Residues in Liquefied Petroleum (LP) Gases: Standard Test Method For
Residues in Liquefied Petroleum (LP) Gases: Standard Test Method For
Residues in Liquefied Petroleum (LP) Gases: Standard Test Method For
Designation: 317/95
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D2158 − 11
given in Table 1. Detailed requirements for centrifuge tubes
appear in Test Methods D96 and D1796.
7.2 Cooling Coil and Cooling Bath, a minimum length of 6
m of 5 to 7-mm outside diameter copper tubing wound to a
diameter of 63.5 6 1.5-mm outside diameter, and assembled in
a suitable cooling bath. (See Fig. 2 as an example.)
7.2.1 Mechanical refrigeration is permitted provided that
the coolant temperature is below −43°C. If dry ice is used, a
non-glass dewar or vessel is recommended.
7.3 Syringe, 2-mL graduated in 0.1 mL and equipped with a
needle 200 6 5 mm long. The needle may be either a sharp
needle (ordinary medical syringe needle) or a safe, non-sharp
syringe needle to avoid a puncture hazard. Alternatively, an
equivalent liquid dispensing device capable of delivering
0.1-mL increments may be used, such as a 0.1-mL pipette.
7.4 Temperature Measuring Device, that is intrinsically
safe, with accuracy equal to or better than Specification E1 or
IP Test Methods - Appendix A shall be used. Thermometers
conforming to Specification E1 or IP Appendix A have been
found to be satisfactory.
Low Range –38°C to + 50°C IP 1C/ASTM 5C
or IP 2C/ASTM 6C
High Range –20°C to + 50°C ASTM 57C
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10.2.1 Add 10 mL of a new sample of solvent to the and does not give a measurable volume, but can still give a ring
centrifuge tube. or stain in the Oil Stain Observation procedure.
10.2.2 Mark the center of the filter paper with a pencil or 11.2 Oil Stain Observation:
other non-pentane-soluble writing tool. 11.2.1 Add sufficient solvent to the centrifuge tube contain-
10.2.3 Fill the syringe or equivalent liquid dispensing de- ing the residue described in 11.1.6 to restore the volume to 10
vice (see 7.3) with a portion of the solvent drawn from the mL. Add the solvent from the wash bottle and carefully wash
centrifuge tube and direct 0.1-mL portions of the solvent to the down the sides of the tube. Stir well so that any residue at the
mark on the paper. bottom of the tube is dissolved uniformly in the solvent.
10.2.3.1 The solvent is added in 0.1-mL increments to Stirring with the syringe needle (see 7.3) or pipette has been
confine the solvent ring to a circle about 30 to 35 mm in found satisfactory. This mixture will be referred to as the
diameter. The filter paper should be held level during the solvent-residue mixture.
solvent addition. One method is to place it on a 250-mL beaker. 11.2.2 Mark the center of a clean white filter paper.
10.2.4 Allow the solvent to evaporate for 2 min, and note 11.2.3 Fill the syringe or equivalent liquid dispensing de-
the persistence of an oil ring. vice (see 7.3), and direct 1.5 mL of the solvent-residue mixture
10.2.4.1 The presence of an oil ring shall be observed by at the center of the paper at an appropriate rate such that the
holding the dry filter paper between the eye and a bright wetted circle is maintained at about 30 to 35 mm in diameter.
incandescent light or strong daylight. If desired, steps 11.2.3 and 11.2.4 may be omitted, and the test
10.2.4.2 If no oil ring appears after 1.5 mL of solvent has continued according to 11.2.5.
been added, the solvent and glassware are satisfactory. 11.2.4 After directing the entire 1.5 mL of residue solution
10.2.4.3 The appearance of an oil ring indicates either onto the filter paper and at the end of a 2-min waiting period,
improperly cleaned glassware or contaminated solvent. if no oil ring persists when holding the dry filter paper between
the eye and a bright incandescent light or strong daylight,
11. Procedure discontinue the test and go to 12.1.
11.1 Residue Measurement: 11.2.5 If a stain or ring is discernible, determine the volume
11.1.1 If the LPG sample is expected to be clean, with no of the solvent-residue mixture at which the oil stain or ring first
residues or contaminants that could result in an oil stain, the persists for 2 min on a new filter paper by adding the
procedure may be performed without a cooling coil. However, solvent-residue mixture in 0.1-mL increments, waiting 2 min
if a residue or oil stain is detected using this screening after each addition, and inspecting the paper for an oil stain at
procedure (that is, a residue is measured at greater than or the end of the 2-min period.
equal to 0.05 mL in 11.1.7, or an oil stain is generated with 11.2.6 Record the volume in millilitres of the solvent-
1.5 mL of test solution in 11.2.4), the test shall be repeated residue mixture required to yield a persistent oil stain or ring as
using a cooling coil. the oil stain observation.
11.1.2 Attach the cooling coil to the LPG sample source, 11.2.7 Alternatively, if a product specification calls for
cool the coil to below the boiling point of the sample, and flush adding a specified amount of solvent-residue mixture to the
the coil and sampling line. filter paper, add the specified quantity in 0.1 mL increments,
11.1.3 Rinse and cool the centrifuge tube with the material and report the result at the specified total amount.
to be sampled and then fill it to the 100-mL mark with a 11.2.7.1 Specification D1835 specifies that 0.3 mL of
representative sample of LPG. solvent-residue mixture shall be deposited on the filter paper in
11.1.4 Immediately insert the copper wire through a clean, 0.1-mL increments.
slotted cork or a clean, loose-fitting plug of cotton or cleansing 11.2.7.2 If there is no oil stain after the addition of 0.3 mL
tissue in the mouth of the centrifuge tube. The wire helps to and a 2-min waiting period, report the result as “Pass.”
prevent superheating and resulting bumping (erratic or exces- 11.2.7.3 If an oil stain is observed at 0.3 mL after a 2-min
sive boiling), and the cork (or plug) will keep out air or waiting period, report the result as “Fail.”
moisture while the sample is weathering. 11.3 Any solvent transferred to the wash bottle for purposes
11.1.5 If more than 10 mL of the sample is lost because of of running the test shall either be used in testing during the
bumping, obtain a new sample and repeat the test. same day or discarded.
11.1.6 Allow the sample to weather, using artificial heating
if the ambient temperature or type of sample requires it. If, 11.4 It has been noted that at low ambient temperatures
when weathering has ceased and the tube has reached ambient (below about 5°C) materials in the gasoline boiling range will
temperature, a visible residue remains, place the tip of the tube leave an oil stain or ring that persists after 2 min. Oil stain
in a water bath at 38°C for 5 min. determinations should be made in a protected area where the
11.1.7 Record the volume of any remaining residue to the temperature is above 5°C. If it is necessary to determine the oil
nearest 0.05 mL, and the presence of extraneous matter, if stain at temperatures below 5°C, allow 10 min for oil stain
observed. persistence.
11.1.8 Perform the oil stain observation described in 11.2
even if there is no apparent or visible residue in the centrifuge 12. Report
tube. Experience has shown that there can be a thin film of oil 12.1 Report the results as:
on the inner surface of the centrifuge tube that is difficult to see 12.1.1 Residue on evaporation to the nearest 0.05 mL, and
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12.1.2 Oil stain observation to the nearest 0.1 mL. 13.2 Bias—The procedure in this test method for measuring
12.2 Alternatively, if the application of this test method calls residues in LP Gas has no bias, because the residues are defined
for passing or failing the oil stain requirement at a specified only in terms of this test method.
volume of solvent-residue mixture, report the result at the
specified volume as “Pass” or “Fail” (see 11.2.7). 14. Keywords
14.1 contaminants; liquefied petroleum gases; LPG; oil
13. Precision and Bias
stain; residue
13.1 Precision—Precision has not been determined on this
method in terms of residue and oil stain results. Precision had
been determined in terms of R and O numbers, as given in
Appendix X1.
APPENDIX
(Nonmandatory Information)
INTRODUCTION
Historically, D2158 has included indices for R and O which give the residue and oil stain results
in whole numbers rather than the decimal results of this test method. These results have been referred
to as “normalized results.” Since no ASTM standards call for R or O results, the description and
calculation of these values have been moved to an appendix for information.
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SUMMARY OF CHANGES
Subcommittee D02.H0 has identified the location of selected changes to this standard since the last issue
(D2158–05) that may impact the use of this standard.
(1) Revised 7.5 and 7.8. (2) Added new 11.1.1 and renumbered rest of Section 11.
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