ASTM D2109-01(2006)e1

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An American National Standard
Designation:D2109–01(Reapproved2006)
Designation:D2109–96 (Reapproved 2000)
Standard Test Methods for
Nonvolatile Matter in Halogenated Organic
Solvents and Their Admixtures
This standard is issued under the fixed designation D 2109; 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.
This standard has been approved for use by agencies of the Department of Defense.
e NOTE—A research report footnote was added in November 2001.
—Removed research report references in Sections 7, 10, and 13 editorially in March 2008.
1. Scope
1.1 These test methods cover the determination of nonvolatile matter in halogenated organic solvents and admixtures.
1.2Three1.2 Five test methods are covered, as follows:
1.2.1 Test Method A— For halogenated organic solvents or admixtures having less than 50 ppm nonvolatile matter; or where
precision greaterbetter than 610 ppm is required.
1.2.2 Test Method B— For halogenated organic solvents or admixtures having more than 50 ppm nonvolatile matter or where
precision of 60.001 % (10 ppm) is satisfactory.
1.2.3 Test Method C—For low-boiling halogenated organic solvents or their admixtures (for example, methylene chloride,
trichlorotrifluoroethane) that may superheat and cause bumping while evaporating to dryness with steam. A precision of greater
than 610 ppm can be attained. — For low-boiling halogenated organic solvents or their admixtures (for example, methylene
chloride, trichlorotrifluoroethane) that may superheat and cause bumping while evaporating to dryness with steam.Aprecision of
greater than6 10 ppm can be attained.
1.2.4 Test Method D— For rapid measurement of nonvolatile matter in halogenated organic solvents and their admixtures and
where precision better than 610 ppm is required.
1.2.5 Test Method E— For halogenated organic solvents or admixtures and where precision better than 610 ppm is required.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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. Terminology
2.1 Definitions of Terms Specific to This Standard:
2.1.1 The term nonvolatile matter should not be construed as equivalent to residue on ignition, ignition residue, or ash content.
Particulates, sediments, and suspended matter should not be considered part of nonvolatile residue.matter. If these solids are
present in the sample, they should be removed by filtration or decantation prior to beginning this test method. Nonvolatile matter
is considered to be “in solution” with the solvent and that which will become residual upon drying the solvent at a specified
temperature.
2.1.2 Nonvolatile matter and nonvolatile residue are interchangeable terms.
3. Significance and Use
3.1 Nonvolatile matter in solvents can adversely affect their cleaning properties. These test methods can be used to control soil
contamination in the boiling solvent, which if allowed to become too high, can decrease the stability of the solvent.
3.2 These test methods can be used to establish manufacturing and purchasing specifications.
4. Apparatus
4.1 Oven, thermostatically controlled at 105 6 5°C.
These test methods are under the jurisdiction ofASTM Committee D26 on Halogenated Organic Solvents and Fire ExtinguishingAgents and are the direct responsibility
of Subcommittee D26.04 on Test Methods.
Current edition approved June 10, 1996. Published August 1996. Originally published as D2109 – 62 T. Last previous edition D2109–92.
Current edition approved June 1, 2006. Published June 2006. Originally approved in 1962 as D 2109 – 62 T. Last previous edition approved in 2001 as D 2109 – 01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D2109–01 (2006)
D2109–96 (2000)
4.2 Evaporating Dish,125-mLcapacity,platinumorhigh-silicaglass.,125-mLcapacity,platinumorhigh-silicaglass,Methods
A, B, C.
4.3 Evaporating Dish (80 3 45 or 115 3 50) (Method D).
4.4 Steam Bath (or hot plate).
4.4Analytical Balance.
4.5 Hot Plate, (Method D).
4.6 Heat Lamp, 250 W, (Method E).
4.7 Analytical Balance, capable of measuring to 0.0001 g.
4.8 Top Loading Balance, capable of weighing to 0.01 g.
4.9 Aluminum Weighing Dish,57 3 18 mm, (Method D).
4.10 Aluminum Weighing Dish, 200 ML capacity, (Method E).
4.11 1000-mL Volumetric Flask (Test Method A).
4.6
4.12 100-mL Volumetric Pipet(Test Method B).
4.71000-mL Graduated Cylinder (Test Method B and E).
4.13 1000-mL Graduated Cylinder (Test Method C).
4.8
4.14 1500-mL Erlenmeyer Flask (Test Method C).
TEST METHOD A
5. Procedure
5.1 Dry a 125-mL capacity platinum (or high-silica glass) evaporating dish in an oven at 105 6 5°C and cool in a desiccator.
Repeat until the weight is constant or within 0.1 mg of the last weighing. Rinse a clean dry 1000-mL volumetric flask with the
solvent and fill to the 1000-mLmark with the solvent to be tested. Invert the evaporating dish, place it over the mouth of the flask,
hold it firmly in place, and invert the flask. In this position place both dish and flask on a steam bath.Adjust a ring support to hold
the flask so the mouth of the flask is approximately 25 mm above the bottom of the evaporating dish. Thus held, the flask
automatically feeds the solvent to the dish during the evaporation. ( Warning—This test method must be run in a ventilated,
dust-free area.)
5.2 Evaporate the 1000-mL sample to dryness. Remove the dish from the steam bath with metal tongs and blot the outside of
the dish with lint-free paper tissue.
NOTE1—Caution:This test method must be run in a ventilated, dust-free area.
5.2Evaporate the 1000-mL sample to dryness. Remove the dish from the steam bath with metal tongs and blot the outside of
the dish with lint-free paper tissue.
NOTE2—Hot plates develop high temperatures on the plate surface. If a hot plate is used to evaporate the solvent, the evaporating dish should be placed
inside a water bath while on the hot plate to prevent the sample from reaching temperatures exceeding 105°C. 1—Hot plates develop high temperatures
on the plate surface. If a hot plate is used to evaporate the solvent, the evaporating dish should be placed inside a water bath while on the hot plate to
prevent the sample from reaching temperatures exceeding 105°C.
5.3 Place the dish and contents in an oven at 105 6 5°C for approximately 1 h. Cool in a desiccator and weigh the dish and
contents.
6. Calculation
6.1 Calculate the nonvolatile matter and report in weight percent or parts per million as follows:
~A! ~10 ! ~A! ~1000!
Nonvolatile matter, ppm by weight 5 5 (1)
~B! ~1000! ~B!
where:
A = grams of residue, and
B = density of sample.
7. Precision and Bias
7.1 Repeatability (Single Analyst)—The standard deviation of results has been estimated to be 0.2 weight ppm. Two such
values should be considered suspect (95 % confidence level) if they differ by more than 0.7 ppm.
7.2 Reproducibility (Multilaboratory)—The standard deviation of results has been estimated to be 1.0 weight ppm. Two such
values should be considered suspect (95 % confidence level) if they differ by more than 4.6 weight ppm.
TEST METHOD B
8. Procedure
8.1 Dry a 125-mL capacity platinum (or high-silica glass) evaporating dish in an oven at 105 6 5°C and cool in a desiccator.
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D2109–01 (2006)
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Repeat until the weight is constant or with
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