Standard Practice for Determination of Soluble Residual Contamination in by Soxhlet Extraction

SIGNIFICANCE AND USE
It is expected that this test method will 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.), 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. Values in parentheses are for information only.  
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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Publication Date
09-Sep-2001
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ASTM G120-01 - Standard Practice for Determination of Soluble Residual Contamination in by Soxhlet Extraction
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:G120–01
Standard Practice for
Determination of Soluble Residual Contamination by
1
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 (e) indicates an editorial change since the last revision or reapproval.
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1. Scope Equipment Used in Oxygen-Enriched Environments
1.1 This practice describes a procedure for the determina-
3. Terminology
tion of residual contamination in systems and components
3.1 Definitions:
requiring a high level of cleanliness, such as oxygen, by
3.1.1 contaminant, n—unwanted molecular and particulate
Soxhlet extraction.
matter that could affect the performance of the components or
1.2 This practice may be used for extracting nonvolatile and
materials upon which they reside.
semivolatile residues from solids such as new and used gloves,
3.1.2 contamination, n—a process of contaminating.
new and used wipes, contaminated test specimens or control
3.1.3 nonvolatile residue (NVR), n—residual molecular and
coupons, small pieces of hardware, component softgoods, etc.
particulate matter remaining following the filtration of a
When used with proposed cleaning materials (wipes, gloves,
solvent containing contaminants and complete evaporation of
etc.), from the cleaning materials this practice may be used to
the solvent at a specified temperature.
determine the potential of the proposed solvent to extract
3.1.4 particle (particulate contaminant), n— a piece of
contaminants (plasticizers, residual detergents, brighteners,
matter in a solid state with observable length, width, and
etc.) and deposit them on the surface being cleaned.
thickness.
1.3 This practice is not suitable for the evaluation of
3.1.4.1 Discussion—The size of a particle is usually defined
particulate contamination.
by its greatest dimension and is specified in micrometres.
1.4 The values stated in SI units are standard.
3.1.5 molecular contaminant , n—non-particulate contami-
1.5 This standard does not purport to address all of the
nation.
safety concerns, if any, associated with its use. It is the
3.1.5.1 Discussion—A molecular contaminant may be in a
responsibility of the user of this standard to establish appro-
gaseous, liquid, or solid state and may be uniformly or
priate safety and health practices and determine the applica-
nonuniformly distributed.
bility of regulatory limitations prior to use.
3.1.5.2 Discussion—Molecular contaminants account for
2. Referenced Documents most of the NVR.
3.1.6 control coupon (witness coupon), n— a coupon made
2.1 ASTM Standards:
2 from the same material and prepared in exactly the same way
D 1193 Specification for Reagent Water
as the test coupons, which is used to verify the validity of the
E 1235 Test Method for Gravimetric Determination of Non-
method or part thereof.
volatile Residue (NVR) in Environmentally Controlled
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3.1.6.1 Discussion—In this test method, the control coupon
Areas for Spacecraft
will be contaminated in the same manner as the test coupons
F 331 Test Method for Nonvolatile Residue of Solvent
and will be subjected to the identical extraction procedure.
Extract from Aerospace Components (Using Rotary Flash
3
Evaporator)
4. Summary of Practice
G93 Practice for Cleaning Methods for Material and
4.1 The sample is placed in an extraction thimble or
between two plugs of glass wool and contaminants are ex-
tracted using an appropriate solvent in a Soxhlet extractor. The
1
This practice is under the jurisdiction of ASTM Committee G04 on Compat-
solvent is brought to the boiling point; the pure solvent vapors
ibility and Sensitivity of Materials in Oxygen Enriched Atmospheres and is the
travel to the condenser where they condense and drip into the
direct responsibility of Subcommittee G04.02 on Recommended Practices.
thimble.When the liquid level in the thimble reaches the top of
Current edition approved Sept. 10, 2001. Published January 2002. Originally
published as G120 – 93. Last previous edition G 120 – 95.
2
Annual Book of ASTM Standards, Vol 11.01.
3 4
Annual Book of ASTM Standards, Vol 15.03. Annual Book of ASTM Standards, Vol 14.04.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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G120–01
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 It is expected that this test method will be suitable to
identify and quantify contaminan
...

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