Standard Test Methods for Nonvolatile Matter in Halogenated Organic<br> Solvents and Their Admixtures

SIGNIFICANCE AND USE
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.
These test methods can be used to establish manufacturing and purchasing specifications.
SCOPE
1.1 These test methods cover the determination of nonvolatile matter in halogenated organic solvents and admixtures.
1.2 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 better than ±10 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 ±0.001 % (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± 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 ±10 ppm is required.
1.2.5 Test Method E—For halogenated organic solvents or admixtures and where precision better than ±10 ppm is required.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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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Publication Date
31-Jul-2011
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ASTM D2109-01(2011) - Standard Test Methods for Nonvolatile Matter in Halogenated Organic<br> Solvents and Their Admixtures
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D2109 − 01(Reapproved2011)
Standard Test Methods for
Nonvolatile Matter in Halogenated Organic
Solvents and Their Admixtures
This standard is issued under the fixed designation D2109; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) 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 2.1.1 The term nonvolatile matter should not be construed
as equivalent to residue on ignition, ignition residue, or ash
1.1 These test methods cover the determination of nonvola-
content. Particulates, sediments, and suspended matter should
tile matter in halogenated organic solvents and admixtures.
not be considered part of nonvolatile matter. If these solids are
1.2 Five test methods are covered, as follows:
present in the sample, they should be removed by filtration or
1.2.1 Test Method A—For halogenated organic solvents or
decantation prior to beginning this test method. Nonvolatile
admixtures having less than 50 ppm nonvolatile matter; or
matter is considered to be “in solution” with the solvent and
where precision better than 610 ppm is required.
that which will become residual upon drying the solvent at a
1.2.2 Test Method B—For halogenated organic solvents or
specified temperature.
admixtures having more than 50 ppm nonvolatile matter or
2.1.2 Nonvolatile matter and nonvolatile residue are inter-
where precision of 60.001% (10 ppm) is satisfactory.
changeable terms.
1.2.3 Test Method C—For low-boiling halogenated organic
3. Significance and Use
solvents or their admixtures (for example, methylene chloride,
trichlorotrifluoroethane) that may superheat and cause bump-
3.1 Nonvolatile matter in solvents can adversely affect their
ing while evaporating to dryness with steam. A precision of
cleaning properties. These test methods can be used to control
greater than6 10 ppm can be attained.
soil contamination in the boiling solvent, which if allowed to
1.2.4 Test Method D—Forrapidmeasurementofnonvolatile
become too high, can decrease the stability of the solvent.
matter in halogenated organic solvents and their admixtures
3.2 These test methods can be used to establish manufac-
and where precision better than 610 ppm is required.
turing and purchasing specifications.
1.2.5 Test Method E—For halogenated organic solvents or
admixtures and where precision better than 610 ppm is
4. Apparatus
required.
4.1 Oven, thermostatically controlled at 105 6 5°C.
1.3 The values stated in SI units are to be regarded as the
4.2 Evaporating Dish, 125-mL capacity, platinum or high-
standard.
silica glass, Methods A, B, C.
1.4 The values stated in SI units are to be regarded as
4.3 Evaporating Dish (80 × 45 or 115 × 50) (Method D).
standard. No other units of measurement are included in this
4.4 Steam Bath (or hot plate).
standard.
4.5 Hot Plate, (Method D).
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.6 Heat Lamp, 250 W, (Method E).
responsibility of the user of this standard to establish appro-
4.7 Analytical Balance, capable of measuring to 0.0001 g.
priate safety and health practices and determine the applica-
4.8 Top Loading Balance, capable of weighing to 0.01 g.
bility of regulatory limitations prior to use.
4.9 Aluminum Weighing Dish, 57 × 18 mm, (Method D).
2. Terminology
4.10 Aluminum Weighing Dish, 200 ML capacity, (Method
2.1 Definitions of Terms Specific to This Standard:
E).
4.11 1000-mL Volumetric Flask (Test Method A).
These test methods are under the jurisdiction of ASTM Committee D26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and are the direct
4.12 100-mL Volumetric Pipet (Test Method B and E).
responsibility of Subcommittee D26.04 on Test Methods.
Current edition approved Aug. 1, 2011. Published November 2011. Originally
4.13 1000-mL Graduated Cylinder (Test Method C).
approved in 1962 as D2109 – 62 T. Last previous edition approved in 2006 as
´1
D2109–01 (2006) . DOI: 10.1520/D2109-01R11. 4.14 1500-mL Erlenmeyer Flask (Test Method C).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2109 − 01(2011)
TEST METHOD A 8.3 Place the dish and contents in an oven at 105 6 5°C for
approximately1h.Coolinadesiccatorandweighthedishand
5. Procedure
contents.
5.1 Dry a 125-mL capacity platinum (or high-silica glass)
9. Calculation
evaporating dish in an oven at 105 6 5°C and cool in a
desiccator.Repeatuntiltheweightisconstantorwithin0.1mg
9.1 Calculate the nonvolatile matter and report in weight
of the last weighing. Rinse a clean dry 1000-mL volumetric
percent as follows:
flask with the solvent and fill to the 1000-mL mark with the
~A!~100! ~A!
solvent to be tested. Invert the evaporating dish, place it over Nonvolatilematter, ppmbyweight 5 5 (2)
B 100 B
~ !~ ! ~ !
the mouth of the flask, hold it firmly in place, and invert the
where:
flask.Inthispositionplacebothdishandflaskonasteambath.
Adjustaringsupporttoholdtheflasksothemouthoftheflask
A = grams of residue, and
is approximately 25 mm above the bottom of the evaporating B = density of sample.
dish.Thusheld,theflaskautomaticallyfeedsthesolventtothe
10. Precision and Bias
dish during the evaporation. (Warning—This test method
must be run in a ventilated, dust-free area.) 10.1 Precision—As the only significant difference between
Test Method B and Test Methods A and C is the sample size
5.2 Evaporate the 1000-mL sample to dryness. Remove the
(100 mL versus 1000 mL), it is reasonable to assume that the
dish from the steam bath with metal tongs and blot the outside
precision is roughly ten times that of Test MethodsAand C or
of the dish with lint-free paper tissue.
2 ppm for repeatability and 10 ppm for reproducibility.
NOTE 1—Hot plates develop high temperatures on the plate surface. If
10.2 The bias of this test method has not been determined.
ahotplateisusedtoevaporatethesolvent,theevaporatingdishshouldbe
placed inside a water bath while on the hot plate to prevent the sample
TEST METHOD C
from reaching temperatures exceeding 105°C.
5.3 Place the dish and contents in an oven at 105 6 5°C for
11. Procedure
approximately1h.Coolinadesiccatorandweighthedishand
11.1 Dry a 125-mL capacity platinum (or high-silica glass)
contents.
evaporating dish in an oven at 105°C and cool in a desiccator.
6. Calculation
Repeat until the weight is constant or within 0.1 mg of the last
weighing.Rinseacleandry1000-mLgraduatedcylinderanda
6.1 Calculate the nonvolatile matter and report in weight
1500-mL Erlenmeyer flask with the solvent to be tested.
percent or parts per million as follows:
11.2 Measure 1000 mL of the sample into the cleaned
A 10 A 1000
~ !~ ! ~ !~ !
Nonvolatilematter, ppmbyweight 5 5 (1)
graduate and transfer 970 mL of it into the clean Erlenmeyer
~B!~1000! ~B!
flask. Evaporate to about 40 mL on a steam bath or warm hot
where:
plate in a fume hood. Do not evaporate to dryness.
A = grams of residue, and
11.3 Transfer the residue to the evaporating dish. Rinse the
B = density of sample.
flask twice with a 15-mL portion of the
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