Liquid Sampling

By: Michael Royce Miller

SPL
Vice President Technical Services

Introduction
Collecting a liquid sample in the field can be challenging. Maintaining the pressure and temperature at
near-line conditions during the sampling event and controlling the sample collection rate are critical factors
for obtaining representative spot samples.

The liquids in the newer shale plays differ from traditional liquids, with increased NGL content. These liquids
present a challenge to personnel responsible for sampling pressurized hydrocarbon liquids.

GPA 2174 and API MPMS Chapter 8 are industry standards for sampling liquid hydrocarbons. GPA 2174 is
the method used for sampling high pressurize hydrocarbon liquids.

Considerations
The focus here will be methods for acquiring a representative spot sample at pressures above 20 psig and
samples below 20 psig.

The first and one of the most important considerations is sample location. A sample should be taken using
a sample probe located in the center 1/3rd of the line. However, in most of the field locations today this has
been neglected. This forces the technician to look for alternative locations. When sampling from a sight
glass, do not empty the sight glass. Regulate the sample procedure to keep product visible in the sight glass.

A static mixer should be upstream of the probe to ensure a proper mixture of the liquids being sampled if
water-cut is the desired test. A static mixer can cause flashing to occur if it causes a high pressure drop.
Use caution when using a static mixer. These locations are usually at the bottom of a sight glass or the drain
port of a strainer. These locations are not ideal but with care a representative sample can be acquired.

The next consideration is an accurate pressure and temperature of the sample being taken. Pressure and
temperature play an important role in bubble point determinations. Taking the pressure and temperature
of the liquid at the sample point will improve consistency between the actual and calculated bubble point.

The next consideration is water cut. The technician should purge the line to make sure that the sample line
is full of hydrocarbon. This can be achieved by purging the sample at the end of the sample line into a clear
or semi-clear Nalgene bottle. A visual inspection should have at least an 80% oil to water ratio. However,
this may present problems in some sample test determinations, so a sample closer to 100% oil is always
recommended.

Another consideration when taking a spot liquid hydrocarbon sample is timing of the sample collection
event. It has been determined that the time you collect the sample after a well cycle can be
critical. Compositional equilibrium can change if well cycles are far apart, and heaters are using the
separator gas and/or the gas exits the separator through the gas sales line.

The collection rate of the sample can also influence the sample results if it is too rapid (and hard to establish
due to the shorter collection time). That is, slower collection rates allow the sampling technician to obtain
the desired collection rate. The “plus fraction” density and molecular weight can be influenced at rapid
collection rates. Data from a recent study will be publicly available in 2018.

Sampling Procedures
There are primarily two procedures listed in GPA 2174:

• Displacement method, utilizes a Constant Volume (CV) cylinder, completely filled with water prior
to the sampling event.

• Constant Pressure (CP) cylinder method, utilizes a piston-cylinder, with gas on the pre-charge side
of the piston at a pressure greater than source sampling pressure.

Procedures for Sample Pressure Above 20 psig CV Cylinder

Using the water displacement method and equipment shown in Figure 1. Start with a CV cylinder
completely filled with water. In this example, we will use a 500 CC cylinder with 1800 psi burst disk
(minus 120 psi), effectively 1680 psi rating for safety.

1. Connect a high-pressure hose to the sample point.

2. Connect the cylinder to the pressure, temperature and purge port at the other end of the hose.
3. Elevate and suspend the 500 CC cylinder over a graduated cylinder.
4. Slowly open the sample valve pressurizing the hose.

5. With a small bent tubing connected to the purge valve slowly purge the liquid into a Nalgene bottle
and check for oil to water ratio. If adequate, note the pressure and temperature of fluid from
manifold.
6. Open cylinder inlet valve fully, allowing the oil to contact the water in cylinder.

7. Slowly drip the water from the bottom valve into the graduate at a rate not to exceed 60 ml per
minute.

8. When water in graduate indicates 80% full, close the inlet and outlet cylinder valves.
9. Slowly open bottom cylinder valve and remove an additional 10% of the water. This will give an
expansion space for the liquid in the case of temperature change during transportation to the lab.
10. Plug or cap both valves for transportation to lab.

11. Make sure all paperwork, bill of lading, chain of custody and sample tag information is filled out and
legible. Close sample valve and purge residual liquid in hose to a grounded bucket.
 Figure 1. Water displacement method sampling apparatus.

Procedures for Sample Pressure Below 20 psig CV Cylinder

1. The connections are the same as having pressures above, except the pressure may be too low to
displace the water in the cylinder.

2. It is recommended to connect a pump device such as an outboard fuel bulb to the outlet of the
cylinder with a short piece of rubber hose, usually on either side of the bulb as in figure 2.
3. Make sure the arrow on the bulb is pointing down to pump the water into the graduated cylinder.
4. If the pressure is so low that the oil will not purge you may need to connect the bulb to the purge
 valve and pump oil into the Nalgene bottle to make sure you are sampling oil and not water.

5. After the purge is completed, open inlet and outlet valves to the cylinder.
6. With the bulb now moved to the bottom of the cylinder, squeeze the bulb to cause the water to
pump to the graduated cylinder.
7. Pump until you have 80% of the graduated cylinder full, then close the inlet valve to the cylinder
and pump an additional 10% for expansion of the product during shipment to the lab.

Figure 2. CV cylinder method sampling Hand pump.

Procedures for Sample Pressure Above 20 psig CP Cylinder

1. Using the Constant Pressure (CP) cylinder method and equipment shown in figure 3.

2. Connect a high-pressure hose to the sample point.

3. Connect the cylinder to the pressure, temperature and purge port at the other end of the hose.
4. Slowly open the sample valve pressurizing the hose.
5. With a small bent tubing connected to the purge valve, slowly purge the liquid into a Nalgene bottle
and check for oil to water ratio. If adequate, note pressure and temperature of fluid from manifold.
 6. On the pre-charged side of the CP cylinder connect a regulator and rotameter as shown in figure
bellow. Place cylinder on flat level surface.

7. Pre-charge pressure should be above line pressure but not to exceed 1200 psi burst disk at both
ends of cylinder 1800 psi burst disk (minus 120 psi), effectively 1680 psi rating for safety.
8. Slowly open cylinder inlet valve. The piston should not move.
9. On the two-stage regulator at the pre-charge side of cylinder, adjust pressure ensuring not to
exceed 200 psig.
10. Slowly open rotameter valve to about 5 on the scale and observe pre-charge pressure drop.

11. When pressure reaches line pressure, cylinder will start to fill. Adjust rotameter to limit fill to 60 ml
per minute or slower.

12. When cylinder indicator is at 80%, close inlet and outlet valve leaving 80% liquid and 10%
backpressure to allow for expansion during transportation to lab.

13. Plug or cap both valves for transportation to lab.

14. Make sure all paperwork, bill of lading, chain of custody and sample tag information is filled out and
legible.

15. Close sample valve and purge residual liquid in hose to a grounded bucket.

Figure 3. CP cylinder method sampling apparatus

Procedures for Sample Pressure Below 20 psig CP Cylinder

1. To sample liquids that are below 20 psig into a CP cylinder, you will need to use a sample pump as
shown in figure 4.
2. To connect a sample pump to the sample probe or sample point, it is a good practice to connect a
small manifold with a temperature and pressure connection at the sample point. This will allow you
to log a good temperature and pressure for the product being sampled.
3. You will need to supply an external pressure source to the actuator of the pump. (I.e. Nitrogen
bottle.)

4. Set the sampler controller to sample every 5 seconds. If the pump cannot recover every 5 seconds,
slow to 10 seconds.
5. With the liquid sampler, you can pump the product into a Nalgene bottle, using its purge valve to
insure you are pumping product and not just water.
6. Connect a small relief valve to the pre-charge outlet valve of the CP cylinder, setting it to around
220 psig or at least 100 lbs above line pressure.

7. Slowly open the pre-charge valve allowing the pre-charge pressure to drop to the relief valve
setting.

8. Close the sampler purge valve, then open the sampler outlet valve to the inlet of the CP cylinder
and start the sampler timer. The indicator will show the cylinder filling up and the pre-charge relief
valve will maintain back pressure.

9. Make sure all paperwork, bill of lading, chain of custody and sample tag information is filled out and
legible.

10. Close sample valve and purge residual liquid in the hose into a grounded bucket.

Figure 4. CP cylinder method sampling apparatus and Spot Automatic Sampler.

Conclusion
It can be a challenge taking a liquid sample correctly, but if done accurately the results will be representative
of the product. The sample is the first and most important step in the hydrocarbon laboratory process. If
the sample is incorrect, the result of the analysis will also be incorrect.

Procedures listed above are based on field experience and repetitive lab results.