S T D - G P A S T D 2140-ENGL 1777
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3 8 2 4 b 7 7 0038475 7 8 2
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GPA Standard 2140-97
Liquefied Petroleum Gas
Specifications and Test Methods
r-
Adopted as Recommended Procedures 1931
Revised 1940-1947-1948-1951-1955-1957-1959-1960-1962-1968
1970-7973-1975-1977-7980- 7984-1986- 7988-1990-1992-1996-1997
Gas ProcessorsAssociatlon
6526 East 60th Street
Tulsa, Oklahoma 74145
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TABLE OF CONTENTS
Disclaimer ........................................................................................
ii
Foreword .........................................................................................
ii
GPA Specificationsfor Liquefied Petroleum Gases .......................................................
1
ASTM D-1265-92: Sampling Liquefied Petroleum Gases .................................................
.2
..........................................
.5
ASTM D-1657-89: Density or Relative Density of Light Hydrocarbons
by PressureHydrometer ............................................................
10
ASTM D-1267-95: Vapor Pressure of Liquefied Petroleum Gases
...............................................
14
ASTM D-1838-91: Copper Strip Corrosion by Liquefied
Petroleum Gases ..................................................................
17
ASTM D-2158-92: Residues in Liquefied Petroleum Gases. ..............................................
.20
ASTM D-1837-94: Volatility of Liquefied Petroleum Gases
ASTM D-2163-91: Analysis of Liquefied Petroleum (LP) Gases and
......................................
ASTM D-2713-91: Dryness of Propane (Valve Freeze Method). ...........................................
Propylene Concentrates by Gas Chromatography.
ASTM D-2784-92: Sulfur in Liquefied Petroleum Gases
(Oxyhydrogen Burner or Lamp). ....................................................
GPA 2174-93:
Obtaining Liquid Hydrocarbon Samples Using a Floating
Pistoncylinder ...................................................................
Propane Dryness Test (Cobalt Bromide Method). ......................................................
Note:
.24
.29
.31
37
.50
ASTM test methods included in this publication have been adopted by GPA, and are included through a
right-to-reprint agreement with, and by special permission of, the American Society of Testing and
Materials, 1916 Race Street, Philadelphia, Pa.
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DISCLAIMER
GPA publications necessarily address problems of a general nature and may be used by anyone desiring to do so.
Every effort has been made by GPA to assure accuracy and reliability of the information contained in its publications. With
respect to particular circumstances, local, state, and federal laws and regulations should be reviewed. It is not the intent of
GPA to assume the duties of employers, manufacturers, or suppliers to warn and properly train employees, or others
exposed, concerning health and safety risks or precautions.
GPA makes no representation, warranty, or guarantee in connection with this publication and hereby expressly
disclaims any liability or responsibility for loss or damage resulting ffom its use or for the violation of any federal, state, or
municipal regulation with which this publication may conflict, or for any infringement of letters of patent regarding
apparatus, equipment, or method so covered.
FOREWORD
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These specifications generally define physical properties and characteristics of liquefied petroleum gases (LP-Gas)
which make them suitable for private, commercial, or industrial applications. These specifications do not purport to
specifically define all possible requirements to meet all possible applications. Therefore the user is cautioned to exercise
judgement informulating final specijications for specific applications.
The Gas Processors Association, its management, and supporting companies claim no specific knowledge of how
manufacturers and users will produce, handle, store, transfer or consume the products defined herein and therefore, are not
responsible for any claims, causes of action, liabilities, losses or expenses resulting from injury or death of persons and/or
damage to property arising directly or indirectly from the use of LP-Gas or these specifications relating to LP-Gas.
LP-gases are composed of hydrocarbon compounds, predominately propane and butane, produced during the
processing of natural gas and also in the conventional processing of crude oil. The composition of LP-gases may vary
depending on the source and the ratios of propane and butane content. They exist as gases at atmospheric pressure and
ambient temperatures, but are readily liquefied under moderate pressures for transportation and utilization
There are many uses for LP-gases, the major ones being as (1) petrochemical, synthetic rubber, and motor gasoline
feedstocks, and as (2) commercial, domestic and industrial fuel. The following may be accepted as a general guide for the
common uses for the four fuel types covered by these specifications:
Commercial Propane is the preferred fuel type for domestic, commercial and industrial fuels. It is also a suitable fuel
for low severity internal combustion engines.
Commercial Butane is used principally as feedstock for petrochemicals, synthetic rubber, and as blending stocks or
feedstocks in the manufacture of motor gasolines. Its use as a fuel is generally limited to industrial applications where
vaporization problems are not encountered; however, small quantities are used as domestic fuel.
Commercial Butane-Propane Mixtures cover a broad range of mixtures, which permits the tailoring of fuels or
feedstocks to specific needs.
Propane HD-5 is less variable in composition and combustion characteristics than other products covered by these
specifications. It is also suitable as a fuel for internal combustion engines operating at moderate to high engine severity.
Additional Considerations
Odorization
For certain applications including, but not limited to, use of LP-gas for residential and commercial fuels, users of LPgas should be aware of additional requirements of other standards, principally NFPA 58 "Storage and Handling of Liquefied
Petroleum Gases"(1) and other regulations (2). NFPA 58 has been adopted widely by local, state and other regulatory bodies
in the form of laws, ordinances, or regulations governing the safe storage, transportation, and use of LP-gas as fuels.
Among other requirements, NFPA 58 (Sec. 14.1.1) stipulates that LP-gases "be odorized by the addition of a warning
agent of such character that they are detectable, by a distinct odor, down to a concentration in air of not over one-fifth the
lower limit of flammability". NFPA notes that "ethyl mercaptan in the ratio of 1.0 Ib. per 10,OOO gallon of liquid LP-Gas has
been recognized as an effective odorant. Other odorants and quantities meeting the requirements of 1-4.1.1 may be used.
Research on odorants has shown that thiophane in a ratio of at least 6.4 lbs. per 10,OOO gallon of liquid LP-Gas may satisfy
the requirements of 1-4.1.".
Ammonia
NFPA 58 also states that LP-gas stored or used in systems within the scope of this standard "shall not contain
ammonia". Although ammonia is not a naturally occurring contaminant of LP-gas, certain industry practices, including the
dual use of transportation or storage equipment, may inadvertently result in contamination of LP-gas by ammonia. When
such a possibility exists, users should test for the presence of ammonia in propane and take appropriate means to eliminate
ammonia from the system, since such contamination may cause stress corrosion cracking of copper bearing alloys in the
distribution system.
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S T D - G P A S T D 21'4O-ENGL
1777
= 3824b77
0018478 b7L 9
Fluorides
Sulfur Compounds
Sulfur compounds such as elemental sulfur, hydrogen sulfide, and carbonyl sulfide may be naturally occurring
contaminates of natural gas from which LP-gas is derived. The Copper Snip Corrosion Test (ASTM D-1838) and the Total
Sulfur Test (ASTM D-2784) assure limitation of objectionable sulfur compounds to prevent corrosion of equipment
containing brass fittings and copper tubing. However this test method is not applicable to liquefied petroleum gases
containing corrosion inhibitors or any other agents which diminish the corrosivity of the sample to the copper strip.
Methanol
There is a possibility that a small amount of methanol may be present in LP-Gas. If methanol is present, ASTM D2713. "Standard Test Method for Dryness of Propane-Valve Freeze Method" is not applicable for determining the dryness
of propane type products.
Residual
LP-gas as produced is normally free of residual matter, which includes those heavier hydrocarbons boiling above
100 OF, including any solid foreign materials. If residuals are present as shown by ASTM D-2158, "Standard Test Method
for Residues in LP-Gas", and are in excess of the amount allowed by these specifications,such material may cause improper
operation of regulators, vaporizers, or combustion apparatus.
(1) NFPA 58 "Storage and Handling Liquefied Petroleum Gases''-National
Park, Quincy, MA 02269
(2) Code of Federal Regulations, CFR 49:173.315@)(1)
Fire Protection Association, Battery-March
Other Trace Constituents
Trace constituents other than those mentioned above can also be present in LP-gas as a natural occurrence or from
processing. These may include olefins, mercury, and arsenic. Users of LP-gas with processes that can be harmed by these
constituents are advised to take appropriate precautions to prevent damage to catalysts and/or process equipment from these
trace materials.
...
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Certain refining processes can, during process upset or malfunction, result in contamination of LP-gas by fluoride
compounds. Such contamination can be extremely destructive in the distribution and end user system. In addition, the
combustion products of fluorides can cause physical damage to property and personal health. Similarly, fluorocarbons,such
as certain refrigerants, can contaminate gas through dual use of storage or tankage facilities. Such contamination is rare but,
if the possibility exists, users of LP-gas should take extreme precautions to insure the absence of fluorides.
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STD=GPA STD 2140-ENGL
1777 W 3824b77 O O L B C O O 0 7 T
(& Designation: D 1265 - 92
An Amencan National Standard
Standard Practice for
Sampling Liquefied Petroleum (LP) Gases (Manual Method)‘
This standard is issued under the fixed designation D 1265; the number immediately following the designation indicates the year of
onginal 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
5. General Information
1.1 This practice covers the procedures for obtaining
representative samples of liquefied petroleum gases such as
propane, butane, or mixtures thereof, in containers other
than those used in laboratory testing apparatus. These
procedures are considered adequate for obtaining representative samples for all routine tests for LP gases required by
Specification D 1835 except analysis by Test Method
D 2 163. They are not intended for obtaining samples to be
used for compositional analysis. A sample procedure that
avoids changes in composition must be used for compositional analysis.
NOTE l-Practice D3700 describes a recommended method for
5.1 Considerable effort is required to obtain a representative sample, especially if the material being sampled is a
mixture of liquefied petroleum gases. The following factors
must be considered:
5. I. 1 Obtain samples of the liquid phase only.
5 . I .2 When it is definitely known that the material being
sampled is composed predominantly of only one liquefied
petroleum gas, a liquid sample may be taken from any part
of the vessel.
5.1.3 When the material being sampled has been agitated
until uniformity is assured, a liquid sample may be taken
from any part of the vessel.
5.1.4 Because of wide variation in the construction details
of containers for liquefied petroleum gases, it is difficult to
spec$ a uniform method for obtaining representative samples of heterogeneous mixtures. If it is not practicable to
agitate a mixture for homogeneity, obtain liquid samples by
a procedure which has been agreed upon by the contracting
parties.
5.1.5 Directions for sampling cannot be made explicit
enough to cover ail cases. They must be supplemented by
judgment, skill, and sampling experience. Extreme care and
good judgment are necessary to ensure samples which
represent the general character and average condition of the
material. Because of the hazards involved, liquefied petroleum gases should be sampled by, or under the supervision
of, persons familiar with the necessary safety precautions.
obtaining a representative sample of a hydrocarbon fluid and the
subsequent preparation of that sample for laboratory analysis.
1.2 This standard does not purport to address all of the
safety problems, 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.
2. Referenced Documents
2.1 ASTM Standards:
D 1835 Specification for Liquefied Petroleum (LP) Gases’
D 2 163 Test Method for Analysis of Liquefied Petroleum
(LP) Gases and Propene Concentrates by Gas
Chromatography’
D 3700 Practice for Containing Hydrocarbon Fluid Samples Using a Floating Piston Cylinder3
NOTE2-Samples to be tested for presence of corrosive compounds
or sulfur compounds should be taken in stainless steel containers
equipped with stainless steel valves; otherwise, determinations of
mercaptans and hydrogen sulfide, for example, can be misleading.
3. Summary of Practice
5.1.6 Hydrocarbon vapors vented during sampling must
be controlled to assure compliance with applicable safety and
environmental regulations.
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3.1 A liquid sample is transferred from the source into a
sample container by purging the container and filling it with
liquid, then providing 20 % outage so that 80 % of the liquid
volume remains.
6. Apparatus
6.1 Sample Container-Use metai sample containers of a
type that ensures maximum safety and are resistant to
corrosion by the product being sampled. A suitable material
is stainless steel. The size of the container depends upon the
amount of sample required for the laboratory tests to be
made. The sample container should be fitted with an internal
outage (ullage) tube to permit release of 20 95 of the
container capacity. The end of the container fitted with the
outage (ullage) tube shall be clearly marked. Typical sample
containers are shown in Figs. 1 and 2. If the container is to be
transported, it must often conform to specifications pubfished in Tariff No. 10, “I.C.C.Regulations for Transportation of Explosives and Other Dangerous Articles,” its supplements, or reissues.
4. Significance and Use
4.1 Samples of liquefied petroleum gases are examined by
various test methods to determine physical and chemical
charactenstics. The test results are often used for custody
transfer and pricing determination. It is therefore essential
that the samples be representative of the product to be tested.
I This practice is under the joint jurisdiction of ASTM Committee D 2 on
Petroleum and Petroleum Roducts and is the direct responsibility of Subcommittee DO2.H on Liquefied Petroleum Gas.
Cumnt edition approved March 15, 1992. Published May 1992. Onginally
published as D 1265 - 53 T.Last previous edition D 1265 - 87.
2 Annual Book of A S T M Standards, Vol 05.0I.
3 Annual Book of A S T M Siandards, Vols 05.02.
2
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S T D - G P A S T D 2140-ENGL 1777
382qb77 0018501 T u b
(m D1265
VALVE
OUTAGE
(UIlAGE)TüBE
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INLET
VALVEC
*
SOURCE
SAMPUNO VALVE
Ht
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VALVE B
FIG. 1 Typical Sample Container and Sampling Connections
OUTAGE
VALVE A
(UiiAGE)TUBE
VALVE D
FIG. 2
Typical Sample Container and Alternate Purging Connections
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S T D = G P A STD 2 L V O - E N G L 1997 m 3 8 2 4 b 7 9 OULA502 942 m
D1265
D. Close outlet valve D and release the remainder of the
sample in the liquid phase by opening vent valve B. Repeat
the purging operation at least three times.
6.2 Sample TransJer Line made of stainless steel tubing or
other flexible metal hose, impervious to the product being
sampled, is required. The most satisfactory line is one
equipped with two valves on the sample-container end, Fig.
1, a control valve, A, and a vent valve, B.
9. Transfer of Sample
9.1 Position the sample container securely in an upright
position with outlet valve D at the top (Fig. 1) and both
valves C and D closed.
9.1.1 Close vent valve B, open the control valve A, open
inlet valve C, and fill container with the sample. Close inlet
valve C and the valve at the product source. Open vent valve
B. After the pressure is fully reduced, disconnect sample
container from the transfer line. Discard the sample if a leak
develops or if either valve is opened during subsequent
handling of the sample container before performing the
outage (ullage) operations outlined in section 10.
PROCEDURE
7. Purging Sample Transfer Line
7.1 Connect the ends of the transfer line securely to the
product source and to the inlet valve C of the container.
Close the control valve A, vent valve B, and inlet valve C,
Fig. 1. Open the valve at the product source and purge the
transfer line by opening the control valve A and the vent
valve B.
8. Purging the Sample Container
8.1 If the history of the sample container contents is not
known or if traces of the previous product could affect the
analysis to be camed out, or both, use the following purge
procedure:
8.1.1 Connect valve D of the sample container to the
sample transfer line with the container in an upright position
and valve C at the top (Fig. 2).
8.1.2 Close valves B, C, and D. Open valve A and then
valves C and D. Fill sample container until liquid issues from
valve C. Close valves C and D, then valve A on the sampling
line.
8.1.3 Loosen the connection joining the sample container
to the sample line and turn container through 180" such that
valve D is at the top. Open valves C and D and drain out
liquid.
8.1.4 Return the sample container to position valve C at
the top. Tighten connection to sample transfer line and
repeat the purging operation at least three times.
8.2 If the history of the sample container contents is
known, use the following purge procedure:
8.2.1 With the container in an upright position, Fig. 1,
and its outlet valve D at the top, close vent valve B and inlet
valve C and open control valve A. Open inlet valve C and
partly fill the container with sample by slowly opening the
outlet valve D. Close the control valve A and allow part of
the sample to escape in the vapor phase through outlet valve
10. Sample Outage (Ullage)
10.1 Immediately after obtaining the sample, place the
container in an upright positioin with the outage (ullage)
tube at the top.
10.1.1 Open outlet valve D slightly. Allow excess liquid to
escape and close the valve at the first sign of vapor. If no
liquid escapes, discard the sample and refill the container.
11 Checking for Leaks
1 1.1 After eliminating the excess liquid so that only 80 %
of the sample remains, immerse in a water bath and check
for leaks. If a leak is detected at any time during the sampling
operation, discard the sample. Repair or replace the leaky
container before obtaining another sample.
12. Care of Samples
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12.1 Place samples in a cool location as soon as possible.
Keep them there until all tests have been completed. Discard
any samples in containers which develop leaks. Protect the
valves on the sample container, either by packing the
container in a crate in an approved manner or by using a
protective cap, so that accidental unseating of the valve or
tampering with it is avoided.
13 Keywords
13.1 liquified petroleum gases; LPG; sampling
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the valid@ of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibil@.
This standard is subject to revision ai any time by the responsible technical committee and must be reviewed every five years and
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 Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments bave not received a fair hearing you should make your
views known to the ASTM Committee on Standards. 1916 Race Sî., Philadelphia, PA 19103.
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S T D - G P A S T D 2340-ENGL
3997 W 3824b77 0038503 889 W
Designation: D 1267 - 95
An American N a t i l Standard
Standard Test Method for
Gage Vapor Pressure of Liquefied Petroleum (LP) Gases
(LP-Gas Method)'
This standard is issued under the fixed designation D 1267; 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
1.1 This test method covers the determination of the gage
vapor pressures of liquefied petroleum gas products at
temperatures of 37.8"C (100°F) up to and including a test
temperature of 70'C (1 58°F).
1.2 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. For specific
hazard statements, see Note 2 and Annex A2.
1.3 The values stated in acceptable metric units are to be
regarded as the standard. The values in parentheses are for
information only.
2, Referenced Documents
2.1 ASTM Standards:
D323 Test Method for Vapor Pressure of Petroleum
Products (Reid Method)*
D i265 Practice for Sampling Liquefied Petroleum (LP)
Gases (Manual Method)2
E i Specification for ASTM Thermometers3
2.2 Institute of Petroleum Standard:
IP 181 Sampling Petroleum Gases4
3. Terminology
3.1 Definition:
3.1. I vapor pressure-the pressure exerted by the vapor of
a liquid when in equilibrium with the liquid.
3.2 Description of Term Specific to This Standard:
3.2.1 liquejied petroleum gases-narrow boiling range
hydrocarbon mixtures consisting chiefly of propane or
propylene, or both, (Warning-see Note i ) butanes and
butylenes, or both, in which the content of hydrocarbon
compounds of higher boiling point than 0°C (32°F) is less
than 5 % by liquid volume, and whose gage vapor pressure at
37.8"C (100°F) is not greater than approximately 1550 kPa
(225 psi).
NOTE 1 : Warning-Extremely
4. Summary of 'Test Method
4.1 The test apparatus, consisting of two interconnected
chambers and equipped with a suitable pressure gage, is
purged with a portion of the sample which is then discarded.
The apparatus is then filled completely with the portion of
the sample to be tested. Thirty-three and one-third to forty
volume percent of the sample content of the apparatus is
immediately withdrawn to provide adequate free space for
product expansion. The apparatus is then immersed in a
water bath maintained at the standard test temperature of
37.8'C (100°F) or, optionally, at some higher test temperature up to and including a test temperature of 70°C (158°F).
4.2 The observed gage pressure at equilibrium, after
correcting for gage error and correcting to a standard
barometric pressure, is reported as the LPG Vapor Pressure
at the selected test temperature.
5. Significance and Use
5.1 Information on the vapor pressures of liquefied petroleum gas products under temperature conditions from 37.8
to 70°C (1O0 to 158°F) is pertinent to selection of properly
designed storage vessels, shipping containers, and customer
utilization equipment to ensure safe handling of these
products.
5.2 Determination of the vapor pressure of liquefied
petroleum gas is important for safety reasons to ensure that
the maximum operating design pressures of storage, handling, and fuel systems will not be exceeded under normal
operating temperature conditions.
5.3 For liquefied petroleum gases, vapor pressure is an
indirect measure of the most extreme low temperature
conditions under which initial vaporization can be expected
to occur. It can be considered a semi-quantitative measure of
the amount of the most volatile material present in the
product.
6. Apparatus
6.1 Vapor Pressure Apparatus, constructed as illustrated
in Fig. A1.1, and the various items of auxiliary equipment,
are completely described in Annex A 1.
6.2 The air chamber of Test Method D 323, may be
interchangeable with the upper chamber of this method.
Similarly, the liquid chamber (two-opening type) of Test
Method D 323 is interchangeable with the Bt 20 % lower
chamber Annex A1.1.4 of this method. Because of this
interchangeability, the apparatus assembly of Test Method
D 323 must pass, as a safety precaution, the hydrostatic test
specified in A1.1.6 before using same in testing liquefied
petroleum gas.
flammable. Harmful when inhaled.
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2.H on Liquefied Petroleum Gas.
Current edition approved April 15, 1995. Published June 1995. Originally
published as D 1267 - 53 T. Last previous edition D 1267 - 89.
2 Annual Book of ASTM Standards, Vol 05.01.
3 Annual Book ofASTM Standards, Vol 14.03.
Available from Applied Science Publishers. Ripple Rd., Barking. Eswx,
England
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7. Sampling and Sample Handling
7.1 Samples shall be obtained and stored in accordance
with Practice D 1265, or IP 18 1, Sampling Petroleum Gases,
unless the test samples can be taken directly from the source
of the material to be tested.
7.2 Any method of coupling the vapor pressure apparatus
to the sample source can be employed. Tubing, 6 to 7 mm
(*/4 in.) in diameter, of minimum length, of suitable-working
pressure, and made of material corrosion-resistant to the
products being sampled, is satisfactory for this purpose. A
flexible tubing connection of a satisfactory type greatly
facilitates the purging and sampling operations. The tubing
should be a conducting material or constructed with a
built-in ground connection to minimize the effect of static
electricity.
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9.3.2 When using the 20 9% lower chamber (Appendix
A I. i .4), close the straight-through valve and again open the
inlet to permit expulsion of the lower chamber contents. As
soon as no more liquid escapes from the lower chamber,
close the inlet valve and immediately open the straightthrough valve.
9.3.3 The upper chamber, prior to this operation, is liquid
full at some temperature that is normally below the environmental temperature. Since any warming of the apparatus
would cause expansion of the liquid content of the upper
chamber, leading to possible rupture of the chamber, it is
necessary that the procedural steps of providing free space in
the apparatus be completed promptly.
9.4 Vapor Pressure Determination:
9.4.1 Invert the apparatus and shake it vigorously. Return
the apparatus to its normal upright position and immerse it
in the constant-temperature water bath maintained at the
test temperature (4.1). The apparatus including the bleeder
valve coupling, but not the pressure gage, must be immersed.
Throughout the determination, the temperature of the water
bath shall be checked periodically by means of the bath
thermometer.
9.4.1.1 At test temperatures of 50°C (122°F) or below,
maintain the bath at +O.l"C (0.2"F).At test temperatures
above 50°C (122"F), up to and including 70°C (158'F),
maintain the bath at t0.3"C (0.5"F).
9.4.1.2 Observe the apparatus assembly throughout the
test period to ensure freedom from leaks. Discontinue the
test and discard the results at any time a leak is detected.
9.4.2 After 5 min have elapsed, withdraw the apparatus
from the water bath, invert it, shake it vigorously, and then
return it to the bath. Perform the shaking operation quickly
to avoid excessive cooling of the apparatus and its contents.
Thereafter, at intervals of not less than 2 min, withdraw the
apparatus from the bath, invert, shake it vigorously, and then
return it to the bath. Prior to each removal of the apparatus
from the water bath, tap the gage lightly and observe the
pressure reading. These operations will normally require 20
to 30 min to ensure equilibrium. After this time, if consecutive observed gage readings are constant, record the pressure
reading as the Uncorrected LP-Gas Vapor Pressure of the
sample at the test temperature.
9.4.3 Without removing the pressure gage from the apparatus or the apparatus from the bath, attach a test gage,
previously calibrated against a dead-weight tester, to the
bleeder valve outlet and open the bleeder valve. At the end of
5 min compare the readings of the two gages. Record any
correction thus determined as gage correction.
8. Preparation of Apparatus
8.1 If the apparatus has been used for testing products
other than the type of product to be tested, disassemble,
clean thoroughly, and purge the parts in a stream of dry air.
8.2 Assemble the apparatus with the inlet valve of the
lower chamber open, the straight-through valve between the
two chambers open, the bleeder valve closed, and with the
proper range pressure gage attached.
9. Procedure
9.1 Safe means for the disposal of vapors and liquids
during this operation and in the subsequent sampling
operation must be provided.
9.2 Purging-With the assembled apparatus in an upright
position, connect the inlet valve of the lower chamber to the
sample source with the sampling connection (7.2). Open the
sample source valve to the apparatus. Cautiously open the
bleeder valve on the upper chamber, permitting the air or
vapors, or both, in the apparatus to escape until the
apparatus is full of liquid. Close the lower chamber inlet
valve and open the bleeder valve to its wide.open position.
Allow the contained liquid to evaporate until the apparatus
is covered with white frost (may require more than one
chilling), then invert the assembly, and expel any residual
material through the bleeder valve. Allow the residual vapors
to escape until the pressure in the apparatus is essentially
atmospheric, then close the bleeder valve.
9.3 Sampling-Return the apparatus, now containing
only vapors, to its normal upright position and open the inlet
valve. As soon as the apparatus attains essentially the same
pressure as the pressure of the sample source, momentarily
open the bleeder valve. If liquid does not promptly emerge,
repeat the purging step (9.2). If liquid appears immediately,
close the bleeder and inlet valves in that order (Note 2).
Close the valve on the sample source, and disconnect the
sampling line. Immediately close the straight-through valve
between the two chambers and open the inlet valve, with the
apparatus in an upright position. Close the inlet valve as
soon as no more liquid escapes, and immediately open the
straight-through valve (Note i).
NOTE 2-Transfer of the sample is facilitated by chilling the appa-
10. Calculation
i O. i Correct the Uncorrected LP-Gas Vapor Pressure for
gage errors.
10.2 Convert the corrected vapor pressure = (test gage
reading)
(gage correction) as calculated in 9.4.3 to a
standard barometric pressure of 760 mm (29.92 in.) Hg by
means of the following equation:
10.2.i LP-gas vapor pressure
= corrected vapor pressure, kPa - (760 - P i )0.1333
(1)
= corrected vapor pressure, psi - (760 - P i )0.0193
(2)
where:
+
ratus with a portion of the material under test.
9.3.1 When using the 33% 9% lower chamber (Aí.l.3)
proceed to 9.4.
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6
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S T D - G P A S T D 2L40-ENGL 1777
m
382qb79 0018505 b5L
m
D 1267
PI = observed barometric pressure, mm Hg.
10.2.2 LP-gas vapor pressure
-
= corrected vapor pressure, kPa - (29.92 P2) 3.3864
= corrected vapor pressure, psi - (29.92 - P2)0.49 12
(3)
(4)
where:
P2 = observed barometric pressure, in. Hg.
10.2.3 Conversion Factors:
1 kPa = 7.50064 mmHg = 0.295301 in. Hg
1 psi = 5 1.7 15 1 mmHg = 2.03603 in. Hg
(5)
(6)
(7)
11. Report
11.1 Report the LP-Gas vapor pressure test results in
terms of kilopascals to the nearest 5 kPa or pounds per
square inch, gage, to the half unit, and the test temperature.
12. Precision and Bias
12.1 The following shall be used as a basis for judging the
acceptability of results (95 % probability).
12.1.1 Repeutabiliry-The difference between two test results, obtained by the same operator with the same apparatus
under constant operating conditions on identical test materials would in the normal and correct operation of the test
method, exceed the following value only in one case in
twenty:
12 kPa ( 1.8 psi)
12.1.2 Reproducibility-The
difference between two
single and independent results obtained by different operators working in different laboratories on identical test material would in the long run, in the normal and correct
operation of the test method, exceed the following value only
in one case in twenty:
19 kPa (2.8 psi)
12.2 Bias-The procedure in Test Method D 1267 for
measuring vapor pressure has no bias because the value of
vapor pressure is defined only in terms of this test method.
13. Keywords
13.1 natural gas liquids; liquified petroleum gases; vapor
pressure
ANNEXES
(Mandatory Information)
Al. 1 Vapor Pressure Apparatus, consisting of two chambers, designated as the upper and lower chambers, shall
conform to the following requirements. To maintain the
correct volume ratio between the upper and lower chambers,
the units shall not be interchanged without recalibrating to
ascertain that the volume ratio is within satisfactory limits.
A 1.1.1 Upper Chamber-This chamber, as shown in Fig.
Al.1 (c), shall be a cylindrical vessel 51 f 3 mm (2 k in.)
in diameter and 254 f 3 mm ( I O t l/8 in.) in length, inside
dimensions, with the inner surfaces of the ends slightly
sloped to provide complete drainage from either end when
held in a vertical position. On one end of the chamber, a
suitable bleeder-valve coupling (Fig. Al.l (e)) shall be
provided to receive the bleeder-valve assembly and the
pressure gage. In the other end of the chamber an opening
approximately 13 mm ( V 2 in.) in diameter shall be provided
for coupling with the lower chamber. Care shall be taken that
the connections to the end openings do not prevent the
chamber from draining completely.
A 1.1.2 Bleeder- Valve Assembly-The bleeder-valve for
purging the apparatus (Fig. Al.l) (d)) shall be a normal 6
mm (V4 in.) valve fitted into the side of the bleeder-valve
coupling (Fig. A I . 1 (e)). The lower end shall be threaded to
fit into the end fitting of the upper chamber, and the upper
end shall be threaded to receive the gage coupling (Fig. AI. 1
(h)).
A 1.1.3 Lower Chamber, 33V3 % (Fig. A l . 1 (b))-This
chamber shall be a cylindrical vessel of such a volume that
the ratio of the volume of the upper chamber to the volume
of the lower chamber is between the limits of 1.97 to 2.03
(Note A 1.2).
A I . 1.4 Lower Chamber, 20 % (Fig. A l . I (b))-This
chamber shall be a cylindrical vessel of such a volume that
the ratio of the volume of the upper chamber to the volume
of the lower chamber is between the limits of 3.95 to 4.05
(Note A 1.2) (Note A 1.3). In one end of the lower chamber,
an opening approximately 19 mm (3/4 in.) in diameter shall
be provided to receive a suitable straight-through valve (Fig.
Al.l (g)) having a minimum internal channel of 13 mm (Y2
in.) in diameter. The other end of the chamber shall be
equipped with a nominal 6 mm ( Y 4 in.) inlet valve.
NOTEAl. 1-In determining the volumetric capacities of the chambers, the volume of the lower chamber is considered as that which is
below the "straight-through" valve closure. The volume above the
"straight-through" valve closure, including the portion of the coupling
attached to the upper chamber, is considered as a part of the upper
chamber volume. The volume ratios of the chambers are determined in
accordance with the procedure outlined in the Appendix of Test Method
D 323.
NOTEAl .3-The apparatus requirements for this method, excluding
the bleeder-valve assembly, are identical with those of Test Method
D 323 with the exception of the 33V3 % lower chamber. Although the
test procedural details are different, the air and liquid chambers of Test
Methcd D 323 may be used in the present method provided they are of
sufficient strength to withstand the higher test pressures (A I 1.6).
I
A1.1.5 Method of Coupling Upper und Lower Chambers-Any method of coupling the chambers can be employed provided the volumetric requirements are met and
that the assembly is free from leaks under the conditions of
the test.
A 1.1.6 Hydrostatic Test-The assembled chambers shall
be certified by the manufacturer to withstand approximately
6920 kPa (loo0 psi) gage hydrostatic pressure without
permanent deformation.
7
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
Al. APPARATUS FOR VAPOR PRESSURE OF LIQUEFIED PETROLEUM (LP) GASES
D1267
'
1G
,
( S T R A I G H T - THROUGH VALVE)
PLINGI
VALVE
COUPLIPJG 1
l
L F( I N L E T
VALVE)
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
FIG. A l . l
Typical LPG Vapor Pressure Apparatus
A I . 1.7 Checking for Freedom from Leaks-Before placing new apparatus in service, and as often as necessary thereafter, the assembled vapor pressure apparatus shall be
checked for freedom from leaks by filling it with air, natural
gas, nitrogen, or other similar gases, to 3460 kPa (500 psi)
gage pressure, and then completely immersing it in a water
bath. Only apparatus that will stand this test without leaking
shaii be used.
A 1.2 Pressure Gage-The pressure gage, shown in Fig.
A l . l (a), shall be a Bourdon-type spring gage of test gage
quality 114 to 140 mm (4% to 5% in.) in diameter provided
with a nominal 6 mm (V4 in.) male thread connection with a
passageway not less than 5 mm (Y16 in.) in diameter from the
Bourdon tube to the atmosphere. The range and graduations
of the pressure gage used shall be governed by the vapor
pressure of the sample being tested, as follows:
Gage to Be Used
LP-Gas Vapor Pressure,
kPa (psi) gage at test
temperature
655 (95) and under
620 (90) to 1750 (250)
1660 (240) to 3460
(5001
Scale
Range,
kPa (psi)
O to 700
(100)
O to 1750
(250)
O to 3500
(500)
considered inaccurate.
A 1.3 Vapor Pressure Bath-The vapor pressure bath
(water) shall be of such dimensions that the vapor pressure
apparatus may be immersed so as to completely cover the
bleeder valve when the assembly is in an upright position.
Means for maintaining the bath at the test temperature (2. I )
within the range as follows: ( I ) Test temperature 50°C
(122°F) and below, +O.l"C (0.2"F); (2) Test temperature
above 50°C (122'F), +0.3"C (0.5"F). In order to check the
bath temperatures, the appropriate bath thermometer shall
be immersed to the test temperature mark on the thermometer scale throughout the vapor pressure determination.
A 1.4 Thermometers-Only thermometers conforming to
specificationsin Specification E 1 or IP Standard Thennometer Specificationsshall be used. The range shall be governed
by the test temperature of the test being used as follows:
Test Temperature
ThermomThermometer
Range 'C
"C
eter No.
35 to 40
18C
34 to 42
50 to 80
65C
50 to 80
Numbered Intermediate
Intervals, Graduations,
kPa (psi) kPa (psi)
70 (IO)
"F
172 (25)
7 (I)
344 (50)
35 (5)
95
Only accurate gages shall be continued in use. When the gage
correction exceeds 2 96 of the scale range, the gage shall be
8
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"F
to 105
18F
94 to 108
125 to 175
65F
122 to 176
A 1.4.1 At other test temperatures a total immersion
thermometer shall be used having a range that brackets the
test temperature and a maximum scale error of O. 1°C (0.2"F).
A 1.5 Dead- Weight Tester-A dead-weight tester of satisfactory range shall be provided as a means for checking the
accuracy of vapor pressure gages.
3.4 (0.5)
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~
~~
~
STDmGPA S T D 21LiO-ENGL 1777 m 382Lib77 0038507 LI2LI m
D 1267
A2. PRECAUTIONARY STATEMENT
A2.1.5 Avoid buildur, of vapors and eliminate all sources
A2.1 ProDane/Butane. or Mixture of Both
.
A2.1.1
A2.1.2
A2.1.3
A2.1.4
I
Vapors can cause flash fires.
Keep away from heat, sparks, and open flame.
Keep container closed.
Use with adequate ventilation.
of ignition, especially nonexplosion-proof electrical apparatus and heaters.
A2.1.6 Avoid prolonged breathing of vapor or spray mist.
A2.1.7 Avoid prolonged or repeated skin contact.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights. and the risk of infringement of such rights. are entirely their own responsibility.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
This standard is subject to revision at any time by the responsible fechnical committee and must be reviewed every five years and
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 Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
9
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4m
Designation: D 1657 - 89
An American National Standard
Standard Test Method for
Density or Relative Density of Light Hydrocarbons by
Pressure Thermohydrometer'
This standard is issued under the fixed designation D 1657; 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
supemript epsilon (e) indicates an editorial change since the last revision or reapproval.
reference temperatures in general use are 15'C and 60'F for both tl and
t2, but other temperatures may be employed for t,.
1. Scope
1.1 This test method covers the determination of the
relative density or density of light hydrocarbons including
liquefied petroleum gases (LPG).
1.2 The prescribed apparatus should not be used for
materials having vapor pressures higher than 1.4 MPa (1 4
bar) at the test temperature. (The SI unit of pressure is the
pascal: 1 Pa = 1 N/m2; lo5 Pa = 1 bar = 1.01972 k&cm2.)
4. Summary of Test Method
4.1 The apparatus is purged with a portion of the sample
before filling with the portion to be used for testing. The
pressure cylinder is filled to a level at which the enclosed
hydrometer floats freely. The hydrometer reading and the
temperature of the sample are noted.
NOTE1-Attention is drawn to the hazards encountered when
working with liquefied petroleum gas or light hydrocarbons. The
requirements of any national, local, or domestic safety code should
always be strictly observed.
5. Significance and Use
5.1 The density or relative density of light hydrocarbons
and liquefied petroleum gases is determined to satis@
transportation, storage, and regulatory requirements. Although this determination does not describe any particular
performancecharacteristic, density or relative density can be
used to indicate approximate component concentrations in
liquefied petroleum mixtures.
1.3 The values in SI units are to be regarded as the
standard. The values in parentheses are for information only.
1.4 This standard may involve hazardous materiais, operations, and equipment. This standard does not purport to
address all of the safety problems 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.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
6. Apparatus4
6.1 Thermohydrometers, made of glass, graduated in density with a range from 500 to 650 ks/m3, or in relative
density with a wide range from 0.500 to 0.650, and conforming to the dimensions given in Table 1.
6.2 Hydrometer Cylinder, constructed of giass or transparent plastic; for example, poly(methy1 methacrylate) or
equivalent material, conforming to the design and dimensions given in Fig. 1. The ends shall be tightly sealed with
neoprene gaskets and metal end plates as shown in Fig. 1.
6.2.1 Caution-A protective shield shall be placed around
the plastic or glass cylinder. Replace any cylinders that show
signs of fogging, crazing, cracking, or etching.
NOTE3-Certain compounds attack plastics and cloud the inner
2. Referenced Documents
2.1 ASTM Standards:
D 1250 Guide for Petroleum Measurement Tables (ASTM
1250/API 2540/IP 200)2
E 100 Specification for ASTM Hydrometers3
3. Terminology
3.1 Dejnitions:
3.1.1 density-the mass of the liquid per unit volume at a
temperature t.
3.1.2 relative density (this term now replaces the former
term "specific gravity")-the
ratio of the mass of a given
volume of the liquid at a temperature t , to the mass of an
equal volume of pure water at a temperature t2.
surface of the cylinder, making it difficult or impossible to read the
hydrometer. Tests showed no attack by ethane, ethylene, propane,
propylene, butane, isobutane, normal butylenes, isobutylene, pentane,
and isopentane, and no attack is expected from butadiene and
acetaldehyde. Users are cautioned, however, to clean the cylinder
thoroughly after each determination.
Ketones and alcohols should not be used for cleaning as they attack
and weaken plastics while aromatics also tend to attack the surface of
plastics and should similarly not be used.
NOTE2-When reporting the density, the units of mass and volume
used, together with the temperature, should be explicitly stated, for
example, kg/m3 at fC. The standard reference temperatures are 15°C
and 60°F.
When reporting the relative density, the temperatures t , and t2 should
be explicitly stated; for example, relative density 60/60'F. The standard
6.2.2 The liquid inlet valve and the liquid outlet valve
shall be tightly connected to a base plate that shall be bored
to give both valves a common inlet to the cylinder. The
* This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum products and Lubricants and is the direct responsibility of Subcommittee W 2 . 0 2 . K on Density.
Current edition approved March 31, 1989. Published May 1989. Onginally
published as D 1657 - 39 T. Last previous edition D 1657 - 83 (1988)''.
Annual Book of ASTM Siandnrds, Vol. 05.01.
Annual Book of ASTM Standards, Vol 14.03.
4Apparatus suitable for this test may be obtained from: EG&G Chandler
Engineering, 7707 E. 38th St., Tulsa, OK 74145; Peter Peterson Scientific
Glassblowing, Inc., 473 Elmira Rd., Guelph, Ontario NIK 1C2; and Refinery
Supply Co., Inc., 6901 E. 12th St., Tulsa, OK 741 12.
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TABLE 1
Thermohydrometer
For Petroleum Products and Other
Liquids of Similar Surface Tensions
i33 dvnes/cm or less)
Thermometer Scale in Body
ASTM Hydrometer No.
Nominal Relative
Density Range
1O1H-62
0.500 to 0.650
Hydrometer
Total length, mm
Body diameter, mm
Stem diameter min, mm
Working pressure min, psi
354 to 366
19 to 22
10.5
200
Hydrometer Scale
Standard temperature, O F
Subdivisions
Intermediate lines at
Main (numbered) lines at
Scale error at any point not to exceed
Length of nominal scale, rnm
60/60
0.001
0.005
0.01o
0.001
125 to 145
Thermometer Scale
30 to 90
total
1
5
10
0.5
Range, O F
Immersion
Subdivisions, O F
Intermediate lines at, O F
Main (numbered)lines at, OF
Scale error at any point not to exceed,
OF
Scale length, mm
50 to 70
LIOUID
INLET
Thermohydrometer (Pressure)
ASTM Hydrometer No.
Density Range,
kglm3
310H
500-650
I
VALVE
\I
I
:EDLE
'LET
Hydrometer
387
16 to 22
10.5
1400
Hvdrometer Scale
Standard temperature, O C
Subdivisions, kg/m3
Intermediate lines at, kg/m3
Main (numbered)lines at, kg/m3
Scale error at any point not to exceed,
kglm3
Length of nominal scale, mm
15
302-1
\.
__.-I
FIG. 1 Pressure Thermohydrometer Cylinder
1
5
10
1
125 to 145
vapor vent valve shall be similarly connected to the top plate,
which shall be bored to provide a vapor outlet from the
pressure cylinder. All valves shall be 6.3 mm ( V 4 in.) or
equivalent needle valves.
6.2.3 The cylinder shall not be operated at a gage pressure
greater than 1.4 MPa (14 bar).
6.3 Water Bath, fitted with a thermostat or other means of
maintaining the bath at a constant temperature of 15 k 0.2"C
(60 k OSOF), and of such dimensions that the cylinder can be
completely immersed.
7. Reference Liquids
7.1 The following reference liquids are required for standardization of the hydrometer:
7.1.1 Propane, pure grade, having a nominal density of
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/
507.6 kg/m3 at 15'C or a relative density 60/60"F of 0.50699.
7.1.2 n-Butane, pure grade, having a nominal density of
584.1 kg/m3 at 15°C or a relative density 60/60"F of 0.5840.
8. Sampling
8.1 The procedure for sampling for calibration of the
apparatus and for subsequent testing is described as follows:
8.1.1 Connect the source of supply of the liquid to be
tested to the inlet valve by suitable fittings so that a
representative sample can be introduced into the cylinder.
Ascertain that these connections are free of leaks. Open the
outlet valve and purge the sampling connections by opening
the inlet valve slightly, permitting the product to flow
through the outlet valve at the bottom of the cylinder.
8.1.2 When the connections have been purged, close the
outlet and vent valves and open the inlet valve, permitting
the liquid to enter the cylinder until it is full. If necessary, the
vent valve can be opened slightly to permit complete filling
of the cylinder and then closed. At no time shall the pressure
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
Nominal length, mm
Body diameter, mm
Nominal stem diameter, mm
Working pressure, kPa
382Lib77 UOL85LU T L 7 U
S T D - G P A STD 2L40-ENGL 2 7 7 7
dm
D 1657
in the cylinder be allowed to rise above a gage pressure of 1.4
MPa.
8.1.3 When the cylinder has been filled, close the inlet
valve and open the outlet valve, permitting the contents of
the cylinder to be withdrawn completely and the pressure
inside the cylinder to be reduced to that of the atmosphere.
8.1.4 Close the outlet valve and open the inlet valve,
filling the cylinder to a level at which the enclosed
thermohydrometer floats freely. If it is necessary to accomplish this filling by venting vapor through the vent valve,
repeat the purging to cool the cylinder sufficiently to permit
its being filled without the necessity of venting.
8.1.5 With all valves closed, examine the apparatus for
leaks. If leaks are detected, discard the sample, reduce the
pressure to atmospheric and repair the leaks. Repeat the
sampling procedure.
the liquid level will improve the visibility of the surface.
Estimate the hydrometer reading to the nearest one-fifth
scale division.
9.8 Repeat with a second sample. Average the two results,
if these differ by less than 0.0005, deduct the average from
the relative density or density of the reference liquid to
obtain the correction to be applied.
9.8.1 If the two results differ by more than 0.0005, repeat
the determinations.
9.8.2 After each determination, empty the cylinder and
vent to reduce the pressure to atmospheric.
10. Procedure
10.1 Purge and empty the apparatus and draw a sample of
the product to be tested as in Section 8.
10.2 Disconnect the cylinder and place it in the water
bath maintained at approximately 15°C or 60'F until the
temperature of the contents has reached 15 +I 0.2"C or 60 f
0.5"F as indicated by the thermometer. In order to accelerate
thermal adjustment, occasionally remove the apparatus from
the water bath, gently invert and tilt, and replace in the water
bath. Exercise care during this operation to prevent damage
to the enclosed thermohydrometer.
10.3 When the product in the cylinder has reached a
constant temperature of 15 f 0.2"C or 60 f 0.5"F, remove
the apparatus from the water bath and while the
thermohydrometer is floating freely, observe and record the
thermohydrometer reading as quickly as possible. Read and
record the temperature to the nearest 0.2"C or 0.5"F.
Immediately after each determination, empty the liquid
from the cylinder and vent to reduce the pressure to
atmospheric. Highly volatile liquids and liquefied petroleum
gases must not be left in the apparatus since at high ambient
temperatures; they might generate sufficient pressure to burst
the cylinder.
10.3.1 If so used, the cylinder must be vented and the test
discarded if the pressure in the cylinder rises above a gage
pressure of 1.4 MPa (14 bar).
9. Calibration of Apparatus
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
9.1 Carefully clean and dry the thermohydrometer and
the inside wall of the pressure cylinder.
9.2 Insert the thermohydrometer in the pressure cylinder.
Connect the source of supply of the reference liquid to the
inlet valve and ascertain that the connections are free of
leaks. Open the outlet valve and purge the connections by
opening the inlet valve slightly.
9.3 When the connections have been purged, close the
outlet and vent valves and open the inlet valve, permitting
the liquid to enter the cylinder until it is full. If necessary, the
vent valve can be opened slightly to permit complete filling,
after which it should be closed. The pressure of the cylinder
must never rise above a gage pressure of 1.4 MPa (14 bar).
9.4 When the cylinder has been filled, close the inlet valve
and open the outlet valve, permitting the liquid to be
withdrawn completely and the pressure inside the cylinder to
be reduced to atmosphere.
9.5 Close the outlet valve and open the inlet valve, filling
the cylinder to a level where the enclosed thermohydrometer
floats freely. If the vapor pressure is too high to permit
adequate filling, the cylinder must be cooled. This is accomplished by repeating the purging operation. When the
cylinder is filled to the normal operating level, close the inlet
valve and examine the apparatus for leaks. If any are
detected, withdraw the liquid, reduce the pressure to atmospheric and repair the leaks. Repeat the purging and filling
operations.
9.6 Disconnect the cylinder from the source of supply of
liquid and place it in the water bath maintained at 15 f
0.2'C or 60 2 0.5"F until thermal equilibrium has been
obtained. To accelerate thermal adjustment, occasionally
remove the cylinder from the water bath, tilt to a horizontal
position, rock gently a few times to ensure mixing, and
replace in the water bath. Exercise care to prevent damage to
the thermohydrometer.
9.7 Remove the cylinder from the water bath, stand it on
a firm level surface, and while the hydrometer is floating
freely, take the hydrometer reading promptly in the following manner: Observe a point slightly below the plane of
the liquid surface and then raise the line of vision until this
surface, seen as an ellipse, becomes a straight line. The point
where this line cuts the hydrometer scale is the reading of the
instrument. A white card held behind the cylinder just below
NOTE&For measurements in the field, this method may be used at
ambient temperatures, with the realization that the accuracy is decreased.
11. Report
1 1.1 Correct the observed thermohydrometer reading and
report the corrected reading to the nearest unit of density or
the nearest 0.001 relative density.
11.2 The result must be reported in accordance with the
Petroleum Measurement Tables (Section 2), using Table 53B
for correction of density to 15'C or Table 23B for correction
of relative density to 6O/6O0F.
12. Precision and Bias
12.1 The precision of procedure in this test method has
not been determined but is under consideration.
12.2 The bias of the procedure in this test method has not
been determined.
12
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The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entireiy their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
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 Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19703.
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[&
Designation: D 1837 - 94
An American Naaonal Standard
Standard Test Method for
Volatility of Liquefied Petroleum (LP) Gases’
This standard is issued under the fixed designation D 1837; 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 epsiion (0indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method is a measure of the relative purity of
the various types of liquefied petroleum (LP) gases and helps
to ensure suitable volatility performance. The test results,
when properly related to vapor pressure and density of the
product, can be used to indicate the presence of butane and
heavier components in propane type LP-gas, and pentane
and heavier components in propane-butane and butane type
fuels. The presence of hydrocarbon compounds less volatile
than those of which the LP-gas is primarily composed is
indicated by an increase in the 95 % evaporated temperature.
1.2 Chromatographic analysis should be used when the
concentration and type of higher boiling compounds must be
identified.
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information only.
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 establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
TABLE 1 Weatherinn Tube Graduation Tolerances
scale
limit of
Range, mL
0.0 to 0.1
0.1 to 0.3
0.3to 0.5
0.5to 1.0
1 .O to 3.0
3.0to 5.0
5.0to 25.0
25.0to 100.0
0.05
0.05
0.05
0.1
0.1
0.5
1 .o
0.02
0.03
0.05
0.05
1 .o
0.1
0.2
0.5
1.o
5. Apparatus
5.1 Weathering Tube-A centrifuge tube, cone-shaped,
conforming to the dimensions given in Fig. 1 and made of
thoroughly annealed heat-resistant glass.4 The shape of the
lower tip of the tube is especially important. The taper shail
be uniform and the bottom shall be rounded as shown in Fig.
1. The tubes shall comply in wall thickness to ASTM
centrifuge tube requirements (Note 1). The graduation
tolerances are given in Table 1.
2.1 ASTM Standards:
D96 Test Methods for Water and Sediment in Crude Oil
by Centrifuge Method (Field Procedure)2
D 1796 Test Method for Water and Sediment in Fuel Oils
by the Centrifuge Method (Laboratory Procedure)2
E 1 Specification for ASTM Thermometers3
NOTE1-Requirements for centrifuge tubes appear in Test Methods
D 96 and D 1796.
3. Summary of Test Method
3.1 The product is refrigerated by means of a cooling coil,
and 100 mL of the liquid is collected in a weathering tube.
The liquid is allowed to weather under specified conditions
’ has evaporated.
and the temperature is observed when 95 %
Correction for variation of barometric pressure is made.
5.2 Tube Support-Means shail be provided for s u p
porting the weathering tube by its neck in a vertical position.
5.3 Water Bath (for use in tests on butane and propanebutane mixture types of liquefied petroleum gas only). A
shallow container filed with clean water having a maintained temperature ranging from 15 to 2 1°C (60 to 70’F) and
a depth of 38 mm (1Y2 in.).
5.4 Thermometer-ASTM Armored Weathering Test
Thermometer having a range from -50 to 5°C (-58 to 41°F)
and conforming to the requirements for Thermometer
99C-92 (99F-86) as prescribed in Specification E 1.
5.5 Sampling Precooling Equipment:
5.5.1 Cooling Vessel-Any suitable wide-mouthed metai
container or Dewar flask at least 64 mm (2V2 in.) in inside
4. Signüícance and Use
4.1 Volatility, expressed in terms of the 95 %
evaporated
i
temperature of the product, is a measure of the amount of
least volatile fuel components present in the product. Cou1 This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee DO2.H on Liquified Petroleum Gas.
Current edition approved July 15, 1994. Published September 1994. Originally
pübhhed as D 1837 - 61 T.Last PXV~OUS edition D 1837 - 92.
2 Annual Book of ASTM Standards, Vol 05.01.
3 Annual Book of ASTM Standarh, Vol 14.03.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
EITOT.mL
pled with a vapor pressure limit, it serves to ensure essentially singlecomponent products in the cases of commercial
propane and commercial butane fuel types. When volatility
is coupled with a vapor pressure limit which has been related
to gravity, as in the case of the commercial PB-mixture type
of fuels, the combination serves to assure essentially two
component mixtures for such fuels. When coupled with a
proper vapor pressure limit, this measurement serves to
assure that specialduty propane products will be composed
chiefly of propane and propylene and that propane will be
the major constituent.
2. Referenced Documents
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~
~
S T D - G P A S T D 2190-ENGL 1997 m 3 8 2 9 b ï î 0018513 7 2 8
[$)9
DI837
TOLEWCE
3 m m (118 in.)
above. Connect the downstream end of the coil to a 3.2 mm
(I/s in.) needle valve having an outlet connection not more
than 76 mm (3 in.) long (see Fig. 2).
5.5.3 Precoolant-This can be the liquefied petroleum gas
from the same container from which a sample is to be taken.
Other refrigerants having a boiling point lower than the
initial boiling point of the sample can be used. Use a
nonflammable precoolant if required.
6. Procedure
6.1 Obtaining a Test Sample-Fiil the cooling vessel with
the precoolant so as to cover the cooling coil. Attach the inlet
of the cooling coil to the source from which the sample is to
be taken with a short line connection of 6.4 mm ( Y 4 in.) pipe
(or larger), having a sampling valve large enough to prevent
vaporization of the material due to the drop in pressure
across the valve seat. Purge the sampling line and cooling coil
by opening both the sampling valve and the 3.2 mm (118 in.)
needle valve on the downstream end of the cooling coil. Fiü
the weathering tube with the sample flowing through the
cooling coil. Empty this first sample, add one or two grains
of charcoal, and then refill the weathering tube to the
100-mL mark with fresh liquid sample passing through the
cooling coil. Carefully inseri the precooled armored thermometer as low as possible into the centrifuge tube (Note 2).
Center the armored thermometer in the tube by means of a
slotted cork.
NOTE2-Do not remove the armor from the thennometer during
the test. Place the bottom of the armor as low in the centrifuge tube as it
will go, pipet in 5 mL of water, and observe the water level in the tube.
3.2 rnrn (118 in.) NEEDLE VALW
SAMPLE VALVE
6 m (20 R.) OF 4.8 mm (3i16 in.) O.D.
4
SOFT COPPER TUBING
-It
METAL OR GLASS
COOLING VESSEL
6.4m m (114in.)
MIN.INSIDE
DIAMETER
NOTE-FOT graduation tderances see TaMe 1.
FIG. 1 Weatheringlube
diameter by 292 mm (1 1 i/z in.) deep.
5.5.2 Cooling Coil-Approximately 6 m (20 fi) of 4.8-mm
(%-in.) outside diameter soft copper tubing, wound around
a hollow mandrel at least 54 mm (2% in.) in outside
diameter, with adjacent turns touching. Run the lower end of
the tube up through the center of the mandrel before winding
so that the finished coil will fit snugly inside the cooling
vessel. When assembled, the top of the coil must be at least
25 mm ( i in.) below the top of the cooling vessel and the
open ends of the coil must not be more than a few inches
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i--1
64 rnm (2 l i 2 in.)
NOTE-The
coils in the drawing are extended for danty.
FIG. 2
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Preceding Equipment
S T D - G P A STD 2 1 4 0 - E N G L 1997
3824679 0018519 bbll
D1837
Take the 5 I
residue readings at this same level with the armored
thermometer in the same position.
6.2 Weathering Butane and Propane-Butane Mixture
Types of Liquefed Petroleum Gas Products-When the
temperature of the sample is below -12'C (10"F), allow it to
weather in the atmosphere until the temperature has reached
-12°C (10°F). At this point, place the weathering tube, with
the armored thermometer still in place, in the water bath in a
vertical position, submerging it to the IVz-mL mark, and
allow the contents to weather.
6.3 Weathering Propane Type of Liquefied Petroleum Gas
Products-Allow the sample to weather in the atmosphere,
taking care to disturb the frost on the tube as little as
possible. An acetone or alcohol swab can be used to remove
frost sufficient to permit reading of the temperature.
6.4 Reading of Temperature-When the liquid level in
the weathering tube, with the armored thermometer still in
place, corresponds with the level previously determined
when the 5 mL of water was put in the weathering tube (see
Note 2), read and record the temperature of the sample in
accordance with 6.2 and 6.3.
6.5 Temperature Correction-Following the final temperature reading (6.4), remove the armored thermometer from
the weathering tube and place it in a bath of finely crushed
ice up to the immersion point. Observe the reading of the
thermometer when a constant reading is obtained. If the
thermometer reading is less than 0°C (32"F),add the fraction
of a degree it is low to the final test reading. If the
thermometer reading is more than 0" (32"F), subtract the
fraction of a degree that it is high from the final test reading.
Discard any thermometer that varies more than 0.5"C (1'F)
in either direction from 0°C (32°F).
NOTE3-A high reading of the thermometer when it is placed in ice
usually indicates that there is a break in the mercury-thallium thread.
This can be corrected by warming the thermometer gently in a warm
water bath to drive the break upward into the expansion chamber at the
top of the thermometer. While the mercury-thallium is continuous in
the upper chamber, tap the bottom of the thermometer on a hard, but
cushioned surface, to join the liquid into a continuous thread. A low
reading in ice usually indicates that some of the liquid has remained in
the expansion chamber. To correct this, allow the thermometer to warm
so the liquid enters the chamber and tap as previously instructed.
( 5 5% residue) for the thermometer error (6.5).
7.2 Correct the observed temperature for the thermometer
error from the observed atmospheric pressure in kPa
(millimetres of mercury) to a base barometric pressure of
101.33 kPa (760 mm).
7.3 In the weathering test for propane, add 0.3"C ( 0 3 ° F )
to the corrected temperature for each 1.3 kPa (10 mm Hg)
that the test is conducted below 101.33 kPa (760 mm)
pressure, or subtract 0.3'C ( 0 3 ° F ) from the observed
temperature for each 1.3 kPa (10 mm Hg) that the test is
conducted above 101.33 kPa (760 mm).
7.4 In the weathering test for butane and propane-butane
mixtures, add 0.4"C (0.7"F)to the corrected temperature for
each 1.3 kPa (10 mm Hg) that the test is conducted below
101.33 kPa (760 mm) pressure, or subtract 0.4"C (0.7"F)
from the observed temperature for each 1.3 kPa (10 mm Hg)
that the test is conducted above 101.33 kPa (760 mm).
8. Precision and Bias
8.1 The following criteria should be used for judging the
acceptability of results (95 % confidence):
8.1.1 Repeatability-The difference between two test results obtained by the same operator with the same apparatus
under constant operating conditions on identical test materials would in the normal and correct operation of the test
method, exceed the following value only in one case in
twenty:
S6'C ( 1 .VF)
8.1.2 Reproducibility-The difference between two single
and independent results obtained by different operators
working in different laboratories on identical test material
would in the long run, in the normal and correct operation of
the test method, exceed the following value only in one case
in twenty:
95°C (1.7'F) for butane and propane-butane mixtures and
1.28"C (2.3"F) for propane.
8.2 Bias-The procedure in this test method for measuring volatility of LP-gases has no bias because the volatility
is defined only in terms of this test method.
9. Keywords
9.1 butane; liquefied petroleum (LP) gases; propane;
LPG; volatility
7. Interpretation of Results
7.1 Correct the thermometer at the 95 9% boiling point
The American Society for Testing and Materials takes no p i t i o n respecting the validity of any palen?rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly edvised that determination of the validity of any such
petent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
il not revised. either reepproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquaaers. Your comments will receive careful consideration at a meeting Ot the responsible
technical committee, which you may attend. If you feel that your comments have no? received a fair hearing you should make your
views known to the ASTM Committee on Standards, 7916 Race St., Philadelphia, PA 19103.
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4Tb
Designation: D 1838 - 91
An American National Standard
Standard Test Method for
Copper Strip Corrosion by Liquefied Petroleum (LP) Gases'
This standard is issued under the fixed designation D 1838; 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 (0 indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method detects the presence of components
in liquefied petroleum gases which may be corrosive to
copper.
NOTE 1-For an equivalent copper strip test applicable to less
volatile petroleum products, see Test Method D 130.
1.2 The values stated in acceptable metric units are to be
regarded as the standard. The values in parentheses are for
information only.
1.3 This standard does not purport to address all of the
safety problems, 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. For specific
hazard statements, see 6.1, 8.3. I , and Annex A l .
6.4 mm (V4-in.) pipe. The whole assembly shall be capable of
withstanding a hydrostatic test pressure of 6895 kPa (loo0
psig). No leak shall be discernible when tested at 3450 kPa
(500 psig) with gas.
5.2 Water Bath, capable of being maintained at 37.8 k
0.5'C (100 k 1°F).Incorporate suitable supports to hold the
test cylinder in an upright position. Make the bath deep
enough so that the entire cylinder and valves will be covered
during the test.
5.3 Thermometer-An
ASTM Density Thermometer
having a range from -20 to 105°C(-5 to +215"F), graduated
in 0.2"C (0.5"F) subdivisions, and conforming to the requirements for Thermometer 12C ( 12F), as prescribed in Specification E 1.
5.4 Strip Polishing Vise, to hold the copper strip firmly
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2. Referenced Documents
2.1 ASTM Standards:
D 130 Test Method for Detection of Copper Corrosion
from Petroleum Products by the Copper Strip Tarnish
Test2
E 1 Specification for ASTM Thermometers3
Needle Valve A
3. Summary of Test Method
3.2 m m I.D.
3.1 A polished copper strip is immersed in approximately
100 mL of the sample and exposed at a temperature of
37.8"C (100°F) for 1 h in a cylinder of suitable working
pressure. At the end of this period, the copper strip is
removed and rated as one of the four classifications of the
ASTM Copper Corrosion Standards.
Neoprene O-Ring
Outage Tube
Mote rial:
4. Significance and Use
4.1 Copper corrosion limits provide assurance that dificulties will not be experienced in deterioration of the copper
and copper-alloy fittings and connections that are commonly
used in many types of utilization, storage, and transportation
equipment.
1 5 2 . 4 mm
(6 i n . )
1
I
76.2 mm
( 3 in.)
6.4 m m Min.
(114 in.)
5. Apparatus
5.1 Corrosion Test Cylinder, constructed of stainless steel
with an O-ring removable top closure according to the
dimensions given in Fig. 1. Provide a flexible aluminum
connecting hose with swivel connections with adapter to a
/ 6.4 mm (1/4in.)
n
Needle Valve B
Metric Equivalents
mm
in.
mm
'/a
3.2
3
76
'14
6.4
6
152
in.
' This test
method is under the jurisdiction of ASTM Commitîee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2.H on Liquefied Petroleum Gas.
Current edition approved Aug. 15, 1991. Published October 1991. Originally
published as D 1838 - 61 T.Last previous edition D 1838 - 89.
*Annual Book ofASTM Siandards, Vol 05.01.
Annual Book ofASTM Siandards, Vol 14.03.
38.1
1 '/z
FIG. 1 Copper Sûip Corrosion Test Cylinder
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without marring the edges. For convenient vises see Test
Method D 130.
6. Materials
6.1 Wash Solvenf-Use acetone or knock test grade
2.2.4 trimethylpentane.
NOTE2: Warning-Extremely flammable. See Annex A 1.
6.2 Copper Strip, 12.5 mm ( V 2 in.) wide, 1.5 to 3.0 mm
('116 to '/E in.) thick, cut 75 mm (3 in.) long from smoothsurfaced, hard-temper, cold-finished copper of 99.9+ percent
purity; electrical bus bar stock is generally suitable. Drill a
3.2 mm (I/8 in.) hole approximately 3.2 mm ('/8 in.) from one
end in the center of the strip. The strips can be used
repeatedly but should be discarded if the surfaces become
deformed.
6.3 Polishing Materials-Silicon carbide grit paper of
various degrees of fineness including 65-pm (24O-fit) paper
or cloth; also a supply of 105ym (150-mesh) silicon carbide
grain and pharmaceutical grade absorbent cotton (cotton
wool).
6.4 Copper Corrosion Standard Plaques are a~ailable.~
Their care and inspection for stability are described in detail
in Test Method D 130.
7. Preparation of Strips
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
7.1 SurJice Preparation-Remove all surface blemishes
from all six sides of the strip with silicon carbide grit paper of
such degrees of fineness as are needed to accomplish the
desired results efficiently. Finish with 65-pm (240-grit)
silicon carbide paper or cloth, removing all marks that were
made by other grades of paper used previously. Immerse the
strip in wash solvent from which it can be withdrawn
immediately for final polishing or in which it can be stored
for future use.
7.1.1 As a practical manual polishing procedure, place a
sheet of the paper on a flat surface, moisten it with wash
solvent and rub the strip against the paper with a rotary
motion, protecting the strip from contact with the fingers
with an ashless filter paper. Alternatively, the strip can be
prepared by use of motor-driven machines using appropriate
grades of dry paper on cloth.
1.2 Final Polishing-Remove
a strip from the wash
solvent. Holding it in the fingers protected with ashless filter
paper, polish first the ends and then the sides with the
105-pm (1 50-mesh) silicon carbide grains picked up from a
clean @ass plate with a pad of absorbent cotton moistened
with a drop of wash solvent. Wipe vigorously with fresh pads
of absorbent cotton and subsequently handle only with
stainless steel forceps; do not touch with the fingers. Clamp
in a vise and polish the main surfaces with silicon carbide
grains on absorbent cotton. Rub in the direction of the long
axis of the strip, carrying the stroke beyond the end of the
strip before reversing the direction. Clean all metal dust from
the strip by rubbing vigorously with clean pads of absorbent
cotton until a fresh pad remains unsoiled. When the strip is
clean immediately attach to the dip tube and immerse it in
the prepared test bomb.
7.2.1 It is important to polish the whole surface of the
strip uniformly to obtain a uniformly stained strip. If the
edges show wear (surface elliptical) they will likely show
more corrosion than the center. The use of a vise will
facilitate uniform polishing.
8. Procedure
8.1 With valve B (Fig. i), open, place approximately 1 mL
of distilled water into a clean test cylinder and swirl to
moisten the walls; allow the remainder to drain from the
cylinder, insert the freshly polished copper strip suspended
from the hook on the dip tube making sure that the bottom
of the strip is at least 6.4 mm (1/4 in.) from the bottom of the
cylinder when assembled. After assembly of the apparatus,
close both valve A (Fig. i), on closure assembly with outage
tube, and valve B.
8.2 Holding the test cylinder upright so as not to wet the
copper strip with water, attach the sample source to the test
cylinder valve A (Fig. 1) by means of a short length of
flexible aluminum tubing that has been purged with the
sample. Admit some sample to the cylinder by opening the
valve at the sample source and then valve A.
8.3 Close valve A without disconnecting the test cylinder
from the sample source. Invert the test cylinder and open
valve B to purge the air from the test cylinder. Return the
test cylinder to the upright position and drain any residual
liquid through the open valve B. Close valve B with the test
cylinder now in its upright position, open valve A and fill the
test cylinder with the sample. When the test cylinder is full,
close valve A, the valve at the sample source, and disconnect
the aluminum tubing.
8.3.1 Warning-Safe means for the disposal of vapors and
liquids during this and subsequent procedures must be
provided.
8.4 As soon as the aluminum tubing is disconnected, and
with the cylinder in its upright position, open valve A slightly
so that all liquid above the end of the outage tube will be
removed from the test cylinder. When vapor first emerges
from valve A, close valve A.
8.5 Immediately after filling, immerse the test cylinder in
the water bath maintained at 37.8 f 0.5'C (100 f 1'F).
Ailow the cylinder to remain in the bath for 1 h f 5 min.
8.6 At the end of the test period remove the cylinder from
the bath and, holding the cylinder in a vertical position, open
the bottom valve to a suitable disposal unit (8.3.1) until all of
the liquid and most of the vapor is discharged.
8.7 When only a slight pressure remains in the cylinder,
disassemble immediately and compare at once the copper
strip that has been exposed to the liquefied petroleum gases
with the ASTM Copper Strip Corrosion Standards.
8.8 If the copper strip shows any appreciable discoloration, the interior of the cylinder should be polished with steel
wool and washed with wash solvent soon after use so as to be
clean for another test.
9. Interpretation of Results
9.1 Handling only with stainless steel forceps, compare
the exposed strip with the ASTM Copper Strip Corrosion
Standards. Hold both the test strip and the standard in such
a manner that light reflected from them at an angle of
approximately 45" will be observed. In handling the test strip
The ASTM Copper Strip Corrosion Standards approved by Committee D-2
are available from ASTM Headquarters. Request Adjunct No. 12-401300-00.
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3777 W 382qb77 0038537 373
during the inspection and comparison, the danger of
marking or staining can be avoided if it is inserted in a flat
test tube which is then stoppered with absorbent cotton.
10. Report
10.1 Report the results in accordance with one of the
classifications listed in Table I . State the duration of the test
and the test temperature.
10.2 The added distilled water frequently causes isolated
brown spots on the copper strip. The presence of these spots
should be disregarded or the test should be repeated.
11. Precision and Bias
1 1.1 In the case of ordinal classification data, no generally
accepted method for determining precision or bias is currently available.
12. Keywords
12.1 corrosivity; liquefied petroleum gases
TABLE 1 ASTM Copper Strip Classifications
___
Classification
Designation
Description"
Freshly polished strip
...
B
1
Slight tarnish
Light orange, almost the same as
a freshly polished strip
Dark orange
2
Moderate tarnish
Claret red
Lavender
Multicoiored with lavender Mue
and/or silver overlaid on claret
red
Silvery
Brassy or gdd
3
Dark tarnish
Magenta overcast on brassy strip
MultiMored with red and green
showing (peacock), but no gray
4
Conosion
Transparent black, dark gray o<
brown with peacock green
barely showing
Graohite or lusterless biack
Glossy or jet black
A The ASTM Copper Corrosion Standard is made up to strips characteristic of
these descriptions.
8 The freshly polished strip is included in a series only as an indication of the
appearance of a properly polished strip before a test run; it is not possible to
duplicate this appearance after a test even with a completely nonmosive sample.
ANNEX
(Mandatory Information)
Al. PRECAUTIONARY STATEMENT
Al.1 2.2.4 Trimethyìpentane
Keep away from heat, sparks, and open flame.
Keep container closed.
Use with adequate ventilation.
Avoid build-up of vapors and eliminate all sources of
ignition, especially non-explosion proof electrical apparatus
and heaters.
Avoid prolonged breathing of vapor or spray mist.
Avoid prolonged or repeated skin contact.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised. either reapproved or withdrawn. Your commnts are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to lhe ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
STD*GPA STD 2340-ENGL
4cRi
Designation: D 2158
- 92
An Americen National Standard
@ Designation: 317195
Standard Test Method for
Residues in Liquefied Petroleum (LP) Gases'
This standard is issued under the fixed designation D 2158; the number immediately following the designation indicates the year of
onginal 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.
2. Referenced Documents
2.1 ASTM Standards:
D 96 Test Methods for Water and Sediment in Crude Oil
by Centrifuge Method (Field Procedure)2
D 1796 Test Method for Water and Sediment in Fuel Oils
by the Centrifuge Method (Laboratory Procedure)2
D 1835 Specification for Liquefied Petroleum (LP) Gases2
E 1 Specification for ASTM Thermometers3
2.2 Other Documents:
GPA Publication 2 1404
IP Appendix AS
3. Terminology
3.1 Descriptions of Terms Specific to This Standard:
3.1.1 residue-the volume, measured to the nearest 0.05
mL, of the residual material boiling above 38°C resulting
from the evaporation of 100 mL of sample under the
specified conditions of this test method.
3.1.2 R Number -the residue multiplied by 200.
3.1.3 oil stain observation-the volume of solvent-residue
mixture required to yield an oil ring that persists for 2 min
under specified conditions on a prescribed filter paper.
3.1.4 O Number -10 divided by the oil stain observation.
4. Summary of Test Method
4.1 A 100-mL sample of liquefied petroleum gas is
weathered in a 100-mL centrifuge tube. The volume of
residue remaining at 38°C is measured and recorded as is
also the appearance of a fdter paper to which the residue has
been added in measured increments.
5. Significance and Use
5.1 Control over the residue content (required by Specification D 1835) is of considerable importance in end-use
applications. In liquid feed systems residues may lead to
troublesome deposits and, in vapor offtake systems, residues
that are carried over can foul regulating equipment. Those
that remain will accumulate, can be corrosive, and will
contaminate following product. Water, particularly if alkaline, can cause failure of regulating equipment and corrosion
of metals.
6. Apparatus
6.1 Centrifuge Tube, 100-mL graduated, conforming to
dimensions given in Fig, 1. The first 0.5 mL shall be
graduated in 0.05-mL increments. The shape of the lower tip
of the tube is especially important. The taper shall be
uniform and the bottom shail be rounded as shown in Fig. 1.
Tubes shall be made of thoroughly annealed heat-resistant
glass. Volumetric graduation tolerances, based on air-free
water at 2VC, are given in Table 1. Detailed requirements
for centrifuge tubes appear in Test Methods D 9 6 and
D 1796.
6.2 Cooling Coil, a minimum length of 6 m of 5 to 7-mm
outside diameter copper tubing wound to a diameter of 63.5
TABLE i . Centrifuge Tube Graduation Tolerances
Range. mL
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2.H on Liquid Petroleum Gas.
Current edition approved Apr. 15, 1992. Published June 1992. Originally
published as D 2 i 58 - 63 T. Last previous edition D 2 I58 - 89.
2 Annual Book ofASTM Standards, Vol 05.01.
3 Annual Book of ASTM Standards, Vol 14.03.
Available from Gas Processors Assn., 6526 E. 60th St., Tulsa, OK 74145.
Available from Institute of Petroleum, 61 Cavendish St., London. 'VIL4 P 4 R
1
0.0to
0.1
0.1 to 0.3
0.3to 0.5
0.5 to 1.0
1.0 to 3.0
3.0to 5.0
5.0 to 25.0
25.0 to 100.0
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scale,
Limit of
Division.
mL
Error,
0.05
0.05
0.05
0.1
0.1
0.5
1.o
0.02
1.o
mL
0.03
0.05
0.05
0.1
0.2
0.5
1.o
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
1. Scope
1.1 This test method covers the determination of the
extraneous materials weathering above 38°C that are present
in liquefied petroleum gases.
1.2 Liquefied petroleum gases that contain alcohols to
enhance their anti-icing behaviour can give erroneous results
by this test method.
1.3 The result can be expressed in terms of measured
volumes or indices derived from these volumes. In either
case, the test method provides an indication of the quantity
and nature of materials in the product that are substantially
less volatile than the liquefied petroleum gas hydrocarbons.
1.4 This standard does not purport to address all of the
safety problems, 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. For specific
precautionary statements, see 6.9.
Copper Wire
3mm NEEDLE VALVE
d 17 z 1 mmiO
SAMPLE VALVE
6mm
6m OF 5mm O.D. SOFT
COPPER TUBING
METALOR GLASS
COOCINGMSSEL
+ 36.W-37 75 mm O 0
I /
7
-
10 mL
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
I
02-90 mm
NOTE-CO¡IS
in the drawing are extended for clarity.
FIG. 2
Precooling Equipment
*
~ino
oi
inside bottom
FIG. 1
7. Reagents and Materials
7.1 Sofvent-Oil-free, reagent-grade pentane or cyclopentane.
INSIDE TAPER SHAPE
Cone-Shaped Centrifuge Tube, 203 mm
NOTE2-Although pentane is the preferred solvent for use in this
test method, cyclopentane can be substituted for pentane whenever the
ambient temperature or altitude is too high to enable the convenient
handling of pentane.
t 1.5 mm outside diameter, and assembled in a suitable
cooling bath. (See Fig. 2.)
6.3 Syringe, 1-mL (ordinary medical syringe), graduated
in 0.1 mL and equipped with a needle 200 f 5 mm long.
Alternatively, a O. 1-mL pipet may be used.
6.4 Thermometers, conforming to Specification E 1 or IP
Appendix A.
Low Range-Minus 38'C to +50"C
High Range-Minus 20°C to +SUC
8. Preparation of Apparatus
8.1 Wash all glassware that is to be used in the test in the
selected solvent. Add 10 mL of a new sample of solvent to
the centrifuge tube. Mark the center of the filter paper. Fill
the syringe or pipet with a portion of the solvent drawn from
the centrifuge tube and direct 0.1 mL of the solvent to the
mark on the paper. Allow the solvent to evaporate and note
the persistence of an oil ring. Attempt to cover a circle of
about 30 to 35 mm in diameter on the filter paper with each
addition. If no oil ring appears after 1.5 mL of solvent has
been added, the solvent and glassware are satisfactory. The
appearance of an oil ring indicates either improperly cleaned
glassware or contaminated solvent.
1P IC/ASTM 5C
ASTM 57C
NOTEI-When
a thermometer or a water bath, or both, are not
available, for example, a field test, a satisfactory alternative for screening
is to warm the tip of the centrifuge tube with the hand.
6.5 Filter Paper, medium-grade, rapid, white, 125-mm
diameter.
6.6 Solvent Wash Bottle.
6.7 Water Bath, controlled at 38 t 2°C.
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*
6.8 Copper Wire, 1.6 0.1-mm diameter, 300 10-mm
long.
6.9 Clamp, suitable for holding the centrifuge tube during
weathering.
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temperature is above 5°C. If it is necessary to determine the
oil ring at temperatures below 5"C,allow 10 min for oil ring
persistence.
8.2 The presence of an oil ring should be observed by
holding the dry filter paper between the eye and a bright
incandescent light or strong daylight.
8.3 The solvent is added in 0.1-mL increments to confine
the solvent ring to a circle of about 30 to 35 mm in diameter.
The filter paper should be held level during the solvent
addition. One method is to place it on the 250-mL beaker.
NOTE3-As an acceptable alternative to the procedure given in 9.2
for use in those cases where a product specification limit has been
established, continued incremental additions of the solvent-residue
mixture that is equivalent to the limiting specification can be made to
the filter paper and, if no persistent oil ring appears, the result of the test
shall be reported as passing.
9. Procedure
9.1 Residue-Attach
the cooling coil to the sample
source, cool the coil to below the boiling point of the sample,
and flush the coil and sampling line.
9.1.1 Rinse the centrifuge tube with the material to be
sampled and then fill it to the 100-mL mark with a
representative sample.
9.1.2 Immediately insert the copper wire through a clean,
slotted cork or a clean, loose-fitting plug of cotton or
cleansing tissue in the mouth of the centrifuge tube. The wire
helps to prevent superheating and resulting bumping (erratic
or excessive boiling), and the cork (or plug) will keep out air
or moisture while the sample is weathering. If more than 10
mL of the sample is lost because of bumping, obtain a new
sample.
9.1.3 Allow the sample to weather, using artificial heating,
if the ambient temperature or type of sample requires it. If,
when weathering has ceased and the tube has reached
ambient temperature, a residue remains, place the tip of the
tube in a water bath at 38°C for 5 min.
9.1.4 Record the volume of any remaining residue to the
nearest 0.05 mL, and the presence of extraneous matter, if
observed.
9.2 Oil Stain Observation-Add sufficient solvent to the
centrifuge tube containing the residue described in 9.1.4 to
restore the volume to 10 mL. Add the solvent from the wash
bottle and carefully wash down the sides of the tube. Stir well
with the syringe needle or pipet so that any residue at the
bottom of the tube is dissolved uniformly in the solvent.
9.2.1 Mark the center of a clean white filter paper. Fill the
syringe or pipet and direct 1.5 mL of the solvent-residue
mixture at a rate such that the wetted circle is maintained at
about 30 to 35 mm in diameter.
9.2.2 If no oil ring persists after a 2-min waiting period
when holding the dry filter paper between the eye and a
bright incandescent light or strong daylight, discontinue the
test.
9.2.3 If a ring is discernible, determine the volume of the
solvent-residue mixture at which the oil ring first persists for
2 min on a new filter paper by adding the solvent-residue
mixture in O. 1-mL increments.
9.2.4 Record the volume in mL of the solvent-residue
mixture required to yield a persistent oil ring as the oil stain
observation.
9.3 Storage of oil-free solvent in a polyethylene wash
bottle for several days contaminates the solvent. Any solvent
transferred to the wash bottle for purposes of running the test
should either be used in testing during the same day or
discarded.
9.4 It has been noted that at low ambient temperatures
(below about 5°C) materials in the gasoline boiling range will
leave an oil ring that persists after 2 min. Oil ring determinations should be made in a protected area where the
10. Calculation
10.1 R Number-Multiply the volume of residue obtained in 9.1.4 by 200.
10.2 O Number-Divide 10 by the oil stain observation
obtained in 9.2.4. If the oil stain observation exceeds 1.5 mL,
the result is recorded as zero.
11. Expression of Results
1 1.1 Volumetric-The results shall be expressed as:
11.1.1 Residue on evaporation to the nearest 0.05 mL,
and
1 1.1.2 Oil stain observation to the nearest O. 1 mL.
1 1.2 Normalized-The results shall be expressed as:
1 1.2.1 R Number to the nearest 10, and
I 1.2.2 O Number to the nearest 1.
12. Precision and Bias
12.1 Precision is only expressed in terms of the normalized reporting units.
12.2 Repeatability-The difference (r) between successive
test results obtained by the same operator with the same
apparatus under constant operating conditions on identical
test material would, in the long run, in the normal and
correct operation of the test method, exceed the values below
only in one case in twenty:
O Number
r
o to 20
20to 40
4
o to ?O
5
6
40 to 100
8
20 to 40
40 to 60
10
20
r
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
12.3 Reproducibilitjp-The difference (R) between two
test results independently obtained by different operators
operating in different laboratories on nominally identical test
material would, in the long run, in the normal and correct
operation of the test method, exceed the values below only in
one case in twenty:
R
R Number
R
6
o to 20
IO
20to 40
8
40 to 100
I?
20 to 40
40 to 60
20
30
O Number
o to
20
12.4 Bias-The procedure in this test method for measuring residues in LP-Gas has no bias because the residues
are defined only in terms of this test method.
13. Keywords
13.1 liquified petroleum gases; LPG; residue
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S T D - G P A S T D 2LYü-ENGL
1777
=
382Lib79 O O L 8 5 2 L 8T4
(tm
D2158
This standard is subject to revision at any time by the responsible technical cornminee and must be reviewed every five years and
il not revised, either reapproved or withdrawn. Your comments are invited either lor revision of this standard or lor additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical cornminee, which you may attend. If you lee/ that your comments have not received a fair hearing you should make your
views known to the ASTM Comminee on Standards, 1916 Race St., Philadelphia. PA 19703.
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
The American Society tor Testing and Materials takes no position respecting the validity of any paient rights asserted in connection
with any item mentioned in this standard Users 01 this standard are expressly advised that determination of the validity 01 any such
patent rights, and the risk o1 mlringement o1 such rights. are entirely their own responsibility
4”
Designation: D 2163 - 91
An American National Standard
@ Designation: 264/79 (85)
Standard Test Method for
Analysis of Liquefied Petroleum (LP) Gases and
Propene Concentrates by Gas Chromatography’
This standard is issued under the fixed designation D 2163; the number immediately following the designation indicates the year of
onginal 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 (z) indicates an editorial cl-ange since the last revision or reapprovai.
1. Scope
5. Significance and Use
1.1 This test method covers the determination of the
composition of liquefied petroleum (LP) gases. It is applicable to analysis of propane, propene, and butane in all
concentration ranges O. 1 % and above.
1.2 This standard does not purport to address all of the
safety problems, 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.
1.3 The values stated in SI units are to be regarded as
standard.
5.1 The component distribution of liquefied petroleum
gases and propene concentrates is often required as a
specification analysis for end-use sale of this material. Its
wide use as chemical feedstocks or as fuel, require precise
compositional data to ensure uniform quality of the desired
reaction products.
5.2 The component distribution data of liquefied petroleum gases and propene concentrates can be used to calculate physical properties such as relative density, vapor
pressure, and motor octane (see Practice D 2598). Precision
and accuracy of compositional data are extremely important
when these data are used to calculate various properties of
these petroleum products.
2. Referenced Documents
2.1 ASTM Standards:
D 242 1 Practice for Interconversion of Analysis of C5 and
Lighter Hydrocarbons to Gas-Volume, Liquid-Volume,
or Weight Basis2
D 2598 Practice for Calculation of Certain Physical Properties of Liquified Petroleum (LP) Gases from Compositional Analysis3
D 3700 Practice for Containing Hydrocarbon Fluid Samples Using a Floating Piston Cylinder3
3. Terminology
3.1 Definition:
3.1.1 propene concentrate-concentrate
than 50 % propene.
6. Gas Chromatograph System
6.1 Detector-The detector shall be a thermal conductivity type or its equivalent in sensitivity and stability. The
system shall be capable of detecting 0.1 9% concentration of
any component of interest. For calculation techniques utilizing a recorder, the signai for the concentration shall be at
least 5 chart divisions above the noise level on a O to 100
scale chart. Noise level must be restricted to a maximum of 1
chart division. When electronic integration is employed the
signal for 0.1 % concentration must be at least twice the
noise level.
6.2 Recorder-A strip-Chari recorder and integrator with
a full-scale range of 10 mV or less shall be required. A
maximum full-scale balance time of 2 s and a minimum
chart speed of */2 in. (12.7 mm)/min shall be required.
6.3 Arfenuator-A multistep attenuator for the detector
output signal shall be necessary to maintain maximum peaks
within the recorder chart range. The attenuator system must
be accurate to 0.5 % in any position.
6.4 Sample Inlet System-Provision shall be made to
introduce up to 0.50 mL of the sample. The sample volume
must be repeatable such that successive runs agree within 1
mm or 1 9% (whichever is larger) on each component peak
height.
6.5 Temperature Control-The analyzer columns shall be
maintained at a temperature constant to 0.3”C during the
course of the sample and corresponding reference standard
runs.
containing more
4. Summary of Test Method
4.1 Components in a sample of LP gas are physically
separated by gas chromatography and compared to corresponding components separated under identical operating
conditions from a reference standard mixture of known
composition or from use of pure hydrocarbons. The
chromatogram of the sample is interpreted by comparing
peak heights or areas with those obtained on the reference
standard mixture of pure hydrocarbons.
1 This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2.W.03 on C4 Test Methods Liquefied Petroleum Gas.
Current edition approved Oct. 15, I99 l . Published December 1991. Originally
published as D 2163 - 63. Last previous edition D 2163 - 87.
2 Annual Book of ASTM Standards, Vol 05.01.
3 Annual Book of ASTM Standards, Vol 05.02.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
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= 382Lib77
S T D - G P A S T D ZL'iU-ENGL 1 7 7 7
0038523 b77
D2163
TABLE 1 Reference Standard Mixtures, Uquid Volume Percent *
~~
Component
Propane
wdh No
ünsaturates
Propane
wdh Low
4
4
93
a7
Ethane
Propane.
Butane
ProPane-
pro(iene
mopene
Butane
Mixtures
with Low
WithHigh
ROaane
RoOane
2
45
6
0.2
4.8
94.9
30
0.1
...
4
3
57
35
1
1
3
1
3
,..
...
...
64
25
6
...
1
1
1
2
2
...
R O W
n-Butane
Isobutane
Butene
isopentam
A
propene
propane
wdh High
Propene
1
3
...
15
...
...
...
0.1
22.6
76.6
0.5
...
0.2
...
The compositii values recorded in this tabie are offered as a guide to laboCatories preparing their Own mixtures irm pure hydrocerbais or to commeráai suppkrs
of standards. In either case, an accurate composition oi the standards must be known to anaiyst.
7. Calibration Sîandard
7.1 Pure components or calibration standard mixtures4
may be used for calibration. If pure components are used,
identical volumes of each component are injected into the
chromatograph and relative area response factors are determined. These factors are valid for a given instrument and
operating conditions and should be redetermined periodically. If pure components are used for calibration, the
\
FIG. 1 Illustration of AI6 Ratio
6.6 Carrier Gas-The instrument shall be equipped with
suitable facilities to provide a flow of camer gas through the
analyzer column at a flow rate that is constant to 1.0 5%
throughout the analysis.
6.7 Columns-Any column may be used provided all
component peaks for compounds present in concentration of
more than 5 %I are resolved so that the ratio A/B shall not be
less than 0.8,
where:
A = depth of the valley on either side of peak B, and
B = height above the baseline of the smaller of any two
adjacent peaks (see Fig. 1).
For compounds present in concentrations of 5 %Y or less, the
ratio of A / B shall not be less than 0.4. In case the smallcomponent peak is adjacent to a large one, it may be
necessary to construct the baseline of the small peak tangent
to the curve as shown in Fig. 2.
I
FIG. 2
calculation should be made in mole percent and converted to
liquid volume percent mote i). Factors repeatable to within
1 % are required. The concentration of each component in
the calibration standard mixtures shall be known to within
0.1 %. The concentration of the major component in the
calibration standard mixture shall not differ from that of the
like component in the sample to be analyzed by more than
10 % if the peak height method of calculation is used. On
propene concentrates, the calibration standard mixtures shall
not differ from that of like component in the sample to be
analyzed by more than 5 %. Typical composition ranges of
suitable calibration standard mixtures are given in Table 1.
NOTEI-TH Method D 2421 may be used whenever a need exists
for such translations.
8. Procedure
8.1 Apparatus Preparation-Mount the column suitable
for the analysis desired (see Appendix Xi) in the
chromatograph and adjust the conditions to optimum for the
column selected (Table 2). Allow sufficient time for the
instrument to reach equilibrium as indicated by a stable base
line.
8.1.1 The test method allows the user a wide latitude in
choice of instrumentation to make the analysis, and most
commercial instrumentation easily meets the requirements
defined in the test method. However, only by strict
adherence to the calibration procedures outlined in the
method can reproducibility between instruments expect to
be achieved.
8.1.2 Proper maintenance of instrumentation is critical to
continued satisfactory performance of this analysis. Clean
sample containers, clean sample inlet systems and clean
detectors are mandatory to achieve the precision and accuracy capabilities of this method.
NOTE2: Warning-Samples and reference mixtures are extremely
flammable. Keep away from heat, sparks,and flames. Use with adequate
Suitable reference standard mixtures of pure hydrocarbonsarc available from
the Phillips Petroleum Co., Special Products Div., Bartlaville, OK.
Illustration of A/B Ratio for Small-Component Peak
25
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
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TABLE 2
Column
Diameter.
Column
Length, m
Silicon 200/500
Benzyl cyanide-silver nitrate
Hexamethylphosphoramide
Dimethylsuifolane pius benzyl cyanide and
silver nitrate
Dimethylsuifolane
Hexamethyl phosphoramide
Di-n-butyl maleate
Tricresyl phosphate plus silicone, 550
Methoxy ethoxy ethyl ether
Instrument Conditions
mm.OD
Substrate,
Mass, %
Temperature,
OC
Flow
Rate,
mLlmin
Carrier G
60 to 70
45 to 55
60 to 70
60 to 70
helium
helium
helium
helium
30
12
helium
helium
helium
helium
helium
-I
4
9
9
6.4
6.4
6.4
27
90
36
17
40
30
7
6.4
36
35
15
6
4
9
9
6.4
3.2
6.4
6.4
6.4
30
25
28
28
25
25
30
30
35
30
60
70
60
TABLE 3 Piecirion Data for LPG Containing Less Than 50 X Propene
Concentration Range of
C o m m n t s . mol %
O to 70
Above 70
Repeatability
Reproducibility
use repeatability curve in Fig. 3
0.2
use reproducibility curve in Fig. 3
ventilation. Cylinders must by supported at all times. Hydrocarbon
vapors that may be vented must be controlled to assure compliance with
applicable safety and environmental regulations. Vapor reduces oxygen
available for breathing. Liquid causes cold bums.
often be attributed to improper sampling procedures. (See
Test Method D 3700.)
8.3 Preparation ofthe Chromatogram-Obtain duplicate
chromatograms of the sample. Adjust the attenuator at each
peak for maximum peak height within the recorder chart
range. Peak heights of like components shall agree within 1
mm or 1 %
! (whichever is larger). If a reference standard
mixture is used for calibration, obtain duplicate chromatograms of the proper reference standard in a similar
manner. Use the same sample size for all runs.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
8.2 Preparation and Introduction of Sample-Attach the
cylinder containing the gas mixture to the sampling valve of
the chromatograph so that a liquid phase sample is withdrawn. Adjust the flow rate from the sample cylinder so that
complete vaporization of the liquid occurs at the cylinder
valve. (An alternative technique is to trap a sample of only
liquid phase in a short section of tubing, and then permit the
entire sample to vaporize into an evacuated container).
Adjust the ratio of the two volumes so that a gage pressure of
69 to 138 kPa (10 to 20 psi) is obtained in the final container.
Then use this sample for the analysis. Fiush the sample loop
for 1 to 2 min at a flow rate of 5 to 10 mL/min before
introducing the sample into the &er gas stream.
8.2.1 On propene concentrates, the sample may be introduced as a liquid by means of a liquid sample valve or by
vaporization of the liquid as above. On propene concentrates
having a propene content of less than 80 %, only the
alternative technique of trapping a sample of liquid and
vaporizing the entire sample into an evacuated container
shall be used.
8.2.2 Sampling at the sample source and at the
chromatograph must always be done in a manner that
ensures that a representative sample is being analyzed. Lack
of precision and accuracy in using this method can most
TABLE 4
COmpOUnd
Ethane
0.0 to 0.1
0.2
Propene
Propane
Butanes
70 to 77
93 to 95
5 to 7
22 to 29
0.0 to 0.1
0.5
NOTE 3-The use of planimeters or integrators is permissible provided their repeatability has been established and the resulting repeatability does not adversely afiìect the repeatability and reproducibility
limits of the method given in Section 10.
Repeatability Reproducibility
0.02
0.05
0.04
0.38
0.34
1.5
0.33
1 .o
0.04
1
0.04
0.1
0.1
0.2
0.07
0.6
Butenes
9. Calculation
9.1 Peak Height Method-Measure the peak height of
each component and adjust this value to the attenuation of
the same component in the reference standard mixture.
Calculate the percentage by mole or liquid volume of each
component as follows:
Concentration, liquid volume or moi percent = (PJP,)x S
where:
P, = peak height of component in the sample,
Po = peak height of component in reference standard
mixture, and
S = percentage of mole or liquid volume of component in
reference standard mixture.
9.2 Area Method-Measure the area of each component
by multiplying the height of the peak by the width at half
height. The width should be measured with the aid of a
magnifying glass (Note 3). Adjust the area to the attenuation
of the same component in the reference standard mixture.
Piecision Data for Propene Concentrates
Concentration, moi %
1 % oí amount present
0.06
1.o
9.2.1 Calculate the percentage by mole or liquid volume
of each component as follows:
1.o
1.7
0.08
Concentration, liquid volume or mol percent = (AJA,) x S
0.2
where:
A, = area of component in sample,
A, = area of component in reference standard mixture, and
0.3
0.5
0.2
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382Lib99 0 0 1 8 5 2 5 L(L(T
1997
Precision, 95 Percent Confidence Limit
FIG. 3 Precision Curves
percentage by mole or liquid volume of component in
reference standard mixture.
9.2.2 If pure components are used for calibration, calculate the composition as follows:
S
=
Concentration, mol percent
= AJAfl
where:
A , = area of component in sample, mm2, and
A, = area sensitivity of component, mm2 per percent.
9.2.3 Total the results and normalize to 100 %.
9.3 Normalization-Normalize the mole or liquid volume percent values obtained in 9.1 or 9.2 by multiplying
each value by 100 and dividing by the sum of the original
values. The sum of the original values should not differ from
100.0 % by more than 2.0 %.
10. Precision and Bias5
10.1 The data in Table 3 and Fig. 3 shall be used for
judging the acceptability of results (95 9% confidence) on
samples containing less than 50 % propene. The data in
Table 4 shall be used for judging the acceptability of results
on samples containing more than 50 % propene.
1O. 1.1 Repeatabifity-The difference between successive
test results, obtained by the same operator with the same
apparatus under constant operating conditions on identical
test material, would in the long run, in the normal and
correct operation of the test method exceed the values shown
in Table 3 or Fig. 3 and Table 4 in only one case in twenty.
1O. 1.2 Reproducibility-The
difference between two
single and independent results, obtained by different operators working in different laboratories on identical test material, in the normal and correct operation of the test method,
exceed the values shown in Table 3 or Fig.
- 3 and Table 4 in
only one case in twenty.
10.2 Bias-Since there is no accepted reference material
suitable for determining the bias for the procedure in this test
method, no statement on bias is being made.
11. Keywords
5
1 1.1 analysis; liquified petroleum gas
The data from which this precision statement is based are not available.
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S T D * G P A S T D 21'4O-ENGL
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APPENDIX
(Nonmandatory Information)
X1. PARTITION COLUMNS
X1.l The following four partition columns have been
cooperatively tested and found suitable for use with materials
given in the scope of this test method.
X 1.1.1 Silicone 200/500 Column-This column separates
ethane, propane, n-butane, isobutane, n-pentane, and
isopentane and is therefore suitable for analyzing LP gases
free from unsaturated hydrocarbons.
X 1.1.2 Benzyl Cyanide-Silver Nitrate Column-This
column separates isobutane, n-butane, the butenes,
n-pentane and isopentane, and accordingly is best suited for
use with LP gas butane containing unsaturated C, hydrocarbons.
X 1.1.3 Hexamethylphosphoramide (HMPA) ColumnThis column separates ethane, propane, propene, isobutane,
n-butane, the butenes, n-pentane, and isopentane, and accordingly is suitable for use with all types of LP gases.
X I. 1.4 Dimethylsufolane (DMS)-Benzyl Cyanide-Silver
Nitrate Column-This column separates ail components in
commercial LP gases.
NOTEX 1 . 1 -There are commercial suppliers of gas chromatography
equipment and columns who can make (and guarantee) that the
columns they provide will meet the specifications (see 6.7 Columns) of
this test method.
NOTEX1.2: Warning-toxic. Precaution-See the product safety
bulletins from the suppiier of the chemicals used in preparing these
columns or before Benzyl Cyanidasilver Nitrate Column; XI. I .3 Hexamethylphosphoramide (HMPA) column, and X 1.1.4 Dimethylsufolane
(DMS) Benzyl Cyanide-Silver Nitrate Column.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights assmed in connection
with any item mentioned in this standard. Users of this standard are expressiy advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibiiity.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
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 Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical comminee, which you may attend. If you feel that your comments have not received a fair hearing you shouki make your
views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
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S T D - G P A S T D ZLqO-ENGL 1997 M 382Lib77 0038527 2L2 M
Designation: D 2713
- 91
An Amencan N a W Standard
Designation: 395/92
Standard Test Method for
Dryness of Propane (Valve Freeze Method)’
This standard is issued under the fixed designation D 27 13; 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 (6) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the measurement of the
dryness of propane-type products such as, but not limited to,
commercial propane (see Specification D 1835).
NOTE1-This test method is not applicable to propane-type prod-
5. Apparatus
5.1 Propane Water Test Valve3-A specially constructed
and calibrated valve manufactured solely for this test (Note
2). The valve has two open positions, a wide open position
for flushing, and a small preset flow position for testing.
ucts containing antifreeze agents. However, the relative freeze times of
such materials tested by this procedure may be an indication of the
tendency of these products to cause freezing in pressure reducing
regulators.
NOTE2-The propane water test valve is a precision instrument and
it should be so treated. It should not be dropped, strained in any way, or
disassembled, except to clean the filter in accordance with the manufacturer’s instructions. Valves suspected of being defective should be
returned to the manufacturer for inspection, reconditioning or
recalibration.
1.2 This standard does not purport to address all of the
safety problems, if any, associated with its use. It is the
responsibility of the user ofthis standard to establish appropriate safety and health practices and determine the appiicability of regulatory limitations prior to use.
1.3 The values stated in SI units are to be regarded as the
standard. The values in parentheses are for information only.
2. Referenced Documents
2.1 ASTM Standards:
D 1265 Practice for Sampling Liquefied Petroleum (LP)
Gases2
D 183 5 Specification for Liquefied Petroleum (LP) Gases2
3. Summary of Test Method
3.1 A liquid-phase sample of the product to be tested is
flowed through the propane water test valve to cool the valve
body. After cooling, the test valve is partiaily closed to a
small preset flow rate and the time required for the valve to
freeze, and thus interrupt the normal flow, is recorded. The
average observed time for several successive observations is
recorded as the observed freeze time.
4. Significance and Use
4.1 This test is a functional test in which the water
concentration in the product is related to product behavior
characteristics in a pressure-reducing system of special design
to arrive at a measure of product acceptability in common
use applications. Experience has demonstrated that excessive
water content (dissolved water) will cause freeze-up difficulties in pressure reducing systems.
This test method is under the jurisdiction of ASTM Committee D2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2.H on Liquified Petroleum Gas.
Current edition approved March 15, 1991. Published July 1991. Originally
published as D 27 13 - 68 T. Last previous edition D 2713 - 86.
2 Annual Book of ASTM Standards, Vol 05.01.
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5.2 Stop Watch.
5.3 Sample Cylinder, having a minimum capacity of 1 1.4
L (3 gai).
5.4 Cloth, dry, clean.
6. Sampling
6.1 The sensitivity of moisture test measurements to
uncontrollable sampling errors is such as to warrant conducting all important tests at the propane supply source
rather than on samples taken from the bulk supply. Referee
tests should be conducted on the bulk supply.
6.2 If the test cannot be run by connecting the apparatus
directly to the bulk propane supply, a sample can be taken
into a sample cylinder having a minimum capacity of 1 1.4 L.
In such cases, the sample shall be taken strictly in accordance
with directions given in Practice D 1265.
7. Procedure
7.1 Connect (Note 3) the propane water test valve to the
liquid line of the bulk product source or to the liquid phase
connection of the sample cylinder described in 6.2, so that
the body of the valve is horizontal and the outlet opening is
aimed vertically upward. The valve should be positioned so
that the internal surfaces of the outlet opening are clearly
visible to the operator. Open the main valve on the sample
source (Note 4) and set the valve on the test apparatus in the
purge position. Purge the sample line and the apparatus for
15 s. Close the test valve for 2 or 3 s, open it for 2 or 3 s, close
it for 2 or 3 s, and continue this intermittent opening and
closing until a uniform frost cover has accumulated on the
housing around the outlet of the test valve. Snap the valve
closed to the test position and simultaneously start the stop
watch. Stop the watch at the instant the liquid propane
ceases to flow through the valve (Note 4).
A list of supplies of LPGas freeze valves is available from ASTM.
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S T D - G P A S T D 21‘40-ENGL
1997
3 8 2 4 b 9 9 0018528 157
4m D2713
NOTE3-Use only clean, dry pipe or metallic tubing for making this
connection. Do not use mbber hose or plastic lined hose.
record the average time for three consecutive determinations
as the freeze-time.
NOTE 5-Failure to purge the apparatus with the valve open to the
purge position for about i 5 s between tests will give erroneous results.
Purging assures that ice formed in the preset opening in the preceding
test will be removed.
7.2 Sample pressure, at the inlet to the test valve, must not
be more than 100 psi (690 kPa) above the vapor pressure of
the product at the sample temperature. When sample source
pressure is above this limit a liquid propane pressure
regulator must be used to hold the pressure, at the inlet to the
test valve, within this limit.
8. Report
8.1 If the valve does not freeze off within 60 s, report the
product as “pass.”
NOTE4-The instant liquid propane stops flowing through the valve,
frost will form on the internal surfaces of the valve outlet. The watch
should be stopped at this instant. The operator is forewarned of this
instant of stoppage if he will watch the frost line climb and roll over the
lip of the valve outlet.
9. Precision and Bias
9.1 In the case of pass-fail data or results from other
qualitative tests, no generally accepted method for determining precision or bias is currently available.
NOTE6-Data from a series of tests conducted in 1967 indicate the
following: At moisture levels of 14 and 26 ppm, all valves can be
7.3 Disregard the observed time for the initial freeze-off
mn.Quickly wipe the test valve outlet threads with a clean,
dry cloth. Open the test valve to the purge position for about
expected to give freeze times over 3 min; at a moisture level of 49 ppm
it can be expected that none of the valves will give freeze times over I8
s; at a moisture level of 93 ppm it can be expected that none of the
valves wiil give freeze times over 5 s.
15 s to ensure the removal of ice from the preset opening.
Repeat the operations as described in the trial run until three
successive freeze-off times check each other to within +2 s.
For freeze-off times of less than 1 min this may require as
many as seven or eight test runs. If the freeze-off time on
three consecutive test runs is 3 min or greater, the test on the
product can be discontinued and the freeze-off time recorded
as greater than 3 min. For freeze-off times shorter than 3 min
9.2 Bias-The procedure in Test Method D 2713 for
measuring dryness of propane has no bias because the value
of dryness is defined only in terms of this test method.
10. Keywords
10.1 dryness; propane.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the rlsk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
it not revised, either reapproved or withdrawn. Your comments are invhed either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comnients will receive careful consideration at a meeting of the responsibte
tachnical committee, which you m y attend. /i you feel that your comments have not received a fair bearing you should make your
views known to the ASTM CommMee on Standards, 1976 Race St.,Philadelphia, PA 19703.
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STD*GPA STD 2140-ENGL
#Tb
Designation: D 2784
1777
m
3824b77 0038527 075
- 92
m
An American National Standard
Standard Test Method for
Sulfur in Liquefied Petroleum Gases (Oxy-Hydrogen Burner or
Lamp)'
This standard is issued under the fixed designation D 2784: the number immediately following the designation indicates the year of
original adoption or. in the case of revision. the year of last re\ ision. A number in parentheses indicates the year of last reapproval. A
superscnpt epsilon ( e ) indicates an editorial change since the last revision or reapproval.
1 . Scope
1.1 This test method covers the determination of total
sulfur in liquified petroleum gases containing more than 1
pg/g. Specimens should not contain more than 100 pg/g of
halogens.
1.2 To attain the quantitative detectability that the
method is capable of, stringent techniques must be employed
and all possible sources of sulfur contamination must be
eliminated. In particular. cleaning agents, such as common
household detergents which contain sulfates, should be
avoided.
1.3 The values given in acceptable metric units are to be
regarded as the standard.
1.4 This standard does not purport to address all OJ the
safety problems, if any. associated wirh its use. I t is the
responsibilitj. of rhe user ofthis srandard to establish appro-
priare safer!, and healtli practices and determine the applicabilitj3 of regitlatorj, litnirations prior to use.
2. Referenced Documents
2.1 .4STM Slandards:
D i56 Test Method for Saybolt Color of Petroleum
Products (Saybolt Chromometer Method)'
D 1265 Practice for Sampling Liquefied Petroleum (LP)
Gases'
D 1266 Test Method for Sulfur in Petroleum Products
(Lamp Method)'
D 1657 Test Method for Density or Relative Density of
Light Hydrocarbons by Pressure Thermohydrometer'
E I l Specification for Wire-Cloth Sieves for Testing
Purposes'
2.2 Institute of Petroleum S~andard."
IP I8 I Sampling Petroleum Gases, Including Liquefied
Petroleum Gases
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3. Summary of Test Method
3.1 The sample is burned in an oxy-hydrogen burner, or
in a lamp in a closed system in a carbon dioxide-oxygen
atmosphere. The latter is not recommended for trace quanI This test method i s under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2.03 on Elemental Analysis.
Current edition approved March IS. 1992. Published May 1992. Onginally
published as D 2784 - 69 T. Last previous edition D 2784 - 89.
Anniral Book ofAST.11 Siandurds. Vol 05.01.
.4nniral Book O(AST.11 Slandards, Vol 14.02.
Available from Amencan National Standards Institute. I I W. 42nd St.. 13th
Floor. New York. NY 10036.
tities of sulfur due to the inordinately long combustion times
needed. The oxides of sulfur are absorbed and oxidized to
sulfuric acid in a hydrogen peroxide solution. The sulfate
ions are then determined by either of the following finishes:
3.1.1 Barium Perchlorate Titration-The
sulfate is
titrated with barium perchlorate using a thorin-methylene
blue mixed indicator.
sulfate is precipitated as
3. I .2 Turbidimetric-The
barium sulfate and the turbidity of a suspension of the
precipitate is measured with a photometer.
4. Significance and Use
4.1 It is important to have the sulfur content of liquefied
petroleum gases at low enough concentration to meet
government regulations. The presence of sulfur can result in
corrosion of metal surfaces. Sulfur can be poisonous to
catalysts in subsequent processing.
5. Apparatus
5.1 Oxy-Hydrogen Combustion Assemblj-The two types
listed below are recommended. Any combustion apparatus
giving equivalent results, however, is satisfactory.
5.1.1 Wickbold-Tjpe Combustion Apparatirs.s as shown
in Fig. 1.
5. i .2 Modtjìed Beckman Burner-Type Apparatus? as
shown in Fig. 2. Each of the above types of apparatus shall
consist of three parts: atomizer-burner, combustion
chamber, and absorber with spray trap. A blowout safety
port in the combustion chamber is desirable. The remainder
of the apparatus shall consist of a suitable support stand with
the necessary needle valves and flow meters for precise
control of oxygen, hydrogen, and vacuum.
5.1.3 Safety Shield-A transparent shield shall be used to
protect the operator in the event an explosive mixture is
formed in the combustion chamber.
5.2 Apparatus for Lamp Cornbusrion:
5.2.1 Absorbers, Chimneys, and Spray Traps, as required
are described in detail in Annex A3 of Test Method D 1266.
5.2.2 Mangold System, consisting of a vacuum manifold
with regulating device, valves. etc. (Fig. 2 of Test Method
D 1266) and a dual manifold (burner and chimney) supplying a gas mixture of approximately 70 % carbon dioxide
(CO,) and 30 5% oxygen (O,) at regulated pressures. The gas
Available from Koehler Instrument Co., h i . . 1595 Sycamore Ave.. Bohemia.
N Y 117 16. with an all-stainless steel burner. or from Atlas Instrument Co.. 8902 E.
1 Iih St.. Tulsa, OK. For the latter. Hoke No. 993 combination flow meter-vahe
assemblies should be substituted for those supplied.
'Available from Scientific Glassblowing Co.. P.O. Box 18353. Houston. TX
77023.
'
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n-w-l
Water
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.
6.2 Purity of Water-Unless otherwise indicated, references to water shall be understood to mean reagent water as
defined by Types II or III of Specification D 1193. Water
conforming to the following specification is required. Sulfate-free deionized water prepared by percolation of water
through a column of mixed anion and cation exchange
resins.
6.3 Standard Sulfate Solution (1 mL = 100 pg S)-Dilute
6.24 & 0.01 mL of 1 N sulfuric acid (H2S0,) with water to
exactly 1 L. Check the dilution by titration against standard
NaOH solution of about the same normality and adjust the
concentration, if necessary, so that each millilitre of this
solution is equivalent to 100 pg of sulfur.
6.4 Hydrogen (Warning-See Note 2), Carbon Dioxide
(Warning-See Note 3), and Oxygen (Warning-See Note
4), meeting the requirement in Note 17.
LT-*
02
“2
1 -Atomizer-burner
2-Sample tube
3-Combustion chamber
4-Three-way stopcock
NOTE2: Warning-Extremely flammable.
NOTE3: Warning-Gas may reduce oxygen available for breathing.
NOTE4: Warning-Oxygen accelerates combustion.
5-Receiver
6-Spray
trap
FIG. 1 Flow Diagram of a Typical Oxy-Hydrogen Combustion
Apparatus
mixture in the chimney manifold shall be maintained at a
nearly constant pressure of 1 to 2 cm of water and the burner
manifold at approximately 20 cm of water. A suitable
arrangement is shown in Fig. 2 of Test Method D 1266 and
described in A3.6 of Annex A3 of Test Method D 1266, but
any other similar system giving equivalent results can be
used.
5.2.3 Blast Type Gas Burner, having dimensions given in
Fig. 3.
5.3 Vacuum Source, having a capacity of at least 1200
L/h. If a vacuum pump is used, it should be protected by a
suitable trap.
5.4 Corrosion-Resistant Metal Cylinder, 75-mL-It shall
be tested at a pressure of 600 psig (4.14 MPa gage) and shall
show no leaks when filled with air or nitrogen to this pressure
and submerged in water. It shall be fitted with a needle valve
for connection to the burner assembly.
5.5 Variable Transformer, 0-120 V, 750-W.
5.6 Carbon Dioxide Pressure Regulator-This regulator
should be of a type that eliminates the refrigeration difficulties occurring with the pressure reduction of carbon d i ~ x i d e . ~
6. Reagents and Materials
6.1 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
’
Victor Type SR 300, which has been found satisfactory for this application, is
available from Victor Equipment Co., Controls Division, 2336 Auburn Blvd.,
Sacramento, CA 95821.
6.5 Scavenger-Rinse-Mix equal volumes of low-sulfur
acetone and isopropanol.
6.6 Hydrogen Peroxide Solution ( 1.5 %) (1+ 19)-Mix 1
volume of concentrated hydrogen peroxide (H20, = 30 ’%)
with 19 volumes of water. Store in a dark-colored, giassstoppered bottle.
7. Sampling Test Specimens and Test Units
7.1 Obtain the test unit in a container by the method
conforming to the recommendations in Practice D 1265, or
IP Method 181,
7.2 Evacuate a clean, dry 75-mL cylinder and weigh to the
nearest 0.05 g. Connect the container to the inverted supply
cylinder and introduce 24 to 40 g of the liquefied gas, taking
care that the container does not become full of liquid. To
prevent this, bleed off a small amount of the liquid phase of
the material after filling but before reweighing. Reweigh the
cylinder to 0.05 g.
NOTE5-The 75-mL, corrosion-resistant metal vessel can be cleaned
as follows: Remove the needle valve. Wash the interior of the vessel and
valve, first with a sulfur-free hydrocarbon, such as n-pentane, and then
wash with acetone. Dry the interior of the vessel with clean compressed
air and rinse it with HCI (1+10). Rinse the interior with water until the
wash water is neutral to a pH test paper. Wash the vessel with acetone
and ailow to drain at least 10 min. Dry the vessel with a stream of clean,
compressed air and reassemble.
NOTE6-If the weight of liquefied petroleum gas is maintained
below 45 g in a 75-mL container, the container cannot become full of
liquid at room temperature.
* “Reagent Chemicals, American Chemical Society Specifications,” Am.
Chemical Soc., Washington, DC.For suggestions on the testing of reagents not
listed by the American Chemical Society, see “Reagent Chemicals and Standards,”
by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United
States Pharmacopeia.”
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NOTE 1-A means for determining when to replace the exchange
resins should be provided. Use of a simple electrical conductivity meter
has been found satisfactory for this purpose.
ìNLET
FIG. 2
Trace Sulfur Apparatus Flow Diagram
0.05 Circulor Hole
Pione
Surfoce)
46k
O0
All dimensions in millimetres
FIG. 3
8. Procedure for Combustion of Sample
8.1 Connect the sample cylinder with stainless steel tubing
to the gas expansion valve. Attach to this another section of
stainless steel tubing which runs to the vicinity of the burner.
Make the final connection to the burner with sulfur-free
rubber tubing. Wrap the expansion valve with heating tape
and connect this to a variable transformer. Insert a thermometer between the heating tape and expansion valve so
that the thermometer bulb is in contact with the valve body.
See Fig. 4.
8.2 Turn on the variable transfomer and allow the
expansion valve to reach 43°C (1 10°F). Alternatively the
expansion valve may be placed in a suitable metal beaker
and covered with water maintained at 11O"F.
8.3 Oxy-Hydrogen Combustion-Assemble the apparatus
according to the manufacturer's directions (see also 14.1).
Add to the absorber 25 mL of the hydrogen peroxide
solution.
NOTE7: Warning-Before attempting subsequent operations, the
operator should ( 1 ) be aware of the various hazards that can exist
Blast-Type Gas Burner
Stainless Steel
R e l i e f Valve
Stainless S t
Connect ions
P
Regulating Valve Maintained at
\ I O O F by Heoting Tope
(4-f t Length, l 4 0 W , 4 5 V )
Controlled by a Variable Transformer
FIG. 4
Burner Assembly for LPG
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
Attach Burner
Here
~
S T D - G P A S T D 23LiO-ENGL 3777 9 3824b77 0038532 b8T 9
4#
through the improper use of hydrogen as a fuel, and (2) Recautionhave the safety shield in place.
8.3.1 Light the burner and insert into the combustion
chamber. If necessary, readjust gas flows. Open the bottom
valve of the sample cylinder. Slowly open the expansion
valve until an optimum burning rate is achieved.
8.4 Lamp Combustion-Add to the absorber 25 mL of
hydrogen peroxide solution. Assemble the chimney, absorber, and spray trap and connect to the C02-02 and
vacuum manifold. Make the necessary vacuum adjustments
(see 5.1 of Test Method D 1266). Set up a control blank
absorber as in 5.3 of Test Method D 1266.
8.4.1 Open the bottom valve of the sample cylinder.
Slowly crack the gas expansion valve. Light the bumer with
an alcohol lamp, and insert the burner into the combustion
chamber (chimney).
8.5 Bum a quantity of sample in accordance with Table 1.
NOTE8-in burning materials with sulfur concentrations greater
~2784
of sulfur from the sample. Likewise subtract any sulfur
obtained in the lamp combustion blank from the total figure.
8.1 I Disconnect the spray trap from the vacuum line and
thoroughly rinse the spray trap and chimney with about 35
mL of distilled water, collecting the rinsings in the absorber.
It is important that any materials clinging to these parts be
transferred to the absorber to avoid low values for sulfur
content.
BARIUM PERCHLORATE TITRATION FINISH
9. Reagents
9.1 Ion-Free Water-Distill
deionized water and store in
tightly capped, highdensity polyethylene bottles.
9.2 Hydrochloric Acid, Standard Alcoholic (O. 1 M)Dilute 20 mL of aqueous 0.5 M HCl with 80 mL of
isopropanol.
9.3 Inhibited Thorin-Methylene Blue Mixed Indicator
Solulion-The indicator is made up as two solutions and
these mixed together in equal volumes once per week as
follows:
than 50 pug, restrict sample sizes to give quantities that will not contain
more than 250 pg of sulfur for the turbidimetric finish or more than 150
pg for the barium perchlorate finish. Alternatively, aliquots of the
absorber solutions which do not contain more than these maximums
can be used.
NOTE9-Minor adjustment of the gas flow rates can be necessary to
maintain those recommended by the manufacturer.
9.4 Fleisher S Methyl Purple Indicator Solution.l o
9.5 Barium Perchlorate (0.005 M)-Dissolve 1.95 g of
barium perchlorate trihydrate" in 200 mL of water and add
800 mL of isopropanol. Adjust the apparent pH to about 3.5
with perchloric acid, using a pH meter.
9.6 Perchloric Acid," 70 %.
9.7 Sodium Hydroxide, Standard Solutions (0.03 M)Prepare by mixing 7 parts of water with 3 parts of standard
O. 1 M sodium hydroxide (NaOH) solution. Concentrate 400
mL of 0.03 N NaOH solution by evaporating to 30 mL, and
determine any sulfate present in accordance with Appendix
A 1, Turbidimetric Procedure for Sulfate of Test Method
D 1266. If sulfate is found, corrections must be made for any
sulfur introduced by the reagent in the alkali titration
following combustion.
9.8 Methylene Blue.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
8.6 After a suficient quantity of sample has been burned,
turn the bottom valve of the cylinder off. Allow the
remaining gas in the tubing and gas expansion valve to bum
itself out. Turn the heat off on the gas expansion valve.
Disconnect the tubing from the sample cylinder and reweigh
the sample cylinder to the nearest 0.05 g. Leave the absorber
solution in the assembled lamp unit. The same absorber
solution will be used for the scavenger-rinse burning. Allow
the expansion valve to cool to ambient temperature.
8.7 If the oxy-hydrogen burner permits, flush the tubing
and valve with 10 mL of scavenger-rinse and bum without
disconnecting the tubing. Otherwise disconnect the tubing
and bum in the normal liquid mode. For the lamp burning
collect the rinsings in a standard lamp sulfur (see Test
Method D 1266) flask. Insert a standard burner equipped
with a wick into the flask and carry out the combustion as
described in Section 7 of Test Method D 1266.
8.8 For the oxy-hydrogen burners, when all of the rinsings
are consumed, shut down the burner as recommended by the
manufacturer.
8.9 After the rinsings have been burned in the lamp,
remove it, turn off the C02-02 supply, and turn off the
vacuum pump.
8.10 For oxy-hydrogen blank determinations bum a hydrocarbon stock with a very low or nondetectable sulfur
content. Make at least two of these prior to the analysis of
samples with trace sulfur contents to ensure that the blanks
are small and constant. Subtract from the total sulfur figures
any blank so obtained. The remainder is the net micrograms
Solution A: 0.8 g thorin?
0.29 g potassium bromate,
water to make 500 mL,
Solution B O. 16 g methylene blue,
0.2 mL of 0.5 M HCl,
water to make 500 mL.
TABLE 1 Sample Sizes
10. Preparation of Working Curve
10.1 Into separate 30-mL beakers pipet each of the
aliquots of the standard sulfate solution given in Table 2. See
6.3. To each aliquot add sufficient water to make 3.4 mL, 12
mL of isopropanol (total volume 15.4 mL) and 3 drops of
mixed thorin-methylene blue indicator solution. Titrate as
indicated below. For each sulfur level given in Table 2, titrate
three of the corresponding aliquots. Plot the millilitres of
titrant used versus micrograms of sulfur. Draw the best
straight line through points. Check at least two points on the
curved at least every 10 days.
~~
SuMir Content, ppm
S a m p Size, g
Turbidimetric Finish
Barium Perchlorate Finish
45
20
5
30
1 to 5
5 to 10
10 to 50
Available from Hach Chemical Co., Ama. IA.
'OAvailable from Reisher Chemical Co., Benjamin Franklin Station.
Washington,DC 20044.
''Ava¡lable from G. Frederick, Smith Chemical Co., P.O.Box 23344,
Columbus. OH 43223.
10
3
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~~
TURBIDIMETRIC FINISH
Sulfur, gg
AligUOtS, rnL
0.40
0.80
1.20
~
2.40
300
3.00
I I . Procedure for Analysis of Solutions
1 1.1 Quantitatively transfer the absorber contents to a
500-mL Erlenmeyer flask, using ion-free water for rinsing.
Add 2 drops of Fleisher’s methyl purple indicator solution to
this solution and titrate to a faint green end point with 0.03
M NaOH solution (Note 12). Add i mL more of the 0.03 M
NaOH solution to the solution and reduce the volume to 2 to
3 mL by evaporation on a hot plate in sulfate-free environment. (Warning-see Note 11): DO NOT BOIL DRY. Cool
the solution to room temperature and measure its volume in
a 10-mL graduate (Note 12). Adjust the volume to 3.0 mL by
adding ion-free water.
NOTE10: Warning-Do not boil.
NOTE1 I-The volume of sodium hydroxide should not exceed 2
mL. More indicates that the sulfur or halogen content is excessive or
that there is a serious air leak in the apparatus.
NOTE12-For high or completely unknown sulfur contents, the
concentrated absorbent can be quantitatively transferred to a 5-mL
volumetric flask, adjusted to 5 mL, and aliquots used. Each aliquot is
then subsequently made up to 3 mL as in 1I. I. Continue as in I 1.2.
11.2 Transfer the absorbent to a 30-mL beaker, rinse the
graduate and the 500-mL boiling flask successively with two
6-mL portions of isopropanol, and add the rinses to the
beaker.
1 1.3 Pipet 0.40 mL of the standard sulfate solution (40 pg
of sulfur) into the beaker. Add 2 drops of the thorinmethylene blue mixed indicator solution. Adjust the resultant gray-green color by adding 0.1 M HC1 dropwise to
the solution until the color changes to bright green.
1 1.4 The 2-mL buret containing standard barium
perchlorate should have its tip positioned just below the
surface of the solution in the beaker. The solution must be
stirred by a small bar on a magnetic stirrer or with a small
propeller stirrer. A white background and good white light
may be helpful in obtaining a precise end point. Add the
barium reagent at a steady rate of O. 1 mL in 5 (A1) s until the
end point is indicated by a rapid, though slight, color change
from green to a bluish gray (Note 13). Shut off the buret at
the point of greatest rate of color change (Note 14).
NOTE 13-It is helpful to match end point colors with solutions
saved from prior standardization titrations performed within the last 15
min and weil stirred to prevent drop-out of the colored barium sulfate
precipitate. People having a low red-green color sensitivity find that
using the blue light of Method D 156, sharpens the end point very
considerably.
NOTE 14-The end point can be. checked by again adding 40 pg of
sulfur (0.4 mL standard sulfuric acid) and retitrating to the end point.
1 1.5 From the working curve, find the total sulfur titrated
to the nearest 1 pg. Subtract the 40 pg added.
11.6 For blank determinations, repeat the operations in
8.3 and 8.7, and burn a hydrocarbon stock with a very low or
nondetectable sulfur content. Burn for the same length of
time as the sample in the normal liquid mode. Subtract from
the sulfur figures in 11.5 any blank so obtained. This is the
net micrograms of sulfur from the sample.
12. Apparatus
12.1 Photometer-Preferably a spectrophotometer having
an effective band width of about 50 nm, and equipped with a
blue-sensitive phototube for use at 450 nm, or alternatively a
filter photometer equipped with a color filter having a
maximum transmission at approximately 450 nm.
12.2 Absorption Cells, having an optical path length of 5
cm. With use the cells may become coated with a film. To
remove this film, wash the cells with a detergent, using a soft
brush. After cleaning, rinse thoroughly with water.
NOTE15-The procedure as written assumes an absorbance change
of about O. 10 for each 100 pg of sulfur in 50 mL of solution measured in
a 5-cm cell. Photometers employing cells of shorter optical paths will not
give the precision of measurement stated in this method.
12.3 Scoop, capable of dispensing 0.30 k 0.01 g of barium
chloride dihydrate as specified in 13.2.
13. Reagents
13.1 Alcohol-Glycerin Mixture-Mix 2 volumes of denatured ethyl alcohol conforming to Formula No. 3A of the
U.S. Bureau of Internal Revenue or ethyl alcohol (99 % by
volume) with 1 volume of glycerin.
13.2 Barium Chloride Dihydrate (BaCl, 2H,O)-Crystals
passing a 20-mesh (850-pm) sieve and retained on a 30-mesh
(600-pm) sieve conforming to Specification E 1 1.
NOTE16-The crystal size of the BaC1,.2H20 is an important
variable that affects the development of turbidity.
13.3 Hydrochloric Acid ( 1+ 12)-Add 77 mL of concentrated hydrochloric acid (HC1, relative density 1.19) to a 1-L
volumetric flask and dilute to the mark with water.
14. Calibration
14.1 Only by the most scrupulous care and attention to
details can reliable results be obtained by this method. Before
using new glassware and thereafter as required, clean the
glassware with concentrated nitric acid. Rinse three times
with tap water and follow with three rinses of deionized
water. Reserve the glassware for use in this method alone.
14.2 Into 50-mL volumetric flasks introduce, by means of
the buret, 0.25, 0.50, 0.75, 1.00, 1.50, 2.00, 3.00, and 5.00
mL of standard sulfate solution (1 mL = 100 pg S ) . See 6.3.
Add 3.0 mL of HCl (1+12) to each flask, dilute to volume
with water, and mix thoroughly. Prepare a reagent blank
standard in a similar way, omitting the standard sulfate.
14.3 Pour the entire contents of each flask into a 100-mL
beaker. Add by means of a pipet 10 f 0.1 mL of alcoholglycerin mixture and mix for 3 min on the magnetic stirrer.
Select a stirring speed just below that which might cause loss
of sample through splashing. Maintain this speed throughout
the entire procedure.
14.4 Allow the solution to stand undisturbed for 4 min.
Transfer to an absorption cell and measure the initial
absorbance, using water as reference.
14.5 Return the solution to the beaker and add 0.30 f
0.01 g of BaCl,-2H,O crystals, either by weighing this
amount or by using the scoop. Stir with the magnetic stirrer
for exactly 3 min. Allow to stand for an additional 4 min,
transfer to the cell, and again measure the absorbance
relative to water.
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
Preparation of Working Curve
40
80
120
240
TABLE 2
15.5 Convert net absorbance to micrograms of sulfur by
using the calibration curve.
14.6 Following steps described in 14.3, 14.4, and 14.5,
obtain a reagent blank reading by subtracting the initial
absorbance of the reagent blank standard from that obtained
after addition of BaC12.2H20. This reading should not
exceed 0.005.
14.7 Obtain the net absorbance for each standard by
subtracting the initial absorbance and reagent blank reading
from the absorbance obtained in accordance with 14.5. Plot
the net absorbance of each standard against micrograms of
sulfur contained in 50 mL of solution and draw a smooth
curve through the points.
14.8 To detect possible shifts, check the calibration curve
daily by making single determinations.
16. Calculation
16.1 Calculate the amount of sulfur in the sample as
follows:
Sulfur content, pg/g = A/ W
(1)
where:
A = micrograms of sulfur as obtained in 1 1.6 or 15.6, and
W = grams of sample burned.
16.1. I Round the result of the test to the nearest 1 pg/g of
sulfur.
16.2 Alternatively calculate the concentration in units of
grains of total sulfur per io0 ft3 as follows:
R (for propane) = 0.083s
R (for butane) = O. 1 1 1S
(2)
R (for propane-butane mixtures)
= S[0.366(G - 0.5077) + 0.0831
where:
R = grains of total sulfur per 100 ft3 of gas at 15.6'C (60'F)
and 0.10132 MPa (760 mm) Hg,
S = sulfur content, pg/g, and
G = relative density of the mixture at 15.6/15.6'C (60/60'F).
15. Procedure for Analysis of Absorber Solutions
15.1 Drain the absorber solution into a 250-mL beaker
and quantitatively rinse the absorber collecting the rinsings
in the beaker.
15.2 Reduce the volume of the absorber solutions to
about 25 mL by evaporation on a hot plate. Quantitatively
transfer the resultant solution to a 50-mL volumetric flask,
rinsing the beaker with several small portions of water. Add 3
mL of HCl (1+ 12) to the flask, make up to volume with
water, and mix thoroughly.
15.3 Into a 100-mL beaker pour the entire contents of the
50-mL volumetric flask containing the solution to be analyzed. Proceed as directed in 14.3, 14.4, and 14.5.
NOTE18-The derivatives of constants used in the above equations
are based on the following properties of propane and butane:
Specific volume for propane (of the real gas at 60'F
and 14.696 psia), ft3/lb of gas
Specific volume for butane (same conditions as
above)
6.3120
NOTE 19-If the relative density of the mixture is not known,
determine it by Test Method D 1657.
NOTE20-Multiply by 2.2883 to convert grains per cubic foot to
grams per cubic metre. Multiply by 35.31 to convert grains per cubic
foot to grams per cubic metre.
NOTE17-Should the blank reading exceed 0.020, the precision
obtainable will be impaired. If so. make an analysis of the reagents alone
to determine whether the atmosphere or reagents are at fault. Place 30
mL of the H202( i .5 %) in the 50-mL volumetric flask, dilute to the
mark with HCI (1 +2 1 5 ) , and proceed as described in 14.6. If this reagent
blank reading exceeds 0.010, results should not be Considered reliable.
17. Precision and Bias
17.1 The precision of this test method has not been
determined. The responsible subcommittee is attempting to
attract volunteers for an interlaboratory study.
17.2 The bias of this test method cannot be determined
since appropriate reference material containing a known
level of sulfur in liquified petroleum gases is not available.
15.4 Obtain the net absorbance of the analysis solution by
subtracting the initial absorbance and the net absorbance for
the oxy-hydrogen combustion blank or the lamp combustion
(depending upon the apparatus used for combustion) from
that obtained after the addition of BaCI, 2H,O.
-
The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asseI1ed in connection
with any item mentioned in this standard. Users ot this standard are expressly advised that determination ot the validity d any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the respsibie technical commirree and must be reviewed every tive years and
1not revised, either reapproved or withdrawn. Your comments are invit8d either for revision of this standard 01 for additional standards
and should be addressed to ASTM Headquarters. Your comments wi// receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your
views known to the ASTM Commirree on Standards, 7976 Race Sr.. Philadelphia, PA 19703.
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8.45 I5
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
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S T D - G P A STD 2140-ENGL 1997
3 8 2 4 b 9 9 0038535 377
=
GPA STANDARD 2174-93
OBTAINING LIQUID HYDROCARBON SAMPLES FOR ANALYSIS BY GAS
CHROMATOGRAPHY
1. SCOPE
1.1 The specific purpose of this method is to describe the
equipment and procedures for obtaining representative samples
of natural gas liquids and the subsequent preparation of those
samples for laboratory analysis by gas chromatography. The
procedures described in this method may be used for obtaining
samples for analysis by methods other than gas chromatography.
A S A M P L E P R O B E M U S T BE U S E D TO O B T A I N A
REPRESENTATIVE SAMPLE.
2. OUTLINE OF METHODS
2.1 A hydrocarbon fluid sample is transferred under
pressure from a source into a sample container by one of the
following methods:
a. Floating Piston Cylinder Method
b. Water Displacement Method 1 (total H 2 0 removal
replaced by hydrocarbons; 20% displaced for outage)
at the bottom. It is strongly recommended that the samples be
obtained under the supervision of a person knowledgeable i n the
phase behavior of hydrocarbon systems and experienced in all
sampling operations.
3.4 T h e s c o p e of t h i s method does not include
recommendations for the location of the sampling point in a line
or vessel, although the importance of the proper sampling
location cannot be overemphasized.
3.5 A certain amount of information about a sample is
necessary before it can be intelligently handled in the laboratory.
Essential information includes the sample source, sample date,
cylinder identification, sample source pressure and temperature,
ambient temperature, type of analysis required, and the sampling
method used. There may be additional related facts such as
field-determined results and operating conditions which will
assist in the evaluation of the analytical data. This information
must accompany the filled sample cylinder.
- 80%
c. Water Displacement Method 2 (partial H 2 0 removal
-
70% replaced by hydrocarbons; 20% displaced for outage; 10%
remaining in cylinder)
d. Ethylene Glycol Displacement Method (total glycol
removal - 80% replaced by hydrocarbons; 20% displaced for
outage)
NOTE 1: Methods b, C, and d may not be aPP1icable to the analysis
of certain samples containing reactive non-hydrocarbons such as sulfur
compounds, carbon dioxide, etc.
3. GENERAL INFORMATION
3.1 The objective of any sampling operation is to secure, in
a suitable container, an adequate portion of a hydrocarbon fluid
under pressure, having the same composition as the stream being
sampled.
3.2 Particular emphasis should be given to the necessity of
obtaining accurate, representative samples for analysis since
analyses, regardless of the care and accuracy of the laboratory
tests, may be useless if the samples are not valid.
3.3 It is not possible, nor is it the intent of this method, to
provide a procedure that will be applicable for all sampling
situations. T h e s a m p l e s o u r c e h e r e is assumed t o b e a
homogeneous, single-phase liquid. All samples must be
obtained using a probe designed to secure product from the
center one-third of the flowing stream. The location of the
probe fitting should be on the top or side of the line rather than
3.6 If the hydrocarbon fluid samples are to be transported by
common carrier within the United States, the sample containers
must meet the specifications of and be labeled and packaged
according to the Hazardous Materials Regulations of the
Department of Transportation.
3.7 This method assumes all procedures begin with clean,
leak-free sample cylinders. Cylinders must be thoroughly
cleaned prior to sampling with an appropriate volatile solvent or
by following
- manufacturers’ recommendations. The use of
detergentlwater solutions or steam is not recommended for the
cleaning of floating piston cylinders.
3.8 For floating piston cylinders, it is desirable in most
cases to use an “inert” charge gas for the piston cylinder which
is not present in the sample so that a leak in the cylinder itself
can be easily detected during the analysis. The use of natural
gas as a back pressure fluid is not recommended because a leak
across the piston may result in compromising the sample with
hydrocarbons (or other components) which were not actually
present at the source. A method to insure a leak-free cylinder is
to pressure test both sides of the piston cylinder. This is
accomplished by pressurizing the displacement chamber with
inert gas to a typical operating pressure with valve C opened
(see Fig. i). Next, close valves C and D and note the pressure
reading-on gauge N. After a period of five minutes, a decrease
in pressure as indicated at gauge N and a corresponding increase
in pressure at gauge M would indicate a leak across the piston.
A pressure drop only at gauge N indicates a leaky fitting, valve,
gauge, or rupture disc. The inert gas should be removed from
the displacement end and the above procedure repeated for the
sample side. It is also possible to analyze the inert gas side of
37
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SAMPLE
SOURCE
C
PROBE
R1
H
L
SAMPLE
FLOATING
PISTON
INERT GAS
I
CYLINDER+
N
INDICATOR ROD
Figure 1. Typical Visual Indicator Sampling System
design) may prevent the flashed product from returning
original homogeneous mixture.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
the cylinder to determine hydrocarbon concentration if leakage
occurs in that direction. Cylinders should be tcstcd at least on an
annual basis.
3.9 Carc must be exercised when sampling liquids having a
vapor pressure higher than atmospheric pressure to prevent
flashing of lighter components when transferring product from
the source to a sample cylinder, or from a primary sample
cylinder to a secondary cylinder. For floating piston cylinders,
precautions should also be taken to ensure that the inert gas
pressure in the piston cylinder never drops below the sampling
pressure or the product’s vapor pressure at the existing source
temperature, thus preventing flashing of the sample.
Theoretically, the product in the vapor state could be returned to
liquid phase, but the physical restrictions of the piston cylinder
(e.g., rupture disc, valve dead space, and stirring assembly
3.10 Duplicate Samples
3.10.1 When resampling is difficult or impossible, it is
advisable to take duplicate samples as a precaution against
accidental loss. These duplicate samples must be taken using
the same sampling method and from the same sampling location.
The sample sequence should be noted on thc sample information
a&
t.!
4. APPARATUS
4.1 Sample Containers
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S T D * G P A STD ZLqO-ENGL 1777
3824b77 0038537 L b 3
4.1.1 Floating Piston Cylinders
4.1.1.2 The cylinder itself contains a moving piston
equipped with O-rings, teflon rings, or other devices to effect a
leak-free seal between the sample and the pressurizing fluid
while allowing it to move freely within the cylinder. The use of
guide rings is recommended to assure smooth piston travel. The
piston and sealing device must be non-reactive to the sample, the
pressurizing fluid, the cleaning solvents, and expected
corrodants.
TIOR Some types of lubricating fluids will absorb
appreciable amounts of the Cd+ fraction from the gas being
sampled, thus compromising the integrity of the sample. It is
recommended that non-absorbing lubricating greases, such as,
but not limited to DuPont's Krytox AC or AD,be wed to prevent
this difficulty. Further details regarding non-absorbing
lubricating greases can be obtained from the piston cylinder
man ufac turers.
4.1.1.3 All valves and safety devices must meet the
appropriate material and pressure requirements for safe design.
The pressure reliefs may be of spring or rupture disc types.
These allow a partial or complete loss of contents due to thermal
expansion or over-pressurization. Should relieving occur, the
sample should be considered compromised.
4.1.1.4 Some piston-type cylinders are fabricated from nonmagnetic materials such as the 300 series stainless steel. The
piston likewise is fabricated of stainless steel but has magnets
attached to the precharge side of the piston. As the piston moves
the'length of the cylinder, the magnetic field generated by the
magnets flips a series of bi-colored flags. This system, or
systems of similar configuration, indicates the piston position
and the volume of product in the cylinder.
4.1.1.5 Some piston-type cylinders are fabricated with a rod
attached to the piston which extends through the end cap on the
inert gas back pressure chamber with appropriate sealing devices
to prevent the inen gas from leaking. The traveling rod provides
an indication of the piston position and the volume of the
product sample in the cylinder. Again, some variations of this
style may exist.
4.1.1.6 Other types of floating piston cylinders are available
which have no visuai method of determining the sample volume
directly. For these cylinders, a displacement cylinder, cylinder
Y (Fig. 2), is fabricated from metal tubing. This cylinder must
be designed to meet the same pressure requirements as the piston
cylinder and have a volume of no more than 80 percent oí the
pressurizing volume of the piston cylinder.
4.1.2 Double Valve Cylinders
4.1.2.1 Metal sample containers of a type which insure
maximum safety and which are corrosion resistant to the product
being sampled should be used. Stainless steel containers are
recommended to minimize problems of surface adsorption of
heavy components (hexanes and heavier components) and to
minimize the reaction of carbon dioxide or other contaminants
with the container. Sample containers and valves must have a
working pressure equal to or exceeding the maximum pressure
anticipated in sampling, storage, or transportation of the sample
container. Soft-seated valves are preferable to those having
metai-to-metai seats. The size of the container depends upon the
amount of sample required for the laboratory tests to be
performed.
NOTE 2: DOT regulations regarding the use of pressure relief
devices on these cylinders must be followed.
4.2 Sample Transfer System
4.2.1 Transfer lines, valves, and gauges in the transfer
system shall be designed consistent with maximum anticipated
pressure and be resistant to all expected corrodants. (Stainless
steel is preferred.) The transfer lines should have a minimum
diameter of 114 inch (6.35 mm) and be as short as is practical.
The use of filters and dryers is discouraged.
4.3 Composite Sampling Mechanism
4.3.1 A composite sampling mechanism is a device which is
used to obtain a representative sample from a flowing product
stream over a given period of time. The unit consists of a
sample probe, either a flow-through sample injection valve,
whether automatic or manual (see Figures 3 and 4) or a probemounted sample pump (Fig. 5) and utilizes a floating piston
cylinder as its collection chamber. The system must include a
method to mix the product sample in the collection chamber.
This is necessary regardless of whether the original floating
piston cylinder is removed and used for laboratory analysis or a
transfer of the product sample is made into a secondary cylinder
as described herein. (Figure 6 depicts a typical automatic
sampler and the various parts required. Figure 5 depicts a
typical proportional sampler using an injection pump and the
vanous parts required.)
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
4.1.1.1 The container required for this method is constructed
of metal tubing, honed and polished on the inside surface. The
cylinder is preferably closed with removable end caps to provide
access to remove and service the moving piston. The end caps
are drilled and tapped for valves, gauges, and relief valves. The
cylinder is designed consistent with the maximum pressure
anticipated during sampling and to be nonreactive to materials
being sampled, the pressurizing fluid, the cleaning solvents and
the expected corrodants. The volume of the cylinder will
depend on the amount of sample needed for the laboratory
analysis.
UMPLE
PISTON
INERT GAS
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
h
CX!NDER
Y
AIR
(ATMOSPH E RIC
PRESSURE)
Figure 2. Displacement Cylinder Sampling System
4.4 Sample Filters
5. SAMPLING PROCEDURES
4.4.1 The sample filter is an optional device used to protect
the sampling valve from scoring due to h e presence of foreign
contaminants such as metal shavings, dirt, etc., in a NGL
sample. The filter should be of a small total volume, of an
inline-type design, and contain a replaceable/disposable element.
5.1 Floating Piston Cylinder Method
5.1.1 Technique of using a cylinder equipped with visual
indicatorfor liquid phase samples of “spot” or “instantaneous”
type (see Figure 1 )
CAUTION; A filter may introduce error if not handled
properly. The filter should be clean and free of any residual
product from previous samples so that a buildup of heavy-end
hydrocarbon components does not result. (This may be
accomplished by a heatinglcmling process or inert gas purge,
etc.) The filter element should be 15 micron size or larger so
that during the purging process NGL is not flashed, causing
fractionation and bubble formation.
5.1.1.1 With sample side of cylinder evacuated (from
cleaning operation) and valve C open, fill displacement end with
inert gas to a pressure at least 10 psi (69 P a ) above sampling
pressure. Close valve D.
5.1.1.2 Open valve A at sample source and thoroughly blow
out any accumulated material. Close valve A at sample source.
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I
?I
i
r ??
i
-
-+- -
---
-
4-73
S T R U M SAMPLE-
/
PROBE
~~
~~
~
Figure 3. Typical Sample Probe Installation
on Orifice Flange
Figure 4. Typical Sample Probe Installation
for a Pump
5.1.1.3 Connect piston cylinder to sampling source at
valve A.
5.1.1.8 Close valves D, C, and A in that order. Open valve
B to release pressure on the sample line. Disconnect the
cylinder from sample source.
5.1.1.4 With valves B and C closed, open source valve A to
full open position. Observe sample pressure on gauge L. Crack
valve B and fitting at valve C to purge line. Do not allow
pressure L to drop below original sample pressure. Discontinue
purging after a sufficient time and only when liquid product is
present. If the product flashes without leaving a liquid residue at
valve B and the fitting at valve C, the operator must use
judgment in determining when to discontinue purging. Close
valve B and tighten fitting at valve C.
5.1.1.9 Do not take outage or reduce pressure on piston
cylinder. Check valves C and D for leaks, cap valves to protect
threads, prepare sample information tag and box for
transportation as per Department of Transportation or applicable
requirements.
5.1.2 Technique of using cylinder not equipped with visual
indicator for liquid phase samples, via displacement cylinder, of
?spot? or ?instantaneous? type (see Figure 2)
NOTE 3: If the diameter of the indicator rod is of significant size
compared to the piston, then the pressure on the inert gas side will be
5.1.2.1 With sample side of the piston cylinder evacuated
(from cleaning operation) and valve C open, fill displacement
end with inert gas to a pressure at least 10 psi (69 kPa) above
sampling pressure. Close valve D.
slightly higher than the sample side, Le., gauge N will read higher than
gauges L and M. This comment applies to all subsequent comments
regarding equal pressures on gauges L.M and N.
5.1.1.5 Adjust pressure on gauge N to equal pressure L by
releasing adequate inert gas through valve D.
5.1.2.2 Open valve A at sample source and thoroughly blow
out any accumulated material. Close valve A at sample sourcc.
5.1.1.6 With valve D closed, slowly open valve C
completely. There should be no pressure change on gauge N
and pressure at gauges L, M and N should all be equal.
5.1.2.3 Connect piston cylinder X to sample source at valve
A and displacement cylinder Y to piston cylinder. Displacement
cylinder Y should be filled with air at atmospheric pressure. For
proper cylinder sizing refer to Section 4.1.1.6.
5.1.1.7 Partially open valve D,slowly allowing inert gas to
vent to the atmosphere. To prevent flashing, do not allow
pressure M to drop below sampling pressure. Continue the
operation until the indicator designates the cylinder contains
80% by volume of product (following manufacturer?s
instructions).
5.1.2.4 With valves B and C closed, open sample source
valve A to full open position. Observe sample source pressure
on gauge L. Crack valve B and fitting at valve C to purge line.
Do not allow pressure L to drop below original sample pressure.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
Product
flow
meter
Minimum
5 Diameters
/
r
Center-stream
sample probe
injection pump
totalizer
___
f
1 P P ~
I
I
I
4
:
Pulse
divider
circuit
i
1 puise per
"X" bbis.
I
:
114" to îJ2"
tubing
I
1
I
I
I
AC - - - - Power
_---
Power
I
I
I
Pressure
recomer
I
Pressure
regulator
I
k4
Pressure
Check valve
Sample transfer tap
Bleed valve
Figure 5. Typical Proportional Sampler Using an Injection Pump
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PRODUCT
FLOW METER
;L--imTfp
STREAM
SAMPLE
3
TOTALIZER
1
)
-
i
1 PPB
AC
POWER
'
i
r---
c
1 PULSE PER
"x" BELS.
--)---
POWER
INTERPOSER
PROBE
A
FILTER
I
Y
DIVIDER
I
3
--
FLOW-TH RU
SAMPLE
INJECTION VALVE
i
--_--
I
I
4
x-
PRESSURE
TUBING
RECORDER
7
I
INERT GAS
PISTON
SAMPLE
a. SAMPLE
TRANSFER TAP
7
PRESSURE
SUPPLY
VALVE
SAMPLE MIXING DEVICE
Figure 6. Typical Automatic Proportional Sampler
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--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
K
5.1.3.4 All samples must be obtained using a probe. (Refer
to Section 3.3 for specifications and location.) A bypass device
that causes a differential pressure, such as an orifice plate or a
small pump, is used to supply fresh liquid to a location for
filling the sample container, either manually or by use of sample
injection valves. The bypass sample line utilizes short lines of a
small diameter connecting the fresh sample source to the
floating piston cylinder receiver (see Figures 3 and 4).
Discontinue purging after a sufficient time and only when liquid
product is present. if the product flashes without leaving a
liquid residue at valve B and the fitting at valve C, the operator
must use judgment in determining when to discontinue purging.
Close valve B and tighten fitting at valve C.
5.1.2.5 With valve E closed, open valve D and observe
pressure on gauge N. Adjust pressure N to equal pressure L by
slowly venting inert gas through valve E. Close valve E.
5.1.3.5 The floating piston cylinder should be connected to
the purged sample line via the composite sampling device. Inert
gas pressure or appropriate pressurizing fluid should be applied
to the cylinder to force the piston to the starting end of the
sampling cylinder. The inert gas pressure should be maintaincd
at a pressure which exceeds by 200 psi (1379 kPa) the
equilibrium vapor pressure of the fluid sampled under expected
varying temperature conditions. At pressure differences less
than 200 psi (1379 kPa) the chance for erroneous samples
increases.
5.1.2.6 With valve E closed, slowly open valve C to full
open position. There should be no pressure change indicated on
gauge N and pressure at gauges L, M and N should all be equal.
5.1.2.7 Close valve D. Open valve E and properly vent
pressure through valve F. Close valve F.
5.1.2.8 Slowly open valve D, allowing inert gas from
cylinder X to flow into cylinder Y. Observe gauge M so as not
to allow pressure M to drop. Continue operation until-pressure
of all three gauges equalizes. At this point, a volume equal to
cylinder Y has been displaced into cylinder X by the product
sample. Sample cylinder X now contains 80% by volume of
sample, leaving sufficient inert gas space to insure safe storage
and transport.
5.1.3.6 The automatic sample injection valves will require
adjusting to obtain incremental samples at a rate such that the
floating piston cylinder will have adequate capacity to hold the
sample during its period of sampling. Care should be exercised
to prevent overfilling of the sample container so that relieving
does not occur, thus changing the composition of the sample and
creating a serious safety hazard.
5.1.2.9 Close valves D, C, and A in that order. Open valves
B and F. Disconnect displacement cylinder Y. Disconnect
piston cylinder X from sample source.
5.1.3.7 Increasing or decreasing the volume of sample
desired can be accomplished by changing the volume of the
incremental sample obtained with the injection valve and/or by
changing the frequency of the proportioning device which
controls the injection valve.
5.1.2.10 Do not take outage or reduce pressure on piston
cylinder X. Check valves C and D for leaks, cap valves to
protect threads, and prepare sample information tag and box for
transport as per Department of Transportation or applicable
requirements.
5.1.3.8 The sample obtained by the sampler apparatus and
stored in the floating piston cylinder must be mixed thoroughly
by either a mechanical device or a liquid pump and circulating
system,
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
5.1.3 Technique of using floating piston cylinders for liquid
phase samples of “composite” type via manual or automatic
systems (see Figures 5 and 6 )
5.1.3.9 The floating piston cylinder used i n the above
system may be removed from the composite sampling device
after the desired product has been sampled.
5.1.3.1 Automatic proportional samplers take small samples
of the flowing stream proportional to the flow rate. Time
increments may be used only when the flow rate is consmt.
CAUTION: Under no circumtances should the cylindcr be
filled beyond 80% of its capacity with sample.
5.1.3.2 Thorough purging of sample lines, pumps and
connections to the sample cylinder is necessary to avoid
contamination of the sample. Sampler systems should be
designed to minimize stagnant areas which could result in the
sample not being representative of the fluid source.
5.1.3.10 Do not take outage or reduce pressure on the
cylinder. Check valves for leaks, cap valves to protect threads,
and prepare sample information tag and box for transport as per
Department of Transportation or applicable requiremenis.
5.1.3.3 Precautions shall be taken to avoid vaporization in
sample loop lines when operating near the equilibrium pressure
of the liquid. In some instances, it may be necessary to insulate
the sample line and sample container, or control the pressure or
temperature of sample containers containing volatile materials.
5.1.3.11 If it is not possible to disconnect the primary
floating piston cylinder from the automatic system, the sample
may be transferred to a secondary floating piston cylinder. Once
the sample in the primary cylinder is adequately mixed, proceed
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S T D - G P A S T D ZLVO-ENGL 1997
as in step 5.1.1, treating the primary cylinder as a flowing
source. (In this particular transfer situation, as sample is
withdrawn, the master sample container will partially
depressurize. The product vapor pressure al the existing master
sampler temperature must be maintained or exceeded to prevent
flashing.)
5.2 WaferDisplacement and Ethylene Glycol Displacement
Methods - Total displacement
5.2.1 A double valve sample cylinder filled with clean
ethylene glycol or water and a vessel to measure the displaced
liquid are required for these two methods (see Figure 7).
3824b99 0038543 4b5
Ethylene glycol must be the glycol t y p used. Water must have
a pH between 5.0 and 7.0. Water with a pH greater than 7.0
must be acidified to bring the pH within the proper range. (0.1
N H2SO4 is a satisfactory acid solution.)
5.2.2 The total volume of the sample cylinder must be
found, then 80% of the total volume should be calculated. (For
example, if the total volume of the cylinder is 500 ml, then 80%
of the total volume is 400 mi.)
5.2.3 Open valve A at sample source and thoroughly blow
out any accumulated material. Close valve A at sample source.
L
SAMPLE
SOURCE
["i
rl
CYLINDER
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
GRADUATED
CYLINDER
b
Figure 7. Liquid Displacement Sampling
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S T D * G P A S T D 2 L 4 0 - E N G L 1997
3 8 2 4 b 9 9 00118544 3 T L
m
5.2.4 Connect the sample cylinder to sampling source at
valve A exactly as shown in Figure 7.
5.3.3 Open valve A at sample source and thoroughly blow
out any accumulated material. Close valve A at sample source.
5.2.5 With valves B, C, and D closed, open sample source
valve A to full open position. Observe sample pressure on
gauge L. Crack valve B and fitting at valve C to purge line. Do
not allow pressure L to drop below original sample pressure.
Discontinue purging after a sufficient time and only when liquid
product is present. If the product flashes without leaving a
liquid residue at valve B and the fitting at valve C, the operator
must use his judgement in determining when to discontinue
purging. Close valve B and tighten fitting at valve C.
5.3.4 Connect the sample cylinder to sampling source at
valve A exactly as shown in Figure 7.
5.3.5 With valves B, C, and D closed, open sample source
valve A to full open position. Observe sample pressure on
gauge L. Crack valve B and fitting at valve C to purge line. Do
not allow pressure L to drop below original sample pressure.
Discontinue purging after a sufficient time and only when liquid
product is present. If the product flashes without leaving a
liquid residue at valve B and the fitting at valve C,the operator
must use his judgement in determining when to discontinue
purging. Close valve B and tighten fitting at valve C.
5.2.6 With valve D still closed, slowly open valve C to full
open position. Pressure at gauges L and M should be equal.
5.2.7 Slowly open valve D to allow a slow discharge of the
glycol or water displacement liquid into the measuring vessel.
To prevent flashing, do not allow pressure M to drop below
sampling pressure. Continue operation until 80% by volume of
the displacement liquid has been displaced by product in the
sample cylinder.
5.3.6 With valve D still closed, slowly open valve C to full
open position. Pressure at gauges L and M should be equal.
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
5.3.7 Slowly open valve D to allow a slow discharge of the
water into the measuring vessel. To prevent flashing, do not
allow pressure M to drop below sampling pressure. Continue
operation until 70% by volume of water has been displaced by
product in the sample cylinder.
5.2.8 Close valves D, C and A in that order. Open valve B
to release pressure on sample line.
5.3.8 Close valves D, C, and A in that order. Open valve B
to release pressure on sample line.
5.2.9 With sample cylinder still attached to source valve A,
slowly open valve D to drain the remaining 20% displacement
liquid from the sample cylinder. After 1 5 ml has been
withdrawn, the operator should reduce the drain rate and
carefully extract the remaining water or glycol. (The
displacement liquid may become cloudy just prior to the end
point, although the effect is less noticeable with glycol.) At this
time, reduce the rate to 10 ml/min maximum. When the first
indication of product appears, usually a flashing bubble, close
valve D immediately with no further loss of product.
Disconnect cylinder from sample source.
5.3.9 With sample cylinder still attached to source valve A,
slowly open valve D to drain another 20% of the water from the
sample cylinder. (At this point, 10% of the water still remains in
the sample cylinder.) Disconnect sample cylinder from sample
source.
5.3.10 Check valves C and D for leaks, cap valves to protect
threads, prepare sample information tag and box for
transportation as per Department of Transportation or applicable
requirements.
5.2.10 Check valves C and D for leaks, cap valves to protect
threads, prepare sample information tag and box for
Uansportation as per Deparunent of Transportation or applicable
requirements.
6. LIQUID PHASE LABORATORY HANDLING AND
PREPARATION
6.1 Recommended Procedures for Liquid Phase Samples
Prior to injection of the Sample into the Test Device
5.3 Waier Displacement Method - Partial Displacement
6.1.1 Floating Piston Cylinders
5.3.1 A double valve sample cylinder filled with clean water
and a vessel to measure the displaced liquid are required for this
method (see Figure 7). The water used must meet the same
requirements as in 5.2.1.
6.1.1.1 For floating piston cylinders refer to Figure 8 and
proceed as follows: Connect a source of inert gas to valve A so
that pressure may be applied to the sample via the floating
piston. Apply a pressure not less than 200 psi (1 379 kPa) above
the vapor pressure of the sample at the temperature of the
sample injection valve by opening the valve on the inert gas
source ard valve A. The inert gas pressure is to be maintained
5.3.2 The total volume of the sample cylinder must be
found; then 70% and 20% of the total volume should be
calculated. (For example, if the total volume of the cylinder is
500 ml, then 70% of the total volume is 350 ml and 20% is 100
mi.)
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S T D n G P A S T D 2140-ENGL L997
3824b77 0018545 238
CAUTION: Extreme care must be used to ensure that no
flashing of sample occurs in the inlet sampling line and valve
system. Any measurements should be taken al sample purge
valve C , never at sample valve B . The sample line and valve
system should remain at 200 psi (1379 kPa) above the vapor
pressure of the product.
on the sample container at all times during the analysis via a
prcchargc regulator or similar device.
6.1.1.2 The sample should be thoroughly mixed per the
cylinder manufacturer’s recommendations, whether it be by
“mixing dasher”, “mixing ball” or equivalcnt, immediately prior
to each analysis.
6.1.1.6 Operate the liquid sample valve either manually or
automatically to inject the liquid sample into the carrier gas flow
immediately ahead of the chromatographic column. The sample
injection valve should be actuated quickly and smoothly to place
the sample onto the column all at once and to ensure continuous
carrier gas flow through the column.
6.1.1.3 Connect the sample end of the cylinder, valve B, to
thc inlet of the chromatograph liquid sample valve. A l l
connections and tubing are to be made of material impervious to
the sample composition with the smallest diameter and shortest
length of plumbing practical, thereby minimizing “dead space”.
All tubing between the sample cylinder and liquid sample valve
should be the same diameter.
6.1.1.7 When sample injection is complete, close valves B
and A in that order, then close valve on inert gas source. Slowly
open valve C and vent any remaining unused sample in the
system through an appropriate vent.
6.1.1.4 With valve C closed, open valve B to fill the sample
valve and associated lines.
6.1.1.8 Disconnect the cylinder from the inlet of the
chromatograph liquid sample valve and the inert gas source.
6.1.1.5 Slowly crack valve C to purge the sample valve and
associated lines. Be sure sufficient volume is displaced to purge
unmixed areas in the sample cylinder as wcll as the sample
injection system. When the purge is complete, close valve C.
6.1.1.9 If the sample is to be reused, do not take an outage
I
‘111.
CARRIER
CARRIER GAS
CHROMATOGRAPH
LIOUIDVALVE
UMPLING
l
FLOATING PISTON
l PRESSURE
N G RNEEDLE
q bVALVE
[
1
1
r
CYLINDER
NEEDLE VALVE
CYLINDER
OUTLET VALVE
NEEDLE
VENT VALVE
o
GAS
RELIEF
VALVE
VALVE
INERT
GAS
1
1
NGL
RELIEF
VALVE
Figure 8. Repressuring System and Chromatograph Valving with Floating Piston
47
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
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or reduce pressure on the piston cylinder. Check valves for
leaks, cap valves to protect threads, and store the cylinder in a
suitable location.
6.1.2 Double Valve Cylinders
6.1.2.1 For double valve displacement cylinders, refer to
Figure 9 and proceed as follows: Connect the sample cylinder Y
to cylinder X so pressurizing fiuid can enter into the bottom of
cylinder Y. (The pressurizing fluid should be same type used to
secure the product.) With this configuration the hydrocarbon
sample will be taken from the upper portion of the cylinder.
Open valve A and pressurize cylinder X w i t h inert gas.
Maintain a pressure at least 200 psi (1379 kPa) above the vapor
pressure of the hydrocarbon sample at operating conditions.
Open valves B and C to admit pressurizing fluid into sample
cylinder Y.
6.1.2.2 Mix the sample thoroughly by gently inverting
cylinder Y several times. Fix cylinder Y in a vertical position by
means of a ringstand or similar device. Allow it to remain
immobile in the vertical position at least 2 minutes before
injection of sample into the chromatograph.
6.1.2.3 Connect the sample outlet valve D on cylinder Y to
the inlet of the chromatograph liquid sample valve. A!l
connections and tubing are to be made of material impervious to
the sample composition, utilizing the smallest diameter and
VENT VALVE
PRESSURE
REGULATOR
r c
CHROMATOGRAPH
LIQUID SAMPLING
CARRIER
GAS
CARRIER GAS
l
l
I
CYLINDER
->
CYLINDER
'Y
-- -- -- LAYER
NGL -
--- -- --
.
.......
.......
.. .. .. .. .. ....
..'GLYCOL' :
;., OR "
. WATER
.-*GLYCOL' :
: . OR
.. WATER
$AS
.,o.
o
e
o.
.*
.:
. . . . ..
. . . .
Figure 9. Repressuring System and Chromatograph Valving with Double Valve Displacement Cylinder
48
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
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shortest length of plumbing practical, thereby minimizing “dead
space”. All tubing between the sample cylinder and liquid
sample valve should be the same diameter.
6.1.2.10 Check the valves for leaks, then cap valves io
protect the threads and store the cylinder in a suitable location.
7. SAFETY PRECAUTIONS
6.1.2.4 With valve E closed, open valve D to fill the sample
valve and associated lines.
6.1.2.5 Slowly crack valve E to purge the sample valve.
When the purge is complete close valve E.
CAUTION: Extreme care must be used I O ensure that no
flashing of sample occurs in the inlet sampling line and valve
sysrem. Any measurements should be taken at sample purge
valve E , never at sample valve D . The sample line and valve
system should remain at 200 psi (1379 kPa) above the vapor
pressure of the product.
6.1.2.6 Operate the liquid sample valve either manually or
automatically to inject the liquid sample into the carrier gas flow
immediately ahead of the chromatographic column. The liquid
sample valve should bc actuated quickly and smoothly to place
the sample onto lhe column ail at once and to ensure continuous
carrier gas flow through the column.
6.1.2.7 When sample injection is complete, close vaives D
and C on cylinder Y and valves B and A on cylindcr X, in that
ordcr, then closc the valve on the inert gas source. Slowly open
valve E and vent any remaining unused sample in the system
through an appropriate vent, (If the sample is to be reused
immediately, do not take an outage or reduce pressure on the
sample cylinder. If the sample is not to bc reused immediately,
procecd to next step, 6.1.2.8.)
6.1.2.8 Disconnect cylinder Y from the inlet of t h e
chromatograph liquid sample valve and disconnect from
cylinder X. Disconnect Cylinder X from the inert gas source.
6.1.2.9 With cylinder Y remaining in the upright position,
remove 20% by volume of the pressurizing fluid for outage.
This is accomplished by slowly opening valve C to allow a slow
discharge of the pressurizing fluid into a measuring vessel.
7.1 Sampling hydrocarbon fluids can be hazardous. Persons
responsible for obJning samples should be familiar wilh and
adhere to safc practices for handling flammable fluids under
pressure.
7.2 In all cases, a 20% (or more) inert gas charge should be
present in all floating piston cylinders and a minimum of 20%
displacement fluid outage in all double valve sample cylinders.
7.3 Disassembly of the Piston Cylinder
CAUTION; D i s a s s e m b l y of the p i s i o n cylinder f o r
maintenance requires special precautions. If either end cap is
removed while pressure is on the cylinder, the end caps and he
piston can be ejected with such a force as I O cause serious injury
to personnel and damage to adjacent equipmenl.
7.3.1 Clamp the piston cylinder firmly to a steady work
surface. Caution should be taken not to dent or bend the
cylinder by applying excessive pressure.
7.3.2 Using a suitable venting apparatus (e.g. vent hood),
properly vent both ends of the cylinder before attempting to
remove either end cap.
7.3.3 The work surface at either end of the cylinder should
be clear before the end plug is loosened.
7.3.4 Provide a mechanical plunger to dislodge the piston
from the cylinders, provided the plunger is of suitable material
as to not scratch the cylinder bore. Do not use fluid Dressure to
flislodnethe piston,
KOTE 4: For reproducible sample volume limils see GPA
publication 2177.
49
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Copyright Gas Processors Association
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PROPANE DRYNESS TEST
(Cobalt Bromide Method)
tube which in turn shall be partially surrounded by a
metal shield. The glass tube shall be sealed at its inlet
end to a pipe fitting and at the other end to a fine
capillary orifice which serves as the outlet. See Fig. 2.
The moisture indicators may be purchased ready for
use or they may be prepared as follows: The cotton
plugs shall be shaped and sized to fit in the glass tube
loosely. Each plug shall be Fpyoximately ?'
in.
i
long. After soaking in a szturated solution of
cobaltous bromide the plugs shall be placed in a test
tube or flask and dried. Drying is accomplished by
heating to a temperature not to exceed 212 F while
simultaneously evacuating the container. When properly
dried the plugr; will be green or blue. They may be
stored in sealed bottles or a desiccator, but the preferable method is to encase each plug in a separate gelatin
capsule.
(b) Pressure Gage. An accurate pressure gage of
suitable range and scaIed in single pounds shall be
provided.
(c) Needle Valve. The needle valve required shall
be capable of accurately controlling the flow of gas
through the equipment with a minimum of adjustment.
(d) Ice Bath. The ice bath shall consist of a container filled with water and cracked ice to a depth sufficient to immerse the cooling COU and all but the tip of
the attached indicator. The temperature of the ice bath
shall be maintained within a range of 32-34 F.
(e) Cooling Coil. The cooling coil shall consist of
at least 2 feet of % in. O.D. copper tubing coiled so
that it may be conveniently immersed in the ice bath.
The inlet of the coil. shall extend well above the bath
and shall be fitted with a suitable connection to accommodate the pressure gage and needle valve. The
outlet of the coil shall point upward so that when
attached to the indicator it can be readily immersed up
to within
in. of the tip of the indicator.
(i) Caps or Plugs. Adequate caps or plugs shall
be provided for the inlet and outlet of the assembly
to prevent moisture from entering the apparatus when
the test is not being performed.
SCOPE
1. This test is intended to give an indication of the
dryness of Commercial Propane and Propane HD 5.
APPARATUS
2. The apparatus shall consist of the following:
(a) The Indicator. The indicator is essentially a
device for intimately contacting a gas or vapor with
finely divided cobaltous bromide under conditions such
that the color of the cobaltous bromide may be observed
at all times. The indicator shall consist of a lightly
folded plug of cotton impregnated with cobaltous
bromide. Thio plug of cotton shall be held in a glass
r-----
R
?
i
$
SAMPLïNG
FIG. I-ASSEMBLED
3. All tests shall be conducted with the apparatus
connected directly to the vapor space of the tank, tank
car or tank truck containing the propane to be tested,
except in cases where local conditions will not permit.
In such cases a dry sample container having a minimum
capacity of 20 gallons shall be used and a liquid sample
of not less than 70 per cent nor more than 80 per cent
of the volume of the sample container shall be obtained.
APPARATUS'
'The required protective cap (see parogroph 2(f)) like that
shown on top of the Indicator wos not shown at the base of the
needle volve for reasons of sketch clarity.
50
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Copyright Gas Processors Association
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S T D - G P A S T D 2LLiO-ENGL
1777
m
3824b77 0038547 9 8 3
Chah
16 Threads R r Inch
--````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`---
lhu13 Threadr
Per Inch
on
'window
Both Sides
7
Cotton Impregnated With
Cobaltous Bromide
A
Glass Tube 1.0. 3/1{
0.0.*y64
v4* Natlonal Plpe Threads
SECTION 8 - 8
MATERIAL
Make From 5/< Hex Brass Bat,
Except Cap To Be Made From
Dlameter Brass Bar.
s/14
SECTION A-A
Finlrh
FIG. 2-DETAIL
OF INDICATOR
51
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- Whlte
Nickel
____
S T D - G P A S T D 2L40-ENGL 1777
ASSEMBLY OF APPARATUS
4. la) The apparatus shall be assembled as shown
in Fig. 2. The needle valve shall be attached to a vapor
outlct of the propane container by means of suitable
pipe or tubing connection of minimum length.
(b) The ôssembled coil and indicator shall be adjusted to a vertical position. The ice bath shall then
be placed in such a position that the coil and all but
rpproximately 1,- in. of the tip of the indicator will
be immcrsed.
PRECAUTIONS
5. (a) All tubing and fittings must be absolutely
dry and free of oil or foreign matter, CO that the
indicator will not be contaminated or the results of
the test obscured.
(b) Keep the caps or plugs on the inlet and outlet
of the asrembly at all times when the apparatus is not
in use and remove the cap on the outlet orifice only
when the actual testing is in progress.
(c) The final color of the indicator will be the
original blue, lavender or pink. Extreme care shall
be exercised in distinguishing blue from lavender color
as any change from the original blue color indicates a
marginal moisture content..
=
=
from the outlet of the indicator.
(b) The needle valve, Fig. 1, shall then be carefully
opened until the pressure gage registers 50 -C 2 pounds
per square inch and shall be edjusted i o maintain this
pressure for the duration of the test. If the container
pressure is less than 50 psig secure a sample as outlined
in Sect. 3.
(c) If the original blue color persists for 30 minutes
of test exposure, the pressure shall then be reduced to
7 pounds t 2 pounds for five minutes. If the original
blue color persists throughout this period, the material
shall be reported as being “dry.” If the color changes
to lavender or pink at reduced pressure, then the
material shall be reported as being “wet.”
(d) If the color changes to lavender or pink during
the 30 minutes of test exposure at 50 f 2 pounds per
square inch (it may occur in a few minutes), the
material is either “wet” or the tubing and fittings contain water. To determine the cause of the color change.
the pressure on the apparatus shall be adjusted to 5
pounds per square inch or less.
(1) If the indicator turns blue it can be assumed
that the tubing and fittings are free of water and
the material shaii be reported as being “wet.”
(2) If the indicator remains lavender or pink
it can De assumed that the tubing and fitti I .s contain water. The apparatus and r.onnections shall be
dried and the test repeated.
TEST PROCEDURE AND INTERPRETATION
6. ia) The valve on the source of propane vapor
to be tested shall be opened and the cap removed
52
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382Lib99 0018550 b T 5
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