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

SIGNIFICANCE AND USE
5.1 It is expected that this test method will be suitable for the quantitative determination of total carbon in water that has been used to clean, extract, or sample parts, components, materials, or systems requiring a high degree of cleanliness, that is, oxygen systems.
SCOPE
1.1 This test method covers the determination of residual contamination in an aqueous sample by the use of a total carbon (TC) analyzer. When used in conjunction with Practice G131 and G136, this procedure may be used to determine the cleanliness of systems, components, and materials requiring a high level of cleanliness, such as oxygen systems. This procedure is applicable for aqueous-based cleaning and sampling methods only.  
1.2 This test method is not suitable for the evaluation of particulate contamination, or contaminants that are not soluble in or that do not form an emulsion with water.  
1.3 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.  
1.4 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

• Status: Published
• Publication Date: 31-Aug-2022
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: G04 - Compatibility and Sensitivity of Materials in Oxygen Enriched Atmospheres
• Drafting Committee: G04.01 - Test Methods

Relations

• Refers: ASTM F331-13(2020) - Standard Test Method for Nonvolatile Residue of Solvent Extract from Aerospace Components (Using Flash Evaporator)
• Effective Date: 01-Apr-2020
• Refers: ASTM G121-18 - Standard Practice for Preparation of Contaminated Test Coupons for the Evaluation of Cleaning Agents
• Effective Date: 01-Dec-2018
• Refers: ASTM G136-03(2016) - Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction
• Effective Date: 01-May-2016
• Refers: ASTM G131-96(2016) - Standard Practice for Cleaning of Materials and Components by Ultrasonic Techniques
• Effective Date: 01-May-2016
• Refers: ASTM F331-13 - Standard Test Method for Nonvolatile Residue of Solvent Extract from Aerospace Components (Using Flash Evaporator)
• Effective Date: 01-Jun-2013
• Refers: ASTM G136-03(2009) - Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction
• Effective Date: 01-Apr-2009
• Refers: ASTM G131-96(2008) - Standard Practice for Cleaning of Materials and Components by Ultrasonic Techniques
• Effective Date: 01-Sep-2008
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM F331-05 - Standard Test Method for Nonvolatile Residue of Solvent Extract from Aerospace Components (Using Flash Evaporator)
• Effective Date: 01-Nov-2005
• Refers: ASTM G121-98(2015)e1 - Standard Practice for Preparation of Contaminated Test Coupons for the Evaluation of Cleaning Agents
• Effective Date: 01-Sep-2004
• Refers: ASTM G121-98(2010)e1 - Standard Practice for Preparation of Contaminated Test Coupons for the Evaluation of Cleaning Agents
• Effective Date: 01-Sep-2004
• Refers: ASTM G136-03 - Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction
• Effective Date: 10-Sep-2003
• Refers: ASTM F331-00 - Standard Test Method for Nonvolatile Residue of Solvent Extract from Aerospace Components (Using Flash Evaporator)
• Effective Date: 10-May-2000
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999

Overview

ASTM G144-01(2022), issued by ASTM International, establishes a standardized test method for determining residual contamination in materials and components by analyzing total carbon content using a high temperature combustion analyzer. This method is especially significant for components and systems that demand a high level of cleanliness, such as those used in oxygen-enriched environments. The procedure is specifically tailored for aqueous-based cleaning and sampling methods, providing a quantitative assessment of residual molecular contamination extracted during cleaning.

Key Topics

• Total Carbon Analysis: Utilizes a high temperature combustion analyzer to measure the total carbon (TC) present in aqueous samples derived from cleaning parts or systems.
• High Cleanliness Demands: Suited for applications where residual contamination could degrade system performance, such as oxygen systems and critical components.
• Excludes Particulate Contamination: The method is designed for molecular (non-particulate) contaminants soluble or emulsifiable in water and is not applicable for insoluble or particulate contaminants.
• Sample Handling: Emphasizes strict protocols for sample collection, preparation, and analysis to avoid external contamination and ensure reliable results.
• Calibration and Verification: Details requirements for calibration standards, reagent purity, and instrument verification to maintain data accuracy and traceability.

Applications

This ASTM standard is widely applicable in sectors where component cleanliness is essential to safety and performance:

• Aerospace Components: Ensures that critical systems, such as those encountered in oxygen service or life support environments, meet stringent cleanliness criteria.
• Manufacturing: Supports quality assurance in the manufacturing of high-precision or sensitive components, helping to detect and quantify residual oils, greases, and other molecular contaminants after aqueous cleaning.
• Materials Testing: Used in verification and validation of cleaning processes by quantifying nonvolatile residue (NVR) as an indicator of cleaning efficiency.
• Cleaning Agent Evaluation: Facilitates comparative assessments of different cleaning agents or processes by providing quantifiable data on residual contaminants.
• Safety Compliance: Supports adherence to international standards and regulatory requirements for cleanliness in various high-risk industries.

Related Standards

For optimal results and comprehensive contamination control, ASTM G144-01(2022) is often used in conjunction with related standards:

• ASTM G131 - Practice for Cleaning of Materials and Components by Ultrasonic Techniques
• ASTM G136 - Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction
• ASTM G121 - Practice for Preparation of Contaminated Test Coupons for the Evaluation of Cleaning Agents
• ASTM F331 - Test Method for Nonvolatile Residue of Solvent Extract from Aerospace Components (Using Flash Evaporation)
• ASTM D1193 - Specification for Reagent Water

Practical Value

Implementing ASTM G144-01(2022) offers several practical benefits:

• Enhanced Reliability: Improves confidence in the cleanliness and performance of components in critical applications.
• Process Validation: Enables manufacturers and quality managers to validate and optimize cleaning protocols.
• Risk Reduction: Decreases the likelihood of contamination-related failures in high-purity and safety-critical systems.
• Regulatory Alignment: Ensures compliance with international guidelines, helping organizations meet global market requirements.

Keywords

total carbon analysis, residual contamination, cleaning validation, nonvolatile residue, high temperature combustion analyzer, aqueous cleaning, oxygen systems, ASTM G144, molecular contaminant, cleanliness testing.

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.
Designation: G144 − 01 (Reapproved 2022)
Standard Test Method for
Determination of Residual Contamination of Materials and
Components by Total Carbon Analysis Using a High
Temperature Combustion Analyzer
This standard is issued under the fixed designation G144; 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 F331 Test Method for Nonvolatile Residue of Solvent Ex-
tract from Aerospace Components (Using Flash Evapora-
1.1 This test method covers the determination of residual
tor)
contamination in an aqueous sample by the use of a total
G121 Practice for Preparation of Contaminated Test Cou-
carbon (TC) analyzer. When used in conjunction with Practice
pons for the Evaluation of Cleaning Agents
G131 and G136, this procedure may be used to determine the
G131 Practice for Cleaning of Materials and Components by
cleanliness of systems, components, and materials requiring a
Ultrasonic Techniques
high level of cleanliness, such as oxygen systems. This
G136 Practice for Determination of Soluble Residual Con-
procedure is applicable for aqueous-based cleaning and sam-
taminants in Materials by Ultrasonic Extraction
pling methods only.
1.2 This test method is not suitable for the evaluation of
3. Terminology
particulate contamination, or contaminants that are not soluble
3.1 Definitions of Terms Specific to This Standard:
in or that do not form an emulsion with water.
3.1.1 contaminant (contamination), n—unwanted molecular
1.3 This standard does not purport to address all of the
and particulate matter that could affect or degrade the perfor-
safety concerns, if any, associated with its use. It is the
mance of the components upon which they reside.
responsibility of the user of this standard to establish appro-
3.1.2 nonvolatile residue (NVR), n—molecular and particu-
priate safety, health, and environmental practices and deter-
late matter remaining following the filtration and controlled
mine the applicability of regulatory limitations prior to use.
evaporation of a liquid containing contaminants.
1.4 This international standard was developed in accor-
3.1.3 Discussion—In this test method, the NVR may be
dance with internationally recognized principles on standard-
uniformly distributed as in a solution or an emulsion, or in the
ization established in the Decision on Principles for the
form of droplets. Molecular contaminants account for most of
Development of International Standards, Guides and Recom-
the NVR.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 3.1.4 particle (particulate contaminant), n— a piece of
matter in a solid state with observable length, width, and
2. Referenced Documents
thickness.
2.1 ASTM Standards: 3.1.5 Discussion—The size of a particle is usually defined
D1193 Specification for Reagent Water
by its greatest dimension and is specified in micrometres.
D2579 Test Method for Total Organic Carbon in Water
3.1.6 molecular contaminant (non-particulate
(Withdrawn 2002)
contamination), n—the molecular contaminant may be in a
gaseous, liquid, or solid form.
This test method is under the jurisdiction of ASTM Committee G04 on
4. Summary of Test Method
Compatibility and Sensitivity of Materials in Oxygen EnrichedAtmospheres and is
the direct responsibility of Subcommittee G04.01 on Test Methods.
4.1 A test method is described for the quantitative analysis
Current edition approved Sept. 1, 2022. Published September 2022. Originally
of aqueous samples and may be used in the determination of
approved in 1996. Last previous edition approved in 2014 as G144 – 01(2014).
contamination on parts, components, and materials used in
DOI: 10.1520/G0144-01R22.
systems requiring a high degree of cleanliness. The residue
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
removed during aqueous cleaning or sampling, using cleaning
Standards volume information, refer to the standard’s Document Summary page on
methods such as Practice G131 and Practice G136, are ana-
the ASTM website.
lyzed using a high-temperature combustion analyzer with a
The last approved version of this historical standard is referenced on
www.astm.org. sensitivity of 60.2 mgC/L (milligrams of carbon per litre).An
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
G144 − 01 (2022)
aqueous sample is injected into the sample port. A stream of necessary to purge dissolved carbon dioxide from the water in
oxygen or air carries the sample into the catalytic combustion order to achieve this level of carbon in the water.
chamber, which is maintained at a temperature high enough to
7.2 Carrier Gas, high-purity oxygen, >99.990 %, <1 ppm
completely pyrolyze the sample. The sample is combusted in
CO and CO , <1 ppm total hydrocarbons. Oxygen of higher
the catalytic combustion chamber and the products are carried
purity may be used if desired.Air that has a hydrocarbon level
by the oxygen or air stream into a nondispersive infrared
less than 1.0 ppm may also be used.
(NDIR)detectorwheretheamountofcarbondioxideinthegas
7.3 Purity of Reagents—Reagent grade chemicals shall be
stream is determined. Additional information on the use and
used in all tests. Unless otherwise indicated, it is intended that
operation of carbon analyzers is provided in Test Methods
all reagents conform to the specifications of the Committee on
D2579.
Analytical Reagents of the American Chemical Society where
4.2 Experience has shown that the bulk of the contaminants 5
such specification are available. Other grades may be used,
are oils and greases; therefore, the samples will typically be
provided it is first ascertained that the reagent is of sufficiently
emulsions rather than solutions. Thus, proper handling and
high purity to permit its use without lessening the accuracy of
preparation techniques are necessary in order to obtain good
the determination.
sample homogeneity.
7.3.1 Anhydrous Potassium Hydrogen Phthalate—
(KC H O ).
8 5 4
5. Significance and Use
7.3.2 Concentrated Phosphoric Acid.
5.1 It is expected that this test method will be suitable for
7.3.3 Concentrated Sulfuric Acid.
the quantitative determination of total carbon in water that has
7.3.4 Concentrated Nitric Acid.
been used to clean, extract, or sample parts, components,
7.3.5 Sodium Hydroxide.
materials, or systems requiring a high degree of cleanliness,
8. Sample Handling
that is, oxygen systems.
8.1 Sample handling is of critical importance in carbon
6. Apparatus
analysis to avoid contaminating the sample. Good laboratory
6.1 A total carbon analyzer consists of a high-temperature
techniques are imperative due to the natural abundance of
TC analyzer that typically utilizes a syringe injection port to carbon in the environment. The following recommendations
introduce the sample into the analyzer, a furnace containing a
are provided for sample handling during collection,
high-temperature catalytic combustion tube to oxidize carbon pretreatment, and analysis.
to carbon dioxide, a NDIR detector to quantitatively determine
8.2 Allglasswareincludingsyringes,shouldbetreatedprior
the carbon dioxide, associated tubing to connect the functional
to use to remove traces of residual carbon. Typical treatments
analytical modules, and a display and control device. A
include sodium hydroxide, hot nitric acid, or hot sulfuric acid.
minimum sensitivity of 60.2 mgC/L is required.
Drain, cool, and rinse with Type II reagent water.
6.1.1 Injection Port—Provides a method for the introduc-
8.3 Use a dedicated syringe for each particular carbon
tion of the sample into the analyzer.
range. When the syringe becomes contaminated, as may be
6.1.2 High-Temperature Furnace—The high-temperature
indicated by incomplete wetting of the inner surface, reapply
furnace maintains the combustion tube at a predetermined
treatment in accordance with 8.2.
value. The combustion tube contains a catalytic bed to oxidize
any organic carbon to carbon dioxide.
9. Preparation of Standard Solutions
6.1.3 NDIR Detector—The nondispersive infrared detector
9.1 Use Specification D1193, Type II water for the prepa-
determines the quantity of carbon dioxide that is eluted from
ration of all standard solutions.The water shall have a TC level
the combustion tube.
of less than 0.2 mgC/L.
6.2 Syringe—Asampling syringe for injection of the sample
9.2 Prepare a standard total carbon stock solution. Weigh
into the TC analyzer.
out 2.126 g of potassium hydrogen phthalate and place into a
6.3 Bottle—Amberborosilicateforstorageofthecalibration
100-mLvolumetric flask.Add 50 to 75 mLof Type II water to
solutions.
dissolve the chemical. Add about 0.1 mL of concentrated
sulfuric or phosphoric acid to adjust the pH below 3, and fill to
6.4 Parts Pan—Stainless steel container, typically with a
the 100-mL mark with Type II water. This will provide a
volume between 1 and 4 L, used to contain the parts during
solution concentration of 10 000 mgC⁄L. The following for-
cleaning.
mula may be used to calculate the mgC/L:
7. Reagents
N 312.01 3wt
mgC/L 5 310 (1)
7.1 Deionized Water, (reagent water), conforming to Speci-
MW
fication D1193, Type II containing less than 0.2 mgC/L. Test
Method D2579 provides detailed instructions if it may become 5
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
SatisfactoryequipmentistheDC-190TCAnalyzerfromRosemountAnalytical Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Inc., Dohrmann Division, 3240 Scott Blvd., P.O. Box 58007, Santa Clara, CA and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
95052-8007. MD.
G144 − 01 (2022)
where: determination. If the value again exceeds 1.0 mgC/L, fresh
reagent water shall be obtained and used for the analysis.
mgC/L = milligrams of carbon per litre of solution,
11.3.2 The average value for the 1.0- and 5.0-mgC/L
N = number of carbon atoms per standard (phthalate)
calibration standards should read 0.85–1.15 mgC/L and
molecule,
4.8–5.2 mgC/L, respectively. If the values for the
...