Gpa 2186-05

GPA Standard 2166-05
Obtaining Natural Gas Samples

for Analysis by Gas Chromatography
Adopted as a Tentative Standard, 1966

Revised and Adopted as a Standard, 1968
Revised 1986, 2005
Gas Processors Association

6526 East 60th Street
Tulsa, Oklahoma 74145
www.gasprocessors.com
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 from 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.
"Copyright ~005 by Gas Processors Association. All rights reserved.

No part of this Report may be reproduced without written
consent of the Gas Processors Association."
INTRODUCTION
This 2005 revision of GPA (Gas Processors Association) Publication 2166 contains major changes from the 1986 version. The
incorporated changes are the result of a cooperative sampling program carried out by the API (American Petroleum Institute)
wOrXgroup on Natural Gas Sampling. Data from the API project combined with data from a GPA project published in 1985 provide
the impetus for this latest revision.
A "definitions" section has been added to help the reader understand the terms used throughout this dOOJment. Words In bold type
are defined in the "definitions" section. First uses of TLAs (Three Letter Acronyms) are followed by an explanation in parentheses.
Subsequent use of the TLA is not followed by a parenthetical explanation.
This publication indudes detailed sampling procedures for each of B test methods:
1. Purging - Fill & Empty Method

2. Purging - Controlled Rate Method
3. Evacuated Container Method
4. Reduced Pressure Method
5. Helium Pop Method
6. Glycol or Water Displacement Method
7. Floating Piston Cylinder Method
8. Portable and On-Line Gas Chromatographs
Not all methods are appropriate for all sampling conditions. Appropriate sampling conditions for each method are disa.assed in this
standard.
It is important to have a thorough knowledge of the phase behavior of the product to be sampled and of the Joule-Thomson Effect
Discussion of the Phase Diagram and the Joule-Thomson Effect can be found in API Chapter 14.1.
The sampling methods listed in this document require that the sampling components are dean and free of contaminants. It may be
necessary to dean sample cylinders and sampling system components between uses. Appendix A of this document discusses
cleaning of sample system components.
The data from the API 14.1 sampling project dearty demonstrated that misuse of the Gas Sampling Separator could distort the
sample. The current revision of this GPA publication includes language to darify the proper use of the separator. It disa.asses when
the Gas Sampling Separator would be appropriate and explores the potential pitfalls associated with its misuse.
3
Obtaining Natural Gas Samples for Analysis by Gas Chromatography
1. ~
1.1. The purpose of this publication is to recommend procedures for obtaining samples from flowing natural gas streams that
represent the composition of the vapor phase portion of the system being analyzed. These representative samples are
subsequently transported to a laboratory and analyzed for composition and/or trace contaminants or analyzed onsile by portable or
on-line chromatographs.
1.2. The methods outlined in this publication are designed for sampling natural gas from systems that are at or above the
Hydrocarbon Dew Point temperature. As the temperature of the flowing stream decreases or the pressure increases to impinge
upon the Hydrocarbon Dew Point, it becomes increasingly difficult to obtain a representative sample of the flowing stream. This
standard does not address accounting for the liquid hydrocarbon portion of two-phase systems.
1.3. The scope of this standard does not indude composite gas sampling (samples taken in increments over relatively long time
periods) systems. For information on composite sampling, the reader is referred to API 14.1 and ASTM 05287.
1.4. Due to a lack of supporting research data, the scope of this standard does not indude sampling from vacuum sources.
2. ~
2.1. General notes
2.1.1. Note 1
Streams containing hydrogen sulfide should be analyzed for hydrogen sulfide on site in the field.
2.1.2. Note 2
Moisture concentration cannot be determined from a sample container in a laboratory. Moisture determination in natural gas
streams must be performed on site in the field or by moisture saturation calculations.
2.1.3. Note 3
All sampling system components between the sample point valve as defined in note 4 and the sample cylinder must be maintained
above the Hydrocarbon Dew Point temperature. To date, the most accurate determination of Hydrocarbon Dew Point is the
Chilled Mirror TesL By definition, the gas-phase portion of the product flowing in a two-phase system is at the Hydrocarbon Dew
Point temperature. Calculated Hydrocarbon Dew Points are only as accurate as the accuracy of the calculation method and the
detail and accuracy of the analysis.
Any component of the sampling system that separates unwanted liquids from the sample stream must be operated at flowing line
temperature and pressure.
Downstream of the sample conditioning components of the sampling system, and where sample is to be purged, the downstream
components must be maintained ~ the Hydrocarbon Dew Point temperature.
For purposes of this publication, the Hydrocarbon Dew Point temperature is considered one of the following: the flowing line
temperature (at flowing line pressure), the value determined by a Chilled Mirror Test (at flowing line pressure), or 30 "F (17C)
above the calculated Hydrocarbon Dew Point temperature. If the product flowing in the line is completely in the vapor phase the
flowing line temperature is, of course, above the Hydrocarbon Dew Point temperature for the line pressure. But if any droplets of
liquid have condensed in the flowing product stream, the flowing line temperature is equal to the Hydrocarbon Dew Point temper-
ature for the line pressure. Therefore, if sample system components are maintained above flowing line temperature and at line
pressure. the sampling system components will be above Hydrocarbon Dew Point temperature (unless the line is 100% liquid full).
2.1.4. Note 4
In Section 9, Sampling Procedures, the term -sample point valve- or "valve at sample poinr refers to the valve at the outlet of the
Sample Probe, regulator, membrane filter. Gas Sampling Separator or combination thereof.
4
2.1.5. Note 5
Pressure drops due to pressure regulators or flow control devices cause reduction in temperature due to the Jou~Thomson
Effect. This can cause condensation in the sampling system. Therefore it may be necessary to heat regulators that are used to
reduce the sample pressure.
For some sampling methods listed, flow control devices such as flow control plugs or valves should be located at the outlet of the
Sample Container. These flow-eontrolling devices can cause cooling due to the Joule-Thomson Effect. To thennally isolate this
cooling effect from the Sample Container, flow control devices should be placed at the outlet end of an Extension Tube
("Pigtail"), which is attached to the outlet of the sample cylinder.
Ambient cooling of the sample system can cause heavy hydrocarbons to condense out of the vapor phase. The presence of any
condensation in the sample inlet system will cause the sample to be non-representative. Condensation must be avoided In the
entire sample system from sample probe to sample cylinder outlet or chromatograph inlel
2.2. Safety Notes
2.2.1. Safety Note 1

Hydrocarbon vapors are flammable and can be explosive. They can also replace breathing air. Refer to employer-provided safety
bulletins. The sampling technician who uses any of these sampling procedures should be property trained in the safe handling of
natural gas and similar hydrocarbon materials.

Natural gas samples may contain components that cause health hazards other than flammability or replacing breathing air.
Hydrogen Sulfide can be particularly dangerous. Prior to performing any sampling or analytical procedures, the analyst or sampler
should be trained to be familiar with all possible hazardous contaminants, how to monitor for these contaminants and how to
respond to various levels of these contaminants.

In some sampling situations and in most laboratory analysis, heating is required. Care should be taken to ensure that any heating
device meets the requirements of all apprlCable codes.
Exceeding temperature limits could result in failure of components, fire and/or explosion. Electrical heating devices should be setf-
limiting to ensure that temperature limits are not exceeded. Electrical heating devices should have at least two methods of
temperature control.
The Compressed Gas Association, Inc. states in CGA P-1-1991 that the temperature of compressed gas cylinder components
should not exceed 125F (51.70C). If it is deemed necessary to heat the sample system components ensure that, acx:ording to
manufacturer's specifications, all components in the sample system are rated for the higher temperature.

If the container is to be transported, it must meet local transportation regulatory specifications and be labeled according to the local
transportation regulations. Containers should meet appropriate pressure and pressure relief requirements and should be safely
secured in the transporting vehide. Those who transport or ship Sample Containers must be trained in the current regulations. In
the United States, refer to Hazardous Materials Regulations of the D.c.T. (CFR 49).

There is a theoretical possibility for auto-ignition of natural gas and air mixtures in gas sample cylinders if improperly filled (rapidly
pressurized). Rapid opening valves should not be used in the sampling system. The only exception is that the outlet of the sample
probe may have a ball valve.
Care should be taken to avoid rapidly opening the sample probe outlet valve to an open cylinder that is filled with air. The
procedures outlined in this method are designed, through valve operation sequences, to prevent rapid filling of the cylinder.
5
Natural gas is often handled at high pressures. The sampling technician must be properly trained to work with compressed gasses.
All sampling equipment should be rated equal to or higher than the highest expected pressure. Pressure reduction from pipeline to
rated sample system pressure must be carried out with appropriately designed pressure regulators. Pressure relief devices should
be used to protect from over pressure conditions.
3. Ust of Methods
3.1. A gas sample is transferred from the source into a Sample Container or gas chromatograph by one of the following
methods:
3.1.1. Purging - RII and Empty Method

3.1.2. Purging - Controlled Rate Method
3.1.3. Evacuated Container Method
3.1.4. Reduced Pressure Method
3.1.5. Helium "Pop" Method
3.1.6. Glycol or Water Displacement Method
3.1.7. Floating Piston Cylinder Method
3.1.8. Portable or On-Une Gas Chromatograph
3.2. The sampling system design and the sampling method selected will depend upon composition, pressure, temperature and
Hydrocarbon Dew Point of the sample at source conditions.
4. General Infonnation
4.1. The objective of the listed sampling procedures is to obtain a representative sample of the gas phase portion of the flowing
stream under investigation. Any SUbsequent analysis of the sample. regardless of the aco.Jracy of the analytical procedure. will not
reflect the true composition of the flowing stream unless a representative sample is obtained. This method assumes all procedures
begin with dean, leak-free Sample Containers. Sample Containers are discussed in section 7.1 and their preparation is
discussed in Appendix A.
4.2. Entrained or free-flowing hydrocarbon liquids are generally collected and accounted for in a condensate recovery system.
These liquids are not desired in the vapor phase portion of the accounting system. Other contaminants such as water. oil, glycol,
amine, etc. are not desirable in the Sample Container. Since free-flowing liquids tend to flow along the bottom of the pipe or flow
along the walls of the pipe. it is necessary to have a Sample Probe extending into the pipe. Sample Probes are discussed in
section 7.5.
4.3. Flow disturbances may cause contaminants to form aerosols that can be ingested by the Sample Probe. These aerosols
should be removed by filtration or separation in the sample system. Care should be taken not to alter the composition of the sample
with these devices. Refer to section 7.3.1.
4.4. A Gas Sampling Separator may help to eliminate contaminants. Gas Sampling Separators are designed and tested to
protect the analyzer from liquid contamination. They should not distort the composition of the sample. Proper use of Gas Sampling
Separator is discussed in Appendix B.
4.5. Permanent or portable filters may be used. It is important to ensure that the filters are dean. Filters should only remove the
unwanted contaminants and allow all components of interest to freely pass. Refer to section 7.3.1.
4.6. It is difficult to write sampling instructions explicit enough to cover all cases. Natural gas samples should be obtained under
conditions that will not aeate condensation or vaporization in the sample system during the sampling process. This requires an
understanding of the Phase Diagram for the stream to be sampled. Condensation due to the Joule-Thomson Effect or from
ambient chilling can distort the sample. Retrograde condensation is difficult to predict without an understanding of the Phase
Diagram for the product to be sampled. Discussion of the Phase Diagram and the Joule-Thomson Effect can be found in API
Chapter 14.1.
6
4.7. Condensation may occur in the Sample Container during shipment. This condensation is not hannful provided that, prior
to withdrawing any sample from the cylinder, the cylinder is heated sufficiently to ensure that all condensed liquids are returned to
the vapor phase. The Sample Container must be heated prior to analysis. This will ensure complete vaporization of any liquid that
has condensed after sample proaJremenl Refer to GPA 2261 for proper handling of gas samples in the laboratory.
5. HydrOcarbon Dew point
5.1. \Nhen the nature of the gas is completely unknown, the safest procedure is to assume that it is at the Hydrocarbon Dew
Point temperature.
5.2. The initial detennination of the system Hydrocarbon Dew Point temperature should be executed as described in API 14.1.
Generally, this involves directly measuring the hydrocarbon (and water) dew point, calculating the dew point from a previous
analysis or by collecting historical data. For any flowing gas stream that has both a vapor and liquid component, the Hydrocarbon
Dew Point temperature of the vapor phase portion of the stream for line pressure is the temperature of the flowing gas stream.
5.3. The Hydrocarbon Dew Point must be considered when designing the sampling system and selecting the sample method.
5.4. The sampling procedure should be selected as specified in Section 6. This section discusses systems that are well above
the Hydrocarbon Dew Point as well as systems that are at or near the Hydrocarbon Dew Point
6. Guide for the Selection of a proper SamDling procedure
See Table 1 for recommended equipment for each sampling procedure.
6.1. Purging - Fill and Empty Method

This method can be used when the vapor phase portion of the flowing stream is at or above the Hydrocarbon Dew Point
temperature. The temperature of the sample equipment downstream of the Sample Valve (Valve 1) must be maintained above the
expected Hydrocarbon Dew Point (see Note 3, section 2.1.3) throughout the sampling process. It is necessary to use an Extension
Tube ("Pigtail; with a flow control drilled plug or valve when using this method. It is important to adhere to the recommended
number of purge cycles (See Table 3) to ensure that a representative sample is secured. Source pressure must be at least 15 psig
(103 kPa guage).
6.2. Purging-Controlled Rate Method

This method can be used only when the vapor phase portion of the flowing stream is above the Hydrocarbon Dew Point (see Note
3, sedion 2.1.3). Source pressure must be sufficient to produce critical flow conditions in flow plug (pressure of 15 psig (103 kPa
guage) or greater and flow tube exhaust to the atmosphere). Extreme care should be used to prevent condensation during the
sampling process. It is necessary to use an Extension Tube ("Pigtail; with a drilled plug when using this method. It is important to
adhere to the recommended purge time (See Charts 1,2,3 and 4) to ensure that a representative sample is secured.
6.3. Evacuated Container Method

temperature. Users are cautioned that most valve styles are not vacuum-tight. Therefore, it is recommended that the cylinder be
evacuated immediately prior to sample proaJrement. Source pressure must be at least 15 psig (103 kPa guage).
6.4. Reduced Pressure Method

temperature. There may be one or two objectives for reducing pressure: to reduce high pipeline pressures down to the pressure
rating of the sampling equipment and/or to reduce the pressure enough to ensure that the sample is comfortably in the vapor phase.
However, it is possible to reduce pressure and produce Retrograde Condensation in the process. This method is only applicable if
the pressure reduction does not aoss the phase boundary. See Section 8, Heating. See API 14.1 for discussion of the Phase
Diagram. Source pressure must be at least 15 psig (103 kPa guage).
Safety Note: All sampling equipment should be rated for the highest expeded sample pressure. Pressure reduction to sample
system rated pressure must be accomplished with appropriately designed pressure regulators and pressure relief devices.
7
6.5. Helium Pop" Method
temperature. The gas source pressure must be greater than the helium pre-charge pressure. This method assumes that the
chromatograph carrier gas is helium, that helium is not a component of interest and that helium does not interfere with any
component of interest Source pressure must be at least 15 psig (103 kPa guage).
6.6. Glycol or Water Displacement Method

temperature. The user is cautioned to remove all glycol or water during the sampling process. The glycol or water, if left in the
Sample Container, may absorb or desorb sample components such as C02 or H2S. Glycol or water can also cause damage to the
analytical equipment This method should not be used when water or other glycol-soluble components are induded in the
components of interest When the ambient temperature is below 320F (O"C), glycol should be the displacement medium. When the
ambient temperature is above 320F (O"C), glycol or water may be used as the displacement medium. Source pressure must be at
least 15 psig (103 kPa guage).
6.7. Floating Piston Cylinder Method

temperature. The user is cautioned that the seals or lubricants used in Floating Piston Cylinders may absorb sample components.
Piston, seal and lubricants should be verified to be inert to sample components. Sample pressure must be sufficient to overcome
the friction of the piston seals, allowing the piston to move. Source pressure must be at least 15 psig (103 kPa guage).
6.8 Portable and On-Une Gas Chromatograph Method

The portable and on-line gas chromatograph sampling method can be used when the vapor phase portion of the flowing stream is
at or above the Hydrocarbon Dew Point temperature. It may be necessary to use a regulator to reduce line pressure to the
required pressure for the portable or on-line gas chromatograph. For a guide to proper sampling of these devices, see Appendix C
(Portable) and Appendix 0 (On-Une). Pressure reduction through the regUlator will cause a drop in temperature, which may cause
the gas to drop below the Hydrocarbon Dew Point. To counteract the effects of the Joule-Thomson Effect., Ambient Cooling or
Retrograde Condensation, it may be necessary to heat trace the regulator and sample tubing. See Section 8, Heating. See API
14.1 for discussion ofthe Phase Diagram. Source pressure must be at least 15 psig (103 kPa guage).
7. APPARATUS
see Table 1 for recommended equipment for each sampling procedure.

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8
7.1. Sample Containers
7.1.1. Single Cavity (Constant Volume) Cylinders (Figure 1)
Figure 1 (Single Cavity Sample Cylinder)
Pressur Outlet
Relief Valve
Sample
Container
Inlet
Valve
7.1.1.1. Use metal Sample Containers of a type that ensures maximum safety and which are corrosion resistant to the product
being sampled. Cylinder components must be non-reactive to materials being sampled, the pressurizing fluid, the deaning solvents
and the expeded corrosive sample stream components. The Sample Container and all associated components should not alter
the composition of the sample during the sampling, storage, and transportation or analysis process. Stainless steel containers are
recommended to minimize problems of surface Adsorption of heavy sample components (hexanes and heavier components) and
to minimize the reaction of carbon dioxide with the container. Ifthe container is to be transported, it must meet local shipping and
labeling regulations. Refer to section 2.2.4, Safety Note 4. The container may be of the one-valve or twa-valve type (depending
upon the sampling procedure selected). Sample Containers and valves must have a wor1(ing pressure equal to or exceeding the
maximum pressure anticipated in sampling, storage, or transportation of the Sample Container. Soft-seated valves are preferable
to those having metal-ta-metal seats. The size of the container depends upon the amount of sample required for the anticipated
laboratory tests and upon handling considerations.
7.1.1.2. Constant volume (single cavity) cylinders used for sampling nalural gas must be dean and free of leaks. See section
Appendix A on Cleaning Requirements.
9
-
7.1.1.3. All valves and safety devices must meet the appropriate material and pressure requirements for safe design. The pressure
relief devices may be of spring or rupture disc type. These allow a partial or complete loss of contents in the event of thermal
expansion or over-pressurization. The safety device should indicate if it has operated. If the safety device has operated, it must be
assumed that the sample has been compromised. For some sample cylinder volumes, a pressure relief device may not be required.
Refer to transportation regulations that may apply.
7.1.2. Floating Piston (Constant Pressure) Cylinders (Figure 2)
Figure 2 Floating Piston Cylinder
Gage N
Inert Gas Valve Inert Gas Valve
Volume Indicator 1,_"///1..,
Sample Inlet GageM

Valve Sample Pressure
Purge Valve
Sample Valve
Valve 1
Sample Outled Valve
Outlet Valve of Sample Probe,
Gas Sampling Separator.
Membrane Probe Regulator
or other sample preparation device.
7.1.2.1. The Floating Piston Cylinder is constructed of metal tubing, honed and polished on the inside surface. A sealed piston
separates the product side of the cylinder from the pressurizing fluid side of the cylinder. The cylinder must have removable end
caps to provide access to remove and service the moving piston. The end caps are drilled and tapped for valves, gauges and relief
valves. Sample Containers and valves must have a working pressure equal to or exceeding the maximum pressure anticipated in
sampling, storage, or transportation of the Sample Container. Cylinder components must be non-reactive to materials being
sampled, the pressurizing fluid, the cleaning solvents and the expected corrosive sample stream components. The Sample
Container and all associated components should not alter the composition of the sample during the sampling, storage and
transportation or analysis process. Soft-seated valves are preferable to those having metal-to-metal seats. If the container is to be
transported, it must meet local shipping and labeling regulations. Refer to section 2.2.4 Safety Note 4.The size of the container
depends upon the amount of sample required for the anticipated laboratory tests and upon handling considerations.
10
7.1.2.2. The cylinder itself contains a moving piston equipped with o-rings, Teflon rings, or other devices to effect a leak-free seal
between the sample and the pressurizing fluid and is able to move freely within the cylinder. Additional guide rings may be installed
to ensure smooth piston travel. The piston and sealing device must be non-reactive to the sample. the pressurizing fluid. the
cleaning solvents and expected corrosive sample stream components.
7.1.2.3. All valves and safety devices must meet the appropriate material and pressure requirements for safe design. The pressure
relief valves may be of spring or rupture disc type. These allow a partial or complete loss of contents due to thennal expansion or
over-pressurization. The safety device should provide indication if it has operated. If the safety device has operated. it must be
assumed that the sample has been compromised.
7.1.2.4. Some piston-type cylinders have provision for indicating the position of the piston. Other types of Floating Piston
Cylinders are available which have no visual method of direetly determining the sample volume. For these cylinders. a magnet of
some type (or magnetic stud finder) is necessary to follow the movement of the piston.
7.1.2.5. Floating PIston-type cylinders used for sampling natural gas must be dean and free of leaks. See section Appendix A on
Cleaning ReqUirements.
7.2. Sample transfer Line
7.2.1. Material
A sample transfer line should be non-reactive to the sample. It should be rated for the maximum expected pressure and must retain
its strength at the maximum or minimum expected temperature. Stainless steel (304 or 316) and Nylon 11 (or similar) have been
proven to be non-reactive to natural gas components. Stainless steel is preferred for pressures over 1000 psig. or for gases
containing hydrogen sulfide (consider silica or other non-reactive material-lined stainless steel tubing for hydrogen sulfide
applications, as stainless steel is known to adsorb H2S).
7.2.2. Size
7.2.2.1. Length
The sample transfer line should be as short as possible. Inches (em) are preferred to feet (meters). Short lines reduce the heat
transfer to ambient surroundings. If ambient temperatures are lower than the temperature of the system being sampled. cooling of
the sample tubing can cause condensation of the heavier (higher boiling point temperature) components. These condensed
components can then drop out or adhere to the wall, causing the sample to be lighter (fewer heavy components, lower heating
value). Or the accumulated droplets can be swept into the Sample Container. causing the sample to be heavier (higher heating
value) than the product to be sampled.
For the portable or on-line gas chromatograph method, sample transport lag time calculations are helpful in determining appropriate
sample bypass purge rate. The below formula will allow the calculation of the actual sample transport time.
=~[ P+15]
Fs 15
X[530 lJ X[~]
T+460 Zp
t = Purge Time
L = Une Length, ft
V = Tubing Volume, ccIft
Fs Standard Flow, cclmin
P = Actual Pressure, PSIG.
T = Actual Temperature, OF
Zp = Compressibility at P Pressure
This formula was taken from Appendix F; pp 579 and 580; "Process Analyzer Sample Conditioning System Technology" by
Robert E. Sherman; Wiley Interscience. and modified for Gas Compressibility by ABB Totalflow Projed Engineering.
11
7.2.2.2. Diameter
The diameter should be as small as possible while ensuring adequate flow through the system.
For spot sampling, the transfer line should have a minimum diameter of 1/4 in (6 mm). To ensure that refrigeration associated with
the Joule-Thomson Effect occurs some distance down stream of the Sample Container, the smallest diameter component in the
spot sample system should be the orifice in the drilled plug at the end of the Extension Tube ("Pigtail") attached to the outlet of
the sample cylinder. The drilled plug can be replaced with a flow control valve provided that the internal diameter of the flow control
valve is smaller than any other component in the sampling system.
For the portable and on-line gas chromatograph method, the sample transfer line would generally have a diameter of 1/16 in (1.5
mm) to % in (6mm). For the portable or on-line gas chromatograph method. sample transport lag time calculations are helpful in
determining appropriate sample line diameter.
7.2.3. Insulation and Heating

Sample transfer lines must be maintained above the Hydrocarbon Dew Point (see Note 3. section 2.1.3). See section Section 8
for heating requirements.
For very short connections between the sample point and the Sample Container, the sample transfer line can be insulated without
supplemental heating. Care should be taken to ensure that this short transfer line is at the same temperature as the sample source
prior to transferring sample to the Sample Container.
7.2.4. Cleaning
Oil in the transfer line can selectively absorb and desorb hydrocarbon components. altering the sample composition. Since new
stainless steel tubing may have machine oil from the manufacturing process, sample transfer lines should be steam cleaned and
dried prior to installation. Refer to Appendix A for cleaning guidelines. Other cleaning methods are acceptable if they can be
demonstrated to leave no residue.
7.3. Sample Une Separators and Filters
7.3.1. Research has shown that misuse of sample line separators and filters can cause sample distortion. Refer to Appendix B.
Separators and Membrane Filters. These devices are intended, and must be appropriately designed, to remove contaminants from
natural gas sampling systems without altering the sample quality. The objective is to remove contaminants without removing
components that are part of the vapor-phase of the flowing gas stream. Contaminants include, but are not limited to, oil. glycol.
amines, water and free-flowing condensed hydrocarbon liquids. Filters should be frequently checked for contamination and cleaned
or replaced if necessary. Separators and filters must have a pressure rating equal to or higher than the pressure of the sample
source.
7.3.1.1. It is imperative that the Gas Sampling Separator temperature and pressure match the flowing natural gas temperature
and pressure throughout the sampling process.
7.3.1.2. It is imperative that the temperature and pressure of filters that are used as a separator (installed upstream of any
pressure-reducing regulator) match the flowing natural gas temperature and pressure throughout the sampling process.
7.3.1.3. Filters that are installed in the sample system after a pressure-reducing regulator must be operated above the Hydrocarbon
Dew Point (see Note 3, section 2.1.3). The Joule-Thomson Effect from the pressure drop across a filter must also be considered
when determining the heating requirements. See Section 8, Heating Requirements.
7.3.2. Special care must be used when using the Gas Sampling Separator (See Figure 3). The separator must be insulated. A
thermometer must be installed to ensure that the separator is operating at line temperature. If the temperature is below line
temperature. it will tend to remove heavy (high temperature boiling point. high heating value) components from the sample stream.
If it is above line temperature. it will tend to increase the concentration of heavy components in the sample. The outlet of the
separator may require supplemental heat to ensure that the product from this point to the sample cylinder is completely in the vapor
phase. See section Section 8. Heating Requirements. The separator is only useful for sample streams containing unwanted
condensed hydrocarbon droplets. oil, amine. glycol, water or other contaminants. For dean. dry sample streams above the
Hydrocarbon Dew Point (see Note 3, section 2.1.3), the separator serves no useful purpose and its misuse could corrupt the
sample. See section Appendix B on the use of the Gas Sampling Separator.
12
Figure 3 Gas Sampling Separator
Separator Outlet Valve

(Valve 1 in Sampling Methods)
Insulation
Thermometer
Extension Tube
Outlet Valve
7.3.3. An acceptable method for removal of unwanted contaminants is a membrane filter (See Figure 4) inserted directly in the
line. This type of filter is, by virtue of its location in the pipe, at the same temperature and pressure as the sample source. This
eliminates condensation or vaporization of heavy components due to changes in temperature or pressure. See section Appendix B
for discussion of the use of membrane filters.
7.3.4. External filters may be used to eliminate contaminants from the sample stream. If the filter is operated at line pressure, it
must be operated at line temperature. If it is above line temperature, it may vaporize liquid contaminants to artificially enrich the
sample. If it is below line temperature, it may condense components to artificially reduce heavy components in the sample.
If extemal filters are used after pressure reduction or after a separator or membrane filter, the filters must be operated above the
Hydrocarbon Dew Point (see Note 3, section 2.1.3).
7.3.5. Separators and filters used for sampling natural gas must be dean and free of leaks. See section Appendix A on Cleaning
Requirements.
13
Figure 4 Membrane insertion probe with regulator
Regulato
Sampl -----NPT
Outlet
~----Tt __.. ol Fins;
Membrane 1-----s('Qt and Poppet

"'s~rtlly
11"'~---"H'GN>n~ IntckQ
Foot Valve As_"*"y
Fixed Probe Style Regulo.tor with MeMbra.ne TIp
7.4. Sample Points
7.4.1. The most current version of API 14.1 should be reviewed prior to installation of a sampling system. (At the time of
publication of this document, the most current version was June 2001).
7.4.2. The sample point should be located at the top of a straight section of horizontal pipe.
7.4.3. Care should be used in selecting the location of sampling points. Flow-disturbing elements such as control valves, headers,
elbows, tees and orifice plates can cause pressure and temperature disturbances in the flowing gas stream immediately
downstream of the disturbance. These disturbances can change the vapor I liquid equilibrium. It is important that the sample point
be separated from flow disturbing elements far enough to avoid the areas of flow disturbance.
7.4.3.1. For samples that are well above the Hydrocarbon Dew Point temperature any probe location will suffice as long as it does
not interfere with the performance of a primary metering element
7.4.3.2 For samples that are at or near the Hydrocarbon Dew Point temperature, the sample point must be separated at least 5
diameters of the flow disturbing element from flow disturbing elements. For example, if a temperature probe has a diameter of 1",
the sample probe must be at lease 5 temperature probe diameters or 5" downstream of the temperature probe.
7.4.4 The sample point must not be installed within the flow measurement portion of the meter tube, since the fitting and probe
could produce disturbances in the flow profile to the meter. Refer to the relevant document for the primary measurement device
being used.
14
7.4.5 The sample point should be within the flowing stream where the product is well mixed.
7.5. Sample Probe (Figure 5)
7.5.1. Contaminants such as oil, water, amine or glycol tend to flow along the inside wall of the pipe. An insertion probe helps to
ensure that the sample is withdrawn from the portion of the product stream that is free of these contaminants.
There exists, along the pipe wall, a laminar flow area which may not represent the product that is flowing through the pipe. At
normal flow velocities, this laminar flow section is very thin. The Sample Probe should ensure that the sample is withdrawn from the
turbulent flow region.
The end of the probe may be square cut or diagonally cut. If the probe is diagonally cut, it should be oriented such that the longer
part of the diagonal is facing upstream. 'Mth this configuration, small droplets entrained in the product stream will generally have
enough inertia to pass by the probe without being withdrawn into the sample system.
Figure 5 Gas Sample Probe
Nipple
PiPelin\
7.5.2. Probe Length

It has been an industry practice that the collection end of the probe be placed within the approximate center one-third of the pipe
cross-section. 'vVhile it is necessary to avoid the area most likely to contain migrating liquids (the pipe wall) it may also be necessary
to limit the probe length to ensure that it cannot fail due to the effects of resonant vibration.
Resonant vibration can occur when the vortex shedding frequency resulting from a probe inserted into a flowing fluid is equal to or
greater the probe's natural resonant frequency. Table 2 provides maximum probe lengths for typical diameters based on a
maximum natural gas velocity of 100 ftlsec.
15
Table 2
Recommended Maximum Sample
Probe Len2tbs
Probe Ouler Recommended
Diameter (inches) Maximum Probe
Length (inches)"
0.250 2.00
0.375 3.25
0.500 4.25
0.750 6.50
Calculations were:: based on a maximum probe
length Strouhal Number of 0.4. :l 0.035 inch
wall thickness. maximum flow velocity of 100
ft.sec. and 316 stainless steel ( E = 28.000.000
PSI. r = 7.96 elcc) orobe construction.
7.5.2.1. Probe Length Calculation SI Units

The maximum insertion probe length (from the end of the probe to the point of attachment) can be calculated (from EEMUA
Publication No. 138:1988) using the following formula:
L= jFrox4.38X OOx 10 x.J (EIr) x(OD' + IDJ)

SxV
'v\Ihere:
L= Permissible Probe Length (mm)

Fm = Virtual mass fador - a constant to take account of the extra mass of the cylinder due to the fluid surrounding it & vibrating
=
with it. For a gas, Fm 1.0 and for water & other liquids Fm 0.9 =
00 = Outside Diameter of the Probe (mm)
10 = Inside Diameter of the Probe (mm)
S = Strouhal number - dependent on the Reynolds number and the shape of the cylinder, but can be taken as 0.4 for worst
case or 02 as suggested by API Chapter 8.
V = Velocity of fluid (m/sec)
E= Modulus of Elasticity of probe material (kglcm2)
r= Density of probe material (kg/m3)
7.5.22. Probe Length Calculation American Engineering System Units
The maximum insertion probe length (from the end of the probe to the point of attachment) can be calculated (based on EEMUA
Publication No. 138:1988) using the following formula:
L = j Fro x 1.194 x 00 x.J (Fir) x (Ool + JD1)

SxV
'v\Ihere:
L = Permissible Probe Length (inches)

Fm = Virtual mass fador - a constant to take account of the extra mass of the cylinder due to the fluid surrounding it & vibrating
=
with it. For a gas. Fm 1.0 and for water & other liquids Fm 0.9 =
00 = Outside Diameter of the Probe (inches)
10 = Inside Diameter of the Probe (inches)
S= Strouhal number - Use 0.4 for worst case
V= Velocity of fluid (ftisec)
E = Modulus of Elasticity of probe material (psi)
r= Density of probe material (glcm3)
16
7.5.3. Under no circumstances should the Sample Probe be longer than 10".
7.5.3. Caution: Harmonics may cause embrittlement of the metal. Poorly designed Sample Probes may bend or break off in the
flowing gas stream.
7.5.4. This section (section 7.5) should be carefully considered when designing a Sample Probe.
7.6. Pressure Regulators

Regulators may be used to reduce sample pressure from the source pressure to a useable pressure for the sampling equipment or
analytical devices. They may also be used to reduce pressure to keep the stream below the Hydrocarbon Dew Point pressure.
The regulator may need to be heated to prevent condensation from the Joule-Thomson Effect cooling or to prevent Retrograde
Condensation.
Pressure regulators can be part of the insertion probe (Figure 4). This allows heat from the flowing product stream to assist in
heating the sample back up to sample point temperature. The flow rate through insertion probe regulator affects the recovery of
product temperature. It is necessary to verify that the sample is sufficiently heated. Supplemental heating may be necessary. See
section 8, Heating Requirements.
7.7. Extension Tube ("Pigtail") (Figure 7)

The smallest diameter portion of the sample system will be the point of maximum pressure drop. This pressure drop causes
reduction in temperature due to the Joule-Thomson Effect. Extension Tubes ("Pigtails") are used to thermally isolate the outlet
valve of Sample Containers from this cooling effect during the purging process. This piece of tubing is typically X" in diameter and
at least 36" in length. If it is coiled. the user is cautioned to leave enough air gaps between coils to prevent thermal coupling of the
coils.
Figure 6 Extension Tube ("Pigtail")
Sample Container
Outlet Valve
Sample Container Extension Tube

or Pigtall"
Sample Container
Inlet Valve
Purge Valve-
l
Extension Tube Outlet Valve
and Drilled Flow Plug
TIp 01 Probe
17
7.7.1. To ensure that cooling from flow regulation occurs at the outlet end of the pigtail, a flow regulating valve or flow regulating
plug must be installed at the end of the pigtail. The internal diameter of the flow regulating valve must be the smallest diameter of all
the sampling system components. The hole in the plugs should be the smallest diameter part of the sample system. Details of the
flow plug are shown in Figures 7 and 8. To achieve the optimum heat-of-eompression results in the Purging-Fill and Empty Method.
the optimum diameter for the hole in the flow control plug or the port diameter of the flow control valve should be 1/16" to 1/8".
Figure 7 Flow Plug 1/8" Port
1/4" NPT Hex Head Pipe Plug
316 Stainless Steel
3/16"
Figure 8 Flow Plug - Various Port Sizes
do Drill Drill L Notes

0.0050 0.0520 55 0.013
0.0100 0.0995 39 0.025
0.0145 79 0.1440 27 0.036
0.0200 76 0.2010 7 0.050
0.2090 4 Same as do 0.523 O. I" Dim Not Held
1/4 in. Hex Head Pipe Plug

316 Stainless Steel
82 deg.
L 0.1 in
18
8. Heating requirements
8.1. General Heating Requirements

The gas being sampled must be maintained above the Hydrocarbon Dew Point throughout the sampling process to ensure the
sample remains in the gas phase from the sample point through the collection vessel. The application of supplemental heat to the
sampling system may be necessary to counteract possible condensation caused by the Joule-Thomson Effect or fractionation of
the sample when the temperature of the sampling apparatus falls below the Hydrocarbon Dew Point It is imperative that the gas
being sampled be maintained above the Hydrocarbon Dew Point (see Note 3, section 2.1.3) throughout the sampling process.
8.1.2. Supplemental heating apparatus

The apparatus used to supply additional heat may be of any type that confonns to applicable codes and regulations. Hot oil,
catalytic heaters, hot water (or water I glycol mix), steam or electrical methods have been used successfully.
Electrical heating tapes must be self-limiting or controlled with temperature limiting devices. Two methods of temperature control
are required. Under no circumstance should any component of the sampling system, such as the sampling probe, regulator, tubing,
valves, filter, regUlator or sample cylinder, be heated above manufacturer's recommended maximum temperatures.
8.2. Sample system heating requirements
82.1. When using a separator or filter to remove unwanted contaminants, the separator or filter should be maintained at the
same temperature and pressure as the gas in the line being sampled. Maintaining the separator at any conditions other than those
of the line may cause sample distortion.
8.2.1.1. If the pressure of the separator or filter is at line pressure but the temperature is higher than fine temperature, unwanted
liquid hydrocarbons may vaporize and artificially enrich (higher BTU value) the sample.
8.2.1.2. If the pressure of the separator or filter is at line pressure but the temperature is lower than line temperature, portions of the
vapor phase may condense, be removed by the separator or filter, and artificially deplete (lower BTU value) the sample.
8.2.1.3. Variations in pressure from line pressure may have similar results
8.2.2. Dead End and Displacement Methods

Generally, additional heat is not required when using the evacuated container, helium "pop", water displacement, glycol
displacement or piston cylinder methods. When additional heat is required, the system must be heated from the sample source
outlet valve through the inlet valve of the sample collection container.
8.2.3. Purge Methods

When using the purge, fill and empty or continuous purge methods and additional heat is required, the system must be heated from
the sample source through the outlet valve of the sample collection container. When using a separator or filter to remove unwanted
contaminants, the separator or filter should be maintained at the same temperature and pressure as the gas in the line being
sampled. Maintaining the separator at any conditions other than those of the line may cause sample distortion by condensing or
vaporizing components, compromising the sample.
8.2.4. Pressure Reduction Methods
8.2.4.1 A separator or filter may be used between the sample point and the point of pressure reduction. When using a separator or
filter to remove unwanted contaminants, the separator or filter should be maintained at the same temperature and pressure as the
gas in the line being sampled. Maintaining the separator at any conditions other than those of the line may cause sample distortion.
See the discussion in section 8.2.1.
8.2.4.2. When using the reduced pressure, portable or on-line gas chromatograph methods and additional heat is required, special
attention should be directed to the pressure reducing devices to ensure the gas is maintained above the expected Hydrocarbon
Dew Point (see Note 3, section 2.1.3) throughout the sampling process. The system must be heated from the sample source
through the pressure-reducing device to prevent condensation due to the Joule-Thomson Effect and downstream of the pressure-
reducing device if ambient conditions require. If extemal fmers are used after pressure reduction or separation, the filters must be
operated above the Hydrocarbon Dew Point (see Note 3, section 2.1.3). Refer to Appendix C and 0 for sampling guidelines.
19
9. SAMpLING PROCEPURES for Soot samoles
9.1. Purging - Fill and Empty Method
The equipment arrangement is shown in Figure 9 and 9a. To minimize the potential for ambient cooling, the tubing and purge valve
section between the sample point outlet valve (Valve 1) and the sample container inlet valve should be kept as short as possible. It
is necessary to connect an Extension Tube ("Pigtail") (refer to section 7.7) with a valve or orifice restriction on the discharge end
to the outlet valve of the container. This arrangement pushes the temperature drop associated with the Joule-Thomson Effect to
the end of the Extension Tube ("Pigtail") and eliminates the possibility of heavy hydrocarbon condensation in the sample
Container outlet valve. To facilitate rapid blow-down for the Purging - Fill and Empty Method, a flow- regulating valve may be used
to replace the flow plug. The internal diameter of the f1ow- regulating valve must be the smallest diameter of all the sampling system
components.
The temperature ofthe sample equipment downstream of \he Sample Valve (Valve 1) must be maintained above the expected
Hydrocarbon Dew Point (see Note 3, section 2.1.3) throughout the sampling process. If the sample cylinder is initially pre-heated
to line temperature, studies have shown that the heal of compression generated during the fill and empty cydes will keep the
sample cylinder above the expected Hydrocarbon Dew Point temperature.
The procedure for sampling by this method is as follows:
Figure 9 Purging. Fill and Empty And Purging, Controlled Rate Methods
Sample Container
Outlet Valve
Extension Tube
Sample Container or "Pigtail"
Sample Container
Inlet Valve
Purge Varve
Sample Valve
l
Valve 1
Sample QuIet V.ve

Outlet Valve at Sample
Probe. Gas Sampling
Sepa~.~brane
Probe Regulator or other Extension Tube Outlet Valve and Drilled Flow Plug
sample preparation
devic;e
20
------------------------------------- -- --
Figure 9a Purging, Fill and Empty And Purging, Controlled Rate Methods
TUbing Should be
as Short as Possible
Sample Valve
Valve 1
Saq>le Oulled Vti.ve
Oullel Vave 01 Sample Probe.
Gas Saqlling s.plRlOf.
Membrane Probe R.lalor
Of OCher slWTlple prep.-ation delrice.
Sample Container
Outlet Valve
Sample Container
Inlet Valve
Extension Tube
or "Pigtail"
9.1.1. Open the valve (Valve 1) at sampling point and thoroughly blow out any accumulated material. Close valve at sampling
point. Purge time should be long enough to blow out contaminants but not so long as to chill the sample point valve.
9.1.2. Install sample Container as shown in Figure 9 or 9a. The container should be in a vertical position. With all valves dosed,
open Sample Valve (Valve 1) at sampling point to fully open position.
9.1.3. Open purge valve at sampling point and gently blowout any accumulated material. Close purge valve.
9.1.4. Slowly open the Sample Container Inlet Valve to pressure Up the Sample Container. (Refer to safety note 5). Open the
Sample Container Outlet Valve. Open the Extension Tube ("Pigtail") Line Valve. Purge the line slowly with gas to displace air.
(Valves 1, Sample Container Inlet Valve, the Sample Container Outlet Valve and the Extension Tube ("Pigtail") Une Valve
should be fully opened. The Purge valve should be shut.)
9.1.5. Close the Extension Tube ("Pigtail") Une Valve and allow the pressure to build up rapidly to sampie supply pressure.
9.1.6. Close the Sample Cylinder Inlet Valve. Open the Extension Tube ("Pigtail") Une Valve and vent the container through the
Extension Tube ("Pigtail") Line Valve to almost atmospheric pressure. Close the Extension Tube ("Pigtail'1line Valve.
9.1.7. Open the Sample Cylinder Inlet Valve and allow the pressure to build up rapidly to sample supply pressure.
21
9.1.8. Repeat steps 9.1.6 and 9.1.7 to comply with Table 3 which gives the minimum number of cydes required to effectively
purge the container of the original gas in the container.
Table 3
Fill and Empty Purge Cycles
Maximum Gas Pressure Number of Fill
in Container, pslg (kPa guage) And Empty Cycles
15-29 (100-200) 13
30-59 (200-405) 8
60-89 (405-615) 6
90-149 (615-1025) 5
150-500 (1025-3450) 4
>500 (>3450) 3
# of Purge Cycles = log (xlY
\fIIhere:
x = atmospheric pressure + fill pressure (psia)
y = maximum allowable mole fraction of contaminants
9.1.9. Close the sample valves in the following order. Extension Tube ("Pigtail") Une Valve, Sample Cylinder Outlet Valve,
Sample Cylinder Inlet Valve and sampling valve (Valve 1).
9.1.10. Slowly open the Extension Tube ("Pigtail") Une Valve. Observe for trace of liquid in the discharge of the Extension Tube
("Pigtail") Line Valve. If liquid appears at the Extension Tube ("Pigtail") Line Valve, discard the sample and re select a sample
method as outlined in Section 6. Also review Heating Requirements as outlined in Section 8.
9.1.11. Open the purge valve slOWly to relieve pressure on the sample connection. Depressurize appropriate portions of the
sampling system.
9.1.12. Remove the Sample Container and check for leaks by immersion of the valves in water or by the use of a commercial leak
detection solution. Plug or cap the valves.
Note: More than one container can be filled at the same time.
9.2. Purging - Controlled Rate Method

The equipment arrangement is shown in Figure 9 and 9a. Source pressure must be sufficient to produce critical flow conditions in
flow plug (pressure of 15 psig or greater and flow tube exhaust to the atmosphere). Deviations from the flow curves will occur when
the gas specific gravity is other than 0.600 and the flowing temperature is not 6QOF, however the variation will 6kely be less than
M
10%. For a flow plug bore diameter of 0.125 purge time should be 1 minute for every 100 cc of sample cylinder volume. The
,
procedure for sampling by this method is as follows:
9.2.1. Open valve (Valve 1) at sampling point and thoroughly blowout any accumulated material. Close valve at sampling point.
Purge time should be long enough to blow out contaminants but not so long as to chill the sample point valve.
9.2.2. Install Sample Container as shown in Figure 90r Sa. The container should be in a vertical position. 'Mth all valves dosed.
open valve (Valve 1) at sampling point to fully open position.
9.2.3. Open purge valve at sampling point and gently blowout any accumulated material. Close purge valve.
9.2.4. Slowly open the Sample Cylinder Inlet Valve fully.
9.2.5. Slowly open the Sample Cylinder Outlet Valve fUlly.
22
9.2.6. Slowly open the Extension Tube ("Pigtail") Une Valve fully.
M
9.2.7. Assuming a O. 125 diameter hole in the flow plug, flow In this manner 1 minute for each 100 cc of the sample cylinder
volume. Charts 1.2,3 and 4 show flow times for various hole diameters and various Sample Container sizes. The calculation for
minimum flow time is:
Cylinder Volume in cc
Purge Time
in Seconds
10.800 x (Hole Diameter in inches)1
Chart 1
Purge TIme for10 Volume Exchange
_.
1100 .-~- -
./
V
- - -
-l
1000
7 -r
900 No. 79 DnI ./
IlOO
I No. 76 M
O.ll2'"DaRowTlbe
/ 0.0145" Dia flow TIbt
... L.-/
. ........ / ./
..
o
o
~
700
600
/ ~
~ V ./
L7
...~ 500
=
>.
o 400
7 V 0.01" Da Row Tlbe " - .
~l
/ ..... ~ -- ~
I
i
----
I
300
./ -:;::::;::;= ;
200
/ ~
100
o
~~
/---- : / -- ~ ...
o 60 120 180 300 360
Seconds
Chart 2
Purge TIme for 10 Volume Exchange. Seconds
.. - .. - ..
~
110 ~ -,"
100
90
/
80
/
0.005" aa. AM TIbt /
..
o
o
~
70
60
"> C7'
~
ic 50
/
~
o ~
/
30
V
20
7
./ I
./
0
0
7 -... '. - -
o 80 120 180 300
Seconds
23
Chart 3
Cylinder Volume Purge Times tor 1G-Volume Exchange
55 . - --,-- ------
5
-;7 ,
.5 / i
-:
"b_ [)-I /7
i...
o
3.5
0.209'" Da_ Row Tube
'- /
Q
o
:>
.,;
) Y
E
ci /' 1
I
.
>
~
~
25
2
./
,
>.
o
1.5
/
/
0.5
/ ;
o 1/
o eo 120 180 2<40 300
Second.
Chart 4
Purge Time for 10 Volume Exchange
_.
1800 -- - ----
c
/'"
1600
/-
1.m
./ !
:7
1200 O_I25"IJa.Aow Tube

/
.
E 1000
:>
~ /
"0
>
:
~
800
// ,
I
>.
o
s.
/
/"
600
~
/
V
200
/ I
i
o
/ :
o 2 3 5 6 7 a 10
9.2.8. Close the sample valves in the following order. Extension Tube ("Pigtail") Une Valve. Sample Cylinder Outlet Valve,
Sample Cylinder Inlet Valve and sampling valve (Valve 1).
9.2.9. Slowly open the Extension Tube ("Pigtail") Une Valve. Observe for trace of liquid in the discharge of the Extension Tube
("Pigtail") Line Valve. If liquid appears at the Extension Tube ("Pigtail") Line Valve, discard the sample and select a sample
method for a fIO'Ning gas stream thai is at the hydrocarbon dew point as outlined in Section 6. Also review Heating Requirements as
outlined in Section 8.
9.2.10. Open purge valve slowly to relieve pressure on the sample connection. Depressurize appropriate portions of the sampling
system.
24
9.2.11. Remove the Sample Container and check for leaks by immersion of the valves in water or by the use of a commercial leak
Note: More than one container can be filled at the same time by using a manifold
9.3. Evacuated Container Method

The equipment arrangement is shown in Figure 10. The procedure for sampling by the evacuated container method is as follows:
Figure 10 Evacuated Container Method, Reduced Pressure Method And Helium Pop Method
Pressure I Vacuum Gage
Auxillia Valve
Sample Container
Outlet Valve
Sample Container
Sample Container
Inlet Valve
Purge Valve-
Sample Valve
Valve 1
Sample Outlet Valve
Outlet Valve of Sample Probe,
Gas SalTl>ling Separator,
or other salTl>le preparation
device.
9.3.1. Evacuate the Sample Container to a pressure of 1 mm Hg or less. (Use a cylinder that has been previously evacuated
and tested to hold 1 mm Hg pressure) Evacuation methods require that a vacuum gauge be permanently affixed to the sampling
cylinder to detect any leaks between the time of evacuation and the time of actual sampling in the field. Since many Sample
Container valves are designed to hold pressure rather than vacuum, it is recommended that the vacuum be pulled in the field
immediately prior to sampling. Since standard vaaJum gauges can only be read to about 5% aCClJracy, it is further recommended
that samples collected by evacuation methods be analyzed on the molecular sieve column to correctly determine the concentration
of free nitrogen (see GPA Standard 2261).
9.3.1.1 To evacuate the cylinder in the field, attach the vaaJum tubing to the outlet of the auxiliary valve. With the Sample
Container inlet valve, Sample Container outlet valve and the auxiliary valve shut, start the vacuum pump. Open the auxiliary valve.
Open the Sample Container outlet valve. Wlen the vacuum gage indicates less than 1mm Hg pressure. Shut the Sample
Container outlet valve. Shut the auxiliary valve.
25
9.3.2. Open Sample Valve (Valve 1) at sampling point and thoroughly blowout any accumulated material. Close Sample Valve
(Valve 1) at sampling point.
9.3.3. Install Sample Container as shown in Figure 10. The container should be in a vertical position. With all valves closed,
9.3.4. Slowly purge the sample line with source gas to displace air by partially opening the purge valve until gas is slowly flowing.
Close purge valve at sampling point
9.3.5. \Nhile monitoring the vaaJumlpressure gage, slowly open the Sample Cylinder Inlet Valve, allowing the container pressure
to increase to the source gas pressure. In some cases condensation may be eliminated by sampling at a pressure less than the
source pressure. (See Reduced Pressure Method.) It is possible to reduce pressure and produce Retrograde Condensation in the
process. See API 14.1 for discussion of the Phase Diagram.
9.3.6. Close the Sample Cylinder Inlet Valve and the sampling valve (Valve 1). Open the purge valve to relieve pressure in the
sample line. Depressurize appropriate portions of the sampling system.
9.3.7. Remove Sample Container and check for leaks by immersion of the valves in water or by the use of a commercial leak
detection solution. (Applicable only for sample pressure greater than 15 psia) Plug or cap the valves.
Note: If the final pressure is below 5 psig the sample pressure should be increased to 15 psig in the laboratory by
pressurizing with a gas that will not interfere with the analysis. If the sample is pressurized, the pressure existing
immediately before and after pressurization shall be recorded.
9.4. Reduced Pressure Method
The reduced pressure method is frequently chosen when the sample pressure is greater than the rated pressure of the Sample
Container. In such a situation, extreme caution should be used in the design of the sampling system. Refer to Safety Note 6. If a
pressure-reducing regulator is used, the outlet valve of the regulator is considered to be Sample valve (Valve 1).
It is possible to reduce pressure and produce Retrograde Condensation in the process. See API 14.1 for discussion of the Phase
Diagram.
The equipment arrangement is shown in Rgure 10. The procedure for sampling by the reduced pressure method is as follows:
9.4.1. Prior to sampling, evacuate the Sample Container to a pressure of 1 mm Hg or less. (Use a cylinder that has been
previously evacuated and tested to hold 1 mm Hg pressure) Evacuation methods require that a vaaJum gauge be permanently
affixed to the sampling cylinder to deted any leaks between evaaJation and adual sampling in the field. Since many Sample
Container valves are designed to hold pressure rather than vacuum. it is recommended that the vacuum be pulled in the field
immediately prior to sampling. Since standard vacuum gauges can only be read to about 5% accuracy, it is further recommended
that samples collected by evacuation methods be analyzed on the molecular sieve column to correctly determine the concentration
of free nitrogen (see GPA Standard 2261).
9.4.1.1 To evacuate the cylinder in the field, attach the vaaJum tubing to the outlet of the auxiliary valve. With the Sample
Container inlet valve, Sample Container outlet valve and the auxiliary valve shut, start the vaaJum pump. Open the auxiliary valve.
Open the Sample Container outlet valve. \Nhen the vacuum gage indicates less than 1mm Hg pressure. Shut the Sample
Container outlet valve. Shut the auxiliary valve.
9.4.2. At the sample point, open valve (Valve 1) at sampling point and thoroughly blow out any accumulated material. Close valve
at sampling point
9.4.3. Install Sample Container as shown in Figure 10. The container should be in a vertical position. With all valves dosed.
26
9.4.5. VVhile monitoring the vaoJUmlpressure gage, slowly open the Sample Container Inlet Valve, allowing the container
pressure to increase to the desired sampling pressure.
9.4.6. Close the Sample Cylinder Inlet Valve and the Sampling Valve (Valve 1). Open the purge valve to relieve pressure in the
sample line. Close sample source valve. Depressurize appropriate portions of the sampling system.
Note: It is not recommended that reduced pressure samples be taken when line pressures are below 100 psig.
9.5. Helium "Pop" Method
The equipment arrangement is shown in Figure 10. The procedure for sampling by the Helium "Pop" Method is as follows:
9.5.1. Prior to sampling, evacuate the cylinder container to a pressure of I mm Hg or less. (Use a cylinder that has been
previously evacuated and tested to hold this vacuum.)
9.5.2. Prior to sampling, loosely connect the helium source to the auxiliary valve with the helium flowing out of the loose
connection to purge the Sample Container auxiliary valve. Tighten the connection at the Sample Container auxiliary valve. Open
the Sample Container auxiliary valve and allow helium to flow into the Sample Container until the pressure reaches approximately
5 psig. Close the Sample Container auxiliary valve. Close helium source valve. Remove container from helium source.
9.5.3. At the sample point. open Sample Valve (Valve 1) and thoroughly blow out any accumulated material. Close valve at
sampling point.
9.5.4. Install Sample Container as shown in Figure 10. The container should be in a vertical position. 'Mth all valves dosed,
9.5.6. Slowly open the Sample Cylinder Inlet Valve, allowing the container pressure to increase to the desired sampling pressure.
In some cases condensation may be eliminated by sampling at a pressure less than the source pressure. (See Reduced Pressure
Method.) It is possible to reduce pressure and produce Retrograde Condensation in the process. See API 14.1 for discussion of
the Phase Diagram.
9.5.7. Close the Sample Cylinder Inlet Valve and the Sample Valve (Valve 1). Open the purge valve to relieve pressure in the
Note: More than one container can be filled at the same time by using a manifold.
9.6. Glycol or Water Displacement Method

The equipment arrangement is shown in Figure 11. The procedure for sampling by the Glycol or Water Displacement Method is as
follows:
9.6.1. A sample cylinder filled with clean glycol or water and a vessel to measure the displaced liquid are required for this method.
Water must have a pH between 5.0 and 7.0. Water with a pH greater than 7.0 must be acidified to bring the pH within the proper
range. (0. 1 N H 2S0 4 is a satisfactory acid solution.) The source gas must displace all glycol or water during sampling.
27
9.6.2. Open Sample Valve (Valve 1) at sampling point and thoroughly blowout any accumulated material. Close Sample Valve
(Valve 1) at sampling point
9.6.3. Install sample Container as shown in Figure 11. The container should be in a vertical position. With all valves dosed,
Figure 11 Displacement Method
Tubing Should be
as Short as Possible
Purge Valve
Sample Valve
Valve 1
Sam.Ple Oullet Valve
Outlet Valve of Sample Probe.
Gas Sampling Sep-arator.
or other sample preparation
device.
Sample Container
Inlet Valve
-
Sample Container
Outlet Valve
Graduated Container
Close purge valve at sampling point.
9.6.5. Slowly open the Sample Cylinder Inlet Valve to fully open position.
9.6.6. Slowly open the Sample Cylinder Outlet Valve to allow a slow discharge of the glycol or water displacement liquid into the
measuring vessel until gas is seen or heard. Immediately dose the Sample Cylinder Outlet Valve.
9.6.7. Close the Sample Cylinder Inlet Valve and the Sample Valve (Valve 1). Open the purge valve to relieve pressure in the
Note: All of the displacement liquids MUST be removed from the cylinder during sampling to prevent noticeable change
in gas composition.
28
l, ~_
Note: Displaced water and glycol must be collected and handled in accordance with all relevant environmental and
safety regulations.
9.7. Floating Piston Cylinder Method
9.7.1. The lubricant on the Floating Piston Cylinder moving parts should be applied as lightly as possible and no component of
the sample can be soluble in the lubricant. (DuPont Krytox AC or AD have been tested and found to be non-absorbing greases.
Refer to Appendix A for deaning recommendations.
9.7.2. It is desirable to use an inert charge gas for the Floating Piston Cylinder, which is not present in the sample so that a leak
in the container itself can be easily detected during the analysis. Natural gas from the sample source can be used in an emergency.
Charge the inert gas side of the rontainer with pressure equal to or greater than the line pressure.
9.7.3. Sampling with a piston rontainer equipped with a visual indicator.
9.7.3.1. Open Sample Valve (Valve 1) and thoroughly blow out any accumulated material. Close Sample Valve (Valve 1).
9.7.3.2. Install the Sample Container as shown in Figure 12.
9.7.3.3. Open Sample Valve (Valve 1) and slowly purge the sample line with source gas by partially opening the Purge Valve until
gas is slowly flowing out of the Purge Valve. Close the Purge Valve.
9.7.3.4. Slowly open the Sample Cylinder Inlet Valve to fully open position and observe pressure on Gauge M.
Figure 12 Floating Piston Method

GageN
Inert Gas Valve Inert Gas Valve
Volume Indicator
Sample Inlet GageM

Sample Pressure
Valv.=e ~Ft~~~~
P urge ~.s:;au-lvKJe"'"__1r11
Sample Valve
Valve 1
s.mpae 0uI'-d V_
0uIl00t VeN. d s.npIe_.
G.a a-pling s.c---.
Mombr_~~
otn- aample pt'eIPlWIIItion doYke.
9.7.3.5. Adjust pressure on Gauge N to equal pressure on Gauge M by releasing inert gas through the Sample Cylinder Inert Gas
Valve.
29
9.7.3.6. Partially open the Sample Cylinder Inert Gas Valve to allow the inert gas to slowly vent to atmosphere. Do not allow the
pressure as indicated by Gauge M to drop below sampling pressure. Continue operation until the indicator designates the container
to be approximately 80% full.
9.7.3.7. Close the Sample Cylinder Inert Gas Valve. the Sample Cylinder Inlet Valve and the Sample Valve (Valve 1).
9.7.3.8. Relieve the pressure on the sample transfer line using the purge valve. Depressurize appropriate portions of the sampling
system.
9.7.3.9. Remove Sample Container and check sample Gauge. Sample Cylinder Inlet Valve and Sample Cylinder Inert Gas Valve
for leaks. Plug or cap the valves.
Note: Some pressure is required to move the piston inside these cylinders. Therefore. this method may not be
appropriate in the sampling of gases of very low pressure.
9.7.4. Sampling with a piston container not equipped with a visual indicator.
9.7.4.1. Open Sample Valve (Valve 1) and thoroughly blow out any accumulated material. Close Sample Valve (Valve 1).
9.7.4.2. Install the Sample Container as shown in Figure 12.
9.7.4.3. Open Sample Valve (Valve 1) and slowly purge the sample line with source gas by partially opening the Purge Valve until
gas is slowly flowing out of the Purge Valve. Close the Purge Valve
9.7.4.4. Slowly open the Sample Cylinder Inlet Valve to fully open position and observe pressure on Gauge M.
9.7.4.5. Adjust pressure on Gauge N to equal pressure on Gauge M by releasing inert gas through the Sample Cylinder Inert Gas
Valve.
9.7.4.6. Partially open the Sample Cylinder Inert Gas Valve to allow the inert gas to slowly vent to atmosphere. Do not allow
pressure Gauge M to drop below sampling pressure. Continue operation until the container is approximately 80% full.
9.7.4.7. Close the Sample Cylinder Inert Gas Valve, the Sample Cylinder Inlet Valve and the Sample Valve (Valve 1).
9.7.4.8. Relieve the pressure on the sample transfer line using the purge valve. Depressurize appropriate portions of the sampling
system.
9.7.4.9. Remove Sample Container and check sample Gauge, Sample Cylinder Inlet Valve and Sample Cylinder Inert Gas Valve
for leaks. Plug or cap the valves.
Note: Some pressure is required to move the piston inside these cylinders. Therefore, this method may not be
appropriate in the sampling of gases of very low pressure.
10. HANDUNG OF SAMPLE CONTAINERS IN THE LABORATORY
10.1 Sample Containers should be stored on shelves or racks.
10.2 If a Sample Container is known to have leaked, secure another sample. If another sample is unavailable, follow company
procedures for a tailed sample.
10.3 Sample Containers should be heated to a minimum of20"F (11C) above the sampling source temperature. Sample
Containers should be held at temperature for at least 2 hours prior to sample analysis.
10.4 After obtaining acceptable analyses, Sample Containers should be emptied in accordance with company safety and
regulatory practices.
30
10.5 Sample Containers should be leak checked, repaired as necessary and cleaned prior to being returned to service. See
Appendix A, Cleaning.
11. SAFETY
11.1. Every precaution should be taken to ensure that proper safety practices are employed.
11.2 Cylinders, sample lines, sampling separators and valves should have working pressures above the sample source
pressure. In particular, copper tubing and copper fittings can be hazardous. These should be used with caution and inspected
frequently for bad connections, flattening and kinks.
11.3. For pressures over 1000 psig. or for gases that contain hydrogen sulfide, stainless steel tubing should be used instead of
copper tubing.
11.4. During sampling, and especially when purging, certain precautions are mandatory. Smoking, open flames, vehicles with
motors running, or the use of matches In the area cannot be tolerated. Caution must be exercised while purging and sampling to
prevent forming a hazardous atmosphere. Special precautions should be taken if hydrogen sulfide is present.
11.5. Cylinder valves should be protected from damage. Cylinder valves may be protected in shipment by protective caps that
cover the entire valve or by crating the cylinders in strong crates or cases. Cylinder valves should be checked for leaks prior to
installing thread caps or plugs. Valve handles should not be forced with wrenches. Hand tightening should be sufficient. Any faulty
valves should be replaced or repaired before using the container. Refer to Safety Note 2.2.4.
11.6. HYDROGEN SULFIDE
11.6.1 Hydrogen Sulfide is a toxic gas. The effect of hydrogen sulfide on the human body varies with its concentration in the
atmosphere and with the length of time a person is exposed to it. The American Conference of Govemmental Industrial Hygienists
has set the threshold limit value for hydrogen sulfide at 10 ppm, ie., the maximum concentration in which a person can work safely
for eight hours. When the concentration reaches 1,000 ppm, death can occur rapidly (less than two minutes). Hydrogen sulfide is
about five times as toxic as carbon monoxide. Uke hydrogen cyanide. in higher concentrations a few breaths may prove fatal. In low
concentrations. hydrogen sulfide seems to be odor1ess after a short exposure because the sense of smell is lost in 2-15 minutes.
11.6.2 The relative density of hydrogen sulfide vapors is 1.192, but its presence (location) is often dependent upon the relative
density of the petroleum product with which it is associated. Depending upon the carTier. hydrogen sulfide may be found in high
areas as well as low areas. Extreme precautions should be taken while sampling gas containing hydrogen sulfide because of its
toxicity.
11.6.3 Length of stain tubes for hydrogen sulfide analyses are available and should be used for quick field checks. (See GPA
Publication 2377, -rentative Method of Test for Hydrogen Sulfide in Natural Gas Using Length of Stain Tubes.;
APPENDIX UST
Appendix A - Cleaning
Appendix B - Separators and Membrane Filters
Appendix C - Portable Chromatographs
Appendix D - On-Line Chromatographs
31
Appendix A
CLEANING
A.1. General Cleaning Requirements
A.1.1. All methods in this document require that the Sample Containers and associated sampling equipment be clean and free of
leaks.
A.1.2. When gasoline-range hydrocarbons are present in a container prior to sample procurement, the sample can become
enriched, yielding an elevated heating value.
A.1.3. Heavier contaminants such as oil or glycol can absorb heavy components of the sample, reducing the heating value of the
sample.
A.1.4. Not all cleaning methods remove both of these ranges of contaminants.
A.1.5. Sample Container cleaning methods should be evaluated for effediveness in removing all potential contaminants. Valves
and containers must be Checked for leaks after cleaning and prior to placing back in service. Sampling equipment such as
separators and associated tubing must be subjected to similar deaning procedures. Refer to API 14.1.
A.2. Contamination of Sample Containers and Associated Sampling Equipment
A.2.1. When contamination occurs during the sampling process, the sample will be non-representative. Personnel responsible for
sample procurement must observe for any potential contaminants at the sample point, the Sample Container, or any associated
sampling equipment. If contaminants are present, the sample should be discarded and the contaminated equipment must be
cleaned.
A.3. Cleaning Procedures
A.3.1. The most effective cleaning agent is wet steam. Wet steam effectively removes both heavy and light contaminants. Water
used in steam cleaning methods must not contain chemicals or contaminants that leave a residue in the Sample Container.
A.3.2. Evacuation methods effedively remove gasoline and lighter range contaminants, but may leave residues from heavier
contaminants.
A.3.3. A combination of steam cleaning and evacuation can remove both light and heavy contaminants.
A.3.4. If a floating piston cylinder is contaminated with heavy contaminants, it may be necessary to disassemble the cylinder for
cleaning. It may also be necessary to replace the seals.
A.3.5. Other methods for cleaning may be used if they pass the perfonnance aiteria evaluation listed in section A.5.
A.4. Leak Testing
A.4.1. Valve damage may occur during the cleaning process. Containers must be tested for leaks after the cleaning process.
One method is to pressurize the cylinder and immerse in water or check with a commercial leak testing solution. The leak test
should ensure that there are no leaks in the cylinder, valve connections, valve stem or valve seat.
A.4.1.1. Needle valves can leak through the valve stem packing when in either the open or closed position, but not necessarily in
the opposite position. The packing should be checked for leaks with the valve in the dosed position and also in the open position
(white capped or plugged)
A.4.1.2. The arrows on the valves should face out from the cylinder to prevent sampled material from leaking out of the cylinder.
32
A.5. Performance Criteria for the Evaluation of Cleaning Methods
A.5.1. Test Solution for Cleaning Methods
A.5.1.1. Prepare a test solution for evaluation of cleaning methods by combining a mixture of 50 % crude oil and 50 % condensate.
Mix the solution thoroughly and fill a Sample Container one-third full of the mixture. leave the mixture in the cylinder overnight
Drain the cylinder and clean the cylinder with the method under evaluation.
A.5.2. Test for Gasoline Range Contaminants
A.5.2.1. Fill the container with a gas used as the carrier gas for the gas chromatograph performing the test. The container must be
heated in a manner that is consistent with the typical sample handling procedures for the facility, or at least two hours at 140
degrees Fahrenheit. The contents of the container are then analyzed by the same method used for samples by gas chromatograph
to determine cleanliness.
NOTE: The total amount of residuals must be less than 140 parts per million by volume.
A.5.3. Test for Heavy Contaminants
A.5.3.1. Depressurize the Sample Container and remove one valve. Use a long-stemmed cotton swab to swab the length of the
container. Check the swab for residues. Rotate the container 45 degrees and repeat the test seven more times.
NOTE: No residues should appear on the swab.
A.5.4. Evaluation of Cleaning Method
A.5.4.1. Any cleaning method that passes both of the above test procedures is acceptable for cleaning Sample Containers and
related sampling equipment. The above tests can be utilized on cylinders in normal use that have been cleaned by the cleaning
method as a form of QA/QC for the cylinder cleaning process.
A.6. Field Cleaning Method
A.6.1. Field cleaning methods should be evaluated for cleaning cylinders and sampling equipment using the above techniques. If
the field method proves effective for one type of contaminant and not both, it should be so noted. The field method would be valid
only for the type contamination that it proved effective.
33
Appendix B
Separators and Membrane Filters
8.1. General
It is important for all sample system components to be clean and free from contaminants. This is equally true for separators and
filters. Refer to Appendix A, Cleaning for cleaning procedures and for procedures to evaluate the effectiveness of cleaning
procedures.
8.1.1. Since entrained or free-flowing hydrocarbon liquids are generally collected and accounted for in a condensate recovery
system, these liquids are not desired in the vapor phase portion of the accounting system.
8.1.2. Other contaminants such as water, oil. glycol, amine. etc. are not desirable in the Sample Container.
8.1.3. Flow disturbances may cause contaminants to fonn aerosols that can be ingested by the Sample Probe. These aerosols
should be removed by filtration or separation in the sample system.

8.1.4. Since free-flowing liquids tend to flow along the bottom of the pipe or flow along the walls of the pipe. it is necessary to
have a Sample Probe extending into the pipe. To prevent failure of the sample probe in the flowing gas stream. Sample Probe
length should be considered with care. Sample Probes are discussed in section 7.5.
8.1.5. A Gas Sampling Separator may help to eliminate contaminants.
B.1.6. The data from the API 14.1 sampling project clearly demonstrated that misuse of the Gas Sampling Separator could
distort the sample. The current revision of this GPA publication includes language to clarify the proper use of the separator. It
discusses when the Gas Sampling Separator would be appropriate and explores some of the potential pitfalls associated with its
misuse.
B.1.7. In a system where the natural gas product is at the Hydrocarbon Dew Point, slight changes in temperature or pressure
can cause liquids to vaporize or vapors to condense.
B.1.7.1. If the change in pressure or temperature causes liquids in the sample to vaporize. the sample no longer represents the
vapor phase of the flowing product stream. The sample has an artificially high concentration of heavy (high boiling point)
hydrocarbons and the BTU value is elevated.
B.1.72. If the change in pressure or temperature causes vapor in the sample to condense. and the condensed liquid is removed
prior to collection in the sample cylinder. the sample no longer represents the vapor phase of the flowing product stream. The
sample has an artificially low concentration of heavy (high boiling point) hydrocarbons and the BTU value is reduced.
B.1.72. In purge type sample methods. if the condensed liquids are subsequently swept back into the sample stream and collected
in the sample cylinder, the sample no longer represents the vapor phase of the flowing product stream. The sample has an
artificially high concentration of heavy (high boiling point) hydrocarbons and the BTU value is elevated.
B.1.8. To effectivety separate the unwanted liquids and to collect a representative sample of the vapor phase of the product
stream, it is imperative that any liquid separation device operates at flowing temperature and pressure conditions.
B.2. Insertion Membrane Filter Probe
B.2.1. The insertion membrane filter probe meets the requirements set forth in 8.1.8 in that the membrane filter is directly
mounted in the product stream.
8.2.2. A heated regulator mounted directly on the outlet of the probe. heating the sample to a temperature greater than JOOF
(17"C) above the Hydrocarbon Dew Point, presents a sample to the sample cylinder inlet valve that is comfortably in the vapor
phase and representative of the vapor phase of the flowing gas stream.
34
8.2.3. Refer to Figure 4 for a typical insertion probe. In this configuration, the outlet valve of the regulator becomes Valve 1 in the
purge methods.
8.3. Gas Sampling Separator
8.3.1. It is imperative that the Gas Sampling Separator be operated at the same temperature and pressure as the sample
source. The drain can be left dosed during the sampling process. In this case. the drain valve extension tube pigtail is not
necessary. If the drain valve is opened very slightly to allow a slow weep (for the purpose of monitoring for liquids in the sample)
and the resultant cooling is so slight that the temperature of the separator is not affected. the drain valve extension tube pigtail is not
necessary. If the drain valve is to be left open during the sampling process (to monitor for contaminants). the pigtail must be used.
8.3.2. The separator must be insulated and have temperature indication.
8.3.3. All connections and tubing should be as short as possible.
8.3.4. Sampling procedure. Refer to Figure 3. Gas Sampling Separator.
8.3.4.1 Open Sample Valve (Valve 1) at sampling point and thoroughly blowout any accumulated material. Close Sample Valve
(Valve 1) at sampling point.
8.3.4.2. With the Gas Sampling Separator inlet connected to the Sample Probe outlet and all valves closed, open the Sample
Probe outlet valve.
8.3.4.3. Open the Gas Sampling Separator inlet valve to pressure up the Gas Sampling Separator.
8.3.4.4. If the extension tube pigtail is used. fully open the Gas Sampling Separator drain valve. If the pigtail is not used. leave the
drain valve closed or very slightly open the valve in accordance with the discussion in section 8.3.1.
8.3.4.5. If the extension tube pigtail is used. slightly open the extension tube outlet valve to allow any accumulated liquids to drain.
The valve should not be opened wide enough to reduce the pressure on the Gas Sampling Separator below sample system
pressure. If liquids are present. verify that the liquids are unwanted liquids and not liquids that have condensed out of the vapor
portion of the sample. Ensure that the temperature and pressure are the same as flowing line temperature and pressure.
8.3.4.6. Open the Gas Sampling Separator outlet valve and purge at a rate just fast enough to bring the Gas Sampling Separator
up to line temperature and slow enough to maintain line pressure on the Gas Sampling Separator.
8.3.4.7. Close the Gas Sampling Separator outlet valve.
8.3.4.8. Attach the appropriate sampling equipment to the Gas Sampling Separator outlet valve.
8.3.4.9. Follow the selected sample procedure with the Gas Sampling Separator outlet valve being Valve 1 for the procedure.
8.4. Filters in the sample system
8.4.1. For some sampling methods. the pressure is reduced at the sample point and the temperature of the sample system after
the regUlator is maintained at least 30F (17"C) above the calculated Hydrocarbon Dew Point throughout the sampling process.
On-line and portable chromatographs frequently have filters installed at the sample inlel Rlters in such systems must be maintained
at least 30"F (17"C) above the calculated Hydrocarbon Dew Point throughout the sampling process.
8.4.2. No component in the sample system should be heated to temperatures above manufacture(s recommendations.
35
Appendix C
Portable Gas Chromatograph Considerations
C.1. The design of the sampling system used for portable gas chromatographs will depend upon the Hydrocarbon Dew Point
of the gas to be analyzed and the pressure and temperature conditions of the source.
C.2. \\'hen the source pressure is greater than the portable Gas Chromatograph's inlet pressure rating, it will be necessary to
use a regulator.
C.3. Under some conditions, the reduction in pressure can cause the product to cross the phase boundary due to Retrograde
Condensation. It may be necessary to heat the regulator to prevent sample distortion.
CA. Any tubing downstream of the regulator should be heated if it will not remain at least 30F (17C) above the calculated
Hydrocarbon Dew Point temperature of the sample at the reduced pressure. Stainless steel tubing and Nylon 11 tubing have
proved acceptable for use with portable gas chromatographs. Both can be heat traced to prevent potential condensation.
C.5. Separators or membrane filters downstream of the regulator must be maintained at least 300F (17C) above the calculated
Hydrocarbon Dew Point temperature of the gas. Separators should be property cleaned. See Appendix A, Cleaning.
C.6. Vacuum systems are not induded in the scope of this publication.
C.B. The connecting tubing at the front of the portable gas chromatograph should be heated at least 30F (17C) above
calculated Hydrocarbon Dew Point temperature of the sample. Failure to do this may cause a loss of heavier hydrocarbons and a
non-representative analysis. Or the accumulated liquids may be injected into the chromatograph, causing a non-representative
analysis or damage to the chromatograph.
36
Appendix 0
Sampling Systems for On-Line Analyzers
0.1. Sampling for on-line analyzers is slightly different than spot or composite sampling. The main objective is to obtain a
current, clean, vapor sample at a temperature well above the vapor's Hydrocarbon Dew Point (API 14.1 recommends 3QoF (17"C)
above the Hydrocarbon Dew Point.) This method usually involves reducing the sample pressure at or very close to the Sample
Probe in order to reduce sample transport lag times and reduce the likelihood of condensation of the vapor sample. Heat must be
added or preserved in this method to prevent aossing of the phase boundary keeping the sample at least JOOF (1r'C) above the
Hydrocarbon Dew Point This reduced pressure sample will continually flow through a bypass, providing the analyzer with a
current sample for analysis.
When designing on-line sample systems, consideration should be given for all sampling conditions, induding plant upsets.
0.2. An example of a typical on line analysis system is shown in the drawing below. In this example. a gas Chromatograph is
shown, but anyon-line analyzer will work in a similar way:
Figure 0.1 Typical On-Une Chromatograph Configuration
Sample System Chromatograph Oven

Bypass
Filter Sample Loop Column Detectors
Vent
Vent
Sample Sample Carrier Air

Return Vent Gas
Chromatograph
Sample Probe Controller
Communication of
Results
Process Line
0.3. In this graphic, the GC has an air-bath oven. However, most GC's for natural gas measurement have mandrill ovens and
do not need instrument air for heat
0.4. In general, all sampling systems for on-line analyzers of any type have several main parts in common:
0.4.1. A Sample Probe with membrane separator and pressure reduction (and heat. if required)
0.4.2. Sample transport tubing
0.4.3. Filtration (for protection of the analyzer from chance liquids or solids not filtered by the probe)
0.4.4. A sample bypass loop (to minimize sample transport lag times)
37
0.4.5. A sample valve loop (to provide a fresh, measured sample to the analyzer)
0.4.6. At least two vents/returns per analyzed stream.
0.5. Components of an On-Une Chromatography System:
0.5.1. Sampling Probes:
0.5.1.1. It has been an industry practice that the collection end of the probe be placed within the approximate center one-third of the
pipe cross-section. While it is necessary to avoid the area most likely to contain migrating liquids (the pipe wal~ it may also be
necessary to limit the probe length to ensure that it cannot fail due to the effects of resonant vibration. Resonant vibration can occur
when the vortex shedding frequency resulting from a probe inserted into a flowing fluid is equal to or greater the probe's natural
resonant frequency. Sample probes are discussed in section 7.5.
0.5.1.2. A membrane filter can be used with the probe to remove liquids from the sample.
0.5.1.3. Reduce the sample pressure to about 1 bar and compensate for any auto-refrigeration due to pressure drop that may occur
by adding heat to maintain at least 30F (11OC) above the expected Hydrocarbon Dew Point temperature throughout the
sampling process.
Figure 0.2 Typical Sample Probe with Regulator Installation
OUTlET
PORT
1I4"NPT
314"NPT
~1- SAMPl.. _
PROBE
GAS SAMPLE R.OW
L - - GAS METER PIPE RUN ~ I

0.5.1.4. The sample should be installed vertically from the top of a horizontal line as is shown above. Refer to section 7.5, Sample
Probes.
0.5.1.6. This reduction in pressure is beneficial because a vapor that is dear of liquid at line pressure will certainly be dear of liquid
when the pressure is dropped to 1 Bar.
0.5.2. Sample transport tubing:
0.5.2.1. The sample transport tubing should be as short as possible.
0.5.2.2. It must also keep "retro-grade" liquid from contaminating the sample. This is liquid that condenses and accumulates in low
spots, sometimes called "drip legsft in the sample tubing. This is not the liquid that forms on the back side of the phase envelope.
0.5.2.3. If the Temperature is expected to drop to 3QoF (17C) above the gas Hydrocarbon Dew Point temperature, heat tracing
should be used.
38
Figure 0.3 Heat tracing with electricity works to keep the transport tubing wann
SAA1PLE SAMPlE TRANSPORT

TRANSPORT TUBING INSULATION
nm~G !
,',..-.,---------------------::7"'f...
GAS A.OW--_~
0.5.2.4. The above drawing illustrates how heat tracing works. If needed this product is available as a package.
0.6. Filtration:
0.6.1. Gas samples must be free from partides as well as liquids to protect the analysis equipment from damage. Filtering should
be done to the degree that the analysis equipment manufacturer specifies. This filtering must be done to prevent plugging of
whatever critical orifice exists in the analyzer equipment Many analyzers today are using "nana" technology and will require very
small particle size filtration.
0.6.2. Fitters should be located where they can be readily changed and should be checked periodically as the condition of the
sample will probably demand that they be changed due to plugging up at some point The manufacturer should be able to specify
to some degree the longevity of a particular filter but, in fact, the sample cleanliness has more to do with how long they will last and
this should be of prime interest.
0.6.3. In-line filters will plug. The dirtier the sample the sooner they will plug. There are filters that are bypass filters and provide
some self-cleaning. These provide longer life but will need to be vented in some way. The gas usage will go up as these are added
to the sampling system.
0.6.4. Rltration methods that change the composition of the sample to be analyzed are not allowed.
0.7. Sample bypass loop:
0.7.1. The sampling system should use a bypass flow if the sample transport lag time requires it. A calculation as desaibed
below will indicate whether this should be done. The bypass filters mentioned in the section above will provide the restriction
needed to give an excellent bypass flow. The diagram below provides a picture of how this bypass works to reduce sample
transport lag times.
Figure 0.4 Sample Bypass loop
Sample System
Bypass
Filler Sample Loop
r---..--__---..:s v
Sample Sample Carrier

Return Vent Gas
Sample Probe
Natural Ga. Pipeline
39
-
0.8. Sample Transport Lag Time
0.8.1. The intemal volume of the sample transport tubing should be calculated or at least estimated using the chart below:
Table 0.1 Tubing Internal Volume
Transport Tubing Transport Tubing Wall Volume per linear Food

Outside Diameter Thickness (inches) (ee)
(inches)
1/8 .02 1
y. .035 5
3/8 .035 15
Y, .035 25
0.8.2. The sample transport lag time should then be calculated using the following formula:
:~ [P::5 J X[~ X[ J
\Nhere:
t Purge Time
L = line Length. ft
V = Tubing Volume, ccIft
Fs = Standard Flow, ccJmin
P = Actual Pressure, PSIG.
T = Actual Temperature, OF
Zp = Compressibility a1 P Pressure
This formula was taken from Appendix F: pp 579 and 580; "Process Analyzer Sample Conditioning System
Technology" by Robert E. Sherman; Wiley Interscience. and modified for Gas Compressibility.
0.8.3. If the sample system has a bypass flow rotometer on it, the flow rate should be set to change the volume in the tubing three
times during the expected analysis cyde time. This should provide a new sample every time an analysis is needed.
0.9. Sample valve loop and VentsJReturns
0.9.1. If the analysis is by gas Chromatography, the sample must be equilibrated to atmospheric pressure by means of some sort
of sample shut off' valve. This equilibration allows the very high repeatability that on-line analyzers are known for. For this reason,
the bypass vent on the sample valve should not be returned to the process or to any pressure of higher or lower than the
barometric. If it is necessary to capture this vent, it should probably go to a flare vent header that has minimum pressure effect on
the sample equilibration.
0.9.2. This barometric equilibration and the fad that the entire sample is analyzed allow "normalization" of the results. This
compensa1es for any barometric pressure changes that can occur between calibrations and gives repeatability results that can be
0.05% or better.
40
12. DEFINITIONS
12.1. Absorption: natural gas constituents are dissolved into a liquid or solid that is not considered to be part of the mixture's
liquid phase.
12.2. Adsorption: a thin film of molecules adheres to a liquid or solid surface.
12.3. Chilled Mirror Test: used to determine dew points (water and/or hydrocarbon) by passing the natural gas over a mirror
while gradually reducing the temperature of the mirror until condensation forms on the surface of the mirror.
12.4. De-sorptlon: adsorbed or absorbed molecules are released from a liquid or solid surface.
12.5. Extension Tube ("Pigtail"): a piece of tubing placed on the end of a Sample Container used to move the point of pressure
drop (point of cooling) away from the sample being acquired.
12.6. Floating Piston Cylinder: a sample container which has a moving piston that has sample pressure on one side of the
piston, balanced by a pre-charge pressure on the other side of the piston.
12.7. Flow-Proportional Composite Sampling: the process of collecting gas over a period of time at a rate that is proportional
to the pipeline flow rate.
12.8. Gas Sampling Separator: a device in the sampling system used to remove contaminant liquids from the natural gas
sample.
12.9. GPA: Gas Processors Association
12.10. Hydrocarbon Dew Point the temperature, for a given pressure, at which hydrocarbon vapor condensation begins. For
purposes of this publication, the Hydrocarbon Dew Point temperature is considered one of:
12.10.1. the flowing line temperature (at flowing line pressure),
12.10.2. the value determined by a Chilled Mirror Test (at flowing line pressure), or
12.10.3. 30 OF (17C) above the calculated Hydrocarbon Dew Point temperature.
12.11. Joule-Thomson Effect A drop in temperature associated with a drop in pressure. This can result in condensation of
heavy hydrocarbons in a natural gas sample. This reduction in temperature is in the order of JOF (4C) per 100 psi (690 kPa) in
pressure drop.
12.12. Multi Phase Flow: two or more phases such as vapor and liquid in the sample stream.
12.13. Nonnal Condensation: Condensation caused by an increase in pressure or a deaease in temperature.
12.14. Nonnal Vaporization: Vaporization caused by a deaease in pressure or an increase in temperature.
12.15. Phase Diagram: An illustration of the change in dew point and bubble point with changes in gas pressure and
temperature.
12.16. Representative Gas Sample: A gas sample that is compositionally identical, or as near to identical, as possible to the
sample source stream.
12.17. Retrograde Condensation: Condensation caused by a decrease in pressure or increase in temperature. (See API 14.1
treatise on the phase envelope)
41
12.18. Retrograde Vaporization: Vaporization caused by an increase in pressure or decrease in temperature. (See API 14.1
treatise on the phase envelope)
12.19. Sample Container: any container used to hold a natural gas sample. Typical Sample Containers are constant volume
cylinders or floating-piston cylinders.
12.20. Sample Probe: a device extending through the meter tube or piping into the stream to be sampled.
12.21. Single-Phase Flow: for natural gas, natural gas flowing at a temperature above the Hydrocarbon Dew Point and free of
compressor oil, water, or other liquid or solid contaminants in the flow stream.
12.22. Water Dew Point the temperature at a specific pressure where water vapor condensation begins.
42

Gpa 2186-05

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GPA Standard 2166-05

Obtaining Natural Gas Samples

Adopted as a Tentative Standard, 1966

Gas Processors Association

"Copyright ~005 by Gas Processors Association. All rights reserved.

1. Purging - Fill & Empty Method

2.1. General notes

2.2. Safety Notes

2.2.1. Safety Note 1

2.2.2. Safety Note 2

2.2.3. Safety Note 3

2.2.4. Safety Note 4

2.2.5. Safety Note 5

3.1.1. Purging - RII and Empty Method

5. HydrOcarbon Dew point

6. Guide for the Selection of a proper SamDling procedure

See Table 1 for recommended equipment for each sampling procedure.

6.1. Purging - Fill and Empty Method

6.2. Purging-Controlled Rate Method

6.3. Evacuated Container Method

6.4. Reduced Pressure Method

6.6. Glycol or Water Displacement Method

6.7. Floating Piston Cylinder Method

6.8 Portable and On-Une Gas Chromatograph Method

see Table 1 for recommended equipment for each sampling procedure.

.... i.. a"".

~RBcPr_Codn T.......... RBcPr_s

7.1.1. Single Cavity (Constant Volume) Cylinders (Figure 1)

Figure 1 (Single Cavity Sample Cylinder)

7.1.2. Floating Piston (Constant Pressure) Cylinders (Figure 2)

Figure 2 Floating Piston Cylinder

Volume Indicator 1,_"///1..,

Sample Inlet GageM

7.2. Sample transfer Line

7.2.3. Insulation and Heating

7.3. Sample Une Separators and Filters

Separator Outlet Valve

Membrane 1-----s('Qt and Poppet

Fixed Probe Style Regulo.tor with MeMbra.ne TIp

7.4. Sample Points

7.5. Sample Probe (Figure 5)

Figure 5 Gas Sample Probe

7.5.2. Probe Length

7.5.2.1. Probe Length Calculation SI Units

L= jFrox4.38X OOx 10 x.J (EIr) x(OD' + IDJ)

L= Permissible Probe Length (mm)

7.5.22. Probe Length Calculation American Engineering System Units

L = j Fro x 1.194 x 00 x.J (Fir) x (Ool + JD1)

L = Permissible Probe Length (inches)

7.6. Pressure Regulators

7.7. Extension Tube ("Pigtail") (Figure 7)

Figure 6 Extension Tube ("Pigtail")

Sample Container Extension Tube

Figure 7 Flow Plug 1/8" Port

1/4" NPT Hex Head Pipe Plug

316 Stainless Steel

Figure 8 Flow Plug - Various Port Sizes

do Drill Drill L Notes

1/4 in. Hex Head Pipe Plug

8.1. General Heating Requirements

8.1.2. Supplemental heating apparatus

8.2. Sample system heating requirements

8.2.2. Dead End and Displacement Methods