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GPA Standard 2166-68 Obtaining Natural Gas Samples for Analysis by Gas Chromatography Adopted as a Tentative Standard, 1966 Fovised and Adopied as @ Standard, 1968 Ravissd 1986 Floprinted 1988, 1990, 1994, 1996 Gas Processors Association 6526 East 60th Street Tulsa, Oklahoma 74145, | I | FOREWORD ‘Thie 1986 revision of GPA Publication 2166 contains major changes from the adopted 1968 standard. The incorporated chenges are the result of three cooperative sampling programs carried out by the GPA Work Group on ‘Natural Gas Sampling. A total of 1050 samples were collected and analyzed resulting in nearly 70,000 data polnta for ‘evaluation of sampling method effects on each of the 10 common components of natural gas. Details of this work wore reported in the Proceedings of the GPA 64th Annuel Convention (1986). ‘The combined data obtained from this sampling project report the degree of accuracy for each method tested to be listed in the following order: 1, Water Displacement Method 2, Purging — Controlled Rate Method 3, Purging ~ Fill & Empty Method 4, Glyool Displacement Method 5. Reduced Pressure Method 6, Floating Piston Cylinder Method 7. Helium “Pop” Method 8, Evacuated Container Method Good samples can be obtained when using any of the eight methods tested, provided extreme care is taken while the samples are being secured. Potential users of these sampling methods are urged to study this report prior to selection of sampling methods, Scksi Dokumentasi + PERPUSTAKAAN & Obtaining Natural Gas Samples for Analysis by Gas Chromatography 1. SCOPE 1.1 The specific purposeof this bulletins to recommend procedures for sompling natural gas for subsequent analysia bby ges chromatography. Thie bulletin describes procedures for obtaining representative “spot” samples of natural gos from vecuum oF pressure sources in containers which are suitable for transporting the sample to a laboratory. Contain- ersmust be selected ao thatthe gas composition isnotaltered {for the tests to be performed during storage or transportetion of the sample. These sampling procedures should be sppli- ible for most situations normally encountered in natural gus sempling, The procedures deseribed in this bulletin may be ‘used for obtaining samples for analysia by methods other than gaa chromatograpiny. Soma of the procedures described in the bultin ae eotable for sampling “wet” (Sc) natural ganee at preaure to ‘There aro no presaure Extilon in supling “dy” Urs) satarel goon Bath sample probe and « GPA separator must be used to obtain good, representative samples. ‘Note 1-Sureams containing hydrogen sulfde should be analyeed for ‘ydrogen sulfide on site inthe fe 2, OUTLINE OF METHODS 2.1 A ges sample is tranaforred from the source into & sample container by one of the following methods: ‘8, Water Displacement Method ’ Purging - Controlled Rate Method ©. Purging - Fill & Empty Method 4. Glycol Displacement Method ©. Reduced Pressure Method {Floating Platon Cylinder Method Helium “Pop” Method 1, Evacuated Container Method 22 The method selected mey depend upon the compo- sition of the sample, pressure and temperature conditions of the sample source and equipment availeble. 8, GENERAL INFORMATION 3.1 The objective of any sampling procedure isto obtain ‘2 representative sample of hydrocarbons from the system under investigation. Any subsequent analysis of the sample, regardless of the accuracy of the analytical test, ia inaccurate unless a representetive sample is obtained. This mothod eanumes all procedures begin with clean, lealvfree sample ‘vlinders. 3.2 Entrained liquids are a chief cause of non-represen- (ative samples when sampling “wet” (rich) geees. These entrained liquide can be eliminated by the correct installation cof sample probes and by the use of a sampling soparator uring sample collection. Sample probes should be installed fon the upper circumference of vessel or pipeline and extend far enough into the vessel or pipeline to insure vapor sampling ‘away from vessel or pipeline walls. Sampling separators can be permanently installed ot the ‘ype) or carried from sampling point to sampling point, The: portable separators muat be thoroughly puzged with the gas to be sampled and no visible liquid should be allowed to remain in the separator during sazapling (cracking the bottom valve daring sampling will insure a “dry” separator). Insulated separators with temperature probe must be used when gas to be sampled is at elevated temperatures ebove ambiect. 33. The cholee of sampling procedure may depend ‘upon the souree pressure, temperature and sample compos tion. The choice of sampling procedure and spparets may also depend upon the particular tests to be made, and whether the samples are to be shipped by common carrier, 8.4 The scope of this bulletin does notinclude composite gas sampling (samples teken in inerements over relatively Yong time periods). Tt should be noted that several “spot” anoles taken appropiate intel any eee for a composite sample. 8.5. The large variations in the composition of natural gases requice thal care he taken in obtaining and handling somples, [tis recommended that samples be obtained under the direction of an individual experienced in sampling pro- cedures because it is difficult to write instructions for sampling which will be explicit enough to cover all cases. If possible, natural gas samples should be taken under conditions ‘which will prevent condensation in the sample container. ‘Should condensation occur in the sampling container during the sampling operation or during shiyment, the conteiner xuvst be heated to a temperature in excese of the eampling temperature and allowed to equilibrate at this temperature for one hour or longer prior to enalyais to ineure complete vaporization of any condensed liquid. For c! phic analysis, itis recoramended to hest samples 20 -50°F above the cempling souree temperature. 4, SELECTION OF SAMPLING PROCEDURE 4.1 The sampling procedure should be oclected as specified in Seetion 5. Inthe event that the nature ofthe gasis completely unknown, the safest procedure is to assume that it ia a "wet" (rich) natural ges and ta choose the eppropriate ampling procedure. Any gas of unknown composition at ¢ pressure greater than 400 psig should bo considered a9 “wet” (rick) gas for sampling purposes. 42 A “dry” (lean) natural gas may be defined as one ‘which does not form condensate on cocling by rapid expansion from source pressure to atmospheric or eny intermediate Pressure, 4.3 A “wet” (rich) neturel gas may be defined as one which partially condenses upon cooling or by a variation in pressure from the source pressure. Since wet gases normally Originsle from a source where th gas in equilibrium with liquid, slight decrease in temperature or variation in pressure may causo partial condensation. 5, GUIDE FOR SELECTION OF PROPER SAMPLING PROCEDURE 5.1 Dry (Lean) Natural Gas 5.1.1 Purging - Fill and Empty Method ‘This method is applicable whore the sample contsiner temperature is equal to or greater than the source tempera- ture, The source prosaure must be greater then atmospheric. 8.1.2 Purging Controlled Rate Method ‘This method is applicable forthe eame conditions specified in 5.11. 5.1.3 Evacuated Container Method ‘This method is applicable where the source pressure in above or below stmosphoriepressure andthe source tempera: ture is greater or lose than the sample container temperature. 5.14 Reduced Pressure Method ‘Thia method is applicable forthe same conditions specified in 5.1.8 except source pressure must be at east 100 psig to provide a 30 psig sample for ges chromatography analysis. 8.1.8 Helium “Pop" Method ‘This method is applicable for the ome conditions epecilied in 6.1.3 except source presaure must be greater than helium charge pressure, 5.18 1:0 Displacement Method ‘This method is applicable for the same conditions specified in 5.1.8 except source presstire must be greater than atmos- herie pressure. 5.1.7 Glycol Displacement Method ‘This method ie applicable forthe seme conditions mpecified in 5.1.8. 8.1.8 Floating Piston Cylinder Method ‘This method is applicable forthe seume conditions specified in5.18. 5.2 Wet (Rich) Natural Gas 5.2.1 Purging — Fil and Empty Method ‘Thin method is applicable where the anmple container temperature is equal to or greatar than the source tempera- ‘ture, The souree pressure muat be greater than atmospheric but less than retfograde pressure. 5.2.2 Purging - Controlled Rate Method ‘This mathod is not recommended for wet natural gas. 5.2.3 Beacuated Container Method ‘This method is applicable where the source pressure is 1100 piig oF less. The source temperature mey be greater or leas than the esmple container temperature. 5.2.4 Reduced Pressure Method ‘This method is applicable for the same conditions specified in 5.2.3. Piling pressure is limited to one-third af the source Dressure over a source pressure range of 100-1100 psig. 5.2.5 Helium “Pop” Method ‘This non-purge sampling method usea a helium charge to keop the cylinder" “air free” prior to sampling. Itie sometimes ‘used after the vacuum sampling to provide sufficient sample ‘presoure to purge sample loop atthe chromatograph. In either tase, the betium charge should not exceed 5-10 pelg. This ‘method is applicable for the same conditions specified in 5.2.8 excepteouree pressure must be greater than the helium charge preseure, 5.2.68 HO Displacement Method ‘This method is applicable for the same conditions epecified in 5.2.3 except source pressure must be greater than atmo- spheric pressure, 5.2.7 Gheol Displacement Method ‘This methodis epplicablefor the same conditions specified in 5.2.6. 5.2.8 Floating Piston Cylinder Method ‘This method is not recommended for wet natural gas unless cylinders have been lubricated with nomabsorbing {greases such as DuPont's Krytox AC or AD. CAUTION: Some types of tbricaing luda wil absorb appreciable enounts of the Cot feton from tee gos Being eampled, thus the integrity ofthe samp. fs recommended tht ren- SSearng lang ret, sak ate ied fo Doth Kentos AC or AD, be used to prevent this difficulty, Further deals rearing non bvring ibiaing ease can be etlnd fom te pistonepinder manufacturer 6. APPARATUS 6.1 Sample Containers 6.1.1 Single and Double Valve Cylinders 6.111 Use metal sample containers of a type which insures masimum safety and which are corrosion resistant to the product being sampled. Stainless steel containers are recommended to minimize problems of surface adsorption of heavy components (hexanes and heavier component) and to rinimize the reaction of carbon dioxide with the container. If the container is to be transported, it must meet DOT specifications and be labeled according to the Hazardous “Msteriala Regulations of the Department of Transportation. ‘The container may be of the one-valve or two-velve type (depending upoa the sampling procedure selected). Saimple containers end valves must have a working preasure equal to or exceeding the maximum pressure anticipated in ssumpling, storage, ortranaportation ofthe semple container. Sof ae valves are preferable to those having métal-to-metal seats. ‘The size ofthe container depends upos the amountof sample required for the laboratory teats thot are to be mado. 6.1.2 looting Piston Cylinders 6.1.2.1 ‘The container required for this method is con- structed of metal tubing, honed and polished on the inside surface. The cylinder is preferably closed with removable end caps to provide access to remove and service the moving piston. The end cape are drilled and tapped for valves, enuges and relief valves. The 5 ia dosigned to exceed the mexizum pressure anticipated during sampling and to be nonreactive to materials being sampled, the pressurizing ‘uid, the cleaning solvents and the expected corrodents. The volume of the cylinder will depend on the amount of sample needed for the laboratory analysis. If the container is to be transported, it must mect DOT specifications and be labeted according to the Hazardous Materials Regulations of the Department of Transportation. 6.1.22 The cylinder itself contains a moving piston ‘equipped with O-rings, tellonrings, crother devices toeffecte leak-free seal between the sample and the pressurizing fluid and allowed to move freely within the cylinder. The use of ‘ide rings is recommended to assure smooth piston travel. ‘The piston and sesling device must be nonreactive to the sample, the pressurizing Muld, the cleaning solvents end expected corrodents 6.1.2.3 All valves and safety devices must meet the appropriate material and pressure requirements for safe design. The pressure reliofs may be of spring or rupture dise ‘ype. These allow a partial or camplote loss of contents due to thermal expansion or over pressurization. Should relieving oceur, the sample may be compromised. 6.1.2.4 Some piston-type eylinders are fabricated from ‘non-magnetic materials such as the 300 series stainless steel. ‘The piston likewise is febricated of stainless steel but has agnets attached to the precharge side of the piston. As the ton moves the length of the cylinder, the magnetic field generated by the magnets flips a series of bi-colored flags. This system or aystems of similar configuration, indicates the piston position and volume of saraple in the cylinder. 6.1.2.5 Some piaton-type cylinders are fabricated with a rod attached to the piston which extends through the end cap, on the inart gos beck-prossure chamber with appropriate sealing devices to prevent the inort ges back-pressure from leaking. The travel rod provides an indication of the piston ‘position and the volume ef the eylinder flied with the sample, ‘Again, some modification of this style may exist. 6.1.2.6 Other types of floating piston cylinders are available which have no visual method of determining the sample volume directly, For these ylinders, a magnetofsome type (or atud fides 2 necessary to follow the overeat of 2 piston. 6.2 Table I gives approximate minimum recommended sample sizes for some of the more common teats: Me Continatar, 280 10" PAT Determination ‘ow Temperature Fractional ‘Analysis Calorimeter Test for Heating Value Mass SpectometerAnaysis Gas Chvomatograpty Analysis 140% 10° 85x 10" 280 ple , steel, copper tubing, or other Noxible metal nonreactive to the product being sampled, is required, Staintess steel is preferred for pressures over 1000 sig or for gases containing hydrogen sulfide. The most ‘satisfactory line is one equipped with two valveson the sample ‘container end (see Figure 1); a control valve, A and a vent volve, B. The transfer ine should have a minimum diameter of ¥ in (6.5mm) and be as short as is practical. 64 Sample Line Separator-When entrained liquids are present at the sample point, a liquid separator must be Installed betaeen the source and the sample container. (See 3.2) A sintered metal filter may also be required to keep solid articles out of the container. Detalt of suggeted gas sampling seperators are shown in Figures 2 ond 3. Soparators should conform to the eppropriate pressure vessel code, (Commercial line separators are available.) 6.5 Sample Points-Care should be used in selecting the location of sampling points. For ges sampling, itis prefersble that the sampling points be located on the top of « horizontal line to reduce the chances of liquid eontaminetion. Sampling Figure 1 ‘Typlcat Layout for Gas Sampling 6 Figure 2 Example of Gas Sempling Separator, Type A ’ rd mer fx" peas insite th tmttiog ore sapratoy stout conto oman wae y Figures Example of Gas Sampling Separator, Type B points should also be located in ¢ section away from bends or ‘obstructions for the same reason. Good sampling mandates that the sample line (probe) extend into the line or vesnel 20 hat liquids on the line or vessel wall will not be withdrawn with the sample. (Commercial probes are available.) Semples should never be taken from stagnant or dead-end sources. 6.8 Duplicate Somples-When resampling is difficult or impossible, it in advisable to take duplicate samples precaution against accidental loss. Duplicate sezmple contain- ers should be connected in parallel and filed simultaneously, 8.7 Preparation of Sample Container-Sample containers ust be thoroughly cleaned before samptes are takin. This is particularly true if the contsiners have previously contained Liguid hydrocarbon samples. Oil films, greese, or sludge should be removed by purging with live steam, by washing ‘with a hot detergont solution, or by washing with auclventand drying, For proparation of Floating Piston Cylinders, refer to GPA Standard 2174, paragraph 3.7. It is preferable to segregate containers used in different services, such a8 liquids, rich gases, or lean gases to facilitate cleaning. ‘7. SAMPLING PROCEDURES 7.1 Purging - Fill and Empty Method-The equipment arrangementis shown in Figure 4. Its necessary to connect an extension tube (length of 2-4{t) with a valve on the discharge ‘end to the outlet valve of the container. This arrangement

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