ASTM G120-01(2008)
(Practice)Standard Practice for Determination of Soluble Residual Contamination in by Soxhlet Extraction
Standard Practice for Determination of Soluble Residual Contamination in by Soxhlet Extraction
SIGNIFICANCE AND USE
It is expected that this practicewill be suitable to identify and quantify contaminants found in systems, system materials, and components used in systems requiring a high level of cleanliness, such as oxygen. Softgoods such as seals and valve seats can be tested as received. Gloves and wipes, or samples thereof, to be used in the cleaning operation can be evaluated prior to use to ensure that the proposed cleaning solvent does not extract contaminants and residues on the surface to be cleaned.
Wipes or other cleaning equipment can be tested after use to determine the amount of contaminant removed from a surface. This procedure can be used to obtain samples for NVR analysis using contaminated control coupons that were subjected to the cleaning process as controls to validate cleaning operations.
The selection of the solvent requires some knowledge of the contaminant (see Practice G 93 for recommendations). If a nonvolatile residue (NVR) analysis is to be performed on the molecular contaminant, the boiling point of the solvent shall be significantly lower than that of the contaminant. For other analytical methods, the tester must know the accuracy of the analytical methods, and the solvent shall be chosen so as not to interfere with the selected analytical method. To identify the composition of the NVR, analytical methods such as infrared spectroscopy or gas chromatography/mass spectroscopy have been used satisfactorily.
SCOPE
1.1 This practice describes a procedure for the determination of residual contamination in systems and components requiring a high level of cleanliness, such as oxygen, by Soxhlet extraction.
1.2 This practice may be used for extracting nonvolatile and semivolatile residues from solids such as new and used gloves, new and used wipes, contaminated test specimens or control coupons, small pieces of hardware, component softgoods, etc. When used with proposed cleaning materials (wipes, gloves, etc.), from the cleaning materials this practice may be used to determine the potential of the proposed solvent to extract contaminants (plasticizers, residual detergents, brighteners, etc.) and deposit them on the surface being cleaned.
1.3 This practice is not suitable for the evaluation of particulate contamination.
1.4 The values stated in SI units are standard.
1.5 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: G120 − 01(Reapproved 2008)
Standard Practice for
Determination of Soluble Residual Contamination by
Soxhlet Extraction
This standard is issued under the fixed designation G120; 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 G93 Practice for Cleaning Methods and Cleanliness Levels
for Material and Equipment Used in Oxygen-Enriched
1.1 This practice describes a procedure for the determina-
Environments
tion of residual contamination in systems and components
requiring a high level of cleanliness, such as oxygen, by
3. Terminology
Soxhlet extraction.
3.1 Definitions:
1.2 This practice may be used for extracting nonvolatile and
3.1.1 contaminant, n—unwanted molecular and particulate
semivolatile residues from solids such as new and used gloves,
matter that could affect the performance of the components or
new and used wipes, contaminated test specimens or control
materials upon which they reside.
coupons, small pieces of hardware, component softgoods, etc.
When used with proposed cleaning materials (wipes, gloves,
3.1.2 contamination, n—a process of contaminating.
etc.), from the cleaning materials this practice may be used to
3.1.3 nonvolatile residue (NVR), n—residual molecular and
determine the potential of the proposed solvent to extract
particulate matter remaining following the filtration of a
contaminants (plasticizers, residual detergents, brighteners,
solvent containing contaminants and complete evaporation of
etc.) and deposit them on the surface being cleaned.
the solvent at a specified temperature.
1.3 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.
1.4 The values stated in SI units are standard.
3.1.4.1 Discussion—The size of a particle is usually defined
by its greatest dimension and is specified in micrometres.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3.1.5 molecular contaminant , n—non-particulate contami-
responsibility of the user of this standard to establish appro-
nation.
priate safety and health practices and determine the applica-
3.1.5.1 Discussion—A molecular contaminant may be in a
bility of regulatory limitations prior to use.
gaseous, liquid, or solid state and may be uniformly or
nonuniformly distributed.
2. Referenced Documents
3.1.5.2 Discussion—Molecular contaminants account for
2.1 ASTM Standards:
most of the NVR.
D1193 Specification for Reagent Water
3.1.6 control coupon (witness coupon), n—a coupon made
E1235 Test Method for Gravimetric Determination of Non-
from the same material and prepared in exactly the same way
volatile Residue (NVR) in Environmentally Controlled
as the test coupons, which is used to verify the validity of the
Areas for Spacecraft
method or part thereof.
F331 Test Method for Nonvolatile Residue of Solvent Ex-
3.1.6.1 Discussion—In this test method, the control coupon
tract from Aerospace Components (Using Flash Evapora-
will be contaminated in the same manner as the test coupons
tor)
and will be subjected to the identical extraction procedure.
This practice is under the jurisdiction of ASTM Committee G04 on Compat-
4. Summary of Practice
ibility and Sensitivity of Materials in Oxygen Enriched Atmospheres and is the
direct responsibility of Subcommittee G04.02 on Recommended Practices.
4.1 The sample is placed in an extraction thimble or
Current edition approved Sept. 1, 2008. Published October 2008. Originally
between two plugs of glass wool and contaminants are ex-
approved in 1993. Last previous edition approved in 2001 as G120 – 01. DOI:
10.1520/G0120-01R08.
tracted using an appropriate solvent in a Soxhlet extractor. The
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
solvent is brought to the boiling point; the pure solvent vapors
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
travel to the condenser where they condense and drip into the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. thimble.When the liquid level in the thimble reaches the top of
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
G120 − 01 (2008)
the Soxhlet siphon, the solvent and extracted soluble contami-
nant are siphoned back into the boiler. This process is allowed
to continue for several hours. The solvent and extract are then
concentrated or dried for analysis.
5. Significance and Use
5.1 Itisexpectedthatthispracticewillbesuitabletoidentify
and quantify contaminants found in systems, system materials,
and components used in systems requiring a high level of
cleanliness, such as oxygen. Softgoods such as seals and valve
seats can be tested as received. Gloves and wipes, or samples
thereof, to be used in the cleaning operation can be evaluated
prior to use to ensure that the proposed cleaning solvent does
not extract contaminants and residues on the surface to be
cleaned.
5.2 Wipes or other cleaning equipment can be tested after
use to determine the amount of contaminant removed from a
surface.ThisprocedurecanbeusedtoobtainsamplesforNVR
analysis using contaminated control coupons that were sub-
jected to the cleaning process as controls to validate cleaning
operations.
5.3 Theselectionofthesolventrequiressomeknowledgeof
the contaminant (see Practice G93 for recommendations). If a
nonvolatile residue (NVR) analysis is to be performed on the
molecularcontaminant,theboilingpointofthesolventshallbe
significantly lower than that of the contaminant. For other
analytical methods, the tester must know the accuracy of the
analytical methods, and the solvent shall be chosen so as not to
interfere with the selected analytical method. To identify the
FIG. 1 Soxhlet Extraction Apparatus
composition of the NVR, analytical methods such as infrared
spectroscopy or gas chromatography/mass spectroscopy have
such specifications are available. Other grades may be used,
been used satisfactorily.
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
6. Apparatus
the determination.
6.1 Soxhlet extractor—500 mL evaporation flask and asso-
NOTE 1—Warning: Solvents such as 2-propanol and 2-butanone are
ciated equipment as shown in Fig. 1.
highly flammable. The reader should refer to appropriate safe handling
6.2 Boiling chips—solvent extracted. procedures.
7.3 Water—shall meet the requirements of D1193, Type II.
6.3 Water bath—heated with temperature control of 65 °C.
6.4 Thimbles—glass or paper.
8. Procedure
6.5 Heating mantle—rheostat controlled. 8.1 Prepare the sample for placement in the extractor.
8.1.1 To determine the amount of extractable material in a
6.6 Balance—range to a minimum of 50 g with an accuracy
wipingcloth(neworused),cutoutatestsectionapproximately
of 0.1 mg.
30 centimetres (cm) square, accurately measure and calculate
6.7 Evaporator—rotary.
the area (A) in square centimetres, and wei
...
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:G120–95 (Reapproved 2001) Designation: G 120 – 01 (Reapproved 2008)
Standard Practice for
Determination of Soluble Residual Contamination in
Materials and Components by Soxhlet
ExtractionDetermination of Soluble Residual Contamination
by Soxhlet Extraction
This standard is issued under the fixed designation G 120; 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 describes a procedure for the determination of residual contamination in systems and components requiring
a high level of cleanliness, such as oxygen, by Soxhlet extraction.
1.2 Thispracticemaybeusedforextractingnonvolatileandsemivolatileresiduesfromsolidssuchasnewandusedgloves,new
and used wipes, contaminated test specimens or control coupons, small pieces of hardware, component softgoods, etc. When used
with proposed cleaning materials (wipes, gloves, etc.), from the cleaning materials this practice may be used to determine the
potential of the proposed solvent to extract contaminants (plasticizers, residual detergents, brighteners, etc.) and deposit them on
the surface being cleaned.
1.3 This practice is not suitable for the evaluation of particulate contamination.
1.4The values stated in SI units are standard. Values in parentheses are for information only.
1.4 The values stated in SI units are standard.
1.5 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 F324Test Method for Nonvolatile Residue of Volatile Cleaning Solvents Using the Solvent Purity Meter
F 331 Test Method for Nonvolatile Residue of Solvent Extract from Aerospace Components (Using Rotary Flash Evaporator)
G 93 Practice for Cleaning Methods and Cleanliness Levels for Material and Equipment Used in Oxygen-Enriched
Environments
3. Terminology
3.1 Definitions:
3.1.1 contaminant, n—unwanted molecular and particulate matter that could affect or degrade the performance of the
components or materials upon which they reside.
3.1.2 contamination, n—a process of contaminating.
3.1.3 nonvolatile residue (NVR), n—residual molecular and particulate matter remaining following the filtration of a solvent
containing contaminants and complete evaporation of the solvent at a specified temperature.
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)molecular contaminant , n—the molecular contaminant may be in
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 G04.01 on Test Methods.
Current edition approved Oct. 10, 1995. Published November 1995. Originally published as G120–93. Last previous edition G120–93.
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. 1, 2008. Published October 2008. Originally approved in 1993. Last previous edition approved in 2001 as G 120 – 01.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
G 120 – 01 (2008)
a gaseous, liquid, or solid state. —non-particulate contamination.
3.1.5.1 Discussion—It may be uniformly or nonuniformly distributed, or be in the form of droplets. Molecular contaminants
account for most of the NVR. —A molecular contaminant may be in a gaseous, liquid, or solid state and may be uniformly or
nonuniformly distributed.
3.1.5.2 Discussion—Molecular contaminants account for most of the NVR.
3.1.6 control coupon (witness coupon), n— a coupon made from the same material and prepared in exactly the same way as
the test coupons, which is used to verify the validity of the method or part thereof.
3.1.6.1 Discussion—In this test method, the control coupon will be contaminated in the same manner as the test coupons and
will be subjected to the identical extraction procedure.
4. Summary of Practice
4.1 The sample is placed in an extraction thimble or between two plugs of glass wool and contaminants are extracted using an
appropriate solvent (see Practice G93 for recommendations) in a Soxhlet extractor. The solvent is brought to the boiling point; the
pure solvent vapors travel to the condenser where they condense and drip into the thimble. When the liquid level in the thimble
reaches the top of the Soxhlet siphon, the solvent and extracted soluble contaminant are siphoned back into the boiler.This process
is allowed to continue for several hours. The solvent and extract are then concentrated or dried for analysis.
5. Significance and Use
5.1 It is expected that this test method will practicewill be suitable to identify and quantify contaminants found in systems,
system materials, and components used in systems requiring a high level of cleanliness, such as oxygen. Softgoods such as seals
and valve seats can be tested as received. Gloves and wipes, or samples thereof, to be used in the cleaning operation can be
evaluated prior to use to ensure that the proposed cleaning solvent does not extract contaminants and deposit chemicalsresidues
on the surface to be cleaned.
5.2 Wipes or other cleaning equipment can be tested after use to determine the amount of contaminant removed from a surface.
This procedure can be used to obtain samples for NVR analysis using contaminated control coupons that were subjected to the
cleaning process as controls to validate cleaning operations.
5.3 The selection of the solvent requires some knowledge of the contaminant (see Practice G 93 for recommendations). If a
nonvolatile residue (NVR) analysis is to be performed on the molecular contaminant, the boiling point of the solvent shall be
significantly lower than that of the contaminant. For other analytical methods, the tester must know the accuracy of the analytical
methods, and the solvent shall be chosen so as not to interfere with the selected analytical method. To identify the composition
of the NVR, analytical methods such as infrared spectroscopy or gas chromatography/mass spectroscopy have been used
satisfactorily.
6. Apparatus
6.1 Soxhlet extractor—500 mL evaporation flask and associated equipment as shown in Fig. 1.
6.2 Boiling chips—solvent extracted.
6.3 Water bath—heated with temperature control of 65 °C.
6.4 Thimbles—glass or paper.
6.5 Heating mantle—rheostat controlled.
6.6 Balance—range to a minimum of 50 g with an accuracy of 0.1 mg.
6.7 Evaporator—rotary.
6.8 500 mL concentrator flask.
7. Reagents
7.1 Solvents that can be used to prepare standard contaminant solutions include the following: 2-propanol, 2-butanone, hexane,
methylene chloride, and perfluorinated carbon fluids.
7.2 Purity of Reagents—Reagent grade chemicals shall be used in al
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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:G120–01 Designation: G 120 – 01 (Reapproved 2008)
Standard Practice for
Determination of Soluble Residual Contamination by
Soxhlet Extraction
This standard is issued under the fixed designation G 120; 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 describes a procedure for the determination of residual contamination in systems and components requiring
a high level of cleanliness, such as oxygen, by Soxhlet extraction.
1.2 Thispracticemaybeusedforextractingnonvolatileandsemivolatileresiduesfromsolidssuchasnewandusedgloves,new
and used wipes, contaminated test specimens or control coupons, small pieces of hardware, component softgoods, etc. When used
with proposed cleaning materials (wipes, gloves, etc.), from the cleaning materials this practice may be used to determine the
potential of the proposed solvent to extract contaminants (plasticizers, residual detergents, brighteners, etc.) and deposit them on
the surface being cleaned.
1.3 This practice is not suitable for the evaluation of particulate contamination.
1.4 The values stated in SI units are standard.
1.5 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 331 Test Method for Nonvolatile Residue of Solvent Extract from Aerospace Components (Using Rotary Flash Evaporator)
G93 Practice for Cleaning Methods and Cleanliness Levels for Material and Equipment Used in Oxygen-Enriched
Environments
3. Terminology
3.1 Definitions:
3.1.1 contaminant, n—unwanted molecular and particulate matter that could affect the performance of the components or
materials upon which they reside.
3.1.2 contamination, n—a process of contaminating.
3.1.3 nonvolatile residue (NVR), n—residual molecular and particulate matter remaining following the filtration of a solvent
containing contaminants and complete evaporation of the solvent at a specified temperature.
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 , n—non-particulate contamination.
3.1.5.1 Discussion—Amolecular contaminant may be in a gaseous, liquid, or solid state and may be uniformly or nonuniformly
distributed.
3.1.5.2 Discussion—Molecular contaminants account for most of the NVR.
3.1.6 control coupon (witness coupon), n— a coupon made from the same material and prepared in exactly the same way as
the test coupons, which is used to verify the validity of the method or part thereof.
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, 2001. Published January 2002. Originally published as G120–93. Last previous edition G120–95.
Current edition approved Sept. 1, 2008. Published October 2008. Originally approved in 1993. Last previous edition approved in 2001 as G 120 – 01.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
G 120 – 01 (2008)
3.1.6.1 Discussion—In this test method, the control coupon will be contaminated in the same manner as the test coupons and
will be subjected to the identical extraction procedure.
4. Summary of Practice
4.1 The sample is placed in an extraction thimble or between two plugs of glass wool and contaminants are extracted using an
appropriate solvent in a Soxhlet extractor. The solvent is brought to the boiling point; the pure solvent vapors travel to the
condenser where they condense and drip into the thimble. When the liquid level in the thimble reaches the top of the Soxhlet
siphon, the solvent and extracted soluble contaminant are siphoned back into the boiler. This process is allowed to continue for
several hours. The solvent and extract are then concentrated or dried for analysis.
5. Significance and Use
5.1 It is expected that this test method willpracticewill be suitable to identify and quantify contaminants found in systems,
system materials, and components used in systems requiring a high level of cleanliness, such as oxygen. Softgoods such as seals
and valve seats can be tested as received. Gloves and wipes, or samples thereof, to be used in the cleaning operation can be
evaluated prior to use to ensure that the proposed cleaning solvent does not extract contaminants and residues on the surface to
be cleaned.
5.2 Wipes or other cleaning equipment can be tested after use to determine the amount of contaminant removed from a surface.
This procedure can be used to obtain samples for NVR analysis using contaminated control coupons that were subjected to the
cleaning process as controls to validate cleaning operations.
5.3 The selection of the solvent requires some knowledge of the contaminant (see Practice G 93 for recommendations). If a
nonvolatile residue (NVR) analysis is to be performed on the molecular contaminant, the boiling point of the solvent shall be
significantly lower than that of the contaminant. For other analytical methods, the tester must know the accuracy of the analytical
methods, and the solvent shall be chosen so as not to interfere with the selected analytical method. To identify the composition
of the NVR, analytical methods such as infrared spectroscopy or gas chromatography/mass spectroscopy have been used
satisfactorily.
6. Apparatus
6.1 Soxhlet extractor—500 mL evaporation flask and associated equipment as shown in Fig. 1.
6.2 Boiling chips—solvent extracted.
6.3 Water bath—heated with temperature control of 65 °C.
6.4 Thimbles—glass or paper.
6.5 Heating mantle—rheostat controlled.
6.6 Balance—range to a minimum of 50 g with an accuracy of 0.1 mg.
6.7 Evaporator—rotary.
6.8 500 mL concentrator flask. flask.
7. Reagents
7.1 Solvents that can be used to prepare standard contaminant solutions include the following: 2-propanol, 2-butanone, hexane,
methylene chloride, and perfluorinated carbon fluids.
7.2 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are available
...
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