Jess Hernando Bermdez David Esteban Hernndez Nicols Fabin Paniagua

ESCUELA DE INGENIERIA DE PETROLEOS

CHATER 4 API RP 40

FLUID SATURATION METHODS

ESCUELA DE INGENIERIA DE PETROLEOS

INTRODUCTION

This section documents the specialized techniques developed for analysis of core samples with different sample physical characteristics and sizes, obtained by various coring methods.

ESCUELA DE INGENIERIA DE PETROLEOS

Rock Type and Recommended Fluid Saturation Testing Method(s

ESCUELA DE INGENIERIA DE PETROLEOS

1-) RETORT METHOD AT ATMOSPHERIC PRESSURE

Oil and water fluid saturations are obtained by a high-temperature retorting process
The gas saturation is determined on an adjacent, lithological similar sample by placing it in a mercury pump

ESCUELA DE INGENIERIA DE PETROLEOS

Apparatus
a. Stainless steel retort(s)
b. Oven
c. Water bath d. Calibrated glass receiving tube e. Rock hammer and crusher f. Diamond saw

h. Centrifuge
g. Mercury pump

ESCUELA DE INGENIERIA DE PETROLEOS

Procedures/Precautions
The basic procedure is normally conducted on samples taken from full-diameter cores
some lithology's such as shale, anhydrite, gypsum, and heavy clays are usually described and skipped in this type of analysis

ESCUELA DE INGENIERIA DE PETROLEOS

ESCUELA DE INGENIERIA DE PETROLEOS

Calculations
The corrected oil and pore water collected for each sample along with the gas volume may be expressed as a percentage of bulk volume as follows:
NDHg = WtHg/BvHg BvRet = WtRet/NDHg GB = (HgInj x 100)/BvHg OB = (OilVol x 100/BvRet WB = WatVol x 100)/BvRet GS = (GB x 100)/(GB + OB + WB) OS = (OB x 100)/(GB + OB + WB) WS = (WB x 100)/(GB + OB + WB)

ESCUELA DE INGENIERIA DE PETROLEOS

Advantages
Fluids are collected from relatively large samples ensuring better representation of the lithology and increasing the potential precision of all measurements

Limitations
Water saturation (and porosity) may be too high if samples contain large amounts of montmorillonite or gypsum that break down at high temperature.

ESCUELA DE INGENIERIA DE PETROLEOS

1.2 Percussion Sidewall Cores

The method is a modification of the basic retort procedure. The main difference is that gas, oil, and water volume measurements are made on the same sample as opposed to the basic procedure where adjacent core pieces are required.

ESCUELA DE INGENIERIA DE PETROLEOS

Apparatus
a. Stainless steel retorts b. Oven c. Calibrated glass receiving tubes

d. Mercury pump e. Apparatus capable of piercing the jar lid

f. A hot wire gas detector g. A gas chromatograph

ESCUELA DE INGENIERIA DE PETROLEOS

Procedures/Precautions
The sample is placed in the cell of a precalibrated mercury pump, and bulk volume is determined by mercury displacement This procedure measures the gas-filled pore volume assuming that the compressibility of the water and/or oil present in the other pore spaces is minimal. Sidewall core material is subject to fluid loss due to evaporation so exposure time to room conditions should be minimized.

ESCUELA DE INGENIERIA DE PETROLEOS

Calculations
The oil, pore water, and gas-filled pore volume may be expressed as percentage of bulk volume as follows: GB = (HgInj x 100)/BV OB = (OilVol x 100)/BV WB = (WatVol x 100)/BV GS = (GB x 100)/(GB + OB +WB) OS = (OB x 100)/(GB + OB + WB) WS = (WB x 100)/(GB + OB + WB)

ESCUELA DE INGENIERIA DE PETROLEOS

Advantages

The method is relatively rapid

Limitations The distilled liquids may form emulsions.

ESCUELA DE INGENIERIA DE PETROLEOS

2 DISTILLATION EXTRACTION METHOD (DEAN STARK

Plug Samples Full Diameter Cores
This procedure is appropriate for plug samples and for rotary sidewall cores. The distillation extraction (Dean-Stark) method of determining fluid saturation depends upon the distillation of the water fraction, and the solvent extraction of the oil fraction from the sample.

The sample is weighed and the water fraction is vaporized by boiling solvent. The water is condensed and collected in a calibrated receiver. Vaporized solvent also condenses, soaks the sample, and extracts the oil. The sample is oven dried and weighed. The oil content is determined by gravimetric difference.

ESCUELA DE INGENIERIA DE PETROLEOS

Pressure-Retained Core Analysis

The objective of pressure-retained core analysis is to provide fluid saturation data on cores for which fluid expulsion has been minimized during core barrel retrieval by preventing pressure depletion from bottom hole to surface conditions.

Sponge Core Analysis

In sponge coring, the core enters a half-inch thick polyurethane or cellulose/polyurethane sponge sleeve inside an aluminum liner. As the core is brought to the surface, expanding gases displace crude oil that is captured by an oil-wet sponge sleeve (or water that is captured by a water-wet sponge sleeve).

ESCUELA DE INGENIERIA DE PETROLEOS

This paragraph covers the special considerations for measuring fluid saturations of the pore space in oil productive shalerocks composed of clay-to-silt-sized particles and potentially oil productive. Analysis of samples from this type formation may need special handling due to their low permeability, possible presence of tightly bound or structural water, and potential for solid organics.

Productive Shale

Tar (Oil) Sand Analysis

The distillation extraction method can be used to determine the fluid saturations of unconsolidated tar (oil) sands. However, certain modifications to the procedure and data presentation are required. The required changes are described in the following paragraphs.

Filtrate Invasion Analysis (Pressure Cores)

The objective of filtrate invasion analysis is to quantify the amount of drilling fluid filtrate that invades the core during the coring operation.

ESCUELA DE INGENIERIA DE PETROLEOS

4.SOLVENT FLUSHING
Karl Fischer Titration Core plug samples are cleaned by dynamic miscible displacement with an appropriate sequence of solvents and the water content of the produced effluents analyzed by Karl Fischer titration

Apparatus
Apparatus appropriate for this method includes: GeneralThe apparatus includes a core flow system for the solvent injections and a Karl Fischer titrimeter for the effluent analysis. Core holder assembly Solvent delivery device Related hardware Karl Fischer titrimeter Analytical balances Syringes Materials and reagents: Toluene Methanol

ESCUELA DE INGENIERIA DE PETROLEOS

Procedures/Precautions
An alternating methanol-toluene solvent injection sequence is performed, beginning with the solvent that is miscible with the mobile phase, i.e., methanol if the brine is mobile or toluene if the oil is mobile. The Karl Fischer titration requires only a small amount of solvent; therefore, the analyzed sample must be representative of the entire solution to yield accurate results.

Calculations
The following calculations should be performed: Water Saturation: Swes = Wes x (Swe Swi) Sws = Sum Swes Swb1 = Sws /[(1 A) x rb] Swb2 = (Swb1 x 100)/PV

ESCUELA DE INGENIERIA DE PETROLEOS

 Oil Saturation: If the sample was fully saturated, oil saturation may be determined by volumetric difference: So = 100 Swb2 If the sample contained an initial gas saturation, the oil saturation must be determined by gravimetric difference: Wo = Wi Wd [Sws /(1 A)] Vo = Wo /ro So= Vo*100/PV

ESCUELA DE INGENIERIA DE PETROLEOS

Advantajes
The Karl Fischer titration is very precise. All saturation levels can be determined.

Limitations
Methanol readily absorbs moisture from the environment. Accuracy of the method is dependent on solvent handling and storage techniques. The analyzed sample must be representative of the bulk effluent.

ESCUELA DE INGENIERIA DE PETROLEOS

SCANNING METHODS
Several laboratory techniques for scanning measurements of water, oil, and gas saturations in core samples have been reported. These techniques include: (a) linear x-ray absorption, (b) microwave absorption, (c) computer assisted (axial) tomography (CT), (d) linear gamma-ray absorption, and (e) nuclear magnetic resonance (NMR). The linear x-ray, gamma-ray, microwave, and CT methods may be considered as emerging technologies for saturation measurement. Other scanning techniques that have been used for saturation determinations are radio wave resonance and neutron attenuation radiography.

ESCUELA DE INGENIERIA DE PETROLEOS

Apparatus
Apparatus for these techniques are generally sophisticated and expensive. X-ray and CT equipment manufactured for medical use are often adequate for saturation measurements. Medical NMR equipment is not often suitable for saturation measurements.

Procedures/ Precautions
Several parameters must be considered for accurate saturation determination when scanning methods are used, such as the power level setting, tagging material and its concentration, tagging fluid-rock and fluid-fluid interaction (refer to the Bibliography for the many procedures and precautions for the individual techniques).

ESCUELA DE INGENIERIA DE PETROLEOS

Calculations
The unknown saturations for the oil-brine system are then calculated based on the following equation: Sw = (Usat Uo)/(Uw Uo)

Advantages
An important advantage of these methods is their ability to provide information on the spatial distribution of the fluid saturation. Another advantage of these techniques is that the measurements are made noninvasively and nondestructively.

ESCUELA DE INGENIERIA DE PETROLEOS

Limitations
A limitation of the x-ray, CT, and gamma-ray techniques is that they can determine saturations in cores only if they are saturated with tagged fluids. Therefore, they may not be suitable for the basic core analyses. A limitation of the NMR technique is the inability to handle cores containing significant ferromagnetic materials, clays, or gas.

ESCUELA DE INGENIERIA DE PETROLEOS

Measurement Capabilities of Scanning Saturation Techniques

ESCUELA DE INGENIERIA DE PETROLEOS

COAL ANALYSIS
The method described here for determining the moisture content of coal involves drying water from a crushed sample in a convection oven and taking successive weight measurements until equilibrium is achieved.

Apparatus
Crusher Drying pans Drying oven Balance Glass desiccator Glass desiccator

ESCUELA DE INGENIERIA DE PETROLEOS

Procedures/Precautions
Sampling
Crushing Sample Size

Weighing
Drying Pan Sample Initial Weight Dry Weight Measurements Do not over-dry the coal sample. Oxidation of the coal occurs if it dries too long in air.

ESCUELA DE INGENIERIA DE PETROLEOS

Calculations
Calculate moisture content using the following equation: M = [(W2 W3)/(W2 W1)] x 100 Where: M = moisture content of coal sample,%. W1 = weight of empty pan, g. W2 = weight of wet coal plus pan, g. W3 = weight of dry coal plus pan, g.

ESCUELA DE INGENIERIA DE PETROLEOS

Advantages
The principle advantage of this method is its simplicity. The procedure does not require a large capital investment in specialized equipment.

ESCUELA DE INGENIERIA DE PETROLEOS

Limitations
Some types of coals have a tendency to oxidize using the technique described here. Moisture content results will be too low if oxidation occurs; oxidation adds weight and will cause the dry weight to be too high.

ESCUELA DE INGENIERIA DE PETROLEOS

OIL SHALES
Oil and water saturations are obtained by a high temperature retorting process. No attempt is made to measure gasfilled pore volume. The fluid saturations are reported in gallons per ton.

ESCUELA DE INGENIERIA DE PETROLEOS

Apparatus
The apparatus is the same as used for the Retort Method at Atmospheric Pressure. The fluids are collected in 15 cm3 centrifuge tubes.

ESCUELA DE INGENIERIA DE PETROLEOS

Procedures/Precautions
The procedure is similar to the procedures described in the RETORT METHOD AT ATMOSPHERIC PRESSURE with the following exceptions: a. The representative sample, approximately two inches in length, is not broken in half. Permeability is a not a consideration in oil shale analysis. b. No attempt is made to screen the crushed sample to exclude fines created during the crushing process.

ESCUELA DE INGENIERIA DE PETROLEOS

Calculations
Calculate moisture content using the following equation:

ESCUELA DE INGENIERIA DE PETROLEOS

Advantages
Large volumes of sample can be used. The method is fairly rapid. All measurements are made directly and independently of others. Standard retorting equipment and procedures can be used.

ESCUELA DE INGENIERIA DE PETROLEOS

Limitations
Limitations of this method include: a. Oil yields may be dependent on rate of heating. b. Due to emulsions, there may be difficulty in reading the meniscus in the collection glassware.

ESCUELA DE INGENIERIA DE PETROLEOS

GYPSUM-BEARING CORES
Such formations are frequently heterogeneous with vugs and/or fractures so that full-diameter core analysis procedures are preferred. However, determination of fluid saturations of gypsum-bearing cores by the distillation extraction method (Dean-Stark) for full diameter cores using toluene as the solvent is not recommended.

ESCUELA DE INGENIERIA DE PETROLEOS

Apparatus
Appropriate apparatus for this method include: a. High temperature retorting equipment b. Low temperature cleaning apparatus, e.g., pressure saturator large enough to pressure cycle a solvent through several samples at one time. c. Boyles law porosimeter.

ESCUELA DE INGENIERIA DE PETROLEOS

Procedures
The core to be analyzed should be laid out on a table and fitted together as in standard practice. The fluid saturation of the trimmed plug ends and/or the remaining material from the segment of core from which the above mentioned plug has been drilled, is determined by the retort method at atmospheric pressure The drilled plug samples should be cleaned in a pressure vessel using an azeotrope mixture of 1/3 acetone, 1/3 cyclohexane, and 1/3 methanol. ESCUELA DE INGENIERIA DE PETROLEOS

Precautions
Care should be exercised drying samples taken from the pressure saturator to prevent dehydration of any gypsum present. Monitor vacuum oven heat with a temperature probe.

ESCUELA DE INGENIERIA DE PETROLEOS

Calculations
Refer to Retort Method at Atmospheric Pressure and Summation-of-Fluids Porosity Calculations Boyles Law Porosity Calculations Soc= Vo /(Vbr x flt) Where:
Vo =volume of oil obtained from the retorting of the trimmed ends or material adjacent to the plug sample, cm3. Vbr =bulk volume of the retorted material, cm3. flt =porosity of the plug after low temperature extraction, fraction. Soc =adjusted oil saturation, fraction.

ESCUELA DE INGENIERIA DE PETROLEOS

Advantages
a. Damage to gypsum is minimized when the sample is cleaned by pressure cycling. Pore volume measurements used to calculate saturations are more representative if the gypsum is not damaged. b. Gypsum content can be estimated by porosity comparisons.

ESCUELA DE INGENIERIA DE PETROLEOS

Limitations
a. The low temperature cleaning process can be time consuming depending on the oil gravity and the permeability of the core material. b. The retort oil and water saturation values are not as precisely determined as for samples that contain no gypsum.

ESCUELA DE INGENIERIA DE PETROLEOS

Calibration
The equipment used to measure porosity by both methods must conform with standards for the appropriate porosity method.

ESCUELA DE INGENIERIA DE PETROLEOS