ASTM G136-03(2016)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: G136 − 03 (Reapproved 2016)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial changes made throughout in May 2017.
1. Scope Areas for Spacecraft
F324 Test Method for Nonvolatile Residue of Volatile
1.1 This practice may be used to extract nonvolatile and
Cleaning Solvents Using the Solvent Purity Meter (With-
semivolatile residues from materials such as new and used
drawn 1987)
gloves, new and used wipes, component soft goods, and so
F331 Test Method for Nonvolatile Residue of Solvent Ex-
forth. When used with proposed cleaning materials (wipes,
tract from Aerospace Components (Using Flash Evapora-
gloves, and so forth), this practice may be used to determine
tor)
the potential of the proposed solvent or other fluids to extract
contaminants (plasticizers, residual detergents, brighteners,
3. Terminology
and so forth) and deposit them on the surface being cleaned.
3.1 Definitions of Terms Specific to This Standard:
1.2 This practice is not suitable for the evaluation of
3.1.1 contaminant (contamination), n—unwanted molecular
particulate contamination.
and particulate matter that could affect or degrade the perfor-
1.3 The values stated in SI units are to be regarded standard.
mance of the components upon which they reside.
No other units of measurement are included in this standard.
3.1.2 contaminate, v—a process of contaminating.
1.4 This standard does not purport to address all of the
3.1.3 nonvolatile residue (NVR), n—residual molecular and
safety concerns, if any, associated with its use. It is the
particulate matter remaining following the filtration and con-
responsibility of the user of this standard to establish appro-
trolled evaporation of liquid containing contaminants.
priate safety and health practices and determine the applica-
3.1.4 particle (particulate contaminant), n—a piece of mat-
bility of regulatory limitations prior to use.
ter in a solid state with observable length, width, and thickness.
1.5 This international standard was developed in accor-
3.1.4.1 Discussion—The size of a particle is usually defined
dance with internationally recognized principles on standard-
by its greatest dimension and is specified in micrometres.
ization established in the Decision on Principles for the
3.1.5 molecular contaminant (non-particulate
Development of International Standards, Guides and Recom-
contamination), n—the molecular contaminant may be in a
mendations issued by the World Trade Organization Technical
gaseous, liquid, or solid state.
Barriers to Trade (TBT) Committee.
3.1.5.1 Discussion—A molecular contaminant may be uni-
2. Referenced Documents
formly or nonuniformly distributed, or be in the form of
droplets. Molecular contaminants account for most of the
2.1 ASTM Standards:
NVR.
D1193 Specification for Reagent Water
E1235 Test Method for Gravimetric Determination of Non- 3.1.6 degas, v—the process of removing gases from a liquid.
volatile Residue (NVR) in Environmentally Controlled
4. Summary of Practice
4.1 A material, glove, hand wipe, and so forth, is placed in
This practice is under the jurisdiction of ASTM Committee G04 on Compat-
a container containing the test fluid. This container is then
ibility and Sensitivity of Materials in Oxygen Enriched Atmospheres and is the
placed in an ultrasonic cleaning bath and treated for a given
direct responsibility of Subcommittee G04.02 on Recommended Practices.
Current edition approved May 1, 2016. Published June 2016. Originally
period of time at the recommended temperature for the test
approved in 1995. Last previous edition approved in 2009 as G136 – 03(2009).
fluid. This results in either a solution if the contaminant is
DOI: 10.1520/G0136-03R16.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
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G136 − 03 (2016)
soluble in the test fluid or an emulsion if the contaminant is not 6.4 Balance, a minimum capacity of 50 g with an accuracy
soluble in the test fluid. The test fluid may then be analyzed for of 0.1 mg.
nonvolatile residue that was extracted from the test specimen.
4.1.1 In the case of aqueous-based agents, the material may 7. Reagents
be treated in accordance with Specification D1193 Type II
7.1 Solvents—the following may be used: tetrachloroethyl-
water or Type II water containing an extracting agent.
ene (perchloroethylene), trichloroethylene, methylene chloride,
4.1.1.1 When Type II water is used, the water and material
and perfluorinated carbon fluids.
may be analyzed without further treatment. Typical methods of
NOTE 3—Warning: Follow appropriate safe handling procedures when
analysis may include weighing the material before and after
using the solvents approved for the use application. Many solvents with
treatment or more sophisticated analytical procedures such as
low TLVs present hazards to personnel working with them as well as to
total carbon (TC) or high-pressure liquid chromatography.
the systems being cleaned. The removal of these solvents from breathing
4.1.1.2 When cleaning agents are used, the materials are gas systems must be assured. Many solvents are not considered to be
compatible with oxygen and must be completely removed from materials
rinsed with Type II water after the removal from the cleaning
before their use in oxygen systems. The preferred solvent removal method
bath and then ultrasonically cleaned in reagent water to ensure
shall be determined by the user.
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.
4.1.2 In the case of solvent-based agents, the weight of the
7.3 Purity of Reagents—Reagent-grade chemicals shall be
material before and after cleaning may be determined or the
used in all tests. Unless otherwise indicated, all reagents shall
solvents may be analyzed using infrared spectroscopy, gas
conform to the specifications of the Committee on Analytical
chromatography, gas chromatography/mass spectroscopy, or
Reagents of the American Chemical Society where such
the NVR determined using Test Methods E1235, F324, or
specifications are available. Other grades may be used, pro-
F331, as appropriate.
vided it is first ascertained and that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
5. Significance and Use the determination. Detergents to be used shall be identified by
the manufacturer and name (registered trademark, if any).
5.1 This practice is suitable for the determination of extract-
able substances that may be found in materials used in systems
8. Procedure
or components requiring a high level of cleanliness, such as
oxygen systems. Soft goods, such as seals and valve seats, may 8.1 Sample Preparations:
be tested as received. Gloves and wipes, or samples thereof, to 8.1.1 Prepare the sample for placement in the ultrasonic
be used in cleaning operations may be evaluated prior to use to bath.
ensure that the proposed extracting agent does not extract or
8.1.1.1 To determine the amount of solvent-extractable
deposit chemicals, or both, on the surface to be cleaned. material in a wiping cloth (new or used), cut out a test section
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
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extraction conditions.
in mg/g or as M3 in mg/cm or as TC in ppm/g or ppm/cm .
The NVR or TC value must be subtracted from that determined
6. Apparatus
for the contaminated cloth.
8.1.1.3 To determine the amount of extractable material in a
6.1 Ultrasonic Bath, with an operating frequency range
glove to be used in a cleaning operation, cut several rectangular
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
determine the mass in grams to the nearest tenth of a milligram,
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
strip in centimetres (cm) and record the total surface area of the
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—Clean the stainless steel sample
bath is to be used.
parts pans. Conduct the extraction procedure selected without
test articles to verify the cleanliness of the parts pans. Use the
NOTE 2—The bracket should be designed to hang in the ultrasonic bath
without contact with the bottom. same volume of cleaning agent for the verification that will be
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G136 − 03 (2016)
used on the test articles. Determine the amount of NVR or TC 8.5.4 Determine the mass (M4) of the nonvolatile residue in
for the parts pan using the analysis procedure that will be used milligrams to the nearest tenth of a milligram using Test
on the actual test articles. Record the amount as the blank (B) Methods E1235, F324, or F331. Ensure that the reported NVR
for the parts pan and cleaning agent. is adjusted by subtracting the NVR of an equivalent volume of
“blank” solvent.
8.3 Preliminary Procedure:
8.3.1 If an extracting agent is being used that requires 8.6 Sampling Procedure for Aqueous Extracted Materials
dilution or special preparation, carefully follow the manufac- and Parts:
turer’s instructions. Use Type II water to prepare the aqueous 8.6.1 Remove the parts pan from the ultrasonic bath and
extracting solutions or as the actual extracting agent. remove the cover. Swirl the parts pan to mix the extracting
8.3.2 Place the support bracket in the ultrasonic bath, fill agent.
with water to the level specified by the manufacturer, heat the 8.6.2 After swirling, quickly decant the extracting agent
ultrasonic bath to the desired temperature, and degas the water from the parts pan.
for 10 min. 8.6.3 Wash the parts pan and parts with a total of 500 mL of
8.3.3 Place the selected parts pan in the support bracket in fresh Type II water in three roughly equal portions and discard
the ultrasonic bath. unless Type II water was used as the extracting agent. If Type
II water was used as the extracting agent, combine the three
8.4 Extraction Procedure:
portions with the water from 8.6.2, and set aside as the sample
8.4.1 Place the material or part(s) to be extracted in the
for analysis. If a surface active compound was used, repeat the
stainless steel parts pan.
procedures in 8.3 – 8.5 using Type II water and use the Type II
8.4.2 Pour a measured amount of the extracting agent into
water as the sample for analysis.
the stainless steel parts pan sufficient to cover the parts. Cover
8.6.4 Determine the NVR of the sample using TC or high
the parts pan with aluminum foil or a stainless steel lid, place
pressure liquid chromatography (see 4.1.1.2).
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
9. Report
extracting agent level in the parts pan, and allow the extracting
agent and bath temperature to equilibrate to the desired 9.1 Report the following information:
temperature. Alternatively, preheat the parts pan and extracting 9.1.1 Identification of the part or material being cleaned
agent prior to the placement of the materials or parts into the (including tradename, part number, serial number, proper
parts pan. Then cover the parts pan with foil and place the parts chemical name, ASTM designation, lot number, batch number,
pan into the bracket in the bath and allow the extracting agent and manufacturer).
to equilibrate to the temperature of the bath. 9.1.2 Cleaning reagent;
8.4.2.1 The ratio of extraction agent to part’s surface area 9.1.3 Cleaning time;
shall not exceed 1000 mL/0.1 m ; the preferred ratio is 500 9.1.4 Cleaning temperature;
mL/0.1 m . 9.1.5 Frequency of the ultrasonic bath, kHz;
8.4.3 Subject the parts to the ultrasonic bath for 10 min. 9.1.6 Power density of the ultrasonic bath, W/L;
Perform the sampling procedure as soon as possible, with a 9.1.7 Volume of extracting agent used, mL;
maximum time limit of 120 min after turning off the ultrasonic 9.1.8 Mass (M1) of parts extracted, g;
bath. 9.1.9 Mass (M2) of material extracted from unused wipes,
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mg/g, or (M3), mg/cm , or TC in ppm/g or ppm/cm ;
8.5 Sampling Procedure for Solvent Extracted Parts:
9.1.10 Mass (M4) of NVR determined using Test Methods
8.5.1 Remove the parts pan from the ultrasonic bath and
E1235, F324, or F331;
remove the cover. Swirl the parts pan to thoroughly mix the
9.1.11 Blank (B) for the parts pan and agent, mg; and,
solvent.
9.1.12 Surface area (S), cm .
8.5.2 After swirling, quickly decant the solvent from the
parts pan.
10. Keywords
8.5.3 Wash the par
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