ASTM G136-96(2002)

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.

General Information

• Status: Historical
• Publication Date: 09-Mar-1996
• ICS: 19.020 - Test conditions and procedures in general
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: G04 - Compatibility and Sensitivity of Materials in Oxygen Enriched Atmospheres
• Drafting Committee: G04.02 - Recommended Practices

Relations

• Replaces: ASTM G136-96 - Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction
• Effective Date: 10-Mar-1996
• Replaced By: ASTM G136-03 - Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction
• Effective Date: 10-Sep-2003
• Referred By: ASTM F2459-18 - Standard Test Method for Extracting Residue from Metallic Medical Components and Quantifying via Gravimetric Analysis
• Effective Date: 10-Mar-1996
• Referred By: ASTM F2847-17 - Standard Practice for Reporting and Assessment of Residues on Single-Use Implants and Single-Use Sterile Instruments
• Effective Date: 10-Mar-1996
• Referred By: ASTM G126-16(2023) - Standard Terminology Relating to the Compatibility and Sensitivity of Materials in Oxygen Enriched Atmospheres
• Effective Date: 10-Mar-1996
• Referred By: ASTM G120-15(2023) - Standard Practice for Determination of Soluble Residual Contamination by Soxhlet Extraction
• Effective Date: 10-Mar-1996
• Referred By: ASTM G144-01(2022) - Standard Test Method for Determination of Residual Contamination of Materials and Components by Total Carbon Analysis Using a High Temperature Combustion Analyzer
• Effective Date: 10-Mar-1996
• Referred By: ASTM G93/G93M-19 - Standard Guide for Cleanliness Levels and Cleaning Methods for Materials and Equipment Used in Oxygen-Enriched Environments
• Effective Date: 10-Mar-1996

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: G 136 – 96 (Reapproved 2002)
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 3.1.2 contaminate, v—a process of contaminating.
3.1.3 nonvolatile residue (NVR), n—residual molecular and
1.1 This practice may be used to extract nonvolatile and
particulate matter remaining following the filtration and con-
semivolatile residues from materials such as new and used
trolled evaporation of liquid containing contaminants.
gloves, new and used wipes, component soft goods, and so
3.1.4 particle (particulate contaminant), n—a piece of mat-
forth. When used with proposed cleaning materials (wipes,
ter in a solid state with observable length, width, and thickness.
gloves, and so forth), this practice may be used to determine
3.1.4.1 Discussion—The size of a particle is usually defined
the potential of the proposed solvent or other fluids to extract
by its greatest dimension and is specified in micrometres.
contaminants (plasticizers, residual detergents, brighteners,
3.1.5 molecular contaminant (non-particulate contamina-
and so forth.) and deposit them on the surface being cleaned.
tion), n—the molecular contaminant may be in a gaseous,
1.2 This practice is not suitable for the evaluation of
liquid, or solid state.
particulate contamination.
3.1.5.1 Discussion—A molecular contaminant may be uni-
1.3 The values stated in SI units are standard.
formly or nonuniformly distributed, or be in the form of
1.4 This standard does not purport to address all of the
droplets. Molecular contaminants account for most of the
safety concerns, if any, associated with its use. It is the
NVR.
responsibility of the user of this standard to establish appro-
3.1.6 degas, v—the process of removing gases from a
priate safety and health practices and determine the applica-
liquid.
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
2.1 ASTM Standards:
a container containing the test fluid. This container is then
D 1193 Specification for Reagent Water
placed in an ultrasonic cleaning bath and treated for a given
E 1235 Test Method for Gravimetric Determination of Non-
period of time at the recommended temperature for the test
volatile Residue (NVR) in Environmentally Controlled
fluid. This results in either a solution if the contaminant is
Areas for Spacecraft
soluble in the test fluid or an emulsion if the contaminant is not
F 324 Test Method for Nonvolatile Residue of Volatile
soluble in the test fluid. The test fluid may then be analyzed for
Cleaning Solvents Using the Solvent Purity Meter
nonvolatile residue that was extracted from the test specimen.
F 331 Test Method for Nonvolatile Residue of Halogenated
4.1.1 In the case of aqueous-based agents, the material may
Solvent Extract from Aerospace Components Using Rotary
be treated in accordance with Specification D 1193 Type II
Flash Evaporator
water or Type II water containing an extracting agent.
3. Terminology
4.1.1.1 When Type II water is used, the water and material
may be analyzed without further treatment. Typical methods of
3.1 Definitions of Terms Specific to This Standard:
analysis may include weighing the material before and after
3.1.1 contaminant (contamination), n—unwanted molecular
treatment or more sophisticated analytical procedures such as
and particulate matter that could affect or degrade the perfor-
total carbon (TC) or high-pressure liquid chromatography.
mance of the components upon which they reside.
4.1.1.2 When cleaning agents are used, the materials are
rinsed with Type II water after the removal from the cleaning
This practice is under the jurisdiction of ASTM Committee G4 on Compat-
bath and then ultrasonically cleaned in reagent water to ensure
ibility and Sensitivity of Materials in Oxygen-Enriched Atmospheres and is the
the removal of the extracting agent. Typical methods of
direct responsibility of Subcommittee G04.02 on Recommended Practices.
analysis may include weighing the material before and after
Current edition approved March 10, 1996. Published August 1996. Originally
published as G 136 – 95. Last previous edition G 136 – 95. cleaning or more sophisticated analytical procedures such as
Annual Book of ASTM Standards, Vol 11.01.
TC or high-pressure liquid chromatography.
Annual Book of ASTM Standards, Vol 15.03.
Discontinued; see 1986 Annual Book of ASTM Standards, Vol 10.05.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
G 136 – 96 (2002)
4.1.2 In the case of solvent-based agents, the weight of the Reagents of the American Chemical Society where such
material before and after cleaning may be determined or the specifications are available. Other grades may be used, pro-
solvents may be analyzed using infrared spectroscopy, gas vided it is first ascertained and that the reagent is of sufficiently
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
that would typically be exposed to the cleaning solvent,
6.1 Ultrasonic Bath, with an operating frequency range
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 record the mass (M1). Determine the dimensions of each
and a temperature controlled bath capable of maintaining a
strip in centimetres (cm) and record the total surface area of the
temperature between ambient and 70°C with an accuracy of
strips (S) in square centimetres.
62°C is to be used.
8.2 Parts Pan Preparation—Clean the stainless steel
6.2 Parts Pans, stainless steel container with volumes
sample parts pans. Conduct the extraction procedure selected
between 1 and 4 L are to be used.
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-
for 10 min.
ethylene, methylene chloride that have relative low threshold limit values.
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,
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
G 136 – 96 (2002)
adjust the water level in the bath such that it is above the 8.6.3 Wash the parts pan and parts with a total of 500 mL of
extracting agent level in the parts pan, and allow the extracting fresh Type II water in three roughly equal portions and discard
agent and bath temperature to equilibrate to the desired unless Type II water was used as the extracting agent. If Type
temperature. Alternatively, preheat the parts pan and extracting II water was used as the extracting agent, combine the three
agent prior to the placement of the materials or parts into the portions with the water from 8.6.2, and set aside as the sample
parts pan. Then cover the parts pan with foil and place the parts for analysis. If a surface active compound was used, repeat the
pan into the bracket in the bath and allow the extracting agent procedures in 8.3-8.5 using Type II water and use the Type II
to equilibrate to the temperature of the bath. water as the sample for analysis.
8.4.2.1 Extraction agent to parts surface area ratio shall not 8.6.4 Determine the NVR of the sample using G TC or high
2 2
exceed 1000 mL/0.1 m ; the preferred ratio is 500 mL/0.1 m . pressure liquid chromatography (see 4.1.1.2).
8.4.3 Subject the parts to the ultrasonic bath for 10 min.
Perform the sampling procedure as soon as possible, with a 9. Report
maximum time limit of 120 min after turning off the ultrasonic
9.1 Report the following information:
bath.
9.1.1 Identification of the part or material being cleaned
8.5 Sampling Procedure for Solvent Extracted Parts:
(including tradename, part number, serial number, proper
8.5.1 Remove the parts pan from the ultrasonic bath and
chemical name, ASTM designation, lot number, batch number,
remove the cover. Swirl the parts pan to thoroughly mix the
and manufacturer).
solvent.
9.1.2 Cleaning reagent;
8.5.2 After swirling, quickly decant the solvent from the
9.1.3 Cleaning time;
parts pan.
9.1.4 Cleaning temperature;
8.5.3 Wash the parts pan and parts with a total of 500 mL of
9.1.5 Frequency of the ultrasonic bath, kHz;
fresh solvent in three roughly equal portions, combine with the
9.1.6 Power density of the ultrasonic bath, W/L;
solvent from 8.5.2, and set aside as the sample for NVR
9.1.7 Volume of extracting agent used, mL;
analysis.
9.1.8 Mass (M1) of parts extracted, g;
8.5.4 Determine the mass (M4) of the nonvolatile residue in
9.1.9 Mass (M2) of material extracted from unused wipes,
milligrams to the nearest tenth of a milligram using Test
2 2
mg/g, or (M3), mg/cm , or TC in ppm/g or ppm/cm ;
Methods E 1235, F 324, or F 331. Ensure that the reported
9.1.10 Mass (M4) of NVR determined using Test Methods
NVR is adjusted by subtracting the NVR of an equivalent
E 1235, F 324, or F 331;
volume of “blank” solvent.
9.1.11 Blank (B) for the parts pan and agent, mg; and,
8.6 Sampling Procedure for Aqueous Extracted Materials
9.1.12 Surface area (S), cm .
and Parts:
8.6.1 Remove the parts pan from the ultrasonic bath and
10. Keywords
remove the cover. Swirl the parts pan to mix the extracting
agent. 10.1 contaminant; contamination; extraction; nonvolatile
8.6.2 After swirling, quickly decant the extracting agent residue; oxygen systems; total carbon (TC); ultrasonic
from the parts pan. extraction
APPENDIX
(Nonmandatory Information)
X1. SELECTION OF ULTRASONIC BATHS
X1.1 Introduction—This appendix describes technical in- X1.2.1 The Tank:
formation useful to th
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