ASTM G136-03(2023)e1
(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
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 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.
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.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
´1
Designation: G136 − 03 (Reapproved 2023)
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—Editorially updated formatting in 7.1 in July 2023.
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, health, and environmental practices and deter-
3.1.4 particle (particulate contaminant), n—a piece of mat-
mine the applicability 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
direct responsibility of Subcommittee G04.02 on Recommended Practices. placed in an ultrasonic cleaning bath and treated for a given
Current edition approved July 1, 2023. Published July 2023. Originally approved
period of time at the recommended temperature for the test
in 1995. Last previous edition approved in 2016 as G136 – 03 (2016). DOI:
fluid. This results in either a solution if the contaminant is
10.1520/G0136-03R23E01.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
G136 − 03 (2023)
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.
7. Reagents
4.1.1 In the case of aqueous-based agents, the material may
7.1 Solvents—the following may be used: tetrachloroethyl-
be treated in accordance with Specification D1193 Type II
ene (perchloroethylene), trichloroethylene, methylene chloride,
water or Type II water containing an extracting agent.
and perfluorinated carbon fluids. Warning—Follow appropri-
4.1.1.1 When Type II water is used, the water and material
ate safe handling procedures when using the solvents approved
may be analyzed without further treatment. Typical methods of
for the use application. Many solvents with low TLVs present
analysis may include weighing the material before and after
hazards to personnel working with them as well as to the
treatment or more sophisticated analytical procedures such as
systems being cleaned. The removal of these solvents from
total carbon (TC) or high-pressure liquid chromatography.
breathing gas systems must be assured. Many solvents are not
4.1.1.2 When cleaning agents are used, the materials are
considered to be compatible with oxygen and must be com-
rinsed with Type II water after the removal from the cleaning
pletely removed from materials before their use in oxygen
bath and then ultrasonically cleaned in reagent water to ensure
systems. The preferred solvent removal method shall be
the removal of the extracting agent. Typical methods of
determined by the user.
analysis may include weighing the material before and after
cleaning or more sophisticated analytical procedures such as
7.2 Purity of Water—The water used shall meet the require-
TC or high-pressure liquid chromatography.
ments of Specification D1193, Type II except that the require-
4.1.2 In the case of solvent-based agents, the weight of the
ment for a maximum TC of 50 kg/L shall not be required.
material before and after cleaning may be determined or the
7.3 Purity of Reagents—Reagent-grade chemicals shall be
solvents may be analyzed using infrared spectroscopy, gas
used in all tests. Unless otherwise indicated, all reagents shall
chromatography, gas chromatography/mass spectroscopy, or
conform to the specifications of the Committee on Analytical
the NVR determined using Test Methods E1235, F324, or
Reagents of the American Chemical Society where such
F331, as appropriate.
specifications are available. Other grades may be used, pro-
vided it is first ascertained and that the reagent is of sufficiently
5. Significance and Use
high purity to permit its use without lessening the accuracy of
5.1 This practice is suitable for the determination of extract-
the determination. Detergents to be used shall be identified by
able substances that may be found in materials used in systems
the manufacturer and name (registered trademark, if any).
or components requiring a high level of cleanliness, such as
8. Procedure
oxygen systems. Soft goods, such as seals and valve seats, may
be tested as received. Gloves and wipes, or samples thereof, to 8.1 Sample Preparations:
be used in cleaning operations may be evaluated prior to use to 8.1.1 Prepare the sample for placement in the ultrasonic
ensure that the proposed extracting agent does not extract or bath.
deposit chemicals, or both, on the surface to be cleaned.
8.1.1.1 To determine the amount of solvent-extractable
material in a wiping cloth (new or used), cut out a test section
5.2 Wipes or other cleaning equipment may be tested after
approximately 30 cm square, accurately measure and calculate
use to determine the amount of contaminant removed from a
the area (S), in square centimetres, and determine the mass of
surface.
the section in grams to the nearest tenth of a milligram (mg).
NOTE 1—The amount of material extracted may be dependent upon the
Record the area and mass.
frequency and power density of the ultrasonic unit.
8.1.1.2 If the residue is to be determined on used wiping
5.3 The extraction efficiency has been shown to vary with
cloths in an effort to assess the cleanliness of a part or system,
the frequency and power density of the ultrasonic unit. The
an extraction and a nonvolatile residue (NVR) or total carbon
unit, therefore, must be carefully evaluated to optimize the
(TC) analysis shall be performed as described in 8.2 – 8.5 on
extraction conditions.
an equivalent sample of unused cloth. Record this NVR as M2
2 2
in mg/g or as M3 in mg/cm or as TC in ppm/g or ppm/cm .
6. Apparatus
The NVR or TC value must be subtracted from that determined
for the contaminated cloth.
6.1 Ultrasonic Bath, with an operating frequency range
8.1.1.3 To determine the amount of extractable material in a
from 25 kHz to 90 kHz, a typical power range from 10 W ⁄L to
glove to be used in a cleaning operation, cut several rectangular
25 W ⁄L, and a temperature-controlled bath capable of main-
strips from the fingers and palm areas of the glove, the areas
taining a temperature between ambient and 70 °C with an
that would typically be exposed to the cleaning solvent,
accuracy of 62 °C is to be used.
determine the mass in grams to the nearest tenth of a milligram,
6.2 Parts Pans, stainless steel container with volumes
and record the mass (M1). Determine the dimensions of each
between 1 L and 4 L are to be used.
strip in centimetres (cm) and record the total surface area of the
6.3 A Bracket, to support the sample pans in the ultrasonic strips (S) in square centimetres.
bath is to be used.
8.2 Parts Pan Preparation—Clean the stainless steel sample
parts pans. Conduct the extraction procedure selected without
NOTE 2—The bracket should be designed to hang in the ultrasonic bath
without contact with the bottom. test articles to verify the cleanliness of the parts pans. Use the
´1
G136 − 03 (2023)
same volume of cleaning agent for the verification that will be 8.5.4 Determine the mass (M4) of the nonvolatile residue in
used on the test articles. Determine the amount of NVR or TC milligrams to the nearest tenth of a milligram using Test
for the parts pan using the analysis procedure that will be used Methods E1235, F324, or F331. Ensure that the reported NVR
on the actual test articles. Record the amount as the blank (B) is adjusted by subtracting the NVR of an equivalent volume of
for the parts pan and cleaning agent. “blank” solvent.
8.3 Preliminary Procedure: 8.6 Sampling Procedure for Aqueous Extracted Materials
8.3.1 If an extracting agent is being used that requires
and Parts:
dilution or special preparation, carefully follow the manufac-
8.6.1 Remove the parts pan from the ultrasonic bath and
turer’s instructions. Use Type II water to prepare the aqueous
remove the cover. Swirl the parts pan to mix the extracting
extracting solutions or as the actual extracting agent.
agent.
8.3.2 Place the support bracket in the ultrasonic bath, fill
8.6.2 After swirling, quickly decant the extracting agent
with water to the level specified by the manufacturer, heat the
from the parts pan.
ultrasonic bath to the desired temperature, and degas the water
8.6.3 Wash the parts pan and parts with a total of 500 mL of
for 10 min.
fresh Type II water in three roughly equal portions and discard
8.3.3 Place the selected parts pan in the support bracket in
unless Type II water was used as the extracting agent. If Type
the ultrasonic bath.
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
8.4 Extraction Procedure:
for analysis. If a surface active compound was used, repeat the
8.4.1 Place the material or part(s) to be extracted in the
procedures in 8.3 – 8.5 using Type II water and use the Type II
stainless steel parts pan.
water as the sample for analysis.
8.4.2 Pour a measured amount of the extracting agent into
8.6.4 Determine the NVR of the sample using TC or high
the stainless steel parts pan sufficient to cover the parts. Cover
pressure liquid chromatography (see 4.1.1.2).
the parts pan with aluminum foil or a stainless steel lid, 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 9. Report
extracting agent level in the parts pan, and allow the extracting
9.1 Report the following information:
agent and bath temperature to equilibrate to the desired
9.1.1 Identification of the part or material being cleaned
temperature. Alternatively, preheat the parts pan and extracting
(including tradename, part number, serial number, proper
agent prior to the placement of the materials or parts into the
chemical name, ASTM designation, lot number, batch number,
parts pan. Then cover the parts pan with foil and place the parts
and manufacturer).
pan into the bracket in the bath and allow the extracting agent
9.1.2 Cleaning reagent;
to equilibrate to the temperature of the bath.
9.1.3 Cleaning time;
8.4.2.1 The ratio of extraction agent to part’s surface area
9.1.4 Cleaning temperature;
shall not exceed 1000 mL/0.1 m ; the preferred ratio is 500
9.1.5 Frequency of the ultrasonic bath, kHz;
mL/0.1 m .
9.1.6 Power density of the ultrasonic bath, W/L;
8.4.3 Subject the parts to the ultrasonic bath for 10 min.
9.1.7 Volume of extracting agent used, mL;
Perform the sampling procedure as soon as possible, with a
9.1.8 Mass (M1) of parts extracted, g;
maximum time limit of 120 min after turning off the ultrasonic
9.1.9 Mass (M2) of material extracted from unused wipes,
bath.
2 2
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 par
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.