ASTM D3448-10(2015)e1

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
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Designation: D3448 − 10 D3448 − 10 (Reapproved 2015)
Standard Test Method for
Specific Aqueous Conductance of Trichlorotrifluoroethane
This standard is issued under the fixed designation D3448; 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.
ε NOTE—Editorial changes were made in 1.3 and X1.1 in June 2015.
1. Scope
1.1 This test method covers the determination of aqueous conductivity due to ionizable contaminants extracted from
trichlorotrifluoroethane. The value of 1.9 μS/cm as maximum specific aqueous conductance corresponds to 0.1 ppm of chloride
ion (100 ppb). It was calculated by putting the solvent specification of 0.1 ppm chloride into the equation of the subject method
to find C − C equals 19.08. The specific conductance due to contaminants from the solvent was then calculated as follows:
2 1
C 2 C C 5 19 0.1 5 1.9 µS/cm (1)
~ ! ~ ! ~ !
2 1 3
1.2 The above is exclusive of the background specific conductance of the water used in the analysis.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 Exception—Values are stated in inch-pound units in Fig. 1.
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 consult and establish appropriate safety and health practices and determine the applicability of
regulatory limitations prior to use. Specific precautionary statements are given in Section 6.
2. Summary of Test Method
2.1 Ionizable impurities in the solvent are extracted with water of known low conductivity. The increase in water conductivity
measures the amount of these impurities present.
3. Significance and Use
3.1 This test method allows for the determination of ionizionizableable contaminants (expressed in terms of ppb of HCl) in
trichlorotrifluoroethane via measurement of specific aqueous conductance.
3.2 This test method can be used for establishing manufacturing and purchasing specifications.
4. Apparatus
4.1 Conductivity Bridge.
4.2 Conductivity Cell, dip-type. dip-type. Cell constant of 0.1 reciprocal centimetre. Electrodes must be bright platinum.
4.3 Polyethylene Beaker, 250-mL.
4.4 Polyethylene Bottles, wide mouth, 300-mL and 500-mL size.
4.4.1 Calibrate and mark the outside of the 300-mL polyethylene bottles to indicate 20, 120, and 220 mL (graduate) of water
volume, using deionized water to determine the liquid levels.
4.5 Polyethylene Tubing, long enough to reach the bottom of the 300-mL polyethylene bottle.
This test method is under the jurisdiction of ASTM Committee D26 on Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct responsibility of
Subcommittee D26.04 on Test Methods.
Current edition approved June 1, 2010June 1, 2015. Published August 2010June 2015. Originally approved in 1975. Last previous edition approved in 20052010 as
D3448 – 85D3448 – 10.(2005). DOI: 10.1520/D3448-10.10.1520/D3448-10R15E01.
The sole source of supply of the apparatus (Serfass Model RCM-15B1) known to the committee at this time is Industrial Instrument Inc., Cedar Grove, NJ. If you are
aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend.
The sole source of supply of the apparatus (Model Cel-A01) known to the committee at this time is Industrial Instrument Inc., Cedar Grove, NJ. If you are aware of
alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D3448 − 10 (2015)
5. Reagents
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
5.2 Alcoholic Hydrochloric Acid (0.01 N)—Dilute 5.0 mL (pipet) of concentrated hydrochloric acid to 6 L with denatured 2B
ethyl alcohol.
5.3 Alumina Gel. Gel.
5.4 Deionized Trichloromonofluoromethane, in 25-kg cylinder. This deionized solvent may be selected pure material or it may
be purified by multiple passes through an alumina gel contactor (see Fig. 1). Check the acceptability of this deionized solvent as
described in 7.4.
NOTE 1—The use of deionized trichloromonofluoromethane will serve as a check on the cleanliness. The deionized standard should be used as required
on a periodic basis when samples are being evaluated. Standards should be checked whenever high values are obtained or there is doubt of the results.
5.5 Deionized Water—Distilled water passed through two mixed resin ion exchangers connected in series and having a
conductance of no greater than 0.5 μS. Check the acceptability of the deionized water in accordance with 7.3.
5.6 Ethyl Alcohol.
NOTE 2—Specially denatured ethyl alcohol conforming to Formula SD-2B of the U.S. Bureau of Internal Revenue may be substituted for ethyl alcohol
(95 %).
5.7 Hydrochloric Acid, concentrated.
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 Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
The sole source of supply of the apparatus (Grade F-3) known to the committee at this time is Aluminum Company of America. If you are aware of alternative suppliers,
please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,
which you may attend.
FIG. 1 Alumina Gel Contractor
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D3448 − 10 (2015)
5.8 Ion-Exchange Cylinders. Cylinders.
6. Safety Precautions
6.1 Both trichlorotrifluoroethane and trichloromonofluoromethane are not flammable and have threshold limit value’s of 1000
ppm by volume in air. The respective boiling points of these solvents are 47.6 and 23.7°C. Avoid repeated skin contact with the
solvents. They remove surface oils from skin.
6.2 Denatured ethyl alcohol is flammable and has a threshold limit value of 1000 ppm by volume in air.
6.3 Hydrochloric Acid—Take all precautions necessary to avoid contact with the body internally and externally. The acid is
corrosive.
7. Procedure
7.1 The basis of this test method is the determination by conductance of ions present in the test solution. Therefore, clean all
equipment carefully to remove all adsorbed ions in the measuring apparatus, otherwise, erroneously high values will be obtained.
Do the initial cleaning and the cleaning of equipment in accordance with 7.2. All equipment must be rinsed with deionized
trichloromonofluoromethane before using in a test.
7.2 Deionizing of Equipment:
7.2.1 Polyethylene Bottles and Stainless Steel Cylinders:
7.2.1.1 Add about 30 g of ion exchange resin from an exchange cylinder to the item to be cleaned. Use an exchange cylinder
as a source of resin for cleaning.
7.2.1.2 Add deionized water to the container until it is about two-thirds full.
7.2.1.3 Close the container and roll for at least 24 h on a ball mill roller or its equivalent.
7.2.1.4 Discard the ion-exchange resin and water, rinse with deionized water and then with deionized trichloromono-
fluoromethane.
7.2.2 Polyethylene Delivery Tubes:
NOTE 3—Use of highly plasticized polyethylene tubing and bottles is not recommended.
7.2.2.1 Place the polyethylene delivery tubes in a 500-mL polyethylene bottle.
7.2.2.2 Clean by following 7.2.1.1 – 7.2.1.4.
7.2.3 Polyethylene Beakers, Dip-Cell, and Other Equipment:
7.2.3.1 Add about 30 g of ion-exchange resin to the beaker.
7.2.3.2 Fill the beaker with deionized water.
7.2.3.3 Stir, shake, or transfer the mixture from one container to another for a
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