ASTM G144-96
(Test Method)Standard Test Method for Determination of Residual Contamination of Materials and Components by Total Carbon Analysis Using a High-Temperature Combustion Analyzer
Standard Test Method for Determination of Residual Contamination of Materials and Components by Total Carbon Analysis Using a High-Temperature Combustion Analyzer
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.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: G 144 – 96
Standard Test Method for
Determination of Residual Contamination of Materials and
Components by Total Carbon Analysis Using a
HighTemperature Combustion Analyzer
This standard is issued under the fixed designation G 144; 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 nonvolatile residue (NVR), n—molecular and particu-
late matter remaining following the filtration and controlled
1.1 This test method covers the determination of residual
evaporation of a liquid containing contaminants.
contamination in an aqueous sample by the use of a total
3.1.3 Discussion—In this test method, the NVR may be
carbon (TC) analyzer. When used in conjunction with Practice
uniformly distributed as in a solution or an emulsion, or in the
G 131, this procedure may be used to determine the cleanliness
form of droplets. Molecular contaminants account for most of
of systems and components requiring a high level of cleanli-
the NVR.
ness, such as oxygen systems. This procedure is applicable for
3.1.4 particle (particulate contaminant), n—a piece of mat-
aqueous-based cleaning and sampling methods only.
ter in a solid state with observable length, width, and thickness.
1.2 This test method is not suitable for the evaluation of
3.1.5 Discussion—The size of a particle is usually defined
particulate contamination, or contaminants that are not soluble
by its greatest dimension and is specified in micrometres.
in or that do not form an emulsion with water.
3.1.6 molecular contaminant (non-particulate contamina-
1.3 This standard does not purport to address all of the
tion), n—the molecular contaminant may be in a gaseous,
safety concerns, if any, associated with its use. It is the
liquid, or solid form.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 A test method is described for the quantitative analysis
2. Referenced Documents of aqueous samples and may be used in the determination of
contamination on parts, components, and materials used in
2.1 ASTM Standards:
systems requiring a high degree of cleanliness. The residue
D 1193 Specification for Reagent Water
removed during aqueous cleaning or sampling, using a clean-
D 2579 Test Methods for Total and Organic Carbon in
ing method such as Practice G 131, is analyzed using a
Water
high-temperature combustion analyzer with a sensitivity of 6
F 331 Test Method for Nonvolatile Residue of Halogenated
0.2 mgC/L (milligrams of carbon per litre). An aqueous sample
Solvent Extract from Aerospace Components (Using Ro-
4 is injected into the sample port. A stream of oxygen or air
tary Flash Evaporator)
carries the sample into the catalytic combustion chamber,
G 121 Practice for Preparation of Contaminated Test Cou-
5 which is maintained at a temperature high enough to com-
pons for the Evaluation of Cleaning Agents
pletely pyrolyze the sample. The sample is combusted in the
G 131 Practice for the Cleaning of Materials and Compo-
5 catalytic combustion chamber and the products are carried by
nents by Ultrasonic Techniques
the oxygen or air stream into a nondispersive infrared (NDIR)
3. Terminology detector where the amount of carbon dioxide in the gas stream
is determined. Additional information on the use and operation
3.1 Definitions of Terms Specific to This Standard:
of carbon analyzers is provided in Test Methods D 2579.
3.1.1 contaminant (contamination), n—unwanted molecular
4.2 Experience has shown that the bulk of the contaminants
and particulate matter that could affect or degrade the perfor-
are oils and greases; therefore, the samples will typically be
mance of the components upon which they reside.
emulsions rather than solutions. Thus, proper handling and
preparation techniques are necessary in order to obtain good
This test method is under the jurisdiction of ASTM Committee G-4 on
sample homogeneity.
Compatibility and Sensitivity of Materials in Oxygen-Enriched Atmospheres and is
the direct responsibility of Subcommittee G04.01 on Test Methods.
5. Significance and Use
Current edition approved Oct. 10, 1996. Published December, 1996.
Annual Book of ASTM Standards, Vol 11.01.
5.1 It is expected that this test method will be suitable for
Annual Book of ASTM Standards, Vol 11.02.
the quantitative determination of total carbon in water that has
Annual Book of ASTM Standards, Vol 15.03.
5 been used to clean, extract, or sample parts, components,
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
G 144
materials, or systems requiring a high degree of cleanliness, 7.3.3 Concentrated Sulfuric Acid.
that is, oxygen systems.
8. Sample Handling
6. Apparatus
8.1 Sample handling is of critical importance in carbon
6.1 A total carbon analyzer consists of a high-temperature
analysis to avoid contaminating the sample. Good laboratory
TC analyzer that typically utilizes a syringe injection port to
techniques are imperative due to the natural abundance of
introduce the sample into the analyzer, a furnace containing a
carbon in the environment. The following recommendations
high-temperature catalytic combustion tube to oxidize carbon
are provided for sample handling during collection, pretreat-
to carbon dioxide, a NDIR detector to quantitatively determine
ment, and analysis.
the carbon dioxide, associated tubing to connect the functional
8.2 All glassware including syringes, should be treated prior
analytical modules, and a display and control device. A
to use to remove traces of residual carbon. Typical treatments
minimum sensitivity of 60.2 mgC/L is required.
include chromic acid or hot sulfuric acid. Drain, cool, and rinse
6.1.1 Injection Port—Provides a method for the introduc-
with Type II reagent water.
tion of the sample into the analyzer.
8.3 Use a dedicated syringe for each particular carbon
6.1.2 High-Temperature Furnace—The high-temperature
range. When the syringe becomes contaminated, as may be
furnace maintains the combustion tube at a predetermined
indicated by incomplete wetting of the inner surface, reapply
value. The combustion tube contains a catalytic bed to oxidize
treatment in accordance with 8.2.
any organic carbon to carbon dioxide.
6.1.3 NDIR Detector—The nondispersive infrared detector
9. Preparation of Standard Solutions
determines the quantity of carbon dioxide that is eluted from
9.1 Use Specification D 1193, Type II water for the prepa-
the combustion tube.
ration of all standard solutions. The water shall have a TC level
6.2 Syringe—A sampling syringe for injection of the sample
of less than 0.2 mgC/L.
into the TC analyzer.
9.2 Prepare a standard total carbon stock solution. Weigh
6.3 Bottle—Amber borosilicate for storage of the calibra-
out 2.126 g of potassium hydrogen phthalate and place into a
tion solutions.
100-mL volumetric flask. Add 50 to 75 mL of Type II water to
6.4 Parts Pan—Stainless steel container, typically with a
dissolve the chemical. Add about 0.1 mL of concentrated
volume between 1 and 4 L, used to contain the parts during
sulfuric or phosphoric acid to adjust the pH below 3, and fill to
cleaning.
the 100-mL mark with Type II water. This will provide a
7. Reagents
solution concentration of 10 000 mgC/L. The following for-
mula may be used to calculate the mgC/L:
7.1 Deionized Water, (reagent water), conforming to Speci-
fication D 1193, Type II containing less than 0.2 mgC/L. Test
N 3 12.01 3 wt
mgC/L 5 3 10 (1)
Methods D 2579 provides detailed instructions if it may
MW
become necessary to purge dissolved carbon dioxide from the
where:
water in order to achieve this level of carbon in the water.
mgC/L 5 milligrams of carbon per litre of solution,
7.2 Carrier Gas, high-purity oxygen, >99.990 %, <1 ppm
N 5 number of carbon atoms per standard (phthalate)
CO and CO , <1 ppm total hydrocarbons. Oxygen of higher
molecule,
purity may be used if desired. Air that has a hydrocarbon level
12.01 5 atomic weight of carbon,
less than 1.0 ppm may also be used.
wt 5 weight of carbon-containing compound, g, and
7.3 Purity of Reagents—Reagent grade chemicals shall be
MW 5 molecular weight of the carbon-containing com-
used in all tests. Unless otherwise indicated, it is intended that
pound.
all reagents conform to the specifications of the Committee on
Store the stock solutions in amber borosilicate bottles with
Analytical Reagents of the American Chemical Society where
PTFE-lined closures at 4°C.
such specification are available. Other grades may be used,
9.2.1 Replace the solution monthly. Date the solution when
provided it is first ascertained that the reagent is of sufficiently
prepared or list the expiration date on the label.
high purity to permit its use without lessening the accuracy of
9.3 Prepare total carbon working standard solutions from
the determination.
the standard stock solution prepared in 9.2, of 1.0 and 5.0
7.3.1 Anhydrous Potassium Hydrogen Phthalate—
mgC/L for expected sample concentrations less than 5.0
(KC H O ).
8 5 4
mgC/L. If sample concentrations are expected to exceed 5.0
7.3.2 Concentrated Phosphoric Acid.
mgC/L, a standard solution at least twice the expected concen-
tration shall be prepared. It is recommended that 1 L of solution
Satisfactory equipment is the DC-190 TC Analyzer from Rosemount Analytical
be prepared for total carbon values of 10 mgC/L and below.
Inc., Dohrmann Division, 3240 Scott Blvd., P.O. Box 58007, Santa Clara, CA
9.3.1 Store the working calibration total carbon standard
95052-8007.
solutions at 4°C in borosilicate bottles with PTFE-lined clo-
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
sures.
listed by the American Chemical Society, see Analar Standards for Laboratory
...
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