An American National Standard

Designation: D 2384 – 83 (Reapproved 2004)

Standard Test Methods for

Traces of Volatile Chlorides in Butane-Butene Mixtures1
This standard is issued under the fixed designation D 2384; 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 halogen-containing combustion products are absorbed in dilute

1.1 These test methods cover the determination of the total sodium carbonate solution.
volatile organic chlorides in concentrations from 10 to 100 3.1.2 Oxy-Hydrogen Combustion—The sample is burned in
ppm in butane-butene mixtures. The amperometric finish is not an oxy-hydrogen atomizer burner, and the combustion products
directly applicable in the presence of other substances that are absorbed in a dilute solution of sodium carbonate.
combine with silver ion or oxidize chloride ion in dilute acid 3.2 Finishes—Either the amperometric titration or spectro-
solution. Bromides, sulfides, ammonia, tobacco smoke, and photometric finish may be used for the chloride ion determi-
more than 25 µg of hydrogen peroxide in the test solution nation.
interfere in the spectrophotometric procedure. 3.2.1 Amperometric Titration—The chloride ion in aqueous
1.2 Dissolved sodium chloride is not quantitatively deter- solution is titrated amperometrically with standard silver ni-
mined using these test methods. trate solution, using a saturated calomel electrode as reference
1.3 The values stated in SI units are to be regarded as the electrode. The diffusion currents are plotted against the corre-
standard. sponding volumes of silver nitrate solution used; the end point
1.4 This standard does not purport to address all of the is taken as the intersection of the two straight-line portions of
safety concerns, if any, associated with its use. It is the the curve.
responsibility of the user of this standard to establish appro- 3.2.2 Spectrophotometric Finish—Chloride ion in the ab-
priate safety and health practices and determine the applica- sorber solution is determined by reaction with mercuric thio-
bility of regulatory limitations prior to use. Specific warning cyanate to release thiocyanate, which forms a reddish orange
statements are given in Sections 5, 8, 11, 14, 19, and Annex A1. complex with Fe +++. The intensity of the color is measured at
460 nm with a spectrophotometer or filter photometer.
2. Referenced Documents
4. Significance and Use
2.1 ASTM Standards: 2
D 329 Specification for Acetone 4.1 These test methods are used to determine trace amounts
D 1266 Test Method for Sulfur in Petroleum Products of volatile chlorides in butane-butene mixtures. Such informa-
(Lamp Method) tion is valuable in cases where chloride is deleterious in the use
of this product; also, chloride contributes to corrosion prob-
3. Summary of Test Methods lems in processing units in instances where further processing
3.1 Combination Test Methods—Either the lamp or oxy- of this material is involved.
hydrogen test method may be used for combustion.
5. Purity of Reagents
NOTE 1—Lamp combustion is readily applicable to multiple testing. 5.1 Purity of Reagents—Reagent grade chemicals shall be
Although an oxy-hydrogen burner does not lend itself to multiple testing,
it affords much more rapid analysis for a single sample than does the lamp
used in all tests. Unless otherwise indicated, it is intended that
combustion. all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
3.1.1 Lamp Combustion—The sample is burned in an atmo- where such specifications are available.3 Other grades may be
sphere of carbon dioxide and oxygen or in purified air; the 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.
1
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
tee D02.D0 on Hydrocarbons for Chemical and Special Uses.
3
Current edition approved Nov. 1, 2004. Published November 2004. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1965. Last previous edition approved in 2000 as D 2384 – 83 (2000)e1. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 D 2384 – 83 (2004)
5.2 References to water shall be understood to mean 8.3 Sodium Carbonate Absorbent (2 g/L)— Dissolve 2.0 g
chloride-free distilled or deionized water. of anhydrous sodium carbonate (Na2CO3) in water and dilute
5.3 (Warning—In view of the common occurrence of to a litre with water.
chloride in reagents and laboratory air, special care must be
taken during preparation and storage of reagents to avoid 9. Procedure
contamination. They should be isolated from other reagents 9.1 Prepare the combustion apparatus as described in Sec-
and used solely for these methods. A blank determination must tion 7 of Test Method D 1266, Preparation of Apparatus, using
be performed each time a reagent is changed to ensure that it 35 mL of Na2CO3 solution to charge the absorber.
is not contaminated with chloride. 9.2 Weigh the vessel containing the sample to the nearest
It is also imperative that all glassware used in this determi- 0.1 g. Support the sample vessel in an upright position so that
nation be cleaned thoroughly and rinsed four times with the sample is burned from the gaseous phase. Connect the
chloride-free distilled or deionized water. Utmost caution must sample vessel to the auxiliary corrosion-resistant regulating
be taken during the analysis to prevent contamination from valve by means of corrosion-resistant metal tubing (Fig. 1)
chlorides.) (Note 2). Connect the bottom valve of the sample vessel to the
regulated hydrogen supply. By means of short lengths of
6. Sampling chloride-free rubber tubing, connect the auxiliary valve outlet
6.1 Steam and dry a 10 to 25-mL corrosion-resistant metal to the side inlet of the gas burner and the lower inlet of the gas
sample cylinder having a 450-psi (3100 kPa) working pressure burner (Test Method D 1266, Annex A3, Apparatus Detail, Fig.
and equipped with a needle valve outlet at each end. 5) to the burner manifold.
6.2 Pressure the prepared cylinder with dry hydrogen to 20 NOTE 2—For steady burning, it may be necessary to surround the
psig (137.5 kPa gage) to afford a gas cushion preventing auxiliary valve with a heat-exchanger system. A convenient means is
rupture due to liquid expansion on increase of temperature. winding insulated heating wire, having a resistance of 40 to 60 V, around
6.3 Obtain a liquid sample from the purged sample line, the auxiliary valve and connecting it to a suitable rheostat. Another means
filling the upright cylinder through the bottom needle valve, is to place the regulating valve in a suitable metal beaker and cover the
valve body with water maintained at 60 to 80°C.
keeping the top valve closed. Do not purge the sample cylinder.
9.3 Open the valve on the sample vessel; then open the
LAMP COMBUSTION TEST METHOD auxiliary valve to allow a small stream of vapor to escape.
Quickly light the burner. Adjust the flow of CO2-O2 mixture
7. Apparatus and the sample so that the flame is approximately 35 mm high
7.1 ASTM Lamp Assembly—Use the apparatus specified in and clear blue in color; this color is reached just beyond the
Test Method D 1266, including the liquefied petroleum gas point at which a yellow color shows at the tip of the flame.
burner assembly. Insert the burner into the chimney and readjust the flame if
necessary. When the sample has burned almost to completion,
8. Reagents open the valve on the bottom of the sample vessel and flush the
8.1 Use the necessary reagents and materials specified in residual sample from the cylinder chamber by passing hydro-
Test Method D 1266, in addition to the absorber solution as gen through the bottom valve for several minutes.
described in 8.3. 9.4 When all of the residual material has been flushed from
8.2 Hydrogen (Warning—Extremely flammable (liquefied) the sample vessel, turn off the hydrogen and close the valves on
gas under pressure. See Annex A1.1.) the sample vessel. Disconnect the hydrogen flushing line and

FIG. 1 Diagrammatic Sketch of Butane-Butene Heat Exchange System

2
 D 2384 – 83 (2004)
the line to the heated auxiliary valve and weigh the sample 11. Reagents and Materials
vessel to the nearest 0.1 g. Draw the combustion atmosphere 11.1 Hydrogen (Warning—Extremely flammable (lique-
through one absorber of a set to serve as a blank on the purity fied) gas under pressure. See Annex A1.1.)
of this atmosphere. Rinse the chimneys and spray traps with 11.2 Oxygen (Warning—Oxygen vigorously accelerates
water and add the rinsings to the absorbers. combustion. See Annex A1.2.)
9.5 Proceed in accordance with either Section 16 or 21. 11.3 Sodium Carbonate, Absorbent (2g/L)—See 8.3.
OXY-HYDROGEN COMBUSTION TEST METHOD— 12. Procedure
ALTERNATIVE TEST METHOD
12.1 Follow the manufacturer’s instructions for preparing
10. Apparatus and operating the apparatus. Place 50 mL of the Na2CO3
absorbent in the absorber. Burn all of the sample from the gas
10.1 Oxy-Hydrogen Burner4—A flow diagram of a typical
phase of the cylinder (Fig. 1) (Warning—Extremely flam-
apparatus is shown in Fig. 2. The apparatus shall consist of
mable (liquefied) gas under pressure. See Annex A1.1.). Flush
the residual gases from the cylinder chamber by passing
hydrogen through the bottom valve for several minutes, burn-
ing the flushed gases.)
12.2 When combustion is completed, rinse all water-cooled
portions of the apparatus and the spray trap with a spray of
water. Collect all rinsings in the absorbent.
12.3 Proceed in accordance with either Section 16 or 21.
12.4 Prepare a blank by placing 50 mL of the Na2CO3
absorbent in the absorber. Operate the apparatus for the same
period of time, under the same conditions that were used for
the combustion of the sample, but without a sample and the
sample inlet closed to the atmosphere. Burn approximately the
same volume of hydrogen as was used to flush the same
cylinder. When combustion of the hydrogen is complete, rinse
all water-cooled portions of the apparatus and the spray trap
with a spray of water. Collect all rinsings in the absorbent.
Proceed as in 12.3.

AMPEROMETRIC TITRATION FINISH

13. Apparatus
13.1 Potentiometer-Galvanometer Assembly, capable of ap-
plying a cell potential up to 3 V with an accuracy of 1 % of full
1—Atomizer-burner 4—Three-way stopcock
2—Sample tube 5—Absorber
scale, and capable of indicating the cell current by means of a
3—Combustion chamber 6—Spray trap galvanometer having a sensitivity of 0.005 to 0.008 µA/mm
FIG. 2 Flow Diagram of a Typical Oxy-Hydrogen Combustion scale division. A multiposition galvanometer shunt for adjust-
Apparatus ment of current measurement sensitivity should also be pro-
vided; shunt ratios to give sensitivities of approximately 0.05
to 0.08, and 0.10 to 0.16 µA/mm should be included.
three parts: atomizer-burner, combustion chamber, and receiver 13.2 Titration Assembly—An apparatus similar to that
with spray trap. A blowout safety port in the combustion shown in Fig. 3, consisting of a rotating (600 rpm) platinum
chamber is desirable. The remainder of the apparatus shall electrode, a saturated calomel reference electrode with salt
consist of a steel support stand with the necessary needle bridge, a means of blanketing the solution with nitrogen, and a
valves and flow meters for precise control of air, oxygen, holder for a 10-mL buret.
hydrogen, and vacuum. 13.3 Calomel Electrode, constructed as shown in Fig. 3.
10.2 Vacuum Pump, having a capacity of at least 1200 L/h, 13.4 Platinum Electrode, rotating-hook type. A suitable
and protected from corrosive fumes by suitable traps. electrode may be constructed as follows: Seal a platinum wire
0.03 to 0.05 in. (0.76 to 1.3 mm) in diameter and 0.75 to 1.0 in.
(19.1 to 25.4 mm) long into the end of a 6-mm outside diameter
4
The Wickbold Burner Apparatus obtainable from the Atlas Instrument Co., soft glass tube that has been shaped into a stirrer blade. Bend
8902 E. 11th St., Tulsa, OK, or the Richfield Burner Apparatus obtainable from the the extending platinum wire upwards at its midpoint to form an
Greiner Glass Blowing Laboratories, 3604 E. Medford St., Los Angeles, CA 90034, angle of 90°. Place a few drops of mercury in the glass tube and
has been found suitable for this purpose. If you are aware of alternative suppliers,
make electrical contact between the mercury and the connec-
please provide this information to ASTM International Headquarters. Your com-
ments will receive careful consideration at a meeting of the responsible technical tion on the amperometric titrator with a piece of copper wire
committee 1, which you may attend. (insulate the exposed wire to prevent shorting).

3
 D 2384 – 83 (2004)

FIG. 3 Schematic Assembly of the Amperometric Titration Cell

13.5 Buret—A 10-mL semi-micro buret, with the tip con- 30 %) with 4 volumes of water. Store in a dark-colored
structed so as to be able to dip below the surface of the solution glass-stoppered bottle.
being titrated. 14.7 Mercury-Calomel Mixture—Prepare a mixture of mer-
cury and calomel (mercurous chloride, Hg2Cl 2) by vigorously
14. Reagents
shaking 10 g of calomel with 50 g of mercury, in a glass-
14.1 Acetone (99.5 %) (Warning—Extremely flammable. stoppered flask, until the calomel becomes uniformly gray in
Vapor may cause fire. See Annex A1.3.)—Refined acetone color. (Warning—Poison: May be harmful or fatal if inhaled
conforming to Specifications D 329. or swallowed. Vapor harmful, emits toxic fumes when heated.
14.2 Agar Solution—Dissolve 2 g of agar-agar powder in Vapor pressure normal room temperature exceeds threshold
100 mL of hot water (80 to 100°C) containing 20 g of limit value for occupational exposure. See Annex A1.4.)
potassium nitrate (KNO3). 14.8 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
14.3 Bromthymol Blue Indicator Solution— Dissolve 0.10 g (HNO3). Bubble nitrogen through the acid until it is colorless,
of the solid indicator in 100 mL of hot water, cool, and add 1 in order to remove oxides of nitrogen.
mL of chloroform as a preservative. Discard the solution when
it is 1 week old. 14.9 Nitric Acid Solution (1 + 28)—Mix 1 volume of con-
centrated nitric acid (HNO3, sp gr 1.42) with 28 volumes of
NOTE 3—Remove possible objectionable amounts of chloride by pass- water.
ing the solution through an ion-exchange resin in the hydroxyl form.
Neutralize the resulting alkaline solution to the bromthymol blue end point 14.10 Nitrogen, oxygen-free tank nitrogen. (Warning—
by titration with HNO 3 (3 + 97). Compressed gas under high pressure. Gas reduces oxygen
available for breathing. See Annex A1.5.)
14.4 Chloride, Standard Solution (10 µg Cl−/mL)—Dilute a
suitable volume of 1 + 10 assayed hydrochloric acid to obtain 14.11 Potassium Nitrate Solution (100 g/L)—Dissolve 100
a solution containing 10 µg Cl−/mL. g of potassium nitrate (KNO3) in water and dilute to 1 L with
14.5 Gelatin Solution (10 g/L)—Dissolve 1 g of gelatin in water.
100 mL of hot water and add 1 mL of chloroform as a 14.12 Potassium Nitrate, Saturated Solution—Prepare a
preservative. Discard the solution when it is 1 week old. saturated solution of KNO3 in water.
14.6 Hydrogen Peroxide Solution—Prepare by diluting 1 14.13 Saturated Calomel Electrolyte— Prepare a solution,
volume of concentrated hydrogen peroxide solution (H2O2, saturated with calomel and potassium chloride (KCl), in water.

4
 D 2384 – 83 (2004)
14.14 Silver Nitrate Solution, Standard (0.1 N)—Prepare 16.2 Add the amount of acetone, HNO3, and gelatin solu-
and standardize a 0.1 N solution of silver nitrate (AgNO3) tion shown in Table 1.
against primary standard sodium chloride crystals. 16.3 Place the beaker in position at the rotating platinum
14.15 Silver Nitrate Solution, Standard (0.01 N)—Dilute electrode assembly and adjust the sensitivity shunt in accor-
100 mL of 0.1 N AgNO3 to 1 L with water. dance with the values given in Table 1. Turn the stirring motor
14.16 Silver Nitrate Solution, Standard (0.001 N)—Dilute on. Adjust the potential divider so that −0.23 6 0.02 V is
10.0 mL of 0.1 N AgNO3 to 1 L with water. applied to the platinum electrode. Maintain this potential
14.17 Sodium Carbonate Solution (2 g/L)—Dissolve 2 g of throughout the titration. Allow the galvanometer to stabilize at
granular anhydrous sodium carbonate (Na2CO3) in water and 1 µA/mm or less; the time needed to achieve this can be
dilute to 1 L with water. markedly reduced by purging the solution with nitrogen.
Record the galvanometer reading.
15. Preparation of Apparatus 16.4 Add AgNO3 solution (Table 1) until the galvanometer
15.1 Platinum Electrode—Clean the electrode by immers- shows a deflection of 30 to 40 scale divisions. When the
ing it in concentrated HNO3 (sp gr 1.42) and washing with galvanometer becomes steady, record the buret and galvanom-
water. Install the electrode on the amperometric titrator so that eter readings. Continue adding AgNO3 solution in suitable
the end of the heavy copper wire dips into the mercury column increments (Table 1); after each addition allow the galvanom-
of the platinum electrode. eter to stabilize and record the buret and galvanometer read-
15.2 Saturated Calomel Reference Electrode—Add suffi- ings. Stop the flow of nitrogen while taking galvanometer
cient mercury to the electrode flask to cover the platinum wire readings. Continue the titration until three or four additional
and to form a mercury seal between the flask and the side arm. points have been obtained to establish a slope.
Cover the mercury with a 5-mm layer of the mercury-calomel
mixture and then fill the cell to within 20 mm of the glass joint 17. Calculations
with the saturated calomel electrolyte solution. Make electrical 17.1 Plot the galvanometer readings against the correspond-
contact between the mercury and the connection on the ing volumes of AgNO3 solution added and draw the best
amperometric titrator with a piece of copper wire (insulate the straight line through these points. Draw a second straight line
exposed wire to prevent shorting). parallel to the milliliter axis and passing through the galva-
15.3 Salt Bridge—Connect the inner glass tube of the salt nometer reading obtained with no added AgNO3 solution. The
bridge to the inlet tube of the reference electrode by means of volume of AgNO3 solution corresponding to the intersection of
a 1-ft (305-mm) section of 6-mm inside diameter polyethylene these lines represents the volume of reagent used by the
tubing; clamp the two glass tubes in a vertical position. Fill the sample.
entire bridge with warm agar solution, taking care that no
bubbles remain in the column of liquid. Close the open ends of NOTE 5—A typical amperometric titration curve (see Fig. 4) consists of
two linear branches and an intermediate curving region. The first linear
the glass tubes with small pieces of loosely rolled filter paper
portion corresponds to the reaction of the substance being titrated with the
and allow to stand until the solution is gelled. Insert the titrating solution and, since excess titrant is never present, the diffusion
reference electrode inlet of the bridge into the electrode flask, current remains constant; a single point suffices to establish this branch.
and the other end through the front panel of the amperometric The second linear branch corresponds to an appreciable excess of titrant.
titrator and into the sleeve tube; fill the sleeve tube with a The intermediate curved portion is due to solubility or mass action effects
saturated solution of KNO3. and is of no value for analytical purposes. The stoichiometric end point
corresponds to the intersection of the extrapolated straight-line branches
NOTE 4—When the amperometric titration apparatus is not in use, of the curve.
immerse the end of the salt bridge and the platinum electrode in the beaker
containing saturated KNO3 solution. 17.2 Calculate the amount of chloride in the sample, in parts
per million by weight, as follows:
16. Procedure Chloride, ppm by weight 5 [~A 2 B! 3 N 3 35 455]/W (1)
16.1 Transfer the absorber solution from either the lamp or
oxy-hydrogen combustion to a 200-mL tall-form titration where:
beaker and reduce its volume to 10 mL if the expected chloride A = millilitres of AgNO3 solution required for titration
content is less than 15 ppm and to about 25 mL if above 15 of the sample,
ppm (see Table 1). B = millilitres of AgNO3 solution required for titration
of the blank,
N = normality of the AgNO3 solution,
TABLE 1 Titration Conditions W = grams of sample used, and
Expected Chloride Content 35 455 = milligram equivalent weight of chlorine 3 10 6
Materials and Operations
Below 15 ppm Above 15 ppm (ppm).
Volume before addition of acetone, mL 10 25
Acetone, mL 20 25 SPECTROPHOTOMETRIC FINISH
Concentrated HNO3, mL 1 2
Gelatin solution (10 g/L), mL 0.3 0.5
Galvanometer sensitivity, µA/mm 0.05 to 0.08 0.10 to 0.16 18. Apparatus
Normality of AgNO3 solution 0.001 0.01
Titrant addition increments, mL 0.25 0.05 to 0.10 18.1 Spectrophotometer—Any spectrophotometer (or filter
photometer) equipped with cells of 5-cm light path and capable

5
 D 2384 – 83 (2004)

FIG. 4 Amperometric Titration Curve

of measuring absorbance at 460 6 10 nm with an accuracy of the corresponding micrograms of chloride present. Make a
0.010 absorbance units. separate calibration for each new batch of composite reagent.
Make the calibration at approximately the same ambient
19. Reagents temperature expected during the analysis.
19.1 Chloride Solution, Standard (10 µg Cl−/mL)—Prepare
as described in 14.4. 21. Procedure
19.2 Composite Reagent—Prepare as needed by thoroughly
21.1 Quantitatively transfer the absorber solution from ei-
mixing 2 volumes of ferric perchlorate (Fe(ClO4) 3·6H2O)
ther the lamp or oxy-hydrogen combustion absorber into a
solution with 1 volume of mercuric thiocyanate (Hg(SCN)2)
200-mL tall form beaker and carefully reduce the volume of
solution. Because the reagent is stable for only about 8 h, a
the solution to 10 mL by evaporation on a hot plate. Cool the
fresh supply must be prepared at least every 8 h.
solution to room temperature. Quantitatively transfer the re-
19.3 Ferric Perchlorate Solution—Dissolve 14.0 g of pure
duced volume of absorber solution into a 25-mL volumetric
iron wire in nitric acid (HNO3, 1 + 2). Add 120 mL of
flask and make up to volume with water.
concentrated perchloric acid (HClO4) and heat to fumes of
HClO4. Continue fuming for 30 min. Cool, add 100 mL of hot 21.2 Pipet a 20-mL (or smaller) aliquot of the absorber
water, and boil for 5 to 10 min, to remove chlorine. Cool and solution into a 25-mL volumetric flask. Add 0.6 mL of HClO4,
dilute to 1 L with water. (Warning—Fuming of HClO4 3.00 mL of the composite reagent, and dilute to volume with
solution must be conducted in hoods constructed for this water. Mix well, transfer to a 5-cm spectrophotometer cell and
purpose only.) measure the absorbance as in Section 20. Obtain the quantity of
19.4 Mercuric Thiocyanate Solution— Prepare a saturated chloride in the aliquot from the calibration curve.
solution of mercuric thiocyanate (Hg(SCN)2) in methyl alco-
hol. Filter to remove the excess Hg(SCN)2. 22. Calculation
19.5 Perchloric Acid (70 %)—Concentrated perchloric acid 22.1 Calculate the chloride content of the sample, in parts
(HClO4). per million by weight, as follows:
20. Preparation of Calibration Curve Chloride, ppm by weight 5 ~C 2 B!/FW (2)

20.1 Pipet 0.0, 1.0, 2.0, 3.0, 4.0, and 5.0-mL portions of the where:
chloride solution (10 µg Cl−/mL) into separate 25-mL volu- C = micrograms of chloride found in aliquot of absorbent
metric flasks. Add 0.6 mL of HClO4, 3.00 mL of the composite analyzed,
reagent, and dilute to volume with water. Mix well, transfer to B = micrograms of chloride found in the blank (same
a 5-cm spectrophotometer cell, and measure the absorbance of aliquot as sample),
the yellow-orange color against water at a wave-length of 460 F = aliquot fraction of absorbent analyzed, and
nm. The color is stable for approximately 1 h, with gradually W = grams of sample used.
increasing absorbance thereafter. Plot the absorbance against

6
 D 2384 – 83 (2004)
23. Precision and Bias operators working in different laboratories on identical test
23.1 Precision—The precision of the method as determined material would, in the long run, in the normal and correct
by statistical examination of interlaboratory results is as operation of the test method, exceed the following values only
follows: in one case in twenty:
23.1.1 Repeatability (Note 6)—The difference between two Volatile Chloride
test results, obtained by the same operator with the same Range, ppm Reproducibility
15 to 70 13
apparatus under constant operating conditions on identical test
material, would in the long run, in the normal and correct 23.2 Bias—The bias of the procedure in this test method has
operation of the test method, exceed the following values only not been determined but is under consideration by the respon-
in one case in twenty: sible committee.
Volatile Chloride
Range, ppm Repeatability NOTE 7—The reproducibility statement is based on results from five
15 to 70 11 laboratories.
NOTE 6—The repeatability statement is based on results obtained in
eight laboratories. 24. Keywords
23.1.2 Reproducibility (Note 7)—The difference between 24.1 butane; butene; chlorides
two single and independent results obtained by different

ANNEX

(Mandatory Information)

A1. WARNING STATEMENTS

A1.1 Hydrogen All equipment and containers used must be suitable and
Warning—Extremely flammable (liquefied) gas under pres- recommended for oxygen service.
sure. Never attempt to transfer oxygen from cylinder in which it is
Keep away from heat, sparks and open flame. received to any other cylinder. Do not mix gases in cylinders.
Use with adequate ventilation. Do not drop cylinder. Make sure cylinder is secured at all
Never drop cylinder. Make sure cylinder is supported at all times.
times. Keep cylinder out of sun and away from heat. Keep cylinder valve closed when not in use.
Stand away from outlet when opening cylinder valve.
Always use a pressure regulator. Release regulator tension
For technical purposes only. Do not use for inhalation
before opening cylinder.
purposes.
Do not transfer cylinder contents to another cylinder. Do not
Keep cylinder out of sun and away from heat.
mix gases in cylinder.
Keep cylinder from corrosive environment.
Keep cylinder valve closed when not in use.
Do not use cylinder without label.
Do not inhale. Do not use dented or damaged cylinders.
Do not enter storage areas unless adequately ventilated. See Compressed Gas Association booklets G-4 and G-4.15
Stand away from cylinder outlet when opening cylinder for details of safe practice in the use of oxygen.
valve.
Keep cylinder from corrosive environment. A1.3 Acetone
Warning—Extremely flammable. Vapors may cause flash
A1.2 Oxygen fire.
Warning—Oxygen vigorously accelerates combustion and Keep away from heat, sparks, and open flame.
can result in an explosion on contact with organic material. Keep container closed.
Keep oil and grease away. Do not use oil or grease on Use with adequate ventilation.
regulators, gauges or control equipment. Vapors may spread long distances and ignite explosively.
Use only with equipment conditioned for oxygen service by Avoid buildup of vapors and eliminate all sources of
carefully cleaning to remove oil, grease and other combus- ignition, especially non-explosion proof electrical apparatus
tibles. and heaters.
Keep combustibles away from oxygen and eliminate ignition Avoid prolonged breathing of vapor or spray mist.
sources. Avoid contact with eyes and skin.
Keep surfaces clean to prevent ignition or explosion, or both,
on contact with oxygen.
Always use a pressure regulator. Release regulator tension 5
Available from Compressed Gas Assoc., 1725 Jefferson Davis Hwy., Arlington,
before opening cylinder valve. VA 22202-4102.

7
 D 2384 – 83 (2004)
A1.4 Mercury Keep container closed.
Warning—Poison. May be harmful or fatal if inhaled or Use with adequate ventilation.
swallowed. Do not enter storage areas unless adequately ventilated.
Vapor harmful, emits toxic fumes when heated. Always use a pressure regulator. Release regulator tension
Vapor pressure at normal room temperature exceeds thresh- before opening cylinder.
old limit value for occupational exposure.
Do not breathe vapor. Do not transfer to cylinder other than one in which gas is
Keep container closed. received. Do not mix gases in cylinders.
Use with adequate ventilation. Do not drop cylinder. Make sure cylinder is supported at all
Do not take internally. times.
Cover exposed surfaces with water, if possible, to minimize Stand away from cylinder outlet when opening cylinder
evaporation. valve.
Do not heat. Keep cylinder out of sun and away from heat.
Keep recovered mercury in tightly sealed container prior to
sale or purification. Do not throw in sink or rubbish. Keep cylinder from corrosive environment.
Do not use cylinder without label.
A1.5 Nitrogen Do not use dented or damaged cylinder.
Warning—Compressed gas under high pressure. Gas re- For technical use only. Do not use for inhalation purposes.
duces oxygen available for breathing.

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of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
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