Residues in Liquefied Petroleum (LP) Gases: Standard Test Method For

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This test method describes how to determine extraneous materials present in liquefied petroleum gases.

This test method covers determining extraneous materials that weather above 38°C in liquefied petroleum gases. It may not detect all contaminants and certain additives can interfere with results.

A 100 mL LPG sample is weathered at 38°C and the residue volume is measured. Solvent is added to dissolve residue and measured volumes are used to create an oil stain on paper.

Designation: D2158 − 11

Designation: 317/95

Standard Test Method for


Residues in Liquefied Petroleum (LP) Gases1
This standard is issued under the fixed designation D2158; 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.

1. Scope* 2. Referenced Documents


1.1 This test method covers the determination of extraneous 2.1 ASTM Standards:2
materials weathering above 38°C that are present in liquefied D96 Test Method for Water and Sediment in Crude Oil by
petroleum gases. The extraneous materials will generally be Centrifuge Method (Field Procedure) (Withdrawn 2000)3
dissolved in the LPG, but may have phase-separated in some D1796 Test Method for Water and Sediment in Fuel Oils by
instances. the Centrifuge Method (Laboratory Procedure)
1.2 Liquefied petroleum gases that contain certain anti-icing D1835 Specification for Liquefied Petroleum (LP) Gases
additives can give erroneous results by this test method. E1 Specification for ASTM Liquid-in-Glass Thermometers
2.2 Energy Institute Document:
1.3 Although this test method has been used to verify IP Test Methods - Appendix A. Specifications - IP standard
cleanliness and lack of heavy contaminants in propane for thermometers4
many years, it might not be sensitive enough to protect some
equipment from operational problems or increased mainte- 3. Terminology
nance. A more sensitive test, able to detect lower levels of
3.1 Definitions of Terms Specific to This Standard:
dissolved contaminants, could be required for some applica-
3.1.1 oil stain observation, n—the volume of solvent-
tions.
residue mixture required to yield an oil stain or ring that
1.4 WARNING—Mercury has been designated by many persists for 2 minutes under specified conditions on absorbent
regulatory agencies as a hazardous material that can cause paper.
central nervous system, kidney and liver damage. Mercury, or 3.1.2 residue, n—the volume, measured to the nearest 0.05
its vapor, may be hazardous to health and corrosive to mL, of the residual material boiling above 38°C resulting from
materials. Caution should be taken when handling mercury and the evaporation of 100 mL of sample under the specified
mercury containing products. See the applicable product Ma- conditions of this test method.
terial Safety Data Sheet (MSDS) for details and EPA’s
website—http://www.epa.gov/mercury/faq.htm—for addi- 3.1.3 solvent-residue mixture, n—a mixture (solution) of 10
tional information. Users should be aware that selling mercury mL of solvent with any residue remaining in the centrifuge
and/or mercury containing products into your state or country tube at the conclusion of the first step in this test method.
may be prohibited by law. 4. Summary of Test Method
1.5 The values stated in SI units are to be regarded as 4.1 A 100-mL sample of liquefied petroleum gas is weath-
standard. No other units of measurement are included in this ered in a 100-mL centrifuge tube. The volume of residue
standard. remaining after heating the tube to 38°C is measured and
1.6 This standard does not purport to address all of the recorded.
safety concerns, if any, associated with its use. It is the
4.2 To dissolve any residue, 10 mL of solvent is added to the
responsibility of the user of this standard to establish appro-
centrifuge tube. Small, measured volumes of solvent-residue
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
1
This test method is under the jurisdiction of ASTM Committee D02 on Standards volume information, refer to the standard’s Document Summary page on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee the ASTM website.
3
D02.H0 on Liquefied Petroleum Gas. The last approved version of this historical standard is referenced on
Current edition approved Jan. 1, 2011. Published February 2011. Originally www.astm.org.
4
approved in 1963. Last previous edition approved in 2005 as D2158–05. DOI: Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
10.1520/D2158-11. U.K. www.energyinstpubs.org.uk

*A Summary of Changes section appears at the end of this standard


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D2158 − 11
mixture are deposited on an absorbent paper in a specified 6. Interferences
manner. The appearance of the absorbent paper to which the
6.1 Solid contaminants such as rust, scale or dirt can
residue solution has been added in measured increments is
interfere with this test method, which is not intended for
observed and recorded.
representative measurement of solid, undissolved contami-
5. Significance and Use nants.
5.1 Control over the residue content (required by Specifica-
7. Apparatus
tion D1835) is of considerable importance in end-use applica-
tions of LPG. In liquid feed systems residues can lead to 7.1 Centrifuge Tube, 100-mL graduated, conforming to
troublesome deposits and, in vapor withdrawal systems, resi- dimensions given in Fig. 1. The first 0.5 mL shall be graduated
dues that are carried over can foul regulating equipment. Those in 0.05-mL increments. The shape of the lower tip of the tube
that remain will accumulate, can be corrosive, and will is especially important. The taper shall be uniform and the
contaminate following product. Water, particularly if alkaline, bottom shall be rounded as shown in Fig. 1. Tubes shall be
can cause failure of regulating equipment and corrosion of made of thoroughly annealed heat-resistant glass. Volumetric
metals. graduation tolerances, based on air-free water at 20°C, are

FIG. 1 Cone-Shaped Centrifuge Tube, 203 mm

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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

NOTE 1—When a thermometer or a water bath, or both, are not


available, for example when conducting a field test, a satisfactory
alternative for screening purposes is to warm the tip of the centrifuge tube
with the hand.
7.4.1 For routine testing, a general purpose thermometer
with 0.5°C subdivisions and a maximum scale error of 0.5°C
NOTE 1—Coils in the drawing are extended for clarity.
may be used. FIG. 2 Precooling Equipment
7.5 Absorbent Paper, white, at least 100-mm diameter.
Medium grade or rapid filter paper has been found to be
satisfactory. In this test method, the paper will be referred to as
8.1.1 Although pentane is the preferred solvent for use in
“filter paper.”
this test method, cyclopentane may be substituted for pentane
7.6 Solvent Wash Bottle, typically polyethylene. whenever the ambient temperature or altitude is too high to
7.7 Water Bath, controlled at 38 6 2°C. enable the convenient handling of pentane.
8.1.2 Storage of solvent in a polyethylene wash bottle for
7.8 Copper Wire, 1 to 2-mm diameter, at least 10 mm longer
several days contaminates the solvent. Therefore, do not use
than the centrifuge tube’s height.
any solvent that has remained in a polyethylene wash bottle for
7.9 Clamp, suitable for holding the centrifuge tube during more than one day.
weathering.
9. Hazards
8. Reagents and Materials
9.1 Note that there is a significant fire hazard from LPG
8.1 Solvent—HPLC-grade pentane or cyclopentane. An- vapors, and since the boiling point of LPG can be as low as
other grade of solvent may be used provided that it meets the −41°C, there is a risk of freezing “burns.” Take appropriate
requirements of 10.2. safety precautions to prevent ignition or fire, and wear suitable
protective equipment to protect against skin contact with liquid
TABLE 1 Centrifuge Tube Graduation Tolerances or vaporizing LPG.
Range, mL
Scale, Division, Limit of Error, 9.2 Operators should wear a grounded antistatic wrist strap.
mL mL
The use of an antistatic floor mat and grounding the sample
0.0 to 0.1 0.05 0.02
0.1 to 0.3 0.05 0.03
cylinder are also advised.
0.3 to 0.5 0.05 0.05
0.5 to 1.0 0.1 0.05 10. Preparation of Apparatus
1.0 to 3.0 0.1 0.1
3.0 to 5.0 0.5 0.2 10.1 Wash all glassware that is to be used in the test in the
5.0 to 25.0 1.0 0.5 selected solvent.
25.0 to 100.0 1.0 1.0
10.2 Verification of cleanliness of glassware and solvent.

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D2158 − 11
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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D2158 − 11
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)

X1. CALCULATION OF R AND O NUMBERS

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.

X1.1 Terminology X1.3.2 Repeatability—The difference (r) between succes-


X1.1.1 Definitions of Terms Specific to this Standard: sive test results obtained by the same operator with the same
X1.1.1.1 O Number, n, 10 divided by the oil stain observa- apparatus under constant operating conditions on identical test
tion (in millilitres). material would, in the long run, in the normal and correct
X1.1.1.2 R Number, n, the residue volume in millilitres operation of the test method, exceed the values below only in
multiplied by 200. one case in twenty:
O Number r R Number r
X1.2 Calculation and Reporting 0 to 20 4 0 to 20 5
20 to 40 6 20 to 40 10
X1.2.1 O Number—Divide 10 by the oil stain observation 40 to 100 8 40 to 60 20
obtained in 11.2.6, in millilitres, and report the result to the
nearest whole number. If the oil stain observation exceeds 1.5 X1.3.3 Reproducibility—The difference (R) between two
mL, record the result as zero. test results independently obtained by different operators
operating in different laboratories on nominally identical test
X1.2.2 R Number—Multiply the residue volume obtained in material would, in the long run, in the normal and correct
11.1.6, in millilitres, by 200, and express the result to the operation of the test method, exceed the values below only in
nearest 10. one case in twenty:
X1.3 Precision and Bias O Number R R Number R
0 to 20 6 0 to 20 10
X1.3.1 Precision has been determined in terms of the 20 to 40 8 20 to 40 20
normalized reporting units. 40 to 100 12 40 to 60 30

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D2158 − 11
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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