ASTM D2109-01(2006)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D2109–01(Reapproved2006)
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.
1. Scope present in the sample, they should be removed by filtration or
decantation prior to beginning this test method. Nonvolatile
1.1 These test methods cover the determination of nonvola-
matter is considered to be “in solution” with the solvent and
tile matter in halogenated organic solvents and admixtures.
that which will become residual upon drying the solvent at a
1.2 Five test methods are covered, as follows:
specified temperature.
1.2.1 Test Method A—For halogenated organic solvents or
2.1.2 Nonvolatile matter and nonvolatile residue are inter-
admixtures having less than 50 ppm nonvolatile matter; or
changeable terms.
where precision better than 610 ppm is required.
1.2.2 Test Method B—For halogenated organic solvents or
3. Significance and Use
admixtures having more than 50 ppm nonvolatile matter or
3.1 Nonvolatile matter in solvents can adversely affect their
where precision of 60.001 % (10 ppm) is satisfactory.
cleaning properties. These test methods can be used to control
1.2.3 Test Method C—For low-boiling halogenated organic
soil contamination in the boiling solvent, which if allowed to
solvents or their admixtures (for example, methylene chloride,
become too high, can decrease the stability of the solvent.
trichlorotrifluoroethane) that may superheat and cause bump-
3.2 These test methods can be used to establish manufac-
ing while evaporating to dryness with steam. A precision of
turing and purchasing specifications.
greater than6 10 ppm can be attained.
1.2.4 Test Method D—For rapid measurement of nonvola-
4. Apparatus
tilematterinhalogenatedorganicsolventsandtheiradmixtures
4.1 Oven, thermostatically controlled at 105 6 5°C.
and where precision better than 610 ppm is required.
4.2 Evaporating Dish, 125-mL capacity, platinum or high-
1.2.5 Test Method E—For halogenated organic solvents or
silica glass, Methods A, B, C.
admixtures and where precision better than 610 ppm is
4.3 Evaporating Dish (80 3 45 or 115 3 50) (Method D).
required.
4.4 Steam Bath (or hot plate).
1.3 The values stated in SI units are to be regarded as the
4.5 Hot Plate, (Method D).
standard.
4.6 Heat Lamp, 250 W, (Method E).
1.4 This standard does not purport to address all of the
4.7 Analytical Balance, capable of measuring to 0.0001 g.
safety concerns, if any, associated with its use. It is the
4.8 Top Loading Balance, capable of weighing to 0.01 g.
responsibility of the user of this standard to establish appro-
4.9 Aluminum Weighing Dish,57 3 18 mm, (Method D).
priate safety and health practices and determine the applica-
4.10 Aluminum Weighing Dish, 200 ML capacity, (Method
bility of regulatory limitations prior to use.
E).
4.11 1000-mL Volumetric Flask (Test Method A).
2. Terminology
4.12 100-mL Volumetric Pipet (Test Method B and E).
2.1 Definitions of Terms Specific to This Standard:
4.13 1000-mL Graduated Cylinder (Test Method C).
2.1.1 The term nonvolatile matter should not be construed
4.14 1500-mL Erlenmeyer Flask (Test Method C).
as equivalent to residue on ignition, ignition residue, or ash
content. Particulates, sediments, and suspended matter should
TEST METHOD A
not be considered part of nonvolatile matter. If these solids are
5. Procedure
5.1 Dry a 125-mL capacity platinum (or high-silica glass)
These test methods are under the jurisdiction of ASTM Committee D26 on
evaporating dish in an oven at 105 6 5°C and cool in a
Halogenated Organic Solvents and Fire Extinguishing Agents and are the direct
responsibility of Subcommittee D26.04 on Test Methods.
desiccator. Repeat until the weight is constant or within 0.1 mg
Current edition approved June 1, 2006. Published June 2006. Originally
of the last weighing. Rinse a clean dry 1000-mL volumetric
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.
D2109–01 (2006)
flask with the solvent and fill to the 1000-mL mark with the 9. Calculation
solvent to be tested. Invert the evaporating dish, place it over
9.1 Calculate the nonvolatile matter and report in weight
the mouth of the flask, hold it firmly in place, and invert the
percent as follows:
flask. In this position place both dish and flask on a steam bath.
~A! ~100! ~A!
Adjust a ring support to hold the flask so the mouth of the flask
Nonvolatile matter, ppm by weight 5 5 (2)
~B! ~100! ~B!
is approximately 25 mm above the bottom of the evaporating
dish. Thus held, the flask automatically feeds the solvent to the
where:
dish during the evaporation. (Warning—This test method
A = grams of residue, and
must be run in a ventilated, dust-free area.)
B = density of sample.
5.2 Evaporate the 1000-mL sample to dryness. Remove the
10. Precision and Bias
dish from the steam bath with metal tongs and blot the outside
of the dish with lint-free paper tissue.
10.1 Precision—As the only significant difference between
Test Method B and Test Methods A and C is the sample size
NOTE 1—Hot plates develop high temperatures on the plate surface. If
(100 mL versus 1000 mL), it is reasonable to assume that the
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 precision is roughly ten times that of Test MethodsAand C or
from reaching temperatures exceeding 105°C.
2 ppm for repeatability and 10 ppm for reproducibility.
10.2 The bias of this test method has not been determined.
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
TEST METHOD C
contents.
11. Procedure
6. Calculation
11.1 Dry a 125-mL capacity platinum (or high-silica glass)
6.1 Calculate the nonvolatile matter and report in weight
evaporating dish in an oven at 105°C and cool in a desiccator.
percent or parts per million as follows:
Repeat until the weight is constant or within 0.1 mg of the last
A! 10 ! A! 1000!
~ ~ ~ ~
weighing. Rinse a clean dry 1000-mLgraduated cylinder and a
Nonvolatile matter, ppm by weight 5 5 (1)
~B! ~1000! ~B!
1500-mL Erlenmeyer flask with the solvent to be tested.
11.2 Measure 1000 mL of the sample into the cleaned
where:
graduate and transfer 970 mL of it into the clean Erlenmeyer
A = grams of residue, and
flask. Evaporate to about 40 mL on a steam bath or warm hot
B = density of sample.
plate in a fume hood. Do not evaporate to dryness.
7. Precision and Bias
11.3 Transfer the residue to the evaporating dish. Rinse the
flask twice with a 15-mL portion of the sample retained in the
7.1 Repeatability (Single Analyst)—The standard deviation
graduate (see
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