GPA 2140 - Liquefied Petroleum Gas Specifications and Test Methods

S T D - G P A S T D 2140-ENGL 1777m 3 8 2 4 b 7 7 0038475 7 8 2 m 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 --````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale, 08/21/2007 09:17:10 MDT 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. --````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 1 Licensee=UK LOCATION/5940240005 Not for Resale, 08/21/2007 09:17:10 MDT 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 --````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`--- 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. 11 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale, 08/21/2007 09:17:10 MDT 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. ... 111 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale, 08/21/2007 09:17:10 MDT --````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`--- 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. S T D - G P A S T D Z L q O - E N G L 1997 Tt = 3 8 2 q b 9 9 0018499 5 2 8 - + 0' 0'0' e n E= Tt xa com in- $32 :?i a v1 I I I I I I u 3& I .. .. . .. .. . --````,,```,,,```,`,,,,,`,,````-`-`,,`,,`,`,,`--- .. .. . 1 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale, 08/21/2007 09:17:10 MDT 1. Because of the hazards involved. I.1 A liquid sample is transferred from the source into a sample container by purging the container and filling it with liquid. A suitable material is stainless steel. Onginally published as D 1265 .1. then providing 20 % outage so that 80 % of the liquid volume remains.. obtain liquid samples by a procedure which has been agreed upon by the contracting parties.Regulations for Transportation of Explosives and Other Dangerous Articles. or reissues. The size of the container depends upon the amount of sample required for the laboratory tests to be made. 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. Typical sample containers are shown in Figs. liquefied petroleum gases should be sampled by. The sample container should be fitted with an internal outage (ullage) tube to permit release of 20 95 of the container capacity. in containers other than those used in laboratory testing apparatus. Scope 5. 2 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.1.87. skill. Published May 1992.. the number immediately following the designation indicates the year of onginal adoption or. It is therefore essential that the samples be representative of the product to be tested. 1 Obtain samples of the liquid phase only. 3. “I. 10.1 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. They must be supplemented by judgment. Vols 05. The test results are often used for custody transfer and pricing determination..0I. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.1.STD=GPA STD 2140-ENGL 1777 W 3824b77 O O L B C O O 0 7 T (& Designation: D 1265 . and sampling experience. They are not intended for obtaining samples to be used for compositional analysis.1 Samples of liquefied petroleum gases are examined by various test methods to determine physical and chemical charactenstics. Apparatus 6. NOTE l-Practice D3700 describes a recommended method for 5.`. 6.`.2 This standard does not purport to address all of the safety problems. A number in parentheses indicates the year of last reapproval. Vol 05...`.Last previous edition D 1265 .02. If it is not practicable to agitate a mixture for homogeneity. --````. 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.`. determinations of mercaptans and hydrogen sulfide.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. 1. 1992. a liquid sample may be taken from any part of the vessel. 5... associated with its use. for example.`--- 3. 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. General Information 1.6 Hydrocarbon vapors vented during sampling must be controlled to assure compliance with applicable safety and environmental regulations.. or under the supervision of. Referenced Documents 2.. 5 . especially if the material being sampled is a mixture of liquefied petroleum gases. 1. butane.3 When the material being sampled has been agitated until uniformity is assured. Summary of Practice 5. 5. I . Significance and Use 4.53 T. otherwise. 2 Annual Book of A S T M Standards. 2. or mixtures thereof.`. if any. a liquid sample may be taken from any part of the vessel.4 Because of wide variation in the construction details of containers for liquefied petroleum gases.H on Liquefied Petroleum Gas..````-`-`. in the case of revision. A sample procedure that avoids changes in composition must be used for compositional analysis.5 Directions for sampling cannot be made explicit enough to cover ail cases. The following factors must be considered: 5.```. Cumnt edition approved March 15.1 Sample Container-Use metai sample containers of a type that ensures maximum safety and are resistant to corrosion by the product being sampled. Extreme care and good judgment are necessary to ensure samples which represent the general character and average condition of the material.1 Considerable effort is required to obtain a representative sample.” its supplements. the year of last revision. 1 and 2. If the container is to be transported..C. The end of the container fitted with the outage (ullage) tube shall be clearly marked.2 When it is definitely known that the material being sampled is composed predominantly of only one liquefied petroleum gas. 4. it is difficult to spec$ a uniform method for obtaining representative samples of heterogeneous mixtures. 08/21/2007 09:17:10 MDT . 5. it must often conform to specifications pubfished in Tariff No.1 This practice covers the procedures for obtaining representative samples of liquefied petroleum gases such as propane. persons familiar with the necessary safety precautions.```.C. obtaining a representative sample of a hydrocarbon fluid and the subsequent preparation of that sample for laboratory analysis. can be misleading. 3 Annual Book of A S T M Siandards. ... 1 Typical Sample Container and Sampling Connections OUTAGE VALVE A (UiiAGE)TUBE VALVE D FIG.````-`-`..```.G P A S T D 2140-ENGL 1777 382qb77 0018501 T u b (m D1265 VALVE OUTAGE (UIlAGE)TüBE --````..S T D .```.`.`.`--- INLET VALVEC * SOURCE SAMPUNO VALVE Ht u - VEKi VALVE B FIG.`.`....`. 2 Typical Sample Container and Alternate Purging Connections 3 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. 08/21/2007 09:17:10 MDT .... 9.. immerse in a water bath and check for leaks.S T D = G P A STD 2 L V O . 1. 11 Checking for Leaks 1 1. and fill container with the sample. is required.2. use the following purge procedure: 8. 2). 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.2 Close valves B.1 Place samples in a cool location as soon as possible. PA 19103. 8.1 Immediately after obtaining the sample. Your comments will receive careful consideration at a meeting of the responsible technical committee.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. The most satisfactory line is one equipped with two valves on the sample-container end.1. 8. 12.. Close the control valve A. Open vent valve B. Close the control valve A and allow part of the sample to escape in the vapor phase through outlet valve 10.````-`-`. discard the sample and refill the container.`.`--- 12. 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.. Protect the valves on the sample container. and inlet valve C. and a vent valve.`. are entirely their own responsibil@. 6.. B. Close inlet valve C and the valve at the product source. Fig.. open inlet valve C. 1) and both valves C and D closed. PROCEDURE 7. Keep them there until all tests have been completed. Fill sample container until liquid issues from valve C. or both. Open inlet valve C and partly fill the container with sample by slowly opening the outlet valve D.2 If the history of the sample container contents is known. If you feel that your comments bave not received a fair hearing you should make your views known to the ASTM Committee on Standards. Repeat the purging operation at least three times. If a leak is detected at any time during the sampling operation. After the pressure is fully reduced. 1916 Race Sî.1.2 Sample TransJer Line made of stainless steel tubing or other flexible metal hose.```. 1. Open valve A and then valves C and D. which you may attend. close vent valve B and inlet valve C and open control valve A.1 Open outlet valve D slightly.1. vent valve B. so that accidental unseating of the valve or tampering with it is avoided. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. 10. disconnect sample container from the transfer line. use the following purge procedure: 8. A. Allow excess liquid to escape and close the valve at the first sign of vapor.4 Return the sample container to position valve C at the top.`. Care of Samples --````. Fig. and the risk of infringement of such rights. If no liquid escapes.. then valve A on the sampling line.1 Connect the ends of the transfer line securely to the product source and to the inlet valve C of the container.1 After eliminating the excess liquid so that only 80 % of the sample remains.`.```.. discard the sample. Sample Outage (Ullage) 10.1 With the container in an upright position. Philadelphia. 1. Purging the Sample Container 8.E N G L 1997 m 3 8 2 4 b 7 9 OULA502 942 m D1265 D..1 Close vent valve B. LPG. open the control valve A. 08/21/2007 09:17:10 MDT .1 liquified petroleum gases. Discard any samples in containers which develop leaks. either reapproved or withdrawn. Transfer of Sample 9.1 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. 9. Users of this standard are expressly advised that determination of the valid@ of any such patent rights... 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. impervious to the product being sampled. Purging Sample Transfer Line 7. C.1.1.. Fig. 8. Open the valve at the product source and purge the transfer line by opening the control valve A and the vent valve B. 13 Keywords 13. 4 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. Close valves C and D.1. Open valves C and D and drain out liquid. either by packing the container in a crate in an approved manner or by using a protective cap. 8.. 8.1 Position the sample container securely in an upright position with outlet valve D at the top (Fig. a control valve. and its outlet valve D at the top. Repair or replace the leaky container before obtaining another sample. Close outlet valve D and release the remainder of the sample in the liquid phase by opening vent valve B.`.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. place the container in an upright positioin with the outage (ullage) tube at the top. and D. Tighten connection to sample transfer line and repeat the purging operation at least three times. Vol 14. associated with its use.8"C (100°F) up to and including a test temperature of 70'C (1 58°F)..````-`-`.S T D .3 The values stated in acceptable metric units are to be regarded as the standard. Available from Applied Science Publishers. is reported as the LPG Vapor Pressure at the selected test temperature. For specific hazard statements. 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.. as a safety precaution. 5. 2. and customer utilization equipment to ensure safe handling of these products. shipping containers. is purged with a portion of the sample which is then discarded.3 For liquefied petroleum gases. in the case of revision. Ripple Rd. I vapor pressure-the pressure exerted by the vapor of a liquid when in equilibrium with the liquid.```. and whose gage vapor pressure at 37. Eswx. in which the content of hydrocarbon compounds of higher boiling point than 0°C (32°F) is less than 5 % by liquid volume.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. if any.. Similarly. at some higher test temperature up to and including a test temperature of 70°C (158°F).03. Terminology 3. are completely described in Annex A 1. The apparatus is then filled completely with the portion of the sample to be tested. and the various items of auxiliary equipment.. 5. the year of last revision..8"C (100°F) is not greater than approximately 1550 kPa (225 psi). Referenced Documents 2.`. the number immediately following the designation indicates the year of original adoption or. The apparatus is then immersed in a water bath maintained at the standard test temperature of 37. Because of this interchangeability. 6. consisting of two interconnected chambers and equipped with a suitable pressure gage.`. 5.1 This test method covers the determination of the gage vapor pressures of liquefied petroleum gas products at temperatures of 37. This test method is under the jurisdiction of ASTM Committee D-2 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2.1 Information on the vapor pressures of liquefied petroleum gas products under temperature conditions from 37.. 1.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 5 Licensee=UK LOCATION/5940240005 Not for Resale. and fuel systems will not be exceeded under normal operating temperature conditions. 1. A superscript epsilon ( e ) indicates an editorial change since the last revision or reapproval. vapor pressure is an indirect measure of the most extreme low temperature conditions under which initial vaporization can be expected to occur.1.01. 3 Annual Book ofASTM Standards.2 The observed gage pressure at equilibrium. (Warning-see Note i ) butanes and butylenes. Originally published as D 1267 . 4.. Last previous edition D 1267 .```.1 Vapor Pressure Apparatus. the hydrostatic test specified in A1.2 The air chamber of Test Method D 323. A number in parentheses indicates the year of last reapproval. Harmful when inhaled. The values in parentheses are for information only.53 T. Scope 1. 3. optionally.G P A S T D 2340-ENGL 3997 W 3824b77 0038503 889 W Designation: D 1267 .`. after correcting for gage error and correcting to a standard barometric pressure. flammable. It can be considered a semi-quantitative measure of the amount of the most volatile material present in the product. Barking. Current edition approved April 15... Published June 1995. handling. 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.1 The test apparatus.. Vol 05.4 of this method.`. 1. constructed as illustrated in Fig. or both. the apparatus assembly of Test Method D 323 must pass.1 Definition: 3.`. Significance and Use 5.1. 2 Annual Book of ASTM Standards. England --````. 6.1. may be interchangeable with the upper chamber of this method.H on Liquefied Petroleum Gas.8 to 70°C (1O0 to 158°F) is pertinent to selection of properly designed storage vessels. 08/21/2007 09:17:10 MDT .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 2.6 before using same in testing liquefied petroleum gas. Summary of 'Test Method 4.1. Apparatus 6. 1995. see Note 2 and Annex A2.. or both.1 liquejied petroleum gases-narrow boiling range hydrocarbon mixtures consisting chiefly of propane or propylene..2 Description of Term Specific to This Standard: 3.89. the liquid chamber (two-opening type) of Test Method D 323 is interchangeable with the Bt 20 % lower chamber Annex A1.2 This standard does not purport to address all of the safety concerns. A1. NOTE 1 : Warning-Extremely 4.2.8'C (100°F) or.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 1267.2 Institute of Petroleum Standard: IP 181 Sampling Petroleum Gases4 3. it is necessary that the procedural steps of providing free space in the apparatus be completed promptly. in the apparatus to escape until the apparatus is full of liquid. the bleeder valve closed. 9.1. shake it vigorously.2. leading to possible rupture of the chamber.i LP-gas vapor pressure = corrected vapor pressure. 8. Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 6 Licensee=UK LOCATION/5940240005 Not for Resale. record the pressure reading as the Uncorrected LP-Gas Vapor Pressure of the sample at the test temperature. psi .3 to a standard barometric pressure of 760 mm (29. clean thoroughly. Close the lower chamber inlet valve and open the bleeder valve to its wide.. 9.) Hg by means of the following equation: 10. Calculation i O.l"C (0.. the straight-through valve between the two chambers open. prior to this operation.. connect the inlet valve of the lower chamber to the sample source with the sampling connection (7.1 At test temperatures of 50°C (122°F) or below. and purge the parts in a stream of dry air. If liquid appears immediately. Close the inlet valve as soon as no more liquid escapes.. tap the gage lightly and observe the pressure reading. --````.4. and then return it to the bath. then invert the assembly.3) proceed to 9. now containing only vapors. 9.l.1 Safe means for the disposal of vapors and liquids during this operation and in the subsequent sampling operation must be provided. Throughout the determination. and immediately open the straight-through valve (Note i). Record any correction thus determined as gage correction. or IP 18 1.`. 10.2 Observe the apparatus assembly throughout the test period to ensure freedom from leaks.At test temperatures above 50°C (122"F). at intervals of not less than 2 min.````-`-`. and expel any residual material through the bleeder valve.4 Vapor Pressure Determination: 9. NOTE 2-Transfer of the sample is facilitated by chilling the appa- 10. 9. Close the valve on the sample source. momentarily open the bleeder valve. Open the sample source valve to the apparatus.(760 . Sampling and Sample Handling 7. invert it. 7. At the end of 5 min compare the readings of the two gages.1).3.2). maintain the bath at t0.3 Without removing the pressure gage from the apparatus or the apparatus from the bath. Allow the residual vapors to escape until the pressure in the apparatus is essentially atmospheric. Sampling Petroleum Gases.`. Tubing.3"C (0.. invert. to the bleeder valve outlet and open the bleeder valve. Return the apparatus to its normal upright position and immerse it in the constant-temperature water bath maintained at the test temperature (4. A flexible tubing connection of a satisfactory type greatly facilitates the purging and sampling operations. close the straight-through valve and again open the inlet to permit expulsion of the lower chamber contents. 9. kPa . with the apparatus in an upright position. As soon as no more liquid escapes from the lower chamber.3. or both. Immediately close the straight-through valve between the two chambers and open the inlet valve.2 Convert the corrected vapor pressure = (test gage reading) (gage correction) as calculated in 9. 9. 8. close the bleeder and inlet valves in that order (Note 2). Discontinue the test and discard the results at any time a leak is detected. As soon as the apparatus attains essentially the same pressure as the pressure of the sample source. is satisfactory for this purpose.1333 (1) = corrected vapor pressure.1.```.2).1 Samples shall be obtained and stored in accordance with Practice D 1265. must be immersed.2 Purging-With the assembled apparatus in an upright position.(760 .2 Any method of coupling the vapor pressure apparatus to the sample source can be employed..`--- 9.92 in.2"F). Since any warming of the apparatus would cause expansion of the liquid content of the upper chamber. previously calibrated against a dead-weight tester. The apparatus including the bleeder valve coupling. and with the proper range pressure gage attached.3 The upper chamber.P i )0. 9. repeat the purging step (9.2 After 5 min have elapsed. if consecutive observed gage readings are constant.5"F). Procedure 9.`.4). the temperature of the water bath shall be checked periodically by means of the bath thermometer. attach a test gage. and made of material corrosion-resistant to the products being sampled. 9. The tubing should be a conducting material or constructed with a built-in ground connection to minimize the effect of static electricity. These operations will normally require 20 to 30 min to ensure equilibrium.) in diameter.2 Assemble the apparatus with the inlet valve of the lower chamber open.3.4.4.7. up to and including 70°C (158'F).0193 (2) where: + ratus with a portion of the material under test.1 If the apparatus has been used for testing products other than the type of product to be tested. Preparation of Apparatus 8. 08/21/2007 09:17:10 MDT . permitting the air or vapors.`.. then close the bleeder valve.2 When using the 20 9% lower chamber (Appendix A I. but not the pressure gage. Thereafter. 6 to 7 mm (*/4 in.1 Invert the apparatus and shake it vigorously. withdraw the apparatus from the bath. of suitable-working pressure. and disconnect the sampling line... unless the test samples can be taken directly from the source of the material to be tested..P i )0.3 Sampling-Return the apparatus. withdraw the apparatus from the water bath. Allow the contained liquid to evaporate until the apparatus is covered with white frost (may require more than one chilling).```. close the inlet valve and immediately open the straightthrough valve. If liquid does not promptly emerge.`. Perform the shaking operation quickly to avoid excessive cooling of the apparatus and its contents. Prior to each removal of the apparatus from the water bath. After this time. of minimum length. disassemble.4.. to its normal upright position and open the inlet valve. 9.1 When using the 33% 9% lower chamber (Aí.4. i Correct the Uncorrected LP-Gas Vapor Pressure for gage errors. i . is liquid full at some temperature that is normally below the environmental temperature. Cautiously open the bleeder valve on the upper chamber. and then return it to the bath.open position. 9. maintain the bath at +O. shake it vigorously.4.4. ) inlet valve. Precision and Bias 12.1.```.1.3 Conversion Factors: 1 kPa = 7.8 psi) 12.295301 in. the volume of the lower chamber is considered as that which is below the "straight-through" valve closure.. consisting of two chambers. A 1..G P A S T D 2L40-ENGL 1777 m 382qb79 0018505 b5L m D 1267 PI = observed barometric pressure.97 to 2. gage.2. including the portion of the coupling attached to the upper chamber.2).1.1 Repeutabiliry-The difference between two test results.(29.6 Hydrostatic Test-The assembled chambers shall be certified by the manufacturer to withstand approximately 6920 kPa (loo0 psi) gage hydrostatic pressure without permanent deformation. kPa .```.. are identical with those of Test Method D 323 with the exception of the 33V3 % lower chamber. The volume above the "straight-through" valve closure..l (e)) shall be provided to receive the bleeder-valve assembly and the pressure gage.) in diameter and 254 f 3 mm ( I O t l/8 in...) valve fitted into the side of the bleeder-valve coupling (Fig. Al. 12.49 12 (3) (4) where: P2 = observed barometric pressure. 1 (e)). exceed the following value only in one case in twenty: 19 kPa (2. 12.3).03603 in.7 15 1 mmHg = 2. 10.. inside dimensions. AI. 7 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.`. A l . In one end of the lower chamber.92 P2) 3. Report 11.03 (Note A 1. 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. A l .1 The following shall be used as a basis for judging the acceptability of results (95 % probability).`--- Al. 08/21/2007 09:17:10 MDT --````.l (g)) having a minimum internal channel of 13 mm (Y2 in.1. The lower end shall be threaded to fit into the end fitting of the upper chamber.2 LP-gas vapor pressure - = corrected vapor pressure. Al. Although the test procedural details are different.4 Lower Chamber. 1-In determining the volumetric capacities of the chambers. Hg (5) (6) (7) 11. a suitable bleeder-valve coupling (Fig.) in diameter shall be provided for coupling with the lower chamber. psi .````-`-`.3864 = corrected vapor pressure. shall conform to the following requirements. vapor pressure ANNEXES (Mandatory Information) Al. exceed the following value only in one case in twenty: 12 kPa ( 1.) in diameter shall be provided to receive a suitable straight-through valve (Fig. and the upper end shall be threaded to receive the gage coupling (Fig.`. is considered as a part of the upper chamber volume. Al. A 1. 33V3 % (Fig.1. excluding the bleeder-valve assembly. 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.`.. liquified petroleum gases. 20 % (Fig.) in length.) in diameter.S T D . as shown in Fig.05 (Note A 1.. in. Al..l) (d)) shall be a normal 6 mm (V4 in. I A1.95 to 4.1 Upper Chamber-This chamber.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.1 (c). Hg 1 psi = 5 1.3-The apparatus requirements for this method.2 Bleeder.8 psi) 12.1 Report the LP-Gas vapor pressure test results in terms of kilopascals to the nearest 5 kPa or pounds per square inch.3 Lower Chamber.2) (Note A 1. 1 (h)). designated as the upper and lower chambers. APPARATUS FOR VAPOR PRESSURE OF LIQUEFIED PETROLEUM (LP) GASES .1. 1 Vapor Pressure Apparatus. an opening approximately 19 mm (3/4 in. NOTEAl . Keywords 13. 10. in the normal and correct operation of the test method. 1. NOTEAl. 13. 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.(29. Care shall be taken that the connections to the end openings do not prevent the chamber from draining completely.6).50064 mmHg = 0. On one end of the chamber.`.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. to the half unit. To maintain the correct volume ratio between the upper and lower chambers.1. with the inner surfaces of the ends slightly sloped to provide complete drainage from either end when held in a vertical position.1 natural gas liquids..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. A I .92 .P2)0. mm Hg. The volume ratios of the chambers are determined in accordance with the procedure outlined in the Appendix of Test Method D 323. the units shall not be interchanged without recalibrating to ascertain that the volume ratio is within satisfactory limits. In the other end of the chamber an opening approximately 13 mm ( V 2 in. The other end of the chamber shall be equipped with a nominal 6 mm ( Y 4 in. Hg. 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.Valve Assembly-The bleeder-valve for purging the apparatus (Fig.2. A I .`. and the test temperature. A 1. shall be a cylindrical vessel 51 f 3 mm (2 k in. A 1. the assembled vapor pressure apparatus shall be checked for freedom from leaks by filling it with air. The range shall be governed by the test temperature of the test being used as follows: Test Temperature ThermomThermometer Range 'C "C eter No.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. shown in Fig.. 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 (2.2"F).```.....`.l"C (0.) in diameter from the Bourdon tube to the atmosphere. nitrogen. The range and graduations of the pressure gage used shall be governed by the vapor pressure of the sample being tested. and then completely immersing it in a water bath. 3.`. kPa (psi) O to 700 (100) O to 1750 (250) O to 3500 (500) considered inaccurate.4 (0.THROUGH VALVE) PLINGI VALVE COUPLIPJG 1 l L F( I N L E T VALVE) --````. shall be a Bourdon-type spring gage of test gage quality 114 to 140 mm (4% to 5% in.5) Licensee=UK LOCATION/5940240005 Not for Resale..Weight Tester-A dead-weight tester of satisfactory range shall be provided as a means for checking the accuracy of vapor pressure gages. l (a).2"F).. (2) Test temperature above 50°C (122'F). Graduations.5 Dead.4.`.7 Checking for Freedom from Leaks-Before placing new apparatus in service. or other similar gases. 08/21/2007 09:17:10 MDT . to 3460 kPa (500 psi) gage pressure. natural gas.3"C (0. A l . 1.. A 1. ( S T R A I G H T . the appropriate bath thermometer shall be immersed to the test temperature mark on the thermometer scale throughout the vapor pressure determination. 35 to 40 18C 34 to 42 50 to 80 65C 50 to 80 Numbered Intermediate Intervals. In order to check the bath temperatures.5"F).2 Pressure Gage-The pressure gage. kPa (psi) kPa (psi) 70 (IO) "F 172 (25) 7 (I) 344 (50) 35 (5) 95 Only accurate gages shall be continued in use.`. +0.) male thread connection with a passageway not less than 5 mm (Y16 in.```. Only apparatus that will stand this test without leaking shaii be used. +O.`. as follows: Gage to Be Used LP-Gas Vapor Pressure.D1267 ' 1G . A 1. l Typical LPG Vapor Pressure Apparatus A I . kPa (psi) gage at test temperature 655 (95) and under 620 (90) to 1750 (250) 1660 (240) to 3460 (5001 Scale Range.`--- FIG. the gage shall be 8 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS "F to 105 18F 94 to 108 125 to 175 65F 122 to 176 A 1.) in diameter provided with a nominal 6 mm (V4 in. When the gage correction exceeds 2 96 of the scale range... I ) within the range as follows: ( I ) Test temperature 50°C (122°F) and below. and as often as necessary thereafter. A l . A 1.````-`-`.4 Thermometers-Only thermometers conforming to specificationsin Specification E 1 or IP Standard Thennometer Specificationsshall be used. 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.6 Avoid prolonged breathing of vapor or spray mist.. are entirely their own responsibility.3 A2..`. of ignition.1.1..`. and open flame.. PA 19103.... 9 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.1. Keep away from heat.`.5 Avoid buildur.. --````. Use with adequate ventilation. which you may attend. and the risk of infringement of such rights. 1916 Race St.. A2. either reapproved or withdrawn. Philadelphia. 08/21/2007 09:17:10 MDT . PRECAUTIONARY STATEMENT A2.```.1 A2.1. Your comments will receive careful consideration at a meeting of the responsible technical committee.1.````-`-`.`. Users of this standard are expressly advised that determination of the validity of any such patent rights. Keep container closed....```.~ ~~ ~ STDmGPA S T D 21LiO-ENGL 1777 m 382Lib77 0038507 LI2LI m D 1267 A2. sparks.7 Avoid prolonged or repeated skin contact. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters.1 ProDane/Butane. A2.`.2 A2. A2. or Mixture of Both .1.`--- 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.4 I Vapors can cause flash fires. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. especially nonexplosion-proof electrical apparatus and heaters. of vapors and eliminate all sources A2.1. the temperatures t .4m Designation: D 1657 . or in relative density with a wide range from 0. 4Apparatus suitable for this test may be obtained from: EG&G Chandler Engineering. the units of mass and volume used. 6. Scope 1.. --````. crazing. graduated in density with a range from 500 to 650 ks/m3. the year of last revision.. isobutylene. 1989.. Vol. propylene...500 to 0. NOTE1-Attention is drawn to the hazards encountered when working with liquefied petroleum gas or light hydrocarbons. lo5 Pa = 1 bar = 1.1 The apparatus is purged with a portion of the sample before filling with the portion to be used for testing.. to clean the cylinder thoroughly after each determination. and no attack is expected from butadiene and acetaldehyde. Inc.1 Dejnitions: 3.```.`. The hydrometer reading and the temperature of the sample are noted.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 . relative density 60/60'F. The requirements of any national. pentane.`. or etching. Ontario NIK 1C2.03. Inc. 1.1 density-the mass of the liquid per unit volume at a temperature t. Replace any cylinders that show signs of fogging. operations.1 This test method covers the determination of the relative density or density of light hydrocarbons including liquefied petroleum gases (LPG). A supemript epsilon (e) indicates an editorial change since the last revision or reapproval. Peter Peterson Scientific Glassblowing. 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 . OK 741 12. Users are cautioned. Last previous edition D 1657 . for example. and regulatory requirements. (The SI unit of pressure is the pascal: 1 Pa = 1 N/m2.89 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 1657.1 Thermohydrometers.````-`-`.39 T. making it difficult or impossible to read the hydrometer. The ends shall be tightly sealed with neoprene gaskets and metal end plates as shown in Fig. the number immediately following the designation indicates the year of original adoption or. 12th St. 08/21/2007 09:17:10 MDT .. 38th St. and equipment. ethylene. Apparatus4 6. butane. and conforming to the dimensions given in Table 1. When reporting the relative density. kg/m3 at fC. Vol 14.. Guelph. normal butylenes. or domestic safety code should always be strictly observed. for example. should be explicitly stated. 1. 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. Tulsa. in the case of revision.3 The values in SI units are to be regarded as the standard. NOTE3-Certain compounds attack plastics and cloud the inner 2. 05.2.2. 1.01.) 4. 1. 473 Elmira Rd. Although this determination does not describe any particular performancecharacteristic.. 3.1 Caution-A protective shield shall be placed around the plastic or glass cylinder.`. Current edition approved March 31.. surface of the cylinder. however. Annual Book of ASTM Standards. together with the temperature. Published May 1989. and Refinery Supply Co.2 Hydrometer Cylinder.4 MPa (1 4 bar) at the test temperature. Annual Book of ASTM Siandnrds. but other temperatures may be employed for t.4 This standard may involve hazardous materiais. and t2 should be explicitly stated. This standard does not purport to address all of the safety problems associated with its use. 6. 7707 E.1. NOTE2-When reporting the density. Referenced Documents 2. Significance and Use 5. made of glass. constructed of giass or transparent plastic. The standard 6.. propane.`--- 6.. 10 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. storage. conforming to the design and dimensions given in Fig. The values in parentheses are for information only. K on Density.. 1.650. 0 2 . 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. Tulsa. Onginally published as D 1657 . 5. Terminology 3. The standard reference temperatures are 15°C and 60°F. density or relative density can be used to indicate approximate component concentrations in liquefied petroleum mixtures.```. reference temperatures in general use are 15'C and 60'F for both tl and t2.2 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.2 The prescribed apparatus should not be used for materials having vapor pressures higher than 1. A number in parentheses indicates the year of last reapproval. OK 74145.`.. isobutane..`.83 (1988)''. poly(methy1 methacrylate) or equivalent material.. cracking.1. for example.1 The density or relative density of light hydrocarbons and liquefied petroleum gases is determined to satis@ transportation. 1. and isopentane. Tests showed no attack by ethane. to the mass of an equal volume of pure water at a temperature t2. Summary of Test Method 4.. local. The pressure cylinder is filled to a level at which the enclosed hydrometer floats freely.01972 k&cm2.1 ASTM Standards: D 1250 Guide for Petroleum Measurement Tables (ASTM 1250/API 2540/IP 200)2 E 100 Specification for ASTM Hydrometers3 3.. 6901 E. 7.. pure grade.1. OF Scale length. having a nominal density of 584..50699.001 125 to 145 Thermometer Scale 30 to 90 total 1 5 10 0. which shall be bored to provide a vapor outlet from the pressure cylinder. OF Scale error at any point not to exceed. close the outlet and vent valves and open the inlet valve.6 kg/m3 at 15'C or a relative density 60/60"F of 0.1. Open the outlet valve and purge the sampling connections by opening the inlet valve slightly. 7. kg/m3 Scale error at any point not to exceed.4 MPa (14 bar).. Sampling 8. the vent valve can be opened slightly to permit complete filling of the cylinder and then closed.001 0. 8.650 Hydrometer Total length.5 1400 Hvdrometer Scale Standard temperature.2 n-Butane.`.5 Range. Nominal Relative Density Range 1O1H-62 0. mm Working pressure..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. kg/m3 Intermediate lines at.1 Propane. mm Stem diameter min.1. __. Reference Liquids 7.-I FIG.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.1 The procedure for sampling for calibration of the apparatus and for subsequent testing is described as follows: 8. kglm3 Length of nominal scale.`. having a nominal density of Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS / 507.```.2 When the connections have been purged. Ascertain that these connections are free of leaks. At no time shall the pressure Licensee=UK LOCATION/5940240005 Not for Resale.`. permitting the liquid to enter the cylinder until it is full. pure grade. kglm3 310H 500-650 I VALVE \I I :EDLE 'LET Hydrometer 387 16 to 22 10.1 kg/m3 at 15°C or a relative density 60/60"F of 0.. psi 354 to 366 19 to 22 10. 1 Pressure Thermohydrometer Cylinder 1 5 10 1 125 to 145 vapor vent valve shall be similarly connected to the top plate.`.01o 0.) or equivalent needle valves.````-`-`. fitted with a thermostat or other means of maintaining the bath at a constant temperature of 15 k 0. kg/m3 Main (numbered)lines at... If necessary. O C Subdivisions. O F Main (numbered)lines at. mm Working pressure min.5840.005 0.5 200 Hydrometer Scale Standard temperature. and of such dimensions that the cylinder can be completely immersed..3 The cylinder shall not be operated at a gage pressure greater than 1. 8.1 The following reference liquids are required for standardization of the hydrometer: 7.2"C (60 k OSOF). mm Nominal stem diameter.```.. kPa . Density Range..3 Water Bath. mm Body diameter. 6. O F Immersion Subdivisions. 08/21/2007 09:17:10 MDT --````. mm 15 302-1 \. mm 50 to 70 LIOUID INLET Thermohydrometer (Pressure) ASTM Hydrometer No. O F Subdivisions Intermediate lines at Main (numbered) lines at Scale error at any point not to exceed Length of nominal scale.3 mm ( V 4 in.500 to 0. rnm 60/60 0.`.2. mm Body diameter. O F Intermediate lines at.`--- Nominal length. permitting the product to flow through the outlet valve at the bottom of the cylinder. 6.1.. All valves shall be 6. Exercise care to prevent damage to the thermohydrometer.2 The bias of the procedure in this test method has not been determined. with the realization that the accuracy is decreased. Report 1 1.1 Correct the observed thermohydrometer reading and report the corrected reading to the nearest unit of density or the nearest 0. To accelerate thermal adjustment.7 Remove the cylinder from the water bath.2'C or 60 2 0. 8. permitting the liquid to be withdrawn completely and the pressure inside the cylinder to be reduced to atmosphere. 9.1.. withdraw the liquid. In order to accelerate thermal adjustment. remove the apparatus from the water bath and while the thermohydrometer is floating freely. reduce the pressure to atmospheric and repair the leaks.6 Disconnect the cylinder from the source of supply of liquid and place it in the water bath maintained at 15 f 0.`. 10. seen as an ellipse. The pressure of the cylinder must never rise above a gage pressure of 1. after which it should be closed. Connect the source of supply of the reference liquid to the inlet valve and ascertain that the connections are free of leaks. 9. Estimate the hydrometer reading to the nearest one-fifth scale division. and replace in the water bath. 9. 12 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.`. Precision and Bias 12.2"C or 0. occasionally remove the apparatus from the water bath.. the liquid level will improve the visibility of the surface.. tilt to a horizontal position.```. Procedure 10.1 If so used. 9. examine the apparatus for leaks..````-`-`. 9.0005. the vent valve can be opened slightly to permit complete filling. and while the hydrometer is floating freely. Immediately after each determination.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. The point where this line cuts the hydrometer scale is the reading of the instrument.`--- 9. the cylinder must be cooled. discard the sample. If any are detected. rock gently a few times to ensure mixing..4 Close the outlet valve and open the inlet valve. 8.001 relative density. close the outlet and vent valves and open the inlet valve.2 Insert the thermohydrometer in the pressure cylinder. 12. 9. deduct the average from the relative density or density of the reference liquid to obtain the correction to be applied.2 The result must be reported in accordance with the Petroleum Measurement Tables (Section 2).1.3 When the connections have been purged. close the inlet valve and examine the apparatus for leaks. repeat the determinations.5"F as indicated by the thermometer.4 MPa (14 bar). Repeat the purging and filling operations. 11.382Lib77 UOL85LU T L 7 U S T D . and replace in the water bath. Read and record the temperature to the nearest 0.1. Average the two results.2 After each determination. repeat the purging to cool the cylinder sufficiently to permit its being filled without the necessity of venting.8. reduce the pressure to atmospheric and repair the leaks..1 Carefully clean and dry the thermohydrometer and the inside wall of the pressure cylinder. 10.8 Repeat with a second sample. permitting the liquid to enter the cylinder until it is full...3 When the product in the cylinder has reached a constant temperature of 15 f 0. If the vapor pressure is too high to permit adequate filling. filling the cylinder to a level at which the enclosed thermohydrometer floats freely. they might generate sufficient pressure to burst the cylinder.5 With all valves closed. When the cylinder is filled to the normal operating level. A white card held behind the cylinder just below NOTE&For measurements in the field.5 Close the outlet valve and open the inlet valve. occasionally remove the cylinder from the water bath. If necessary. If leaks are detected.2"C or 60 f 0.`. 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.. 12.4 When the cylinder has been filled. 9. Exercise care during this operation to prevent damage to the enclosed thermohydrometer. observe and record the thermohydrometer reading as quickly as possible. 10.5"F.3 When the cylinder has been filled. becomes a straight line.1 The precision of procedure in this test method has not been determined but is under consideration. If it is necessary to accomplish this filling by venting vapor through the vent 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. This is accomplished by repeating the purging operation. the cylinder must be vented and the test discarded if the pressure in the cylinder rises above a gage pressure of 1.3. 9. Open the outlet valve and purge the connections by opening the inlet valve slightly.5"F until thermal equilibrium has been obtained.`. 9. 08/21/2007 09:17:10 MDT .`. this method may be used at ambient temperatures.1 Purge and empty the apparatus and draw a sample of the product to be tested as in Section 8. stand it on a firm level surface. if these differ by less than 0. 10. Highly volatile liquids and liquefied petroleum gases must not be left in the apparatus since at high ambient temperatures.4 MPa. Calibration of Apparatus --````.1 If the two results differ by more than 0. using Table 53B for correction of density to 15'C or Table 23B for correction of relative density to 6O/6O0F.. empty the liquid from the cylinder and vent to reduce the pressure to atmospheric.4 MPa (14 bar).0005.5"F. close the inlet valve and open the outlet valve. empty the cylinder and vent to reduce the pressure to atmospheric. 11.2 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. close the inlet valve and open the outlet valve. Repeat the sampling procedure.8.2"C or 60 f 0. gently invert and tilt.. 9. filling the cylinder to a level where the enclosed thermohydrometer floats freely. .. either reapproved or withdrawn..`. Your comments will receive careful consideration at a meeting of the responsible technical committee.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. 08/21/2007 09:17:10 MDT . 1916 Race St...`.````-`-`. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. which you may attend..`--- 13 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.```..`.`. --````..```. Philadelphia... 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. are entireiy their own responsibility. Users of this standard are expressly advised that determination of the validity of any such patent rights. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. PA 19703..`. and the risk of infringement of such rights.. 1.0 to 0.`.mL pled with a vapor pressure limit. When coupled with a proper vapor pressure limit. 1. A superscript epsiion (0indicates an editorial change since the last revision or reapproval.4 This standard does not purport to address all of the safety concerns. the year of last revision. the number immediately following the designation indicates the year of original adoption or. Vol 05. and pentane and heavier components in propane-butane and butane type fuels.3 0. 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. Referenced Documents Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Division.05 0.5 0.92.o 0..0 25. Originally pübhhed as D 1837 .Last PXV~OUS edition D 1837 . 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. and the temperature is observed when 95 % Correction for variation of barometric pressure is made.5 Sampling Precooling Equipment: 5. The tubes shall comply in wall thickness to ASTM centrifuge tube requirements (Note 1).. The values given in parentheses are for information only.2 Chromatographic analysis should be used when the concentration and type of higher boiling compounds must be identified.0to 5.2 Tube Support-Means shail be provided for s u p porting the weathering tube by its neck in a vertical position. Signüícance and Use 4.4 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.O to 3. Current edition approved July 15.61 T.03 0. Published September 1994.0to 100.1 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. and 100 mL of the liquid is collected in a weathering tube. 5.5 1.1 Weathering Tube-A centrifuge tube. the combination serves to assure essentially two component mixtures for such fuels. 3.. if any.`. Summary of Test Method 3. as in the case of the commercial PB-mixture type of fuels.0 3. 1. When volatility is coupled with a vapor pressure limit which has been related to gravity. The graduation tolerances are given in Table 1. 2 Annual Book of ASTM Standards.. can be used to indicate the presence of butane and heavier components in propane type LP-gas. 5. TABLE 1 Weatherinn Tube Graduation Tolerances scale limit of Range.05 0. Scope 1. in the case of revision. 1. 5.`.05 1 ...```.`.2 0. 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.3to 0.5.. 14 Licensee=UK LOCATION/5940240005 Not for Resale. is a measure of the amount of least volatile fuel components present in the product.4 The shape of the lower tip of the tube is especially important.03. 5.05 0.1 Cooling Vessel-Any suitable wide-mouthed metai container or Dewar flask at least 64 mm (2V2 in.0 5.H on Liquified Petroleum Gas.3 The values stated in SI units are to be regarded as the standard.0to 25. Vol 14.1 0. cone-shaped.1 The product is refrigerated by means of a cooling coil.0 0. The liquid is allowed to weather under specified conditions ’ has evaporated. when properly related to vapor pressure and density of the product. 1 and made of thoroughly annealed heat-resistant glass. The taper shail be uniform and the bottom shall be rounded as shown in Fig. A number in parentheses indicates the year of last reapproval.1 0. conforming to the dimensions given in Fig.0 1 . 2.).[& Designation: D 1837 . The test results.1 0.o 5. it serves to ensure essentially singlecomponent products in the cases of commercial propane and commercial butane fuel types.1 0.. expressed in terms of the 95 % evaporated i temperature of the product. --````. 1.5to 1. 2.) in inside 4. associated with its use.05 0.o 0. 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. Apparatus 5. rnL Borosilicate @ass has been found satisfactory for this purpose.3 Water Bath (for use in tests on butane and propanebutane mixture types of liquefied petroleum gas only).02 0.`--- EITOT..5 1 .01.`. mL 0. 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. 1994..1 to 0. 08/21/2007 09:17:10 MDT . 3 Annual Book of ASTM Standarh.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.```.````-`-`.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 1796.1 Volatility.. ```.. wound around a hollow mandrel at least 54 mm (2% in. and then refill the weathering tube to the 100-mL mark with fresh liquid sample passing through the cooling coil. Center the armored thermometer in the tube by means of a slotted cork.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.. 08/21/2007 09:17:10 MDT Preceding Equipment . Other refrigerants having a boiling point lower than the initial boiling point of the sample can be used. 4 SOFT COPPER TUBING -It METAL OR GLASS COOLING VESSEL 6.4 mm ( Y 4 in.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS i--1 64 rnm (2 l i 2 in.) above. Place the bottom of the armor as low in the centrifuge tube as it will go..5.~ ~ S T D .`.) pipe (or larger).) long (see Fig. 5. Purge the sampling line and cooling coil by opening both the sampling valve and the 3.) deep. 5. Carefully inseri the precooled armored thermometer as low as possible into the centrifuge tube (Note 2). Empty this first sample..) NOTE-The coils in the drawing are extended for danty.`. Use a nonflammable precoolant if required.2 mm (118 in.4m m (114in.`.5. FIG.) in outside diameter. pipet in 5 mL of water.1 Obtaining a Test Sample-Fiil the cooling vessel with the precoolant so as to cover the cooling coil.) outside diameter soft copper tubing.```..2 Cooling Coil-Approximately 6 m (20 fi) of 4. 3. having a sampling valve large enough to prevent vaporization of the material due to the drop in pressure across the valve seat. Procedure 6.2 rnrn (118 in.) below the top of the cooling vessel and the open ends of the coil must not be more than a few inches --````.`.. When assembled.. Connect the downstream end of the coil to a 3.. 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.````-`-`.) O. NOTE2-Do not remove the armor from the thennometer during the test. 6.8-mm (%-in. 2). Fiü the weathering tube with the sample flowing through the cooling coil. 1 Weatheringlube diameter by 292 mm (1 1 i/z in.) needle valve having an outlet connection not more than 76 mm (3 in.D.) needle valve on the downstream end of the cooling coil. and observe the water level in the tube.) NEEDLE VALW SAMPLE VALVE 6 m (20 R.2 mm (I/s in..3 Precoolant-This can be the liquefied petroleum gas from the same container from which a sample is to be taken.`. FIG. 2 15 Licensee=UK LOCATION/5940240005 Not for Resale. add one or two grains of charcoal. with adjacent turns touching.INSIDE DIAMETER NOTE-FOT graduation tderances see TaMe 1...) MIN. the top of the coil must be at least 25 mm ( i in.8 mm (3i16 in. 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.) OF 4. 7'F) for butane and propane-butane mixtures and 1. If the thermometer reading is less than 0°C (32"F).1 The following criteria should be used for judging the acceptability of results (95 % confidence): 8.4"C (0.33 kPa (760 mm) pressure.28"C (2. Keywords 9. 7. A low reading in ice usually indicates that some of the liquid has remained in the expansion chamber.VF) 8.G P A STD 2 1 4 0 .`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 16 Licensee=UK LOCATION/5940240005 Not for Resale. Observe the reading of the thermometer when a constant reading is obtained. propane. tap the bottom of the thermometer on a hard..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). ( 5 5% residue) for the thermometer error (6. and the risk of infringement of such rights. If you feel that your comments have no? received a fair hearing you should make your views known to the ASTM Committee on Standards.. in the normal and correct operation of the test method.33 kPa (760 mm). in the water bath in a vertical position. To correct this. are entirely their own responsibility.33 kPa (760 mm) pressure. Discard any thermometer that varies more than 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.3'C ( 0 3 ° F ) from the observed temperature for each 1.add the fraction of a degree it is low to the final test reading. add 0.3 Weathering Propane Type of Liquefied Petroleum Gas Products-Allow the sample to weather in the atmosphere. 08/21/2007 09:17:10 MDT .`. 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. read and record the temperature of the sample in accordance with 6.3 kPa (10 mm Hg) that the test is conducted below 101.```.3. with the armored thermometer still in place. liquefied petroleum (LP) gases.33 kPa (760 mm).. 7.S T D .4).7"F)to the corrected temperature for each 1. to join the liquid into a continuous thread. or subtract 0. but cushioned surface.. 8.7"F) from the observed temperature for each 1.1. 6.1 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.1. or subtract 0. taking care to disturb the frost on the tube as little as possible.3 In the weathering test for propane. At this point. corresponds with the level previously determined when the 5 mL of water was put in the weathering tube (see Note 2).`.1 butane. which you may attend. Interpretation of Results 7.. 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. and allow the contents to weather. exceed the following value only in one case in twenty: S6'C ( 1 . 6.. 6. PA 19103. add 0. Your comments will receive careful consideration at a meeting Ot the responsible technical committee. LPG.`. Precision and Bias 8..```..4 Reading of Temperature-When the liquid level in the weathering tube.3 kPa (10 mm Hg) that the test is conducted above 101..5"C (1'F) in either direction from 0°C (32°F). volatility 7. 9.1 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.`.3"C ( 0 3 ° F ) to the corrected temperature for each 1.3 kPa (10 mm Hg) that the test is conducted above 101.2 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. 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.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. subtract the fraction of a degree that it is high from the final test reading.33 kPa (760 mm).. --````.2 and 6. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquaaers.`. submerging it to the IVz-mL mark.3 kPa (10 mm Hg) that the test is conducted below 101. Philadelphia. While the mercury-thallium is continuous in the upper chamber. 8.4"C (0. 7.2 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. either reepproved or withdrawn. 7916 Race St. Users of this standard are expressly edvised that determination of the validity of any such petent rights. exceed the following value only in one case in twenty: 95°C (1. allow it to weather in the atmosphere until the temperature has reached -12°C (10°F). with the armored thermometer still in place.5 Temperature Correction-Following the final temperature reading (6. An acetone or alcohol swab can be used to remove frost sufficient to permit reading of the temperature..3"F) for propane. If the thermometer reading is more than 0" (32"F).````-`-`. 6.4 In the weathering test for butane and propane-butane mixtures. place the weathering tube.5).. remove the armored thermometer from the weathering tube and place it in a bath of finely crushed ice up to the immersion point. allow the thermometer to warm so the liquid enters the chamber and tap as previously instructed. see Test Method D 130. Make the bath deep enough so that the entire cylinder and valves will be covered during the test.) 5. 5..01.. in the case of revision.3 This standard does not purport to address all of the safety problems. No leak shall be discernible when tested at 3450 kPa (500 psig) with gas. 6.D.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.`.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. as prescribed in Specification E 1. 5.`. 1. The whole assembly shall be capable of withstanding a hydrostatic test pressure of 6895 kPa (loo0 psig).2"C (0. see 6. storage.1 1 '/z FIG.```. 1... Provide a flexible aluminum connecting hose with swivel connections with adapter to a / 6.4 mm (1/4in. *Annual Book ofASTM Siandards. I . 8. the number immediately following the designation indicates the year of original adoption or. if any. 38.1 This test method detects the presence of components in liquefied petroleum gases which may be corrosive to copper.8 k 0. 1991.2 Water Bath... to hold the copper strip firmly --````. (114 in.2 m m I. Apparatus 5.1 Corrosion Test Cylinder. and transportation equipment.89. Annual Book ofASTM Siandards. constructed of stainless steel with an O-ring removable top closure according to the dimensions given in Fig.5'C (100 k 1°F). associated with its use. The values in parentheses are for information only.. Originally published as D 1838 . Neoprene O-Ring Outage Tube Mote rial: 4.2 3 76 '14 6.`. mm '/a 3.3 Thermometer-An ASTM Density Thermometer having a range from -20 to 105°C(-5 to +215"F). ) 1 I 76.61 T. 15.H on Liquefied Petroleum Gas. 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.4 Strip Polishing Vise. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 5.2 The values stated in acceptable metric units are to be regarded as the standard. Significance and Use 4.1 A polished copper strip is immersed in approximately 100 mL of the sample and exposed at a temperature of 37.4 m m Min. 1 5 2 .`.) 6. 1.) pipe. and conforming to the requirements for Thermometer 12C ( 12F). Current edition approved Aug. A number in parentheses indicates the year of last reapproval.. Published October 1991.3. the copper strip is removed and rated as one of the four classifications of the ASTM Copper Corrosion Standards.````-`-`. capable of being maintained at 37. 3. graduated in 0.8"C (100°F) for 1 h in a cylinder of suitable working pressure.1. and Annex A l .. 4 mm (6 i n . Vol 14.`--- 2. Scope 1.Incorporate suitable supports to hold the test cylinder in an upright position. 08/21/2007 09:17:10 MDT .4 mm (V4-in.03.Last previous edition D 1838 . NOTE 1-For an equivalent copper strip test applicable to less volatile petroleum products. For specific hazard statements.```.5"F) subdivisions. 1. Vol 05. At the end of this period. Referenced Documents 2.. 1 Copper Sûip Corrosion Test Cylinder 17 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.4Tb Designation: D 1838 .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.`.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. the year of last revision.2 mm ( 3 in. Summary of Test Method 3.) n Needle Valve B Metric Equivalents mm in.. 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.2 Holding the test cylinder upright so as not to wet the copper strip with water. 8.`--- 7.1 Handling only with stainless steel forceps. i). attach the sample source to the test cylinder valve A (Fig..3 Close valve A without disconnecting the test cylinder from the sample source. open. 9. For convenient vises see Test Method D 130.2 mm ('/8 in. 7. Interpretation of Results 9.5 Immediately after filling. Finish with 65-pm (240-grit) silicon carbide paper or cloth. Holding it in the fingers protected with ashless filter paper. NOTE2: Warning-Extremely flammable.5 to 3. close both valve A (Fig.````-`-`. close valve A. allow the remainder to drain from the cylinder. do not touch with the fingers. i). open the bottom valve to a suitable disposal unit (8..`.0 mm ('116 to '/E in.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.. 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. hard-temper.. 8. electrical bus bar stock is generally suitable. close valve A. Invert the test cylinder and open valve B to purge the air from the test cylinder.) long from smoothsurfaced. Alternatively.5'C (100 f 1'F). 1) by means of a short length of flexible aluminum tubing that has been purged with the sample. 12-401300-00. 8.6 At the end of the test period remove the cylinder from the bath and.1 As a practical manual polishing procedure. 12. 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.3. Procedure 8. When the strip is clean immediately attach to the dip tube and immerse it in the prepared test bomb.```. 1.2. cut 75 mm (3 in. and with the cylinder in its upright position.. 08/21/2007 09:17:10 MDT ..1 Wash Solvenf-Use acetone or knock test grade 2. 8. 7. The strips can be used repeatedly but should be discarded if the surfaces become deformed. and disconnect the aluminum tubing. Clean all metal dust from the strip by rubbing vigorously with clean pads of absorbent cotton until a fresh pad remains unsoiled.) thick.1 It is important to polish the whole surface of the strip uniformly to obtain a uniformly stained strip.7 When only a slight pressure remains in the cylinder.3. cold-finished copper of 99. 18 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.9+ percent purity.) from the bottom of the cylinder when assembled.1 With valve B (Fig. When vapor first emerges from valve A.4 Copper Corrosion Standard Plaques are a~ailable.~ Their care and inspection for stability are described in detail in Test Method D 130.. Ailow the cylinder to remain in the bath for 1 h f 5 min... 8.1 Warning-Safe means for the disposal of vapors and liquids during this and subsequent procedures must be provided. If the edges show wear (surface elliptical) they will likely show more corrosion than the center. Request Adjunct No.5 mm ( V 2 in.4 mm (1/4 in.. Drill a 3. 7. place a sheet of the paper on a flat surface.2 mm (I/8 in.2 Copper Strip.4 trimethylpentane. removing all marks that were made by other grades of paper used previously. Wipe vigorously with fresh pads of absorbent cotton and subsequently handle only with stainless steel forceps. When the test cylinder is full. After assembly of the apparatus.without marring the edges. on closure assembly with outage tube. 8.`. 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.3 Polishing Materials-Silicon carbide grit paper of various degrees of fineness including 65-pm (24O-fit) paper or cloth. the strip can be prepared by use of motor-driven machines using appropriate grades of dry paper on cloth. open valve A and fill the test cylinder with the sample. Close valve B with the test cylinder now in its upright position. 6. place approximately 1 mL of distilled water into a clean test cylinder and swirl to moisten the walls. also a supply of 105ym (150-mesh) silicon carbide grain and pharmaceutical grade absorbent cotton (cotton wool). In handling the test strip The ASTM Copper Strip Corrosion Standards approved by Committee D-2 are available from ASTM Headquarters. 8.1. 8. and valve B. Materials 6. 1. compare the exposed strip with the ASTM Copper Strip Corrosion Standards. 6. open valve A slightly so that all liquid above the end of the outage tube will be removed from the test cylinder. Admit some sample to the cylinder by opening the valve at the sample source and then valve A.`.) from one end in the center of the strip.2 Final Polishing-Remove a strip from the wash solvent.) hole approximately 3. 8. protecting the strip from contact with the fingers with an ashless filter paper.`. The use of a vise will facilitate uniform polishing. immerse the test cylinder in the water bath maintained at 37. 6.8 If the copper strip shows any appreciable discoloration. the valve at the sample source.) wide.. Preparation of Strips --````. moisten it with wash solvent and rub the strip against the paper with a rotary motion. 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 6.2.`. carrying the stroke beyond the end of the strip before reversing the direction. Clamp in a vise and polish the main surfaces with silicon carbide grains on absorbent cotton. Return the test cylinder to the upright position and drain any residual liquid through the open valve B.4 As soon as the aluminum tubing is disconnected. 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.```. See Annex A 1.1) until all of the liquid and most of the vapor is discharged. holding the cylinder in a vertical position. 6.8 f 0. Rub in the direction of the long axis of the strip. 10. 10. 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. Precision and Bias 1 1. no generally accepted method for determining precision or bias is currently available.. either reapproved or withdrawn.`--- STD*GPA STD 2340-ENGL .. 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..4 Trimethyìpentane Keep away from heat. it is not possible to duplicate this appearance after a test even with a completely nonmosive sample. Use with adequate ventilation. Keywords 12. are entirely their own responsibility. 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). Avoid build-up of vapors and eliminate all sources of ignition.. but no gray 4 Conosion Transparent black. 08/21/2007 09:17:10 MDT --````. which you may attend. Philadelphia. ANNEX (Mandatory Information) Al. 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.2. Avoid prolonged breathing of vapor or spray mist.````-`-`. B 1 Slight tarnish Light orange..1 corrosivity. and open flame... liquefied petroleum gases TABLE 1 ASTM Copper Strip Classifications ___ Classification Designation Description" Freshly polished strip .. The presence of these spots should be disregarded or the test should be repeated.3777 W 382qb77 0038537 373 during the inspection and comparison..```. Keep container closed. 19 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. 11..1 In the case of ordinal classification data. Your commnts are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters.. 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. Report 10. 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. Your comments will receive careful consideration at a meeting of the responsible technical committee. sparks.```. 1916 Race St.`.1 2.`. Avoid prolonged or repeated skin contact.`. State the duration of the test and the test temperature. PA 19103.. 12.. If you feel that your comments have not received a fair hearing you should make your views known to lhe ASTM Committee on Standards. PRECAUTIONARY STATEMENT Al.`.1 Report the results in accordance with one of the classifications listed in Table I .2 The added distilled water frequently causes isolated brown spots on the copper strip. 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..`. especially non-explosion proof electrical apparatus and heaters. 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.`. 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. Available from Gas Processors Assn. Scope 1.0to 0.1 0.4 O Number -10 divided by the oil stain observation. Current edition approved Apr.0 to 100. 3 Annual Book of ASTM Standards.1 A 100-mL sample of liquefied petroleum gas is weathered in a 100-mL centrifuge tube. 4.3to 0.5 TABLE i . Apparatus 6.`. 1.2 R Number -the residue multiplied by 200. conforming to dimensions given in Fig.3 0.1 Centrifuge Tube...01.3 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.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. Terminology 3. see 6. 08/21/2007 09:17:10 MDT scale. in the case of revision..````-`-`. 'VIL4 P 4 R 1 0.5 1.1 This test method covers the determination of the extraneous materials weathering above 38°C that are present in liquefied petroleum gases. 1. 100-mL graduated.03. Available from Institute of Petroleum.05 mL.1 to 0..89. can cause failure of regulating equipment and corrosion of metals.H on Liquid Petroleum Gas.05 0. 3. .5 to 1.. 1992. Originally published as D 2 i 58 . Published June 1992.0 3. a minimum length of 6 m of 5 to 7-mm outside diameter copper tubing wound to a diameter of 63.. can be corrosive.. Significance and Use 5.05 0.4 This standard does not purport to address all of the safety problems.5 0.. Tubes shall be made of thoroughly annealed heat-resistant glass. Vol 14.```. 2.1. 6.5 1.```.0 25.. based on air-free water at 2VC.05 0. OK 74145.0 to 25.5 mL shall be graduated in 0.9. and will contaminate following product. 1.63 T. Tulsa.1 0.4cRi Designation: D 2158 .1 0. associated with its use. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. In liquid feed systems residues may lead to troublesome deposits and.o --````.. residues that are carried over can foul regulating equipment.03 0. 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.0 to 3. Vol 05.o mL 0.0 1.o 0. 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. if any. Last previous edition D 2 I58 .1 residue-the volume. The first 0. Referenced Documents 2.1 Descriptions of Terms Specific to This Standard: 3.2 Cooling Coil.. Limit of Division.1. 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. are given in Table 1.02 1. mL Error. 60th St.0 20 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. 6526 E.`. The shape of the lower tip of the tube is especially important. particularly if alkaline.2 Other Documents: GPA Publication 2 1404 IP Appendix AS 3..1.2 0. 15. London.05 0. Those that remain will accumulate. 3.`. Summary of Test Method 4.1 0. 61 Cavendish St. In either case. 6. in vapor offtake systems. Centrifuge Tube Graduation Tolerances Range.`--- 1. 5. 1.2 Liquefied petroleum gases that contain alcohols to enhance their anti-icing behaviour can give erroneous results by this test method. 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.3 The result can be expressed in terms of measured volumes or indices derived from these volumes.05 0.. 0..1 Control over the residue content (required by Specification D 1835) is of considerable importance in end-use applications. 3. 2 Annual Book ofASTM Standards. For specific precautionary statements. the year of last revision. 1.0 5. measured to the nearest 0.0to 5.`. Water. Volumetric graduation tolerances.1.05-mL increments. Detailed requirements for centrifuge tubes appear in Test Methods D 9 6 and D 1796. A number in parentheses indicates the year of last reapproval. The taper shall be uniform and the bottom shail be rounded as shown in Fig. SOFT COPPER TUBING METALOR GLASS COOCINGMSSEL + 36.. Fill the syringe or pipet with a portion of the solvent drawn from the centrifuge tube and direct 0. Attempt to cover a circle of about 30 to 35 mm in diameter on the filter paper with each addition. 6. controlled at 38 t 2°C. a O. 6.D. 300 10-mm long. or both.Copper Wire 3mm NEEDLE VALVE d 17 z 1 mmiO SAMPLE VALVE 6mm 6m OF 5mm O.````-`-`. 6.. Add 10 mL of a new sample of solvent to the centrifuge tube. If no oil ring appears after 1. 2.5 mm outside diameter.4 Thermometers. reagent-grade pentane or cyclopentane.) 6.7 Water Bath. Mark the center of the filter paper. (See Fig. 1-mL (ordinary medical syringe).`.W-37 75 mm O 0 I / 7 - 10 mL --````. and assembled in a suitable cooling bath..`.6 Solvent Wash Bottle. 2 Precooling Equipment * ~ino oi inside bottom FIG. 1P IC/ASTM 5C ASTM 57C NOTEI-When a thermometer or a water bath. 1-mL pipet may be used.5 mL of solvent has been added. white.1 mL of the solvent to the mark on the paper. 1. Preparation of Apparatus 8.1 mL and equipped with a needle 200 f 5 mm long. conforming to Specification E 1 or IP Appendix A. for example. a satisfactory alternative for screening is to warm the tip of the centrifuge tube with the hand.. cyclopentane can be substituted for pentane whenever the ambient temperature or altitude is too high to enable the convenient handling of pentane.1 Sofvent-Oil-free.1-mm diameter.`--- I 02-90 mm NOTE-CO¡IS in the drawing are extended for clarity... 21 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS * 6.. a field test. Alternatively. Low Range-Minus 38'C to +50"C High Range-Minus 20°C to +SUC 8. 6. medium-grade.5 Filter Paper. 08/21/2007 09:17:10 MDT . 1 7.```.1 Wash all glassware that is to be used in the test in the selected solvent. Allow the solvent to evaporate and note the persistence of an oil ring. t 1. 203 mm NOTE2-Although pentane is the preferred solvent for use in this test method. 125-mm diameter. Reagents and Materials 7.`. 6..```. The appearance of an oil ring indicates either improperly cleaned glassware or contaminated solvent. FIG.6 0. graduated in 0.3 Syringe. INSIDE TAPER SHAPE Cone-Shaped Centrifuge Tube. rapid..`.. suitable for holding the centrifuge tube during weathering.8 Copper Wire.`.9 Clamp. Licensee=UK LOCATION/5940240005 Not for Resale. are not available. the solvent and glassware are satisfactory.. 4 Record the volume in mL of the solvent-residue mixture required to yield a persistent oil ring as the oil stain observation. loose-fitting plug of cotton or cleansing tissue in the mouth of the centrifuge tube..2..2 Oil stain observation to the nearest O.2. LPG. continued incremental additions of the solvent-residue mixture that is equivalent to the limiting specification can be made to the filter paper and. 08/21/2007 09:17:10 MDT . 9. One method is to place it on the 250-mL beaker.````-`-`.05 mL. 8. 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 --````.1. The filter paper should be held level during the solvent addition.2. slotted cork or a clean.1.`. If it is necessary to determine the oil ring at temperatures below 5"C.2.4 by 200.3 Allow the sample to weather.05 mL. in the normal and correct operation of the test method. The wire helps to prevent superheating and resulting bumping (erratic or excessive boiling).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..3 Storage of oil-free solvent in a polyethylene wash bottle for several days contaminates the solvent. the result of the test shall be reported as passing. NOTE3-As an acceptable alternative to the procedure given in 9. Procedure 9. 9.1. 1 mL. when weathering has ceased and the tube has reached ambient temperature.2 for use in those cases where a product specification limit has been established.2 Normalized-The results shall be expressed as: 1 1.```.1. and flush the coil and sampling line.. obtain a new sample.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.. if the ambient temperature or type of sample requires it.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.1. 12. using artificial heating. the result is recorded as zero. Calculation 10.1 liquified petroleum gases. and I 1.2 O Number to the nearest 1. 9. If.. 9.1-mL increments to confine the solvent ring to a circle of about 30 to 35 mm in diameter. 10.3 If a ring is discernible.1 Rinse the centrifuge tube with the material to be sampled and then fill it to the 100-mL mark with a representative sample. Expression of Results 1 1. 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. Oil ring determinations should be made in a protected area where the 10. cool the coil to below the boiling point of the sample. 9.1 R Number-Multiply the volume of residue obtained in 9. 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.allow 10 min for oil ring persistence.4 to restore the volume to 10 mL. 9.5 mL. 9. a residue remains. 9.2.1 Residue on evaporation to the nearest 0. Fill the syringe or pipet and direct 1. If more than 10 mL of the sample is lost because of bumping. if no persistent oil ring appears.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.1 Residue-Attach the cooling coil to the sample source.4 Record the volume of any remaining residue to the nearest 0.`. in the normal and correct operation of the test method. 9. in the long run.3 Reproducibilitjp-The difference (R) between two test results independently obtained by different operators operating in different laboratories on nominally identical test material would.1 Volumetric-The results shall be expressed as: 11.1. 11.1. 12.. 1-mL increments.2 Oil Stain Observation-Add sufficient solvent to the centrifuge tube containing the residue described in 9. 9. Stir well with the syringe needle or pipet so that any residue at the bottom of the tube is dissolved uniformly in the solvent.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.```. 13.1 R Number to the nearest 10. 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. 1 1. in the long run. discontinue the test. place the tip of the tube in a water bath at 38°C for 5 min. 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.`. residue 22 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS R Number Licensee=UK LOCATION/5940240005 Not for Resale.2 Immediately insert the copper wire through a clean. Precision and Bias 12. and the cork (or plug) will keep out air or moisture while the sample is weathering. Keywords 13. if observed.`.2 O Number-Divide 10 by the oil stain observation obtained in 9.`--- 12. If the oil stain observation exceeds 1.1 Precision is only expressed in terms of the normalized reporting units. 9.temperature is above 5°C.2..3 The solvent is added in 0.1 Mark the center of a clean white filter paper.. and the presence of extraneous matter. Add the solvent from the wash bottle and carefully wash down the sides of the tube.4...2.`. and 1 1. 8. are entirely their own responsibility . Philadelphia..`.. 08/21/2007 09:17:10 MDT --````.. If you lee/ that your comments have not received a fair hearing you should make your views known to the ASTM Comminee on Standards..```. Your comments are invited either lor revision of this standard or lor additional standards and should be addressed to ASTM Headquarters.`.`.`--- 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. which you may attend. 23 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.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.```. and the risk o1 mlringement o1 such rights...````-`-`. PA 19703. Your comments will receive careful consideration at a meeting of the responsible technical cornminee.... 1916 Race St.. .01. and butane in all concentration ranges O.3”C during the course of the sample and corresponding reference standard runs. require precise compositional data to ensure uniform quality of the desired reaction products.4 Sample Inlet System-Provision shall be made to introduce up to 0. Vol 05. The chromatogram of the sample is interpreted by comparing peak heights or areas with those obtained on the reference standard mixture of pure hydrocarbons.1.87. 2 Annual Book of ASTM Standards.1 propene concentrate-concentrate than 50 % propene..03 on C4 Test Methods Liquefied Petroleum Gas. Terminology 3. Scope 5. Significance and Use 1.````-`-`. in the case of revision.`.```.5 Temperature Control-The analyzer columns shall be maintained at a temperature constant to 0.4” Designation: D 2163 . Precision and accuracy of compositional data are extremely important when these data are used to calculate various properties of these petroleum products. Referenced Documents 2.2 The component distribution data of liquefied petroleum gases and propene concentrates can be used to calculate physical properties such as relative density.W.`. 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. the year of last revision. A maximum full-scale balance time of 2 s and a minimum chart speed of */2 in. For calculation techniques utilizing a recorder. A number in parentheses indicates the year of last reapproval.1 ASTM Standards: D 242 1 Practice for Interconversion of Analysis of C5 and Lighter Hydrocarbons to Gas-Volume.1 Definition: 3..`. 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. The system shall be capable of detecting 0. When electronic integration is employed the signal for 0.. 6. Current edition approved Oct.02. (12.2 Recorder-A strip-Chari recorder and integrator with a full-scale range of 10 mV or less shall be required. Vol 05.1 This test method covers the determination of the composition of liquefied petroleum (LP) gases.. Published December 1991. 5.. It is applicable to analysis of propane. 6.. vapor pressure.1 % concentration must be at least twice the noise level.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. Last previous edition D 2163 .1 Detector-The detector shall be a thermal conductivity type or its equivalent in sensitivity and stability. 1. 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.`--- 24 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. Noise level must be restricted to a maximum of 1 chart division.`.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. containing more 4. 1. and motor octane (see Practice D 2598).. --````..```. propene.. Gas Chromatograph System 6. 1 % and above. 6.7 mm)/min shall be required. 6. 5. I99 l . 6. The attenuator system must be accurate to 0.2 This standard does not purport to address all of the safety problems.63. 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. Originally published as D 2163 . 3 Annual Book of ASTM Standards.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. A superscript epsilon (z) indicates an editorial cl-ange since the last revision or reapprovai. Its wide use as chemical feedstocks or as fuel. 08/21/2007 09:17:10 MDT . Summary of Test Method 4. associated with its use. 15..3 The values stated in SI units are to be regarded as standard. 1. the signai for the concentration shall be at least 5 chart divisions above the noise level on a O to 100 scale chart. the number immediately following the designation indicates the year of onginal adoption or.`. 2. if any. Liquid-Volume.1 9% concentration of any component of interest.5 % in any position.3 Arfenuator-A multistep attenuator for the detector output signal shall be necessary to maintain maximum peaks within the recorder chart range.50 mL of the sample. . 7. Butane ProPane- pro(iene mopene Butane Mixtures with Low WithHigh ROaane RoOane 2 45 6 0.8 94.`.```.. In case the smallcomponent peak is adjacent to a large one. the \ FIG.`. Factors repeatable to within 1 % are required. the calibration standard mixtures shall not differ from that of like component in the sample to be analyzed by more than 5 %. 15 .... . where: A = depth of the valley on either side of peak B. For compounds present in concentrations of 5 %Y or less..... NOTE2: Warning-Samples and reference mixtures are extremely flammable.. Allow sufficient time for the instrument to reach equilibrium as indicated by a stable base line.1 22. 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.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale..and flames.= 382Lib77 S T D .`.2 .```. Illustration of A/B Ratio for Small-Component Peak 25 --````.. 1 1 1 2 2 .6 76... identical volumes of each component are injected into the chromatograph and relative area response factors are determined. Special Products Div. In either case. Calibration Sîandard 7.. 6.1 %. 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.1 ...6 0.. Use with adequate Suitable reference standard mixtures of pure hydrocarbonsarc available from the Phillips Petroleum Co..5 .1.8. . The concentration of each component in the calibration standard mixtures shall be known to within 0. OK. clean sample inlet systems and clean detectors are mandatory to achieve the precision and accuracy capabilities of this method. R O W n-Butane Isobutane Butene isopentam A propene propane wdh High Propene 1 3 .4. 2. 08/21/2007 09:17:10 MDT . sparks. 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.G P A S T D ZL'iU-ENGL 1 7 7 7 0038523 b77 D2163 TABLE 1 Reference Standard Mixtures.. 8.1.. 1 Illustration of AI6 Ratio 6.`... 0... and most commercial instrumentation easily meets the requirements defined in the test method.2 4. On propene concentrates.. 64 25 6 . If pure components are used for calibration. Uquid Volume Percent * ~~ Component Propane wdh No ünsaturates Propane wdh Low 4 4 93 a7 Ethane Propane.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. These factors are valid for a given instrument and operating conditions and should be redetermined periodically. If pure components are used.. only by strict adherence to the calibration procedures outlined in the method can reproducibility between instruments expect to be achieved....1 The test method allows the user a wide latitude in choice of instrumentation to make the analysis. 2 calculation should be made in mole percent and converted to liquid volume percent mote i).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). an accurate composition oi the standards must be known to anaiyst. it may be necessary to construct the baseline of the small peak tangent to the curve as shown in Fig. .2 Proper maintenance of instrumentation is critical to continued satisfactory performance of this analysis..````-`-`. However.0 5% throughout the analysis.. 0.. Bartlaville. 8. I FIG. and B = height above the baseline of the smaller of any two adjacent peaks (see Fig.`. Clean sample containers. 1)... 8. the ratio of A / B shall not be less than 0. .1 Pure components or calibration standard mixtures4 may be used for calibration. Procedure 8.9 30 0.7 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.. Keep away from heat. 4 3 57 35 1 1 3 1 3 .. . On propene concentrates having a propene content of less than 80 %. (An alternative technique is to trap a sample of only liquid phase in a short section of tubing. Hydrocarbon vapors that may be vented must be controlled to assure compliance with applicable safety and environmental regulations.04 1 0.08 Concentration. Use the same sample size for all runs..4 6.. = area of component in sample.2 use reproducibility curve in Fig.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.6 Butenes 9. 3 ventilation.1 Calculate the percentage by mole or liquid volume of each component as follows: 1.34 1.06 1.04 0. Calculate the percentage by mole or liquid volume of each component as follows: Concentration.. moi % 1 % oí amount present 0. mol % O to 70 Above 70 Repeatability Reproducibility use repeatability curve in Fig. Then use this sample for the analysis. (See Test Method D 3700.04 0.2 Area Method-Measure the area of each component by multiplying the height of the peak by the width at half height. 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.1 On propene concentrates. 9.5 0.```.07 0.3 Preparation ofthe Chromatogram-Obtain duplicate chromatograms of the sample.`--- 8.4 36 35 15 6 4 9 9 6.38 0. 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. 08/21/2007 09:17:10 MDT . 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.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. 3 0.2 where: A.2 Propene Propane Butanes 70 to 77 93 to 95 5 to 7 22 to 29 0. Lack of precision and accuracy in using this method can most TABLE 4 COmpOUnd Ethane 0.33 1 .2 6. Column Length.. If a reference standard mixture is used for calibration.2.0 to 0. Po = peak height of component in reference standard mixture... The width should be measured with the aid of a magnifying glass (Note 3). Cylinders must by supported at all times. obtain duplicate chromatograms of the proper reference standard in a similar manner. OC Flow Rate. 8. and then permit the entire sample to vaporize into an evacuated container).1 0. 550 Methoxy ethoxy ethyl ether Instrument Conditions mm.2. Repeatability Reproducibility 0.7 0.) x S 0. 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 6.1 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. % Temperature.OD Substrate.`. = peak height of component in the sample.`.4 6. liquid volume or moi percent = (PJP.o 9. and 0. the sample may be introduced as a liquid by means of a liquid sample valve or by vaporization of the liquid as above.4 6.`.)x S where: P.`.. Mass. often be attributed to improper sampling procedures. Piecision Data for Propene Concentrates Concentration.o 1.1 0.3 0.) 8.4 3. = area of component in reference standard mixture. Peak heights of like components shall agree within 1 mm or 1 % ! (whichever is larger).02 0.````-`-`. Adjust the attenuator at each peak for maximum peak height within the recorder chart range..4 27 90 36 17 40 30 7 6.4 6. Vapor reduces oxygen available for breathing.o 0. Adjust the flow rate from the sample cylinder so that complete vaporization of the liquid occurs at the cylinder valve. 8.1 0.05 0. Liquid causes cold bums.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 ..0 to 0.1 0. Adjust the area to the attenuation of the same component in the reference standard mixture.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 10.2 26 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. A.`. liquid volume or mol percent = (AJA. Calculation 9.TABLE 2 Column Diameter.2 0. --````. and S = percentage of mole or liquid volume of component in reference standard mixture.5 0.```. only the alternative technique of trapping a sample of liquid and vaporizing the entire sample into an evacuated container shall be used..2. obtained by the same operator with the same apparatus under constant operating conditions on identical test material. mm2 per percent.````-`-`.. 1O. mm2.`.2 Reproducibility-The difference between two single and independent results. 11. 9.`--- S T D * G P A S T D 21'4O-ENGL 27 Licensee=UK LOCATION/5940240005 Not for Resale..0 % by more than 2. Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS = --````.```. calculate the composition as follows: S = Concentration. and A. 9. 3 shall be used for judging the acceptability of results (95 9% confidence) on samples containing less than 50 % propene. 9.382Lib99 0 0 1 8 5 2 5 L(L(T 1997 Precision. exceed the values shown in Table 3 or Fig..3 and Table 4 in only one case in twenty. = area sensitivity of component..3 Normalization-Normalize the mole or liquid volume percent values obtained in 9. . = area of component in sample.```. no statement on bias is being made.`. The data in Table 4 shall be used for judging the acceptability of results on samples containing more than 50 % propene.3 Total the results and normalize to 100 %. Precision and Bias5 10.. The sum of the original values should not differ from 100.`.`. obtained by different operators working in different laboratories on identical test material. 3 Precision Curves percentage by mole or liquid volume of component in reference standard mixture.2 by multiplying each value by 100 and dividing by the sum of the original values.. 08/21/2007 09:17:10 MDT . 10.`. 10.2.2. 1. would in the long run. 3 and Table 4 in only one case in twenty.... in the normal and correct operation of the test method exceed the values shown in Table 3 or Fig.2 If pure components are used for calibration. liquified petroleum gas The data from which this precision statement is based are not available.1 The data in Table 3 and Fig. Keywords 5 1 1.1 analysis. 1.. in the normal and correct operation of the test method.1 Repeatabifity-The difference between successive test results. 95 Percent Confidence Limit FIG.1 or 9.2 Bias-Since there is no accepted reference material suitable for determining the bias for the procedure in this test method.. 1O. mol percent = AJAfl where: A .0 %. APPENDIX (Nonmandatory Information) X1. Users of this standard are expressiy advised that determination of the validity of any such patent rights..2: Warning-toxic.```.4 Dimethylsufolane (DMS) Benzyl Cyanide-Silver Nitrate Column. isobutane.7 Columns) of this test method.`. Philadelphia. 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. isobutane. --````.`. n-pentane.````-`-`..1 Silicone 200/500 Column-This column separates ethane. hydrocarbons.. and isopentane and is therefore suitable for analyzing LP gases free from unsaturated hydrocarbons. I .. and accordingly is best suited for use with LP gas butane containing unsaturated C. Precaution-See the product safety bulletins from the suppiier of the chemicals used in preparing these columns or before Benzyl Cyanidasilver Nitrate Column. XI. n-butane. X I. 1916 Race St.1. 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.`. n-pentane..4 Dimethylsufolane (DMS)-Benzyl Cyanide-Silver Nitrate Column-This column separates ail components in commercial LP gases. and isopentane. If you feel that your comments have not received a fair hearing you shouki make your views known to the ASTM Committee on Standards. the butenes. 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. the butenes.. NOTEX1.1. X 1. propane.2 Benzyl Cyanide-Silver Nitrate Column-This column separates isobutane. X 1.1... n-butane.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.. PARTITION COLUMNS X1.```. 28 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.. either reapproved or withdrawn.. X 1. and accordingly is suitable for use with all types of LP gases. PA 19103. n-butane. 08/21/2007 09:17:10 MDT . NOTEX 1 .. n-pentane and isopentane. propane. which you may attend. and X 1. and the risk of infringement of such rights.3 Hexamethylphosphoramide (HMPA) column.`. propene. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters.3 Hexamethylphosphoramide (HMPA) ColumnThis column separates ethane. Your comments will receive careful consideration at a meeting of the responsible technical comminee.`. 1.1. 3 Sample Cylinder. a wide open position for flushing. Sampling 6. Vol 05.4 Cloth. Procedure 7. Referenced Documents 2.1 A liquid-phase sample of the product to be tested is flowed through the propane water test valve to cool the valve body..G P A S T D ZLqO-ENGL 1997 M 382Lib77 0038527 2L2 M Designation: D 2713 . if any.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.. Experience has demonstrated that excessive water content (dissolved water) will cause freeze-up difficulties in pressure reducing systems. NOTE2-The propane water test valve is a precision instrument and it should be so treated. 2 Annual Book of ASTM Standards. In such cases.```..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. 08/21/2007 09:17:10 MDT . However. Scope 1. reconditioning or recalibration. A superscript epsilon (6) indicates an editorial change since the last revision or reapproval.4 L.1 This test method covers the measurement of the dryness of propane-type products such as. associated with its use. Apparatus 5.S T D .`.```. a sample can be taken into a sample cylinder having a minimum capacity of 1 1.`. 1. the number immediately following the designation indicates the year of original adoption or. NOTE1-This test method is not applicable to propane-type prod- 5. strained in any way. A list of supplies of LPGas freeze valves is available from ASTM.````-`-`. Stop the watch at the instant the liquid propane ceases to flow through the valve (Note 4). the test valve is partiaily closed to a small preset flow rate and the time required for the valve to freeze. 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.01.. Published July 1991. 5. 1991. 6. 2. The valve should be positioned so that the internal surfaces of the outlet opening are clearly visible to the operator. 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.. the year of last revision.1 Propane Water Test Valve3-A specially constructed and calibrated valve manufactured solely for this test (Note 2). The values in parentheses are for information only. It should not be dropped.4 L (3 gai). commercial propane (see Specification D 1835). the sample shall be taken strictly in accordance with directions given in Practice D 1265.2 If the test cannot be run by connecting the apparatus directly to the bulk propane supply. A number in parentheses indicates the year of last reapproval.. Referee tests should be conducted on the bulk supply.2 This standard does not purport to address all of the safety problems. 4. Last previous edition D 2713 . After cooling. 1. open it for 2 or 3 s.`. Summary of Test Method 3.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 5. Significance and Use 4. 5. The average observed time for several successive observations is recorded as the observed freeze time. and thus interrupt the normal flow. or disassembled. dry. in the case of revision.86.2 Stop Watch. 6. Close the test valve for 2 or 3 s. This test method is under the jurisdiction of ASTM Committee D2 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2. so that the body of the valve is horizontal and the outlet opening is aimed vertically upward. clean. except to clean the filter in accordance with the manufacturer’s instructions. Originally published as D 27 13 . 29 Licensee=UK LOCATION/5940240005 Not for Resale. --````... Valves suspected of being defective should be returned to the manufacturer for inspection. close it for 2 or 3 s.1 ASTM Standards: D 1265 Practice for Sampling Liquefied Petroleum (LP) Gases2 D 183 5 Specification for Liquefied Petroleum (LP) Gases2 3.2. having a minimum capacity of 1 1. The valve has two open positions. 7. and a small preset flow position for testing.3 The values stated in SI units are to be regarded as the standard.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. 1. but not limited to. Current edition approved March 15.. Open the main valve on the sample source (Note 4) and set the valve on the test apparatus in the purge position.`.`. is recorded. and continue this intermittent opening and closing until a uniform frost cover has accumulated on the housing around the outlet of the test valve...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. ucts containing antifreeze agents. Purge the sample line and the apparatus for 15 s.68 T.H on Liquified Petroleum Gas. Snap the valve closed to the test position and simultaneously start the stop watch. ```. dry pipe or metallic tubing for making this connection. Repeat the operations as described in the trial run until three successive freeze-off times check each other to within +2 s. dry cloth. are entirely their own responsibility. Report 8. all valves can be 7.1 dryness.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 30 Licensee=UK LOCATION/5940240005 Not for Resale. --````.. 8.. 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.Philadelphia. /i you feel that your comments have not received a fair bearing you should make your views known to the ASTM CommMee on Standards. 08/21/2007 09:17:10 MDT .1 If the valve does not freeze off within 60 s.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. Your comnients will receive careful consideration at a meeting of the responsibte tachnical committee. must not be more than 100 psi (690 kPa) above the vapor pressure of the product at the sample temperature. 9.2 Sample pressure.````-`-`.`. propane. 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.`.1 In the case of pass-fail data or results from other qualitative tests.`.. at a moisture level of 49 ppm it can be expected that none of the valves will give freeze times over I8 s.. the test on the product can be discontinued and the freeze-off time recorded as greater than 3 min..3 Disregard the observed time for the initial freeze-off mn. Open the test valve to the purge position for about expected to give freeze times over 3 min.. record the average time for three consecutive determinations as the freeze-time. 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. The watch should be stopped at this instant. Purging assures that ice formed in the preset opening in the preceding test will be removed. no generally accepted method for determining precision or bias is currently available. report the product as “pass. frost will form on the internal surfaces of the valve outlet.” NOTE4-The instant liquid propane stops flowing through the valve. Keywords 10. at the inlet to the test valve.. 1976 Race St.S T D .```. 10. at the inlet to the test valve. and the rlsk of infringement of such rights. If the freeze-off time on three consecutive test runs is 3 min or greater.. within this limit.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.. 15 s to ensure the removal of ice from the preset opening. which you m y attend.. Your comments are invhed either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. When sample source pressure is above this limit a liquid propane pressure regulator must be used to hold the pressure. Precision and Bias 9. Do not use mbber hose or plastic lined hose. For freeze-off times shorter than 3 min 9.`.. at a moisture level of 93 ppm it can be expected that none of the valves wiil give freeze times over 5 s.Quickly wipe the test valve outlet threads with a clean. For freeze-off times of less than 1 min this may require as many as seven or eight test runs. 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. Users of this standard are expressly advised that determination of the validity of any such patent rights. NOTE6-Data from a series of tests conducted in 1967 indicate the following: At moisture levels of 14 and 26 ppm..`. 7. either reapproved or withdrawn. PA 19703. . with an all-stainless steel burner. 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. 1. stringent techniques must be employed and all possible sources of sulfur contamination must be eliminated. Onginally published as D 2784 . Summary of Test Method 3. The presence of sulfur can result in corrosion of metal surfaces.4nniral Book O(AST.````-`-`.2 Mangold System. 5.`.2 Apparatus for Lamp Cornbusrion: 5.`.03 on Elemental Analysis.2. The oxides of sulfur are absorbed and oxidized to sulfuric acid in a hydrogen peroxide solution. For the latter.```.. as required are described in detail in Annex A3 of Test Method D 1266. or from Atlas Instrument Co.`--- 3. A blowout safety port in the combustion chamber is desirable. Significance and Use 4. 1595 Sycamore Ave. etc. Box 18353. Last previous edition D 2784 . and vacuum. 2 of Test Method D 1266) and a dual manifold (burner and chimney) supplying a gas mixture of approximately 70 % carbon dioxide (CO.. In particular. hydrogen. Houston.2 Institute of Petroleum S~andard.. 1 . valves.. The gas Available from Koehler Instrument Co..) and 30 5% oxygen (O.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. Chimneys. cleaning agents. P. litnirations prior to use. 1992... 42nd St.1 Wickbold-Tjpe Combustion Apparatirs. Referenced Documents 2. (Fig. A superscnpt epsilon ( e ) indicates an editorial change since the last revision or reapproval..02. i ." IP I8 I Sampling Petroleum Gases. Vol 05..89.O. if any. Specimens should not contain more than 100 pg/g of halogens. 5. Published May 1992. Sulfur can be poisonous to catalysts in subsequent processing.2 Modtjìed Beckman Burner-Type Apparatus? as shown in Fig.1 It is important to have the sulfur content of liquefied petroleum gases at low enough concentration to meet government regulations.`.2 To attain the quantitative detectability that the method is capable of.2. associated wirh its use.. 2.`. Tulsa. 1. in the case of revision. 'Available from Scientific Glassblowing Co. A number in parentheses indicates the year of last reapproval. Current edition approved March IS. . Scope 1.. Available from Amencan National Standards Institute. and healtli practices and determine the applicabilitj3 of regitlatorj. I I W. of rhe user ofthis srandard to establish appro- priare safer!. Apparatus 5. 2. N Y 117 16. TX 77023. such as common household detergents which contain sulfates. 1 Iih St.. Hoke No. Any combustion apparatus giving equivalent results.11 Siandurds. and absorber with spray trap.1 Barium Perchlorate Titration-The sulfate is titrated with barium perchlorate using a thorin-methylene blue mixed indicator.STD*GPA STD 2140-ENGL #Tb Designation: D 2784 1777 m 3824b77 0038527 075 . is satisfactory.s as shown in Fig. 5. New York.. sulfate is precipitated as 3.4STM 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' 2.1 The sample is burned in an oxy-hydrogen burner. ' 31 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale..```..1 This test method covers the determination of total sulfur in liquified petroleum gases containing more than 1 pg/g.1. Vol 14. Anniral Book ofAST.2 Turbidimetric-The barium sulfate and the turbidity of a suspension of the precipitate is measured with a photometer. consisting of a vacuum manifold with regulating device. 1. combustion chamber.1 Absorbers. Including Liquefied Petroleum Gases --````.01..4 This standard does not purport to address all OJ the safety problems. the year of last re\ ision. I .11 Slandards. however. 8902 E.3 The values given in acceptable metric units are to be regarded as the standard. Each of the above types of apparatus shall consist of three parts: atomizer-burner. should be avoided. 08/21/2007 09:17:10 MDT . 5. . NY 10036. 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. 4.1.3 Safety Shield-A transparent shield shall be used to protect the operator in the event an explosive mixture is formed in the combustion chamber. Bohemia.1.1 .1 Oxy-Hydrogen Combustion Assemblj-The two types listed below are recommended. tities of sulfur due to the inordinately long combustion times needed. or in a lamp in a closed system in a carbon dioxide-oxygen atmosphere.`. 5. The sulfate ions are then determined by either of the following finishes: 3. 13th Floor. 1.) at regulated pressures.69 T. 5. I t is the responsibilitj. OK. 993 combination flow meter-vahe assemblies should be substituted for those supplied. h i . and Spray Traps. Water conforming to the following specification is required.. 2 of Test Method D 1266 and described in A3. bleed off a small amount of the liquid phase of the material after filling but before reweighing. provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.5 Variable Transformer.`--- NOTE 1-A means for determining when to replace the exchange resins should be provided. is available from Victor Equipment Co. 3. 6.3 Standard Sulfate Solution (1 mL = 100 pg S)-Dilute 6. 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.3 Blast Type Gas Burner... Store in a dark-colored.1 Obtain the test unit in a container by the method conforming to the recommendations in Practice D 1265. Check the dilution by titration against standard NaOH solution of about the same normality and adjust the concentration. Chemical Soc. first with a sulfur-free hydrocarbon..’ Other grades may be used. it should be protected by a suitable trap. the container cannot become full of liquid at room temperature.`.`.01 mL of 1 N sulfuric acid (H2S0. 5.05 g. Wash the interior of the vessel and valve. 5. Inc. 5-Receiver 6-Spray trap FIG. 5. NOTE6-If the weight of liquefied petroleum gas is maintained below 45 g in a 75-mL container.) with water to exactly 1 L.6 of Annex A3 of Test Method D 1266. Wash the vessel with acetone and ailow to drain at least 10 min.2.. NOTE3: Warning-Gas may reduce oxygen available for breathing. Connect the container to the inverted supply cylinder and introduce 24 to 40 g of the liquefied gas. 5. Sacramento.. 6. Use of a simple electrical conductivity meter has been found satisfactory for this purpose.2 Purity of Water-Unless otherwise indicated. D. such as n-pentane.6 Hydrogen Peroxide Solution ( 1. = 30 ’%) with 19 volumes of water. . it is intended that all reagents shall conform to the specifications of the ’ Victor Type SR 300.4 Hydrogen (Warning-See Note 2). 7. Dry the interior of the vessel with clean compressed air and rinse it with HCI (1+10)....```. * “Reagent Chemicals. NY. corrosion-resistant metal vessel can be cleaned as follows: Remove the needle valve. 75-mL-It shall be tested at a pressure of 600 psig (4.4 Corrosion-Resistant Metal Cylinder. and the “United States Pharmacopeia. It shall be fitted with a needle valve for connection to the burner assembly.`. having dimensions given in Fig. giassstoppered bottle.For suggestions on the testing of reagents not listed by the American Chemical Society. If a vacuum pump is used. 08/21/2007 09:17:10 MDT --````. and then wash with acetone. Washington. and Oxygen (Warning-See Note 4). 6. or IP Method 181.” 32 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. LT-* 02 “2 1 -Atomizer-burner 2-Sample tube 3-Combustion chamber 4-Three-way stopcock NOTE2: Warning-Extremely flammable.`.. 7. having a capacity of at least 1200 L/h. but any other similar system giving equivalent results can be used. DC. taking care that the container does not become full of liquid.`.” by Joseph Rosin. Controls Division.24 & 0. references to water shall be understood to mean reagent water as defined by Types II or III of Specification D 1193.. 750-W. Reagents and Materials 6. Carbon Dioxide (Warning-See Note 3).. To prevent this. Sulfate-free deionized water prepared by percolation of water through a column of mixed anion and cation exchange resins. New York.. 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 . Van Nostrand Co. CA 95821.n-w-l Water Committee on Analytical Reagents of the American Chemical Society. American Chemical Society Specifications.05 g.2 Evacuate a clean.. A suitable arrangement is shown in Fig. NOTE4: Warning-Oxygen accelerates combustion. compressed air and reassemble.3 Vacuum Source. meeting the requirement in Note 17. if necessary. Reweigh the cylinder to 0. Rinse the interior with water until the wash water is neutral to a pH test paper. NOTE5-The 75-mL.5 %) (1+ 19)-Mix 1 volume of concentrated hydrogen peroxide (H20. Sampling Test Specimens and Test Units 7. see “Reagent Chemicals and Standards. Unless otherwise indicated.````-`-`. where such specifications are available..1 Purity of Reagents-Reagent grade chemicals shall be used in all tests..```. Dry the vessel with a stream of clean. so that each millilitre of this solution is equivalent to 100 pg of sulfur.” Am. ~ 6. which has been found satisfactory for this application. 0-120 V. 6.14 MPa gage) and shall show no leaks when filled with air or nitrogen to this pressure and submerged in water. dry 75-mL cylinder and weigh to the nearest 0.5 Scavenger-Rinse-Mix equal volumes of low-sulfur acetone and isopropanol. 2336 Auburn Blvd. 6. ìNLET FIG.```. 4. 08/21/2007 09:17:10 MDT --````.. Alternatively the expansion valve may be placed in a suitable metal beaker and covered with water maintained at 11O"F.`. Insert a thermometer between the heating tape and expansion valve so that the thermometer bulb is in contact with the valve body. Wrap the expansion valve with heating tape and connect this to a variable transformer.. 8. NOTE7: Warning-Before attempting subsequent operations. 2 Trace Sulfur Apparatus Flow Diagram 0.2 Turn on the variable transfomer and allow the expansion valve to reach 43°C (1 10°F).````-`-`.. Procedure for Combustion of Sample 8...1).. 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..05 Circulor Hole Pione Surfoce) 46k O0 All dimensions in millimetres FIG.`.1 Connect the sample cylinder with stainless steel tubing to the gas expansion valve. 3 8. l 4 0 W ...`.`. 8. Add to the absorber 25 mL of the hydrogen peroxide solution. Make the final connection to the burner with sulfur-free rubber tubing.3 Oxy-Hydrogen Combustion-Assemble the apparatus according to the manufacturer's directions (see also 14..`.`--- Attach Burner Here ..```. 4 Burner Assembly for LPG 33 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. 4 5 V ) Controlled by a Variable Transformer FIG. See Fig. Attach to this another section of stainless steel tubing which runs to the vicinity of the burner. . NOTE9-Minor adjustment of the gas flow rates can be necessary to maintain those recommended by the manufacturer. 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. For each sulfur level given in Table 2. 10 3 34 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. collecting the rinsings in the absorber. 1 M sodium hydroxide (NaOH) solution. OH 43223. To each aliquot add sufficient water to make 3. Draw the best straight line through points.5 M HCl.3.6 After a suficient quantity of sample has been burned. Light the bumer with an alcohol lamp. Disconnect the tubing from the sample cylinder and reweigh the sample cylinder to the nearest 0.10 For oxy-hydrogen blank determinations bum a hydrocarbon stock with a very low or nondetectable sulfur content.. Turbidimetric Procedure for Sulfate of Test Method D 1266. Slowly open the expansion valve until an optimum burning rate is achieved. 0..03 N NaOH solution by evaporating to 30 mL.G P A S T D 23LiO-ENGL 3777 9 3824b77 0038532 b8T 9 4# through the improper use of hydrogen as a fuel. --````. 08/21/2007 09:17:10 MDT . Frederick. ppm S a m p Size. Concentrate 400 mL of 0. Solution B O.. 8.`. readjust gas flows. Preparation of Working Curve 10.8 g thorin? 0. Slowly crack the gas expansion valve.. shut down the burner as recommended by the manufacturer.. Adjust the apparent pH to about 3. when all of the rinsings are consumed. turn the bottom valve of the cylinder off.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. Washington. Standard Alcoholic (O.`.05 g.2 mL of 0. Set up a control blank absorber as in 5.Box 23344. 9.DC 20044. Assemble the chimney. 8.4 mL) and 3 drops of mixed thorin-methylene blue indicator solution..6 Perchloric Acid.4 Lamp Combustion-Add to the absorber 25 mL of hydrogen peroxide solution. P. and spray trap and connect to the C02-02 and vacuum manifold. The same absorber solution will be used for the scavenger-rinse burning.4. 12 mL of isopropanol (total volume 15. 8.7 If the oxy-hydrogen burner permits.95 g of barium perchlorate trihydrate" in 200 mL of water and add 800 mL of isopropanol.03 M)Prepare by mixing 7 parts of water with 3 parts of standard O. Leave the absorber solution in the assembled lamp unit.1 Light the burner and insert into the combustion chamber. Titrate as indicated below.l o 9.29 g potassium bromate.1 Open the bottom valve of the sample cylinder. 1 M)Dilute 20 mL of aqueous 0." 70 %. using a pH meter. corrections must be made for any sulfur introduced by the reagent in the alkali titration following combustion. 9. and (2) Recautionhave the safety shield in place.O. Alternatively. 16 g methylene blue. Smith Chemical Co. TABLE 1 Sample Sizes 10. For the lamp burning collect the rinsings in a standard lamp sulfur (see Test Method D 1266) flask.8 Methylene Blue.. 8.````-`-`. 9.~ S T D .5 M HCl with 80 mL of isopropanol. The remainder is the net micrograms Solution A: 0. NOTE8-in burning materials with sulfur concentrations greater ~2784 of sulfur from the sample. Ama. Reagents 9. Likewise subtract any sulfur obtained in the lamp combustion blank from the total figure. 9. 8.2 Hydrochloric Acid. highdensity polyethylene bottles. Benjamin Franklin Station. 8. 8. 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. Allow the expansion valve to cool to ambient temperature.9 After the rinsings have been burned in the lamp. If necessary. Subtract from the total sulfur figures any blank so obtained. 9. and determine any sulfate present in accordance with Appendix A 1.`. Otherwise disconnect the tubing and bum in the normal liquid mode.. and insert the burner into the combustion chamber (chimney).3. ''Ava¡lable from G.3 of Test Method D 1266. See 6. flush the tubing and valve with 10 mL of scavenger-rinse and bum without disconnecting the tubing. Turn the heat off on the gas expansion valve. It is important that any materials clinging to these parts be transferred to the absorber to avoid low values for sulfur content..1 Ion-Free Water-Distill deionized water and store in tightly capped. If sulfate is found..5 Bum a quantity of sample in accordance with Table 1. g Turbidimetric Finish Barium Perchlorate Finish 45 20 5 30 1 to 5 5 to 10 10 to 50 Available from Hach Chemical Co.8 For the oxy-hydrogen burners. Standard Solutions (0. Columbus. 9. aliquots of the absorber solutions which do not contain more than these maximums can be used.005 M)-Dissolve 1. ~~ SuMir Content.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. Plot the millilitres of titrant used versus micrograms of sulfur. turn off the C02-02 supply.4 mL.```. 8. 'OAvailable from Reisher Chemical Co.5 with perchloric acid. IA. BARIUM PERCHLORATE TITRATION FINISH 9. 8. Open the bottom valve of the sample cylinder.`. water to make 500 mL. remove it. Allow the remaining gas in the tubing and gas expansion valve to bum itself out. water to make 500 mL. Make the necessary vacuum adjustments (see 5.5 Barium Perchlorate (0. titrate three of the corresponding aliquots.1 of Test Method D 1266).`. absorber.1 Into separate 30-mL beakers pipet each of the aliquots of the standard sulfate solution given in Table 2... and turn off the vacuum pump. 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.`--- 8..```.7 Sodium Hydroxide. Check at least two points on the curved at least every 10 days.4 Fleisher S Methyl Purple Indicator Solution. 3 Pour the entire contents of each flask into a 100-mL beaker.````-`-`. NOTE1 I-The volume of sodium hydroxide should not exceed 2 mL. Rinse three times with tap water and follow with three rinses of deionized water. either by weighing this amount or by using the scoop.00. Before using new glassware and thereafter as required. Calibration 14. and burn a hydrocarbon stock with a very low or nondetectable sulfur content.50. wash the cells with a detergent.`. Photometers employing cells of shorter optical paths will not give the precision of measurement stated in this method. and 5. More indicates that the sulfur or halogen content is excessive or that there is a serious air leak in the apparatus. by means of the buret.```.`--- Preparation of Working Curve 40 80 120 240 TABLE 2 .1 M HC1 dropwise to the solution until the color changes to bright green.3 Scoop. and add the rinses to the beaker.2.. Subtract the 40 pg added. 1 1.. 1. 13.3 and 8. 14. Add 3. 14. Allow to stand for an additional 4 min. 13.2H20 is an important variable that affects the development of turbidity.25.2 Transfer the absorbent to a 30-mL beaker.O crystals..6 For blank determinations. clean the glassware with concentrated nitric acid. People having a low red-green color sensitivity find that using the blue light of Method D 156. 11. using water as reference.40 300 3. or alternatively a filter photometer equipped with a color filter having a maximum transmission at approximately 450 nm.5 From the working curve.4 Allow the solution to stand undisturbed for 4 min.20 ~ 2.03 M NaOH solution (Note 12). using a soft brush.50. Adjust the volume to 3.3.00. After cleaning. Add 2 drops of the thorinmethylene blue mixed indicator solution. Continue as in I 1.`. Select a stirring speed just below that which might cause loss of sample through splashing.1 Alcohol-Glycerin Mixture-Mix 2 volumes of denatured ethyl alcohol conforming to Formula No.30 f 0. 14. and equipped with a blue-sensitive phototube for use at 450 nm. rinse the graduate and the 500-mL boiling flask successively with two 6-mL portions of isopropanol.O)-Crystals passing a 20-mesh (850-pm) sieve and retained on a 30-mesh (600-pm) sieve conforming to Specification E 1 1.. 3. Cool the solution to room temperature and measure its volume in a 10-mL graduate (Note 12).2 Into 50-mL volumetric flasks introduce.00. With use the cells may become coated with a film.3 Hydrochloric Acid ( 1+ 12)-Add 77 mL of concentrated hydrochloric acid (HC1.19) to a 1-L volumetric flask and dilute to the mark with water. NOTE16-The crystal size of the BaC1.2. 08/21/2007 09:17:10 MDT --````.5 Return the solution to the beaker and add 0.1 Quantitatively transfer the absorber contents to a 500-mL Erlenmeyer flask. Reagents 13. NOTE12-For high or completely unknown sulfur contents. and aliquots used.80 1. though slight. Shut off the buret at the point of greatest rate of color change (Note 14).5 any blank so obtained. the concentrated absorbent can be quantitatively transferred to a 5-mL volumetric flask.-2H. See 6. 12. checked by again adding 40 pg of sulfur (0. Add i mL more of the 0. gg AligUOtS. sharpens the end point very considerably.30 k 0. 1.. Apparatus 12.. capable of dispensing 0.00 I I ..~~ TURBIDIMETRIC FINISH Sulfur. NOTE10: Warning-Do not boil.1 Photometer-Preferably a spectrophotometer having an effective band width of about 50 nm. 1 1.01 g of barium chloride dihydrate as specified in 13. 11.3 Pipet 0.2 Absorption Cells.00 mL of standard sulfate solution (1 mL = 100 pg S ) .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. 12.`.0 mL by adding ion-free water. 1 mL in 5 (A1) s until the end point is indicated by a rapid.1 Only by the most scrupulous care and attention to details can reliable results be obtained by this method. Adjust the resultant gray-green color by adding 0.75. color change from green to a bluish gray (Note 13).`.. 1 1. 2H.7. repeat the operations in 8. rinse thoroughly with water.0 mL of HCl (1+12) to each flask. 14.. 12. Stir with the magnetic stirrer for exactly 3 min.. relative density 1. omitting the standard sulfate. and mix thoroughly. 3A of the U.`. NOTE15-The procedure as written assumes an absorbance change of about O. This is the net micrograms of sulfur from the sample. 0. A white background and good white light may be helpful in obtaining a precise end point. Add 2 drops of Fleisher’s methyl purple indicator solution to this solution and titrate to a faint green end point with 0..40 mL of the standard sulfate solution (40 pg of sulfur) into the beaker. Subtract from the sulfur figures in 11. The solution must be stirred by a small bar on a magnetic stirrer or with a small propeller stirrer. 10 for each 100 pg of sulfur in 50 mL of solution measured in a 5-cm cell. adjusted to 5 mL. 0.S. Add the barium reagent at a steady rate of O. 14. Prepare a reagent blank standard in a similar way. Reserve the glassware for use in this method alone.. having an optical path length of 5 cm.40 0. and again measure the absorbance relative to water. 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.01 g of BaCl. Burn for the same length of time as the sample in the normal liquid mode. I. Each aliquot is then subsequently made up to 3 mL as in 1I.4 The 2-mL buret containing standard barium perchlorate should have its tip positioned just below the surface of the solution in the beaker.1 mL of alcoholglycerin mixture and mix for 3 min on the magnetic stirrer. find the total sulfur titrated to the nearest 1 pg. Procedure for Analysis of Solutions 1 1. transfer to the cell. 13. Maintain this speed throughout the entire procedure. dilute to volume with water. Add by means of a pipet 10 f 0. Transfer to an absorption cell and measure the initial absorbance. 35 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.2 Barium Chloride Dihydrate (BaCl. 0.4 mL standard sulfuric acid) and retitrating to the end point. NOTE 14-The end point can be.```. (Warning-see Note 11): DO NOT BOIL DRY. To remove this film. Bureau of Internal Revenue or ethyl alcohol (99 % by volume) with 1 volume of glycerin. 2. rnL 0. using ion-free water for rinsing. determine it by Test Method D 1657. 14.6'C (60/60'F). and 14. 08/21/2007 09:17:10 MDT . 15.2883 to convert grains per cubic foot to grams per cubic metre.2H20. rinsing the beaker with several small portions of water.4. dilute to the mark with HCI (1 +2 1 5 ) . If so.1 Calculate the amount of sulfur in the sample as follows: Sulfur content.2 Alternatively calculate the concentration in units of grains of total sulfur per io0 ft3 as follows: R (for propane) = 0. 14.5077) + 0.5.6/15.020. 16. NOTE17-Should the blank reading exceed 0. pg/g. Proceed as directed in 14.`. Procedure for Analysis of Absorber Solutions 15. make up to volume with water. 14.1. and proceed as described in 14. 7976 Race Sr.8 To detect possible shifts. and W = grams of sample burned.005..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.```.0.. check the calibration curve daily by making single determinations.3120 NOTE 19-If the relative density of the mixture is not known.. Your comments are invit8d either for revision of this standard 01 for additional standards and should be addressed to ASTM Headquarters. 17. NOTE20-Multiply by 2.. and G = relative density of the mixture at 15. I Round the result of the test to the nearest 1 pg/g of sulfur.```. 2H. and mix thoroughly..3 Into a 100-mL beaker pour the entire contents of the 50-mL volumetric flask containing the solution to be analyzed.0831 where: R = grains of total sulfur per 100 ft3 of gas at 15.`.. 15. Calculation 16. which you may attend. 16.````-`-`.083s R (for butane) = O.4.7 Obtain the net absorbance for each standard by subtracting the initial absorbance and reagent blank reading from the absorbance obtained in accordance with 14..45 I5 --````. 17. 14. ft3/lb of gas Specific volume for butane (same conditions as above) 6.366(G . 1 1 1S (2) R (for propane-butane mixtures) = S[0. The responsible subcommittee is attempting to attract volunteers for an interlaboratory study.6 Following steps described in 14.. results should not be Considered reliable. Philadelphia.`.3.31 to convert grains per cubic foot to grams per cubic metre.2 Reduce the volume of the absorber solutions to about 25 mL by evaporation on a hot plate. Users ot this standard are expressly advised that determination ot the validity d any such patent rights. pg/g = A/ W (1) where: A = micrograms of sulfur as obtained in 1 1. Multiply by 35.6 or 15. This standard is subject to revision at any time by the respsibie technical commirree and must be reviewed every tive years and 1not revised. - 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.3. obtain a reagent blank reading by subtracting the initial absorbance of the reagent blank standard from that obtained after addition of BaC12. Place 30 mL of the H202( i . If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Commirree on Standards.10132 MPa (760 mm) Hg.`..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. Your comments wi// receive careful consideration at a meeting of the responsible technical committee. are entirely their own responsibility..6. 36 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 8. 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.696 psia). S = sulfur content. the precision obtainable will be impaired.`.1 The precision of this test method has not been determined.6.. and the risk of infringement of such rights. 16. 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.O. PA 19703.`--- Licensee=UK LOCATION/5940240005 Not for Resale. and 14. Add 3 mL of HCl (1+ 12) to the flask.5.6'C (60'F) and 0.15.. If this reagent blank reading exceeds 0.5.010. 15.5 Convert net absorbance to micrograms of sulfur by using the calibration curve. make an analysis of the reagents alone to determine whether the atmosphere or reagents are at fault. 15. This reading should not exceed 0. either reapproved or withdrawn. Precision and Bias 17. 14. Quantitatively transfer the resultant solution to a 50-mL volumetric flask.1 Drain the absorber solution into a 250-mL beaker and quantitatively rinse the absorber collecting the rinsings in the beaker.5 %) in the 50-mL volumetric flask. sample date. 20% displaced for outage.`. 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.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. 3..S T D .. single-phase liquid. 10% remaining in cylinder) d. 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. The procedures described in this method may be used for obtaining samples for analysis by methods other than gas chromatography.8 For floating piston cylinders. The inert gas should be removed from the displacement end and the above procedure repeated for the sample side.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.7 This method assumes all procedures begin with clean.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. GENERAL INFORMATION 3. The location of the probe fitting should be on the top or side of the line rather than 3. 3. There may be additional related facts such as field-determined results and operating conditions which will assist in the evaluation of the analytical data. 3.. 3. It is also possible to analyze the inert gas side of 37 --````.`. All samples must be obtained using a probe designed to secure product from the center one-third of the flowing stream. Water Displacement Method 2 (partial H 2 0 removal - 70% replaced by hydrocarbons.80% replaced by hydrocarbons.5 A certain amount of information about a sample is necessary before it can be intelligently handled in the laboratory. and d may not be aPP1icable to the analysis of certain samples containing reactive non-hydrocarbons such as sulfur compounds. 08/21/2007 09:17:10 MDT . 3. leak-free sample cylinders. 3.. etc.1 The objective of any sampling operation is to secure. cylinder identification. 2.1 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.3 It is not possible. close valves C and D and note the pressure reading-on gauge N. gauge.```. 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.2 Particular emphasis should be given to the necessity of obtaining accurate. Floating Piston Cylinder Method b.manufacturers’ recommendations. although the importance of the proper sampling location cannot be overemphasized. Water Displacement Method 1 (total H 2 0 removal replaced by hydrocarbons. 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. nor is it the intent of this method. Next. SCOPE 1. Essential information includes the sample source.80% c.`.`. Ethylene Glycol Displacement Method (total glycol removal . 20% displaced for outage) NOTE 1: Methods b. representative samples for analysis since analyses. may be useless if the samples are not valid.`. the sample containers must meet the specifications of and be labeled and packaged according to the Hazardous Materials Regulations of the Department of Transportation. having the same composition as the stream being sampled. 20% displaced for outage) at the bottom. type of analysis required. in a suitable container..1 A hydrocarbon fluid sample is transferred under pressure from a source into a sample container by one of the following methods: a. A method to insure a leak-free cylinder is to pressure test both sides of the piston cylinder. to provide a procedure that will be applicable for all sampling situations. regardless of the care and accuracy of the laboratory tests. Cylinders must be thoroughly cleaned prior to sampling with an appropriate volatile solvent or by following . A pressure drop only at gauge N indicates a leaky fitting. 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... ambient temperature. sample source pressure and temperature. This is accomplished by pressurizing the displacement chamber with inert gas to a typical operating pressure with valve C opened (see Fig. and the sampling method used.. or rupture disc. This information must accompany the filled sample cylinder.. 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. carbon dioxide.````-`-`.```.. i). . OUTLINE OF METHODS 2. valve.6 If the hydrocarbon fluid samples are to be transported by common carrier within the United States. The use of detergentlwater solutions or steam is not recommended for the cleaning of floating piston cylinders. an adequate portion of a hydrocarbon fluid under pressure. C. 3. After a period of five minutes.. ```. 08/21/2007 09:17:10 MDT .SAMPLE SOURCE C PROBE R1 H L SAMPLE FLOATING PISTON INERT GAS I CYLINDER+ N INDICATOR ROD Figure 1. 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.`.10 Duplicate Samples 3.`...g. and stirring assembly 3.. These duplicate samples must be taken using the same sampling method and from the same sampling location.1 Sample Containers 38 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS LO the Licensee=UK LOCATION/5940240005 Not for Resale. but the physical restrictions of the piston cylinder (e. it is advisable to take duplicate samples as a precaution against accidental loss. For floating piston cylinders..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.`.. valve dead space.`. or from a primary sample cylinder to a secondary cylinder. Typical Visual Indicator Sampling System design) may prevent the flashed product from returning original homogeneous mixture... thus preventing flashing of the sample.`--- the cylinder to determine hydrocarbon concentration if leakage occurs in that direction.! 4. 3.1 When resampling is difficult or impossible. the product in the vapor state could be returned to liquid phase..```.`.. Theoretically. --````. rupture disc...10. APPARATUS 4.. Cylinders should be tcstcd at least on an annual basis. The sample sequence should be noted on thc sample information a& t.````-`-`. (Stainless steel is preferred. The volume of the cylinder will depend on the amount of sample needed for the laboratory analysis. cylinder Y (Fig.4 Some piston-type cylinders are fabricated from nonmagnetic materials such as the 300 series stainless steel.) 39 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.```. The traveling rod provides an indication of the piston position and the volume of the product sample in the cylinder. or transportation of the sample container. thus compromising the integrity of the sample.2 The cylinder itself contains a moving piston equipped with O-rings. gauges. some variations of this style may exist. and relief valves.`. The end caps are drilled and tapped for valves. the pressurizing fluid. The use of filters and dryers is discouraged.1. the pressurizing fluid. a displacement cylinder.1. 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. These allow a partial or complete loss of contents due to thermal expansion or over-pressurization.) The transfer lines should have a minimum diameter of 114 inch (6.1. the magnetic field generated by the magnets flips a series of bi-colored flags.6 Other types of floating piston cylinders are available which have no visuai method of determining the sample volume directly. such as.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. teflon rings. This system.`. Should relieving occur. The size of the container depends upon the amount of sample required for the laboratory tests to be performed.S T D * G P A STD ZLqO-ENGL 1777 3824b77 0038537 L b 3 4. The piston and sealing device must be non-reactive to the sample. TIOR Some types of lubricating fluids will absorb appreciable amounts of the Cd+ fraction from the gas being sampled.2 Double Valve Cylinders 4. 4. 4. 08/21/2007 09:17:10 MDT --````.be wed to prevent this difficulty..1. The pressure reliefs may be of spring or rupture disc types. 4.`. is fabricated from metal tubing...1. The system must include a method to mix the product sample in the collection chamber. 4. The use of guide rings is recommended to assure smooth piston travel.1.1. or systems of similar configuration.1 Transfer lines.1. Figure 5 depicts a typical proportional sampler using an injection pump and the vanous parts required. (Figure 6 depicts a typical automatic sampler and the various parts required.1. either a flow-through sample injection valve.`. Sample containers and valves must have a working pressure equal to or exceeding the maximum pressure anticipated in sampling. . 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. The cylinder is preferably closed with removable end caps to provide access to remove and service the moving piston. 4. 4. NOTE 2: DOT regulations regarding the use of pressure relief devices on these cylinders must be followed.3 Composite Sampling Mechanism 4. 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.1 Metal sample containers of a type which insure maximum safety and which are corrosion resistant to the product being sampled should be used..1. 4. honed and polished on the inside surface.2.`. The unit consists of a sample probe. 2). It is recommended that non-absorbing lubricating greases.1.1.. whether automatic or manual (see Figures 3 and 4) or a probemounted sample pump (Fig. valves. and expected corrodants. The piston likewise is fabricated of stainless steel but has magnets attached to the precharge side of the piston. Soft-seated valves are preferable to those having metai-to-metai seats. 5) and utilizes a floating piston cylinder as its collection chamber. and gauges in the transfer system shall be designed consistent with maximum anticipated pressure and be resistant to all expected corrodants.1 The container required for this method is constructed of metal tubing. storage. Further details regarding non-absorbing lubricating greases can be obtained from the piston cylinder man ufac turers.....3 All valves and safety devices must meet the appropriate material and pressure requirements for safe design. The cylinder is designed consistent with the maximum pressure anticipated during sampling and to be nonreactive to materials being sampled. the cleaning solvents and the expected corrodants. but not limited to DuPont's Krytox AC or AD.. indicates the piston position and the volume of product in the cylinder. As the piston moves the'length of the cylinder.1 Floating Piston Cylinders 4.`--- 4.2 Sample Transfer System 4. the sample should be considered compromised. For these cylinders.```.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.````-`-`.35 mm) and be as short as is practical. Again.1.2.. the cleaning solvents. 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.1.1.3. 1.`--- h CX!NDER Y AIR (ATMOSPH E RIC PRESSURE) Figure 2. SAMPLING PROCEDURES 4.1. in a NGL sample..````-`-`..1. Close valve A at sample source.`.`.1.1 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.1. causing fractionation and bubble formation. 5.1 Technique of using a cylinder equipped with visual indicatorfor liquid phase samples of “spot” or “instantaneous” type (see Figure 1 ) CAUTION.`. of an inline-type design. (This may be accomplished by a heatinglcmling process or inert gas purge..```. 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..1 With sample side of cylinder evacuated (from cleaning operation) and valve C open.1 Floating Piston Cylinder Method 5. fill displacement end with inert gas to a pressure at least 10 psi (69 P a ) above sampling pressure... 5..) The filter element should be 15 micron size or larger so that during the purging process NGL is not flashed.4 Sample Filters 5. 40 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. dirt...`. The filter should be of a small total volume. A filter may introduce error if not handled properly. 08/21/2007 09:17:10 MDT . 5.`.. etc. and contain a replaceable/disposable element.2 Open valve A at sample source and thoroughly blow out any accumulated material. Displacement Cylinder Sampling System 4.4..```. etc. Close valve D.UMPLE PISTON INERT GAS --````.. Close valve A at sample sourcc.1.- --- - 4-73 S T R U M SAMPLE- / PROBE ~~ ~~ ~ Figure 3.1. This comment applies to all subsequent comments regarding equal pressures on gauges L. 5. Do not allow pressure L to drop below original sample pressure..`.1. Disconnect the cylinder from sample source.. 5. gauge N will read higher than gauges L and M.2 Technique of using cylinder not equipped with visual indicator for liquid phase samples. Continue the operation until the indicator designates the cylinder contains 80% by volume of product (following manufacturer?s instructions). 5.1. open sample source valve A to full open position. Crack valve B and fitting at valve C to purge line.I ?I i r ?? i - -+. For proper cylinder sizing refer to Section 4.1. C. There should be no pressure change on gauge N and pressure at gauges L.1. 5. cap valves to protect threads. Close valve D. 08/21/2007 09:17:10 MDT . then the pressure on the inert gas side will be 5. --````.`--- 41 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. 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. 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. slowly open valve C completely.1. M and N should all be equal..2. Le.`.6.8 Close valves D. Do not allow pressure L to drop below original sample pressure... 5. Typical Sample Probe Installation on Orifice Flange Figure 4. Open valve B to release pressure on the sample line.2 Open valve A at sample source and thoroughly blow out any accumulated material.5 Adjust pressure on gauge N to equal pressure L by releasing adequate inert gas through valve D. 5. Observe sample source pressure on gauge L.1.9 Do not take outage or reduce pressure on piston cylinder..1.7 Partially open valve D. 5.`.M and N. do not allow pressure M to drop below sampling pressure.2.````-`-`. 5.1.`.4 With valves B and C closed.slowly allowing inert gas to vent to the atmosphere.1. fill displacement end with inert gas to a pressure at least 10 psi (69 kPa) above sampling pressure. Check valves C and D for leaks.1....1.1. Displacement cylinder Y should be filled with air at atmospheric pressure.1.1. the operator must use judgment in determining when to discontinue purging. Typical Sample Probe Installation for a Pump 5. 5.4 With valves B and C closed. 5..```.1. slightly higher than the sample side.. To prevent flashing. Crack valve B and fitting at valve C to purge line.```.3 Connect piston cylinder X to sample source at valve A and displacement cylinder Y to piston cylinder. via displacement cylinder.2.1. Observe sample pressure on gauge L. Close valve B and tighten fitting at valve C. prepare sample information tag and box for transportation as per Department of Transportation or applicable requirements.6 With valve D closed.3 Connect piston cylinder to sampling source at valve A. and A in that order.1..1.1.2.`.1 With sample side of the piston cylinder evacuated (from cleaning operation) and valve C open. open source valve A to full open position. `...Power _--- Power I I I Pressure recomer I Pressure regulator I k4 Pressure Check valve Sample transfer tap Bleed valve Figure 5.--````.````-`-`..```.....`..`--- 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 . 08/21/2007 09:17:10 MDT . Typical Proportional Sampler Using an Injection Pump Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 42 Licensee=UK LOCATION/5940240005 Not for Resale.```.`.. `.````-`-`..```. SAMPLE TRANSFER TAP 7 PRESSURE SUPPLY VALVE SAMPLE MIXING DEVICE Figure 6.`...`...`..L--imTfp STREAM SAMPLE 3 TOTALIZER 1 ) - i 1 PPB AC POWER ' i r--- c 1 PULSE PER "x" BELS. Typical Automatic Proportional Sampler Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 43 Licensee=UK LOCATION/5940240005 Not for Resale..`.```.. --)--- 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...`--- K . 08/21/2007 09:17:10 MDT --````.PRODUCT FLOW METER .. is used to supply fresh liquid to a location for filling the sample container. Disconnect piston cylinder X from sample source. Discontinue purging after a sufficient time and only when liquid product is present. CAUTION: Under no circumtances should the cylindcr be filled beyond 80% of its capacity with sample.```.1.5 The floating piston cylinder should be connected to the purged sample line via the composite sampling device. Observe gauge M so as not to allow pressure M to drop. 5.10 Do not take outage or reduce pressure on the cylinder.5.3 for specifications and location.`.3. Close valve F.7 Close valve D. slowly open valve C to full open position.1.6 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. In some instances.1. allowing inert gas from cylinder X to flow into cylinder Y.3. 5. 5. leaving sufficient inert gas space to insure safe storage and transport. Continue operation until-pressure of all three gauges equalizes. such as an orifice plate or a small pump. and A in that order.1..2 Thorough purging of sample lines.1. 5. and prepare sample information tag and box for transport as per Department of Transportation or applicable requiremenis.3.1 Automatic proportional samplers take small samples of the flowing stream proportional to the flow rate.10 Do not take outage or reduce pressure on piston cylinder X. and prepare sample information tag and box for transport as per Department of Transportation or applicable requirements. or control the pressure or temperature of sample containers containing volatile materials. the operator must use judgment in determining when to discontinue purging. C. Open valves B and F. 5. if the product flashes without leaving a liquid residue at valve B and the fitting at valve C.`. 5.2. --````.1.11 If it is not possible to disconnect the primary floating piston cylinder from the automatic system. 5. Time increments may be used only when the flow rate is consmt. (Refer to Section 3. it may be necessary to insulate the sample line and sample container.) A bypass device that causes a differential pressure.`--- 5. Once the sample in the primary cylinder is adequately mixed. 5.3.1. 5.2. 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). Adjust pressure N to equal pressure L by slowly venting inert gas through valve E.. pumps and connections to the sample cylinder is necessary to avoid contamination of the sample.. 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.3. thus changing the composition of the sample and creating a serious safety hazard. the sample may be transferred to a secondary floating piston cylinder. a volume equal to cylinder Y has been displaced into cylinder X by the product sample.3.1. 08/21/2007 09:17:10 MDT . either manually or by use of sample injection valves. 5.8 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. cap valves to protect threads. Check valves for leaks.1.7 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..1. cap valves to protect threads.4 All samples must be obtained using a probe.1.3. There should be no pressure change indicated on gauge N and pressure at gauges L.`.1. 5. Care should be exercised to prevent overfilling of the sample container so that relieving does not occur. Check valves C and D for leaks. Close valve B and tighten fitting at valve C. Disconnect displacement cylinder Y.. 5.. At pressure differences less than 200 psi (1379 kPa) the chance for erroneous samples increases.2.2.3 Precautions shall be taken to avoid vaporization in sample loop lines when operating near the equilibrium pressure of the liquid. 5.3. Open valve E and properly vent pressure through valve F.````-`-`.2.9 Close valves D.1. proceed 44 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.3.. 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.1. Sampler systems should be designed to minimize stagnant areas which could result in the sample not being representative of the fluid source. open valve D and observe pressure on gauge N.2..3. M and N should all be equal.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 ) 5.3.`.6 With valve E closed. 5. Sample cylinder X now contains 80% by volume of sample. At this point.8 Slowly open valve D.. Close valve E.1.9 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.1.`.5 With valve E closed.. 2 WaferDisplacement and Ethylene Glycol Displacement Methods .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).2. Close valve A at sample source.0.`. then 80% of the total volume is 400 mi.`.2 The total volume of the sample cylinder must be found. The product vapor pressure al the existing master sampler temperature must be maintained or exceeded to prevent flashing. (For example. (0.`..) 5. then 80% of the total volume should be calculated.```.Total displacement 5.2.1 N H2SO4 is a satisfactory acid solution. 08/21/2007 09:17:10 MDT .. if the total volume of the cylinder is 500 ml.G P A S T D ZLVO-ENGL 1997 as in step 5.1... L SAMPLE SOURCE ["i rl CYLINDER --````..2.0 must be acidified to bring the pH within the proper range..S T D . Water must have a pH between 5.0 and 7. 3824b99 0038543 4b5 Ethylene glycol must be the glycol t y p used. Water with a pH greater than 7.````-`-`.`.) 5. (In this particular transfer situation..) 5.`... Liquid Displacement Sampling 45 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. the master sample container will partially depressurize.3 Open valve A at sample source and thoroughly blow out any accumulated material.. as sample is withdrawn.```.`--- GRADUATED CYLINDER b Figure 7.. treating the primary cylinder as a flowing source.1. ) Disconnect sample cylinder from sample source.`. 5. Continue operation until 80% by volume of the displacement liquid has been displaced by product in the sample cylinder.2.5 With valves B.. 5.4 Connect the sample cylinder to sampling source at valve A exactly as shown in Figure 7..2.1 Recommended Procedures for Liquid Phase Samples Prior to injection of the Sample into the Test Device 5.`. slowly open valve C to full open position. Open valve B to release pressure on sample line. Continue operation until 70% by volume of water has been displaced by product in the sample cylinder. (At this point.```.```. Pressure at gauges L and M should be equal. usually a flashing bubble. cap valves to protect threads. the operator should reduce the drain rate and carefully extract the remaining water or glycol.9 With sample cylinder still attached to source valve A. Crack valve B and fitting at valve C to purge line. LIQUID PHASE LABORATORY HANDLING AND PREPARATION 6. prepare sample information tag and box for Uansportation as per Deparunent of Transportation or applicable requirements.`--- 5. slowly open valve D to drain the remaining 20% displacement liquid from the sample cylinder. 5... Observe sample pressure on gauge L.7 Slowly open valve D to allow a slow discharge of the water into the measuring vessel. 5. Discontinue purging after a sufficient time and only when liquid product is present.3.Partial Displacement 6. 6.10 Check valves C and D for leaks. Observe sample pressure on gauge L.1. Pressure at gauges L and M should be equal.2. 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 5.8 Close valves D. C and A in that order. Close valve B and tighten fitting at valve C.) 46 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.) At this time. then 70% of the total volume is 350 ml and 20% is 100 mi. --````. prepare sample information tag and box for transportation as per Department of Transportation or applicable requirements. do not allow pressure M to drop below sampling pressure. 5.3 Open valve A at sample source and thoroughly blow out any accumulated material.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. 5.3.S T D * G P A S T D 2 L 4 0 . do not allow pressure M to drop below sampling pressure...1. Discontinue purging after a sufficient time and only when liquid product is present. and D closed.3.`..4 Connect the sample cylinder to sampling source at valve A exactly as shown in Figure 7.10 Check valves C and D for leaks.2. Do not allow pressure L to drop below original sample pressure. 5. then 70% and 20% of the total volume should be calculated. To prevent flashing.1.3..````-`-`. Close valve A at sample source. open sample source valve A to full open position.3 Waier Displacement Method . Crack valve B and fitting at valve C to purge line.3. open sample source valve A to full open position.2.3. 5.3. 5.7 Slowly open valve D to allow a slow discharge of the glycol or water displacement liquid into the measuring vessel.5 With valves B. cap valves to protect threads. C. 5. 6. 5. 5. Do not allow pressure L to drop below original sample pressure.9 With sample cylinder still attached to source valve A.3.2. When the first indication of product appears.the operator must use his judgement in determining when to discontinue purging.3. C. The water used must meet the same requirements as in 5. After 1 5 ml has been withdrawn.1. (For example. slowly open valve D to drain another 20% of the water from the sample cylinder. Disconnect cylinder from sample source. 10% of the water still remains in the sample cylinder.2.8 Close valves D.E N G L 1997 3 8 2 4 b 9 9 00118544 3 T L m 5.3. if the total volume of the cylinder is 500 ml.`.6 With valve D still closed. Close valve B and tighten fitting at valve C.2 The total volume of the sample cylinder must be found.`. If the product flashes without leaving a liquid residue at valve B and the fitting at valve C. close valve D immediately with no further loss of product. the operator must use his judgement in determining when to discontinue purging. 08/21/2007 09:17:10 MDT .1 Floating Piston Cylinders 5. C. If the product flashes without leaving a liquid residue at valve B and the fitting at valve C. Open valve B to release pressure on sample line. slowly open valve C to full open position. and D closed..2. (The displacement liquid may become cloudy just prior to the end point. reduce the rate to 10 ml/min maximum. 5. although the effect is less noticeable with glycol.6 With valve D still closed.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).. and A in that order.. To prevent flashing. 1.```.. thereby minimizing “dead space”. The sample line and valve system should remain at 200 psi (1379 kPa) above the vapor pressure of the product. 6.7 When sample injection is complete.```. When the purge is complete.9 If the sample is to be reused. never at sample valve B .`. Any measurements should be taken al sample purge valve C .. then close valve on inert gas source.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.1.. on the sample container at all times during the analysis via a prcchargc regulator or similar device. close valve C.````-`-`...1.. 08/21/2007 09:17:10 MDT .8 Disconnect the cylinder from the inlet of the chromatograph liquid sample valve and the inert gas source. open valve B to fill the sample valve and associated lines.1. do not take an outage I ‘111. 6. close valves B and A in that order.1. 6. 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 8.1.`. 6..1.1. to thc inlet of the chromatograph liquid sample valve. 6.`.3 Connect the sample end of the cylinder. All tubing between the sample cylinder and liquid sample valve should be the same diameter.1.1.1.`.. 6. valve B.1.1.1. Be sure sufficient volume is displaced to purge unmixed areas in the sample cylinder as wcll as the sample injection system. 6.6 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. Slowly open valve C and vent any remaining unused sample in the system through an appropriate vent.4 With valve C closed. 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. whether it be by “mixing dasher”. 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.1.5 Slowly crack valve C to purge the sample valve and associated lines... “mixing ball” or equivalcnt.1.. 6.`.2 The sample should be thoroughly mixed per the cylinder manufacturer’s recommendations.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. Repressuring System and Chromatograph Valving with Floating Piston 47 --````. immediately prior to each analysis. .. . utilizing the smallest diameter and VENT VALVE PRESSURE REGULATOR r c CHROMATOGRAPH LIQUID SAMPLING CARRIER GAS CARRIER GAS l l I CYLINDER -> CYLINDER 'Y -. 6.) With this configuration the hydrocarbon sample will be taken from the upper portion of the cylinder. Maintain a pressure at least 200 psi (1379 kPa) above the vapor pressure of the hydrocarbon sample at operating conditions.. 6. o e o. .: . Allow it to remain immobile in the vertical position at least 2 minutes before injection of sample into the chromatograph..2 Double Valve Cylinders 6.1.'GLYCOL' : .... 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..or reduce pressure on the piston cylinder. and store the cylinder in a suitable location.LAYER NGL - --.. A!l connections and tubing are to be made of material impervious to the sample composition..-. Check valves for leaks..2..... .. . WATER $AS . OR " .. WATER . (The pressurizing fluid should be same type used to secure the product. . OR .1.. .`..`..1 For double valve displacement cylinders..* .```.. .. ..`. .2..1.2.-- ..`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.````-`-`.o. . Fix cylinder Y in a vertical position by means of a ringstand or similar device. . Figure 9.-*GLYCOL' : : .1.`. . . .-.```.. 08/21/2007 09:17:10 MDT ...`... . cap valves to protect threads... 6.2 Mix the sample thoroughly by gently inverting cylinder Y several times... . . Open valves B and C to admit pressurizing fluid into sample cylinder Y.. Open valve A and pressurize cylinder X w i t h inert gas.. . Repressuring System and Chromatograph Valving with Double Valve Displacement Cylinder 48 --````.3 Connect the sample outlet valve D on cylinder Y to the inlet of the chromatograph liquid sample valve.-. 1. provided the plunger is of suitable material as to not scratch the cylinder bore. never at sample valve D . Persons responsible for obJning samples should be familiar wilh and adhere to safc practices for handling flammable fluids under pressure.9 With cylinder Y remaining in the upright position.```.. 7.3 The work surface at either end of the cylinder should be clear before the end plug is loosened.8 Disconnect cylinder Y from the inlet of t h e chromatograph liquid sample valve and disconnect from cylinder X. 6.1.2.`. procecd to next step.`. Caution should be taken not to dent or bend the cylinder by applying excessive pressure. 6.1. thereby minimizing “dead space”. 7. 7.. 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.5 Slowly crack valve E to purge the sample valve. close vaives D and C on cylinder Y and valves B and A on cylindcr X.. 7.) 6. All tubing between the sample cylinder and liquid sample valve should be the same diameter.1 Clamp the piston cylinder firmly to a steady work surface.2.1 Sampling hydrocarbon fluids can be hazardous. vent hood). 08/21/2007 09:17:10 MDT .g. Disconnect Cylinder X from the inert gas source.2. If either end cap is removed while pressure is on the cylinder.3.1.1. KOTE 4: For reproducible sample volume limils see GPA publication 2177.2. open valve D to fill the sample valve and associated lines.````-`-`.. The sample line and valve system should remain at 200 psi (1379 kPa) above the vapor pressure of the product.7 When sample injection is complete. in that ordcr. 6..10 Check the valves for leaks. Do not use fluid Dressure to flislodnethe piston. 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.4 With valve E closed. If the sample is not to bc reused immediately. 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.2 Using a suitable venting apparatus (e.`. then cap valves io protect the threads and store the cylinder in a suitable location. then closc the valve on the inert gas source.shortest length of plumbing practical. properly vent both ends of the cylinder before attempting to remove either end cap..2. 6. CAUTION: Extreme care must be used I O ensure that no flashing of sample occurs in the inlet sampling line and valve sysrem. 49 --````.. 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. 6.. (If the sample is to be reused immediately.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.. When the purge is complete close valve E.`.`.```. This is accomplished by slowly opening valve C to allow a slow discharge of the pressurizing fluid into a measuring vessel.2.4 Provide a mechanical plunger to dislodge the piston from the cylinders.1. Slowly open valve E and vent any remaining unused sample in the system through an appropriate vent.8. remove 20% by volume of the pressurizing fluid for outage. Any measurements should be taken at sample purge valve E .1. 7.. SAFETY PRECAUTIONS 6. 7.3. do not take an outage or reduce pressure on the sample cylinder.2 In all cases. 7.2.1.3..3. 6.3 Disassembly of the Piston Cylinder CAUTION. 7.2.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale. (e) Cooling Coil. 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.```. 2. (d) Ice Bath. The indicator shall consist of a lightly folded plug of cotton impregnated with cobaltous bromide. 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. except in cases where local conditions will not permit.. shall extend well above the bath and shall be fitted with a suitable connection to accommodate the pressure gage and needle valve. See Fig. The inlet of the coil. SCOPE 1.. (i) Caps or Plugs. will be green or blue. I-ASSEMBLED 3. 08/21/2007 09:17:10 MDT . but the preferable method is to encase each plug in a separate gelatin capsule. 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. The temperature of the ice bath shall be maintained within a range of 32-34 F. copper tubing coiled so that it may be conveniently immersed in the ice bath.PROPANE DRYNESS TEST (Cobalt Bromide Method) tube which in turn shall be partially surrounded by a metal shield. i long. 50 --````. tank car or tank truck containing the propane to be tested. Drying is accomplished by heating to a temperature not to exceed 212 F while simultaneously evacuating the container. They may be stored in sealed bottles or a desiccator. (c) Needle Valve. 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. This test is intended to give an indication of the dryness of Commercial Propane and Propane HD 5.. The needle valve required shall be capable of accurately controlling the flow of gas through the equipment with a minimum of adjustment. (b) Pressure Gage. Thio plug of cotton shall be held in a glass r----- R ? i $ SAMPLïNG FIG. 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.`--- Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.. An accurate pressure gage of suitable range and scaIed in single pounds shall be provided.. Each plug shall be Fpyoximately ?' in.`. The outlet of the coil shall point upward so that when attached to the indicator it can be readily immersed up to within in. The apparatus shall consist of the following: (a) The Indicator.`.`. When properly dried the plugr...D. After soaking in a szturated solution of cobaltous bromide the plugs shall be placed in a test tube or flask and dried...```. O. of the tip of the indicator. The cooling coil shall consist of at least 2 feet of % in.````-`-`. APPARATUS 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.. All tests shall be conducted with the apparatus connected directly to the vapor space of the tank. 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..`.`. .G P A S T D 2LLiO-ENGL 1777 m 3824b77 0038547 9 8 3 Chah 16 Threads R r Inch --````.0.8 MATERIAL Make From 5/< Hex Brass Bat.```.Whlte Nickel .`. 08/21/2007 09:17:10 MDT . 2-DETAIL OF INDICATOR 51 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS Licensee=UK LOCATION/5940240005 Not for Resale.0....*y64 v4* Natlonal Plpe Threads SECTION 8 ..`.. 3/1{ 0.`.S T D .```. s/14 SECTION A-A Finlrh FIG..`--- lhu13 Threadr Per Inch on 'window Both Sides 7 Cotton Impregnated With Cobaltous Bromide A Glass Tube 1.````-`-`.`.`. Except Cap To Be Made From Dlameter Brass Bar..... .. 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..in.” (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). 2. the pressure shall then be reduced to 7 pounds t 2 pounds for five minutes..`. lavender or pink. (c) The final color of the indicator will be the original blue. If the original blue color persists throughout this period.```.. the pressure on the apparatus shall be adjusted to 5 pounds per square inch or less. of the tip of the indicator will be immcrsed. the material shall be reported as being “dry. The ice bath shall then be placed in such a position that the coil and all but rpproximately 1. 1. (a) All tubing and fittings must be absolutely dry and free of oil or foreign matter. (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... then the material shall be reported as being “wet. 08/21/2007 09:17:10 MDT . (c) If the original blue color persists for 30 minutes of test exposure. (b) The ôssembled coil and indicator shall be adjusted to a vertical position. la) The apparatus shall be assembled as shown in Fig.s contain water.`. = = from the outlet of the indicator. the material is either “wet” or the tubing and fittings contain water. The apparatus and r. Fig. (b) The needle valve. To determine the cause of the color change.```.`--- Licensee=UK LOCATION/5940240005 Not for Resale.. TEST PROCEDURE AND INTERPRETATION 6. PRECAUTIONS 5. CO that the indicator will not be contaminated or the results of the test obscured...” If the color changes to lavender or pink at reduced pressure. 3.G P A S T D 2L40-ENGL 1777 ASSEMBLY OF APPARATUS 4.____ S T D ... (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. Extreme care shall be exercised in distinguishing blue from lavender color as any change from the original blue color indicates a marginal moisture content.`.onnections shall be dried and the test repeated. ia) The valve on the source of propane vapor to be tested shall be opened and the cap removed 52 Copyright Gas Processors Association Provided by IHS under license with GPA No reproduction or networking permitted without license from IHS 382Lib99 0018550 b T 5 --````..” (2) If the indicator remains lavender or pink it can De assumed that the tubing and fitti I . 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.`. If the container pressure is less than 50 psig secure a sample as outlined in Sect.````-`-`.`.