ASTM G144-01(2006)

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
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 G 131 and G 136, 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.
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: 30-Sep-2006
• 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

• Replaces: ASTM G144-01 - Standard Test Method for Determination of Residual Contamination of Materials and Components by Total Carbon Analysis Using a High-Temperature Combustion Analyzer
• Effective Date: 01-Oct-2006
• Referred By: ASTM G120-15(2023) - Standard Practice for Determination of Soluble Residual Contamination by Soxhlet Extraction
• Effective Date: 01-Oct-2006
• 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: 01-Oct-2006
• Referred By: ASTM G126-16(2023) - Standard Terminology Relating to the Compatibility and Sensitivity of Materials in Oxygen Enriched Atmospheres
• Effective Date: 01-Oct-2006

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: G144 − 01(Reapproved 2006)
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 Ultrasonic Techniques
G136 Practice for Determination of Soluble Residual Con-
1.1 This test method covers the determination of residual
taminants in Materials by Ultrasonic Extraction
contamination in an aqueous sample by the use of a total
carbon (TC) analyzer. When used in conjunction with Practice
3. Terminology
G131 and G136, this procedure may be used to determine the
3.1 Definitions of Terms Specific to This Standard:
cleanliness of systems, components, and materials requiring a
3.1.1 contaminant (contamination), n—unwanted molecular
high level of cleanliness, such as oxygen systems. This
and particulate matter that could affect or degrade the perfor-
procedure is applicable for aqueous-based cleaning and sam-
mance of the components upon which they reside.
pling methods only.
3.1.2 nonvolatile residue (NVR), n—molecular and particu-
1.2 This test method is not suitable for the evaluation of
late matter remaining following the filtration and controlled
particulate contamination, or contaminants that are not soluble
evaporation of a liquid containing contaminants.
in or that do not form an emulsion with water.
3.1.3 Discussion—In this test method, the NVR may be
1.3 This standard does not purport to address all of the
uniformly distributed as in a solution or an emulsion, or in the
safety concerns, if any, associated with its use. It is the
form of droplets. Molecular contaminants account for most of
responsibility of the user of this standard to establish appro-
the NVR.
priate safety and health practices and determine the applica-
3.1.4 particle (particulate contaminant), n— a piece of
bility of regulatory limitations prior to use.
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
F331 Test Method for Nonvolatile Residue of Solvent Ex-
gaseous, liquid, or solid form.
tract from Aerospace Components (Using Flash Evapora-
tor)
4. Summary of Test Method
G121 Practice for Preparation of Contaminated Test Cou-
4.1 A test method is described for the quantitative analysis
pons for the Evaluation of Cleaning Agents
of aqueous samples and may be used in the determination of
G131 PracticeforCleaningofMaterialsandComponentsby
contamination on parts, components, and materials used in
systems requiring a high degree of cleanliness. The residue
removed during aqueous cleaning or sampling, using cleaning
This test method is under the jurisdiction of ASTM Committee G04 on
methods such as Practice G131 and Practice G136, are ana-
Compatibility and Sensitivity of Materials in Oxygen EnrichedAtmospheres and is
the direct responsibility of Subcommittee G04.01 on Test Methods.
lyzed using a high-temperature combustion analyzer with a
Current edition approved Oct. 1, 2006. Published December 2006. Originally
sensitivity of 60.2 mgC/L (milligrams of carbon per litre).An
approved in 1996. Last previous edition approved in 2001 as G144 – 01. DOI:
aqueous sample is injected into the sample port. A stream of
10.1520/G0144-01R06.
oxygen or air carries the sample into the catalytic combustion
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
chamber, which is maintained at a temperature high enough to
Standards volume information, refer to the standard’s Document Summary page on
completely pyrolyze the sample. The sample is combusted in
the ASTM website.
the catalytic combustion chamber and the products are carried
The last approved version of this historical standard is referenced on
www.astm.org. by the oxygen or air stream into a nondispersive infrared
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
G144 − 01 (2006)
(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
such specification are available. Other grades may be used,
4.2 Experience has shown that the bulk of the contaminants
provided it is first ascertained that the reagent is of sufficiently
are oils and greases; therefore, the samples will typically be
high purity to permit its use without lessening the accuracy of
emulsions rather than solutions. Thus, proper handling and
the determination.
preparation techniques are necessary in order to obtain good
7.3.1 Anhydrous Potassium Hydrogen Phthalate—
sample homogeneity.
(KC H O ).
8 5 4
7.3.2 Concentrated Phosphoric Acid.
5. Significance and Use
7.3.3 Concentrated Sulfuric Acid.
5.1 It is expected that this test method will be suitable for
7.3.4 Concentrated Nitric Acid.
the quantitative determination of total carbon in water that has
7.3.5 Sodium Hydroxide.
been used to clean, extract, or sample parts, components,
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
analysis to avoid contaminating the sample. Good laboratory
6. Apparatus
techniques are imperative due to the natural abundance of
6.1 A total carbon analyzer consists of a high-temperature
4 carbon in the environment. The following recommendations
TC analyzer that typically utilizes a syringe injection port to
are provided for sample handling during collection,
introduce the sample into the analyzer, a furnace containing a
pretreatment, and analysis.
high-temperature catalytic combustion tube to oxidize carbon
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
rationofallstandardsolutions.Thewatershallhavea TClevel
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
where:
Method D2579 provides detailed instructions if it may become
mgC/L = milligrams of carbon per litre of solution,
necessary to purge dissolved carbon dioxide from the water in
N = number of carbon atoms per standard (phthalate)
order to achieve this level of carbon in the water.
molecule,
7.2 Carrier Gas, high-purity oxygen, >99.990 %, <1 ppm
12.01 = atomic weight of carbon,
CO and CO , <1 ppm total hydrocarbons. Oxygen of higher
purity may be used if desired.Air that has a hydrocarbon level
less than 1.0 ppm may also be used. 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 (2006)
prepare new calibration standards. The standard deviation
wt = weight of carbon-containing compound, g, and
should not exceed 60.2 mgC/L.
MW = molecular weight of the carbon-containing
compound.
12. Procedure
Store the stock solutions in amber borosilicate bottles with
12.1 Determine the TC content of samples obtained from
PTFE-lined closures at 4°C.
parts that have been extracted withType II water in accordance
9.2.1 Replac
...