PVT Laboratory Procedures and Report: Gas-Crude Oil Sample The laboratory procedure for sample analysis generally

follows this procedure: 1. Determine the mole fraction composition of the subsurface sample, or of the individual gas and oil surface samples. 2. Determine shrinkage for surface separator samples. 3. Recombine the surface oil and gas samples according to test data. 4. Perform a relative total volume or PV test. 5. Perform a differential liberation test at reservoir temperature in the test cell. 6. Perform a flash separation test at various separation pressures and temperatures. 7. Determine the fluid viscosity over a range of pressures at reservoir temperature. The first page or two of a report generally is a cover letter which includes a statement of the field quality check on the samples and of the tests performed. The bubble-point pressure at reservoir temperature, the total solution gas and relative volume factor for differential liberation, the range of oil viscosities, and the optimum separator pressure are usually summarized in the text. Following this is a listing of formation characteristics, well characteristics, and sampling conditions. All of these data are obtained before or during the sampling procedure. Some testing laboratories may include more extensive amounts of the field test data and conditioning procedures. Most important are the reservoir pressure, gas and oil rates, and reservoir temperature, although all of the data are helpful and possibly critical in interpreting the test results. Hydrocarbon Compositional Analysts Next in the report we will find the compositional analyses of the reservoir fluid. If a surface recombination sample has been taken, the composition of the individual separator gas and liquid samples is listed along with the composition of the recombined reservoir fluid. The basis of recombination is always given, as well as the molecular weight and density of the heptanes-plus (C7+) fraction and the properties of separator gas and liquid. Composition may be determined by fractionation in a low or high temperature fractionating column, by mass spectrometer, or, more commonly, by gas chromatography. A chromatograph ( Figure 1 , Gas chromatograph used for compositional analysis of hydrocarbon mixtures) separates the components according to boiling point, in a special column.

Liquids are analyzed by capillary gas chromatography up to a certain molecular weight (C35), and the heavier fraction is characterized by molecular weight and density. Molecular weight measurements are performed on the heavier fraction by cryoscopy. In this technique the freezing point of a mixture of benzene and the oil's heavy ends is measured and compared to the freezing point of pure benzene. This allows a determination of the heavy fraction's molecular weight and density. As mentioned earlier, the recombination of the gas and oil samples must be made based on the separator GOR expressed with respect to separator liquid. If a separator-stock tank oil shrinkage factor was not measured in the field, it must be determined in the laboratory by recreating separator and stock tank conditions and measuring the difference in volumes of the separator and stock tank liquid. Only on this basis can the samples be recombined and the fluid composition analyzed. Relative Total Volume Test After the representative fluid sample is transferred into the test cell, usually a highpressure, high-temperature, mercury cell ( Figure 2 , High-pressure, high-temperature mercury test cell for relative volume determinations.

Viewing mirror allows view glass to be pointed away from operator), the flash separation procedure shown in Figure 3 may be carried out.

(Schematic of (a) flash liberation and (b) differential liberation. The degree to which oil volume is effected by the separation process is dependent on the composition of the oil. In the case of a low shrinkage oil (c), differential liberation provides for a larger volume of stock tank oil. A high shrinkage oil (d) is affected differently.) The pressure on the sample is decreased from above reservoir pressure by withdrawing mercury at reservoir temperature. The pressure and volume changes allow the plotting of a graph to determine the bubble point. Once gas begins to appear, the sample is brought to equilibrium after each volume change by rocking the cell. The resulting data are expressed as the relative total volume and are found in the PVT report as a columnar table. The volume is expressed relative to the volume at the bubble-point or saturation pressure. No material is removed from the cell during this procedure. Usually, the data entered in the PVT report is "smoothed" to account for the errors in reading very small changes in volume. This smoothing is done by fitting the total relative volume data to a "Y" function curve:

(9) The compressibility of the reservoir oil above the bubble-point pressure is usually presented here also, since it is obtainable from the pressure-relative volume data by calculating the change in volume per unit change in pressure.

Differential Liberation Test Usually the results of a differential liberation test appear next in our PVT report. Once again, the pressure is incrementally lowered in the test cell, increasing the volume by withdrawal of mercury ( Figure 2 ). When gas has evolved from the oil, it is displaced from the cell at a constant pressure by injecting mercury (Figure 3 ). The volumes of the free gas and remaining oil are measured at cell conditions, and the free gas is also measured at standard conditions. This procedure is repeated (perhaps 10 or 12 times) until only oil remains in the cell at reservoir temperature and atmospheric pressure. The residual oil is then cooled to standard temperature in order to measure its change in volume. This residual oil is not the same as stock tank oil, because the differential process of gas liberation is not equivalent to flash liberation. Differential liberation is carried out at reservoir temperature, thus the residual oil will have more of the lighter ends "cooked off." This results in the gravity of the residual oil being lower than that of an oil resulting from a flash liberation carried out at separator temperature. In the differential liberation test, material is removed from the system, changing the overall composition of the hydrocarbon mixture in the cell. The relative oil volume data presented in the PVT report are given relative to a volume of residual oil at standard conditions. The solution gas-oil ratio is also presented, based on the volume of gas liberated in each incremental pressure drop and the total gas released. The compressibility factor, formation volume factor, and gas gravity are determined for the gas released during each pressure decrement, and presented in the report. The oil density also is reported here. The relative oil volume data measured so far are not equivalent to the oil formation volume factor we wish to obtain for use in material balance and reserve calculations. In order to adjust the differential liberation data to obtain B0, we need to simulate the flash liberation process that takes place in the separator and results in stock tank oil. This is done in the flash separation test. Flash Separation Tests In this test, part of the reservoir fluid is ejected from the test cell at reservoir temperature and saturation pressure into a small-scale stage-separation system. The separation pressures and temperatures are carefully controlled and generally determined by the engineer requesting the test. The volume of gas liberated at each stage and the volume of remaining liquid are measured. Normally the test is carried out for two stages of separation. The first-stage separator pressure is generally varied to include at least four possible separator pressures at ambient temperature, and the second stage is generally carried out under stock tank conditions of o psig (1 atmosphere) at ambient temperature. The data presented for this test include the GOR in gas volumes per separator barrel and per stock tank barrel. The formation volume factor given here is the volume of saturated oil at bubble-point pressure and reservoir temperature per volume of stock tank oil at standard conditions. The gravity of the oil and the gravity of the flashed gas are also reported for each separator pressure. These data may be plotted as a function of separator pressure ( Figure 4 , Formation volume factor and oil gravity versus separator pressure) to reveal the optimum separator

pressure.

The optimum pressure is that which maximizes stock tank oil gravity and volume. Assuming that we will be able to install a separator that operates at this optimum pressure, we can use the flash separation data from the stage separation closest to this optimum pressure to adjust our earlier differential data, thus obtaining B0 for the proposed field conditions. This is done by multiplying each differential liberation volume factor by the ratio of the flash separation volume factor and the differential liberation volume factor at the bubble point. In Figure 5 (Adjustment of differential oil relative volume curve to separator conditions) we see the adjustment.

Similarly, the solution GOR curve must be adjusted as shown in Figure 6 (Adjustment of differential solution GOR curve to separator conditions).

The Rs and B0 values generated in this manner may be used to predict reservoir performance when surface separation equipment performs as expected. Some laboratories present adjusted formation volume factor and solution GORs in their reports based on the optimal separator pressure. Other labs leave the selection of an optimal separator pressure up to the engineer. Fluid Viscosity Reservoir fluid viscosity is measured at reservoir conditions using a rolling-ball viscosimeter ( Figure 7 , Rolling-ball viscosimeter used for determining fluid viscosity at high pressures and temperatures).

This instrument electronically measures the time required for a steel ball to roll a given distance through a tube filled with the fluid to be tested. The clearance between the tube and the ball is varied according to the general magnitude of the fluid viscosity. The viscosity of the oil above the bubble point and below the bubble point is measured in this manner. Gas viscosities are generally determined from the gas analysis using correlations. By performing a compositional analysis on the gas liberated at any point during differential liberation or flash separation tests, the gas viscosity can be determined. When measured, gas viscosities are usually measured by determining the pressure drop for flow through a capillary tube. The PVT report generally includes plots of all the important tabular data, along with a plot of the subsurface pressure survey if a subsurface sample was taken. Although not part of a typical PVT report, the determination of equilibrium ratios for a reservoir fluid may be done at special request. A test cell is charged with a reservoir fluid sample and the sample is flashed by withdrawing mercury and dropping the pressure. Samples of the equilibrium oil and gas are individually withdrawn and analyzed using gas chromatography. The equilibrium ratio at the particular pressure and reservoir temperature can be determined from the analyses. The process is repeated with a fresh sample to a lower pressure than the previous one. This is done several more times over a desired range of pressures.