the nonvolatile residue in
9.1.7 Volume of extracting agent used, mL;
milligrams to the nearest tenth of a milligram using Test
9.1.8 Mass (M1) of parts extracted, g;
Methods E 1235, F 324, or F 331. Ensure that the reported
9.1.9 Mass (M2) of material extracted from unused wipes,
NVR is adjusted by subtracting the NVR of an equivalent 2 2
mg/g, or (M3), mg/cm , or TC in ppm/g or ppm/cm ;
volume of “blank” solvent.
9.1.10 Mass (M4) of NVR determined using Test Methods
8.6 Sampling Procedure for Aqueous Extracted Materials
E 1235, F 324, or F 331;
and Parts:
9.1.11 Blank (B) for the parts pan and agent, mg; and,
8.6.1 Remove the parts pan from the ultrasonic bath and
9.1.12 Surface area (S), cm .
remove the cover. Swirl the parts pan to mix the extracting
agent.
10. Keywords
8.6.2 After swirling, quickly decant the extracting agent
from the parts pan. 10.1 contaminant; contamination; extraction; nonvolatile
8.6.3 Wash the parts pan and parts with a total of 500 mL of residue; oxygen systems; total carbon (TC); ultrasonic extrac-
fresh Type II water in three roughly equal portions and discard tion
APPENDIX
(Nonmandatory Information)
X1. SELECTION OF ULTRASONIC BATHS
X1.1 Introduction—This appendix describes technical in- X1.2.1.1 Volume—cubic measure or gallons.
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