Method for fluid chemistry determination during well drilling and fluid production

FIELD: in-situ or remote measurement and analysis of drilling mud, completion fluid, completion fluid, industrial solutions and reservoir fluids.

SUBSTANCE: method involves taking liquid samples from predetermined liquid sample taking points where drilling mud, completion fluid, completion fluid, industrial solutions and reservoir fluid flow or are stored; introducing the samples in chemical analyzing microfluid system linked to computer device; performing one or several selected tests in said microfluid device with the use of test result detecting and data creation means; converting said data with analytic test results obtaining; monitoring said results to control selected parameters of drilling operation, reservoir penetration and operation.

EFFECT: decreased amount of sample and test reagents.

12 cl, 3 ex, 3 tbl, 5 dwg

 

The technical field

The present invention relates to the measurement and analysis of drilling fluids, fluids for drilling, solutions for completions, production fluids and reservoir fluids on the rig floor or in a remote laboratory. In particular, it relates to microfluidics (i.e. the microelectronic device type or MEMS) technology, the measurement of drilling fluids, fluids for well completion, solutions for drilling, production fluids and formation fluids in real-time, on-site drilling or remotely, faster, more reliable, and more economical with the best reproducibility of the results. Examples of properties of drilling fluids, indicators which can be measured by the proposed method include, for example, measuring the concentration of ions in fluids, such as chloride concentration, water hardness (Ca2+, Mg2+), the concentration of bromide ions, heavy metals such as Zn, Ba, and Cd, the reactive groups of slate, Zeta-potential, enzymes and biopolymers.

On the basis of these tests it is possible to optimize the properties of drilling muds and fluids for completion of the reservoir to improve their performance characteristics, to meet higher standards to protect the environment and improve the economic and technological is of pokazateli, can also be periodic intervention to minimize the damage caused by the incompatibility of solutions for dissection of productive and production of the reservoir.

Prior art

In the process of drilling solids, fluids and gases are carried to the surface of the drilling fluid (mud)collected and analyzed. The drilling fluid, the solution for drilling and mortar for completion is usually analyzed several times a day on several key chemical properties to ensure technological properties, compliance with the requirements of environmental protection and the safety of drilling fluids. Examples of the properties tested for the drilling fluids, fluids for well completion and production solutions are as follows: alkalinity, chloride, polymer concentration, density, hardness, iron, test methylene blue, pH, potassium, the concentration of silicate, the concentration of sulfides, salinity, the content of the shale inhibitor, the content of the hydrate inhibitor, the inhibitor content of asphaltene precipitation, the concentration of heavy metals and compatibility of formation fluid with a solution to the reservoir.

Usually these tests are wire is provided by one or twice a day measurement solution simplified, although relatively long, analytical methods. When conducting a more detailed analysis. Given the complexity of liquid systems, the high cost of drilling and completion of wells and the risk of production losses, such tests are not satisfactory analytical tests. It would be desirable if there was a faster and more flexible way to analyze the chemical properties of the drilling fluid, the solution for the opening production of the formation or production of a solution, which would provide higher reproducibility of the results.

Chemical sensors and especially Mikroelektronika device (MEM), which measure the performance of biochemical properties that are under development in the biomedical industry. Device through which carry out measurements may include optical mass spectroscopy (UV, visible, infrared, and near infrared), a potentiometer, a calorimeter, a selective chemical sensors, instruments, optical rotation, diffusion and chromatographs.

Measurement principles for chemical sensors and chemical sensors for liquids and gases in some cases similar, but the use, as a rule, very different due to large differences in the complexity and variability of the target substances. So, is serenia gas include chemically very simple matter, usually do not interact significantly with each other in the gas phase or in the analytical system. In contrast, liquids, particularly those associated with drilling, reservoir opening and operation of the wells contain a complex mixture of solids, ionic substances, surface-active agents of various types, hydrocarbons, water and polymers. Specialists in this field will understand that not all devices mentioned above, suitable for gases and liquids, and that even when the principles are similar, the scope of the devices differ significantly.

In U.S. patent 5306909 disclosed method of analysis of drilling fluids, which includes the use of reflective infrared spectroscopy. The method uses the standard components of the drilling fluid for calibration and provides an assessment of the concentrations of various polymers in water and oil drilling muds, water, and chemical activity of water and quartz and other minerals in oil drilling fluids with an accuracy of 10-20%. Declared the possibility of estimating parameters for the various properties of the drilling fluid by using a calibration of the fluid for which the parameters mentioned properties are known. Important points that should be noted are as follows: the method is based on the calibration set of well-studied is the materials, which may or may not correspond to the materials for use in the field, and the method has very limited accuracy for mineralogical assessments without specifying the accuracy of other estimates. In addition, although stated that does not require sample preparation, the importance of indicators of dispersion limits the distribution of particle sizes in the samples to be analyzed. Therefore, at the place of application of the above method will be limited.

In U.S. patent 6176323 disclosed method of analysis of the chemical composition of drilling fluids, as well as concentrations of trace elements in these solutions. In particular, the patent pending measurement capability: "(a) in the mud of interest hydrocarbon; (b) the presence of mud water; (C) the amount of solids in the drilling fluid; (d) the density of the drilling fluid; (e) the composition of the downhole drilling fluid; (f) the pH of the drilling fluid, and (g) (H2S in the mud". These measurements are carried out using only optical spectroscopy only total reflection and optical spectroscopy in combination with the Sol/gelinas technology with the receiving environment for the reactions of chemical compounds in the mud with chemicals in porous glass with getting painted centers, which can be detected optically. The chemical is such a connection in the mud can be added as part of the formulation of the drilling fluid or may be present as a result of inflow of deposits during drilling.

Full reflection system requires the use of two separate detectors, one for the incoming drilling mud and other drilling mud fluid passing through the drill bit, with the subtraction of the spectrum of the first (or intensity at one wavelength) of the spectrum of the last (or intensity at one wavelength), the difference represents the range (or intensity) of interesting compounds. It should be noted that the drilling fluid that passes through the drill bit (for drilling mud in the annulus), contains solids drilling fluid, particles of different sizes resulting from drilling, the diameter of which varies from a micron or two to centimeters. The total reflectivity, as is well known to specialists in this field, essentially depends on the size of the particles in turbid solutions and it is difficult to quantify in the laboratory. Thus, the subtraction operation applied to the two profiles, which are not quantified characteristics are unlikely to give valuable information.

Sol/Galina technology feasible for a single measurement, if the target compound can interact with the formation of colored fragments that can be detected by the optical system. Of contaminants mud below, one is th impurity, most likely detected by the reaction with the formation of colored compounds, is H2S. For this reason, the following will be discussed in this material. The method is based on diffusion of the target of the analyzed compounds through a porous glass medium and clash it with chemical compounds designed to interact with him with the formation of a colored product. The system requires the use of drilling mud is water-based for optimal reactivity, because the glass is wetted with water, and the reactions take place in aqueous medium. Therefore, it is doubtful that this method can be implemented for the synthetic/oil-drilling muds, which contain hydrocarbons as the external phase. For drilling fluids, water-based pH is usually about 9, and often higher, which leads to the presence of several or even several hundred ppm H2's not considered a problem; detection at the surface is appropriate. Operators who are concerned about the possibility of the presence of H2S, usually increase the pH of drilling mud, add a buffer to provide additional protection to the pH, and/or add acceptor sulfide, some of which are commercially available.

A key element of the Sol/gelinas technology is the fact that after the molecule was browseinterval with the formation of the connection, determined by optical spectroscopy, it cannot be reused. Thus, the method cannot be used to estimate the chemical composition of the downhole drilling mud in the usual way.

In the mentioned patent 6176323 stated that the detection methods include the use of "visible light, infrared, near-infrared, ultraviolet, radio frequency field, electromagnetic energy, and nuclear energy", but they are not confirmed by the description of the patent. Electromagnetic energy includes all previous types in this list, the patent does not disclose the use of nuclear energy, only considered non-radioactive atomic label, deuterium.

The use of Microsystems known in areas related to biology, medicine and explosives. Sandia National Laboratories (U.S. Department of the organization on energy - a United States Department of Energy organization) revealed the use of Microsystems for detection of various products. This organization has investigated the use of microscale gas chromatography in combination with surface acoustic wave sensors for detection of explosives among other materials. In addition, she has developed a handheld device, which with a microscale chromatography, for the particular application for the detection of explosives. Sandia has also developed two methods of chemical detection of explosives and weapons of mass destruction. In the underwater installation for explosives used the ion mobility spectrometer to identify the chemical characteristics of the materials. Steam block-based acoustic wave sensors designed for specific compounds. It is important to note that these systems were applied only to explosives and that the blocks are disposable is not applicable for fluid systems in which it is necessary to make repeated measurements. Concept analysis of aerosol particles patented by Sandia U.S. patent 6386015: "a Device for the collection, classification, concentration and characterization of particles formed by the gas.

Researchers at the University of Washington, Seattle, develop continuous measurements of different concentrations of the analyzed substances, but the main area of application of the invention - medicine (see, for example, U.S. patents№№5716852, 5948684, 5972710, 5974867, 5932100, 6134950 and 6387290).

In U.S. patent 5910286 disclosed chemical sensor, which is based on the "molecular fingerprint", in which the cavity formed by Poperechnaya polymer has the same size and shape as the target analyzed pedestal this approach - one-time definition of a chemical substance. A particular application is not specified.

In U.S. patent 5984023 disclosed downhole measurement on the physical and chemical properties of the cores during the selection process, including porosity, bulk density, Mineralogy and saturation of the liquid. The main goal is the determination of the properties of rocks and limited aspects of the analysis of liquids, which is so common, that they cannot be applied for the analysis of mud mortar for the opening production of the reservoir or to analyze the working solution.

In U.S. patent 6023540, which is based on two earlier U.S. patent No. 5244636 and 5250264, describes how the development of bundles of optical fibers with multiple matrices, microspheres coated with specific materials that interact with the target being analyzed substance by providing a unique characteristic properties. Although not specified a specific field of application or type of application, the approach is based on a one-time use and is not suitable for use in a fluid environment.

In U.S. patent 6070450 disclosed is a gas sensor for detecting methane and carbon monoxide in a single device using a layered structure in which the surface of the sensor for "town gas" (methane etc) is the sensor for the incompletely burned gases, the same is how the carbon monoxide. This device is intended for use as part of the alarm system and is intended for individual use.

In U.S. patent 5822473, which is based on U.S. patent 5760479, disclosed a method of manufacturing a chemical sensor based on an integrated microchip that is intended to determine whether a single connection for individual use. Again, these systems individual use are not suitable for fluid systems in which it is necessary to conduct repeated measurements.

In U.S. patent No. 5610708 and 5502560 disclosed device for measuring microscale sample reflective light spectroscopy for process monitoring. Scope relates to the recognition of tree sizes of the particles in aqueous solution.

Center for process analytical chemistry, University of Washington the Center for Process Analytical Chemistry (CPAC) at the University of Washington (UW)) sponsors NeSSI (the New Sampling/Sensor Initiative) to develop new miniaturized systems for sampling-based semiconductors, adapted for use to obtain feedback in real time on the concentrations of many chemical compounds in chemical processes, but no patents on microfluidic test or device is not received. The aim is rather to develop ways of processing the information, than the development of new sensors.

Other research directions CPAC offer: 1) programmnoe detection and identification of volatile organic compounds used for a variety of simple compounds in terms of individual application; 2) surface plasmon resonance sensors with the intended applications for the analyzed biological compounds; 3) Raman spectroscopy for process monitoring and evaluation of material properties (historically, this approach was limited white solid or colorless solutions, as a large laser power is absorbed by the darker colored materials, leading to a rapid temperature increase. The above does not allow to apply the techniques for drilling fluids, the use of techniques for drilling fluids is limited due to the complexity of the spectrum and insensitive to ions of metals; 4) technological liquid chromatography and sampling at the microscale, which are under development; and 5) the concept of "lab-on-a-valve" for monitoring fermentation. Not known no patents on any of these concepts.

APS Technology, Hellertown, PA, has a contract for a three-year project to develop downhole sensor for technological solutions, however, he only considers the very Grubu the assessment of water gas and oil.

Microfluidic technique is a term used to identify a chemical analysis conducted in the micro-channels etched on the glass plate. Earlier microfluidic device was issued U.S. patent 5376252, Pharmacia Biosensor. Microfluidic sensors and devices are designed mainly for medicine and biotechnology. Analyses, such as the characterization of DNA and RNA, were conducted on small chips. For example, in U.S. patents№6358387, 6306659, 6274337, 6267858, 6150180, 6150119, 6132685, 6046056 and 5942445, Caliper Technologies, Inc., disclosed microfluidic devices and methods that can be used to implement high-performance research. Review microfluidic technology described in the publication Whitesides, G.M., Strock, A.D. [2001] "Flexible Methods for Microfluidics", Physics Today, 54 (6), 42-48.

In the art there is a need for a convenient way continuous or periodic measurement and analysis of chemical compounds mud. It would be especially desirable if such a method was required only small amounts of sample and reagents, and would give reliable, reproducible results. Insufficient content of some compounds in the mud or the presence of impurities could be determined in real time, to avoid well control or dangerous situations, it would be the OS which may serve as a basis appropriate treatment, to avoid costly downtime associated with the use of drilling mud, and to minimize costly processes of closing the production wells. Such a system could more effectively to solve problems in chemistry (composition) of drilling fluids related to flocculation of the mud and chemical imbalance and dangerous tributaries H2S, CO2and CH4.Furthermore, the method could also provide important measurements of concentrations of hydrocarbon gases, noxious gases, crude oil, water, traces of other elements and inhibitor (deposits of soot and asphaltenes, hydrate formation).

Summary of the invention

The technical task of the present invention is to provide a method for determining the chemical composition of the drilling mud, which enables automated measurement of concentrations of chemical compounds in drilling fluids, solutions for dissection production of reservoir fluids for well completion, production fluids and formation fluids using microfluidic technology, which requires only small amounts (for example, microlitres) solution and reagents for testing, thus allowing to use the minimum cycle time, the minimum sample size, minimal detrimental effect helices is their compounds on humans and the environment due to the use of the lowest effective concentrations. The present invention also allow for the compatibility tests of machining fluids with formation fluids, to optimize the concentration of the inhibitor and to improve control over the mud.

The present invention may be included in a desktop appliance, running on the application site, the current tool or downhole chemical analyzer.

In accordance with the foregoing, the present invention is a method of performing periodic or continuous analysis of fluids used or produced in the drilling process, drilling and operation of wells containing:

1) collecting samples of fluid from a liquid stream,

2) sample preparation,

3) carrying out the selected analytical tests on liquid chemical analyzer using microfluidic methods

4) use of detection results of the tests and the formation of data

5) convert the specified data with the results of the specified analytical test

6) monitoring (monitoring) of these results to tune the selected aspects of drilling operations, drilling, completion or operation.

The following is an explanation of each step of the method.

(1) the Sample can be selected from fluid flow to or from the Kvasiny, near the drill bit, or at pre-defined points of the selection of the sample, where three or stored drilling fluid, solution reservoir, the solution for well completion, reservoir fluid, or production solution. Sample requirements - less than one cubic centimeter of fluid. Preferably, but not necessarily, to filter the selected fluid through the filter (for example, a rigid circular paper filter).

(2) the Sample fluid must be prepared in such a way as to ensure the necessary measurements. Such preparation may include, for example, dilution of the sample to achieve a uniform viscosity of all liquids (including fluorescent dyes, buffers and standard solution) or to reach the same concentration of chemical compounds, which lies within the sensitivity of a fluorescent dye. Sample preparation may include additional filtering solution.

(3) Microfluidic devices are glass or plastic plates that are pre-specified schema, etched, printed or molded channels and cavities on them. Depression or the so-called cavity on these plates hold the liquid sample and, depending on the selected test, can also contain buffer solutions, fluorescent dyes is liquid solutions of chemical compounds chemical reactions, or mixtures of liquids. Such channels or cavities can be pre-treated to change the surface properties of glass or polymer, they may contain typical Mikroelektronika devices, such as pumps, valves, or heating elements. The movement of the solution inside the channels is due to the action of electrokinetic forces (i.e. by application of an electric field) or by application of a pressure gradient over the cross section of the channels.

(4) using the known methods it is possible to measure the concentration of a sample by comparison with a known standard liquid (for example, when using fluorescent dyes or formation of a standard and measured curves), or to measure the resistivity of the solution, the relative flow in the channel, the compatibility of two or more liquids or viscous liquids.

The measurement of the concentration of the sample can be carried out, for example, the formation of a standard curve using well-known standard solution that contains a known concentration of the analyte. Suitable fluorescent dye is added to the standard solution and measure the increase or decrease of the intensity of the dye of the analyzed substance when using the standard detection methods fluorescence (for example, photome is sustained fashion tubes). May be effected by an additional dilution on the spot. In the same or separate microfluidic Protocol, on the same or separate plate gain curve measurements using the same a suitable fluorescent dye. May be effected by an additional dilution of the sample on the spot. Comparing thus obtained standard and test curves, it is possible to determine the concentration of the sample.

(5) converting the measured data to obtain the results of the test can be carried out by comparing the standard curve and the curve of the sample using the equations or known by automated computer programs. For example, the measurement of the resistance of the fluid can be carried out according to the following equations

Voltage=Resistance·Current

(6) Monitoring (monitoring) chemical properties allows you to define the imbalance in the chemical compositions of fluids that could potentially affect the technological properties of drilling mud, mud for drilling and solution for completion, in compliance with the requirements of environmental protection to the above solutions or productive capacity of the well. The concentration of some chemical compounds can be adjusted by adding cm is causig action of chemical substances, such as acceptors oxygen, corrosion inhibitors, biocides or anti-fouling, hydrates or inhibitors, asphaltene precipitation, in response to the result of a specific dimension.

Brief description of drawings

The invention is further explained in the description of the preferred variants of the embodiment with reference to the accompanying drawings, in which:

figure 1 depicts a chart speed of response when measuring the resistance of the standard solutions and filtrates mud;

figure 2 depicts the time-averaged a graph of the results of the resistance measurements of the standard solutions and drilling mud filtrate, according to the invention;

figure 3 depicts a graph of the intensity of fluorescence of the mud filtrate, containing NaCl, fluorescent dye is extinguished by the presence of chloride in the filtrate, according to the invention;

figure 4 depicts a graph of the intensity of fluorescence of the mud filtrate, containing fresh water, a fluorescent dye is extinguished by the presence of chloride, according to the invention;

figure 5 depicts a chart measuring the concentration of calcium.

A detailed description of the preferred variant embodiment of the invention

The method according to the invention allows automatic measurement of the concentration of a chemical connection is on, it only requires a small amount (i.e. Microlitre) solution and reagents for carrying out these tests, allowing you to provide the minimum cycle time, the minimum sample size, minimal impact of chemical compounds on humans and the environment due to the use of the lowest effective concentrations. The present invention also allows compatibility tests of the processed fluids with formation fluids, to optimize the concentration of inhibitors and improve the management of the flow of drilling mud.

The method according to the invention can be used to increase the efficiency of drilling through monitoring of chemicals in the drilling fluid and the presence and concentrations of ions, polymers and inhibitors added for security and improve performance.

The method can be used for tests that are currently in use in the normal analysis, and tests that are too difficult for ordinary measurements using traditional methods of analysis.

Examples of tests that can be used microfluidic methods are the measured concentrations of, for example, chloride, polymer concentration, water hardness (calcium ions and/or magnesium), iron content, is the actual content of potassium, the concentration of silicate, salinity, concentrations of heavy metals, the concentration of inhibitors slate amine type, presence of acceptors oxygen production on the detection of traces of chemical elements, bromide ions, sulfides, thiosulfates, phosphates, biocides and the concentration of inhibitor hydrates. Examples of typical tests include compatibility: the compatibility of the formation fluid with a solution for completion in the well, the definition of crude oil and emulsions, the measurement of the reactive groups of slate and compatibility acids and brines to completion with the formation fluids. Typical dimensions for testing reactive groups of slate are: test methylene blue, Zeta-potential and the effectiveness of the polymers. Examples of other tests which can be applied microfluidic technology are: alkalinity, determination of enzymes, specific biopolymers and pH.

When implementing the present invention are selected samples, continuously or intermittently, from the process stream for analysis. The sample solution can be located, but is not limited to this, on the lines of the feed solution into the well and from the well, the bottom node of the wells near the drill bit, under cutting shale shakers and on the remote station for sample preparation production line.

The present invention can be included in table a device for use in a linear device or downhole chemical analyzer.

Liquid chemical analyzer

Liquid chemical analyzer for testing solutions can be a sensor of any type, micro system or tool for analysis in this area, which is not limited to individual use. Analyzing instrument preferably is microfluidized a device made of a glass plate or a plastic plate, which is applied to a predefined scheme for two-dimensional or three-dimensional etched, molded, or printed channels with cavities in them. Typically, these channels or cavities will have at least one transverse dimension that ranges from about 0.1 to about 500 microns, and preferably from about 1 to about 100 microns. Dimensions can also be in the range from about 5 μm to about 100 μm. Using the dimensions of this procedure allows you to implement a greater number of channels, cavities or cells for the sample in a small area and use smaller volumes of reagents, samples and other liquids for the preparation or analytical operations that are required on the sample. Such devices are disclosed, for example, the U.S. patents No. 5165292 and 5876675. The channels or cavities can be pre-treated to change the surface properties of the glass or polymer channels, and they may contain typical Mikroelektronika devices, such as pumps, valves, or heating elements. The movement of the fluid inside the channels can be done using electrokinetic forces (for example, when the application of an electric field) or by the application of pressure gradient over the cross section of the channels. Inside the channels can be made simple chemical reactions. Types of measurements in such microfluidic devices may include the determination of concentrations of the sample, reactive groups, relative velocity, viscosity, hydraulic or electrical resistance.

Suitable microfluidic device typically has at least three or more cavities, etched or cut into the plate with channels connecting the camera. These cavities serve as reservoirs for the retention of such reagents as the sample solution, standard solution, the dilution buffer or a fluorescent dye and the cavity for the spent solution. The cavity is connected with the above-mentioned channels so that between these solutions can be confusing. For example, the cavity containing the sample solution, can be connected with the cavity of the La buffer, with a cavity for dye and with a cavity for the spent solution. The fluids are moved through the channels under the action of pumps or electrokinetic forces. The photomultiplier may be directed to any point of the network channels, but preferably in the portion of the channel, where there is a mixture, and where you can observe the interaction of sample or standard liquid dye.

The fluid flow in microfluidic devices

Microfluidic device used in the present invention for analysis of liquids, characterized by the presence of systems of movement and direction, using either mechanical pumps or valves (see, for example, U.S. patent 6171067), or by the application of external pressure or electrokinetic flow for selective movement and direction of fluids through various vzaimosoedinenie channels or chambers contained in the device or system. One example of a controlled electro-osmotic flow is described in the published international patent application no WO 96/04547. When appropriate, the liquid is placed in a channel or pipe for liquids, the surface of which has a functional group, these groups can ionize. For example, if the surface of the channel includes hydroxyl functional groups on the surface, for example, as in the case dioxide to Omnia, protons can leave the surface of the channel and move into the solution. In such conditions, the surface will have a total negative charge, whereas the solution will have an excess of protons or positive charge is localized near the interface between the surface of the channel and solution. When application of the electric field along the length of channel cations will flow to the negative electrode. The movement of positively charged fragments in solution leads to saturation of the solvent. Stationary speed of the movement of the solution in the channel is directly proportional to the Zeta-potential (electrokinetic potential) surface in contact with a roaming solution (see, for example, U.S. patent No. 5304487 and 5800690).

Microfluidic dimension

A typical method is based is not limited to downhole fluids and provides standard and the measured curve. The method or Protocol of measurement, is preferably determined in advance and recorded in the form of a simple program, through which you can control pumps, voltage or current supplied across the channels or cavities. The test liquid, standard liquid, fluorescent dyes and, if necessary, other reagents, such as buffer fluid is introduced into the receiving tank or cavity on microfluidic plates. The introduction is of small amounts of test compounds can be carried out manually by pipette or automatically, using, for example, electrotyped (see, for example, U.S. patent No. 5779868). Mentioned receiving tanks or cavity usually require less than 25 microliters solutions.

A standard curve obtained using well-known standard solution that contains known concentrations of the analyzed compounds. Suitable fluorescent dye (the intensity of which increases or decreases in the present of the analyzed compounds) is added to the standard solution. Fluorescent dye is excited under the action of a suitable light source such as a mercury lamp, an argon lamp, a xenon lamp, LED lamp or laser. A set of mirrors for excitation, emission, and dichroic mirrors is chosen so that the wavelengths of fluorescence excitation and emission were optimized. Can be used broadband filters to optimize the excitation spectra and emission.

The damping or amplification of the intensity of the dye under the action of the analyzed compounds was measured using standard methods for the determination of fluorescence (e.g., photomultiplier tubes). Can be made more dilute at the place of use. The intensity of the fluorescence recorded. Using the same microfluidic plate which is jut curve measurements using the same fluorescent dye. Can be an additional dilution of the sample on the spot. The fluorescence intensity of the dye is measured and recorded. When comparing the standard and test curves it is possible to determine the concentration of the sample.

Microfluidized the device can be mounted in a desktop device, which enables the use of microfluidic technology and may include microfluidic device with cavities and channels, excitation source, suitable filters and photomultipliers, and the storage device test results. The design of the device allows the use of the method for illumination and detection using lamps of a wide range, such as mercury, argon, or lamps narrower range, such as LED with a predetermined bandwidth. The detector of the analyzed compounds can be placed close to the viewing area of the substrate to determine the formation of products and/or passage of the reactants along the side of the substrate. The computer may be operatively connected to the detector analyte monitoring of formation of the reactants (see, for example, U.S. patent 6046056).

In the method according to the invention these operations can be used to obtain a number of key dimensions. The following are tests that can be performed on the drilling fluid, R is the sites for drilling, well completion, reservoir fluids and production solutions in real-time, on site or remotely, with faster, more reliable, and more economical with the best reproducibility of the results.

Reactive group slate and Zeta-potential can be measured with the use of such dyes as polymethine dyes, including but not limited to this, stillove dyes, oxanol, cyanine, especially carbocyanine, and merocyanine 540. Other suitable dyes include sulfur compounds, including rhodamine.

Ion concentrations far exceeding those that can be observed in biological systems, can be measured using indicators with low affinity or dilution of the sample is enough to shift the concentration of ions in the sample in the region of dyes with high affinity. Suitable examples are indicators of calcium, including but not limited to this, the PTS, Mag-Fura-2, Mag-Fura-5 and Mag-Indo-1 (disclosed in U.S. patent 5501980)supplied by the company Molecular Probes.

The calcium concentration can be measured using a dye that increases the intensity with added calcium, such as fluo-5n (disclosed in U.S. patent 5049673), or alternatively Oregon Green (antakarana salt BAPTA-2)supplied by the company Molecular Probes.

Inhibitors cancelling type can be measured using dyes, they join to amine groups of proteins and enzymes can be determined using dyes that are specific for proteins or which are connected to amines. Such measurements can be used for quantitative monitoring during drilling. Acceptable dyes for these tests include, for example, the number of derivatives of carboxyfluorescein, including, but not limited to, dyes Alexa (Alexa), an example of which is Alexa Fluor supplied by Molecular Probes (Alexa Fluor is a trademark).

Biopolymers in the fluid can be identified by their interaction with enzymes containing specific fragments, and then the determination of glucose, the end product of the enzymatic activity. Suitable substrates include dihydroprogesterone (also known as fluorescine), dihydrorhodamine and 10-acetyl-3,7-dihydroxyquinoxaline sold under the trademark Amplex Red. (see U.S. patent 6265179).

Can be measured acceptors oxygen. This test is especially important in high-temperature wells to increase the efficiency of the polymers in drilling fluids, water-based. Suitable dyes include those that are used to measure reactive oxygen compounds, and include, but are not limited to, Luminal (Luminol) and kr is the bearers acridine group, such as Lucigenin (Lucigenin).

Crude oil and emulsions can be determined using sensitive lipid dyes selected from hydrophobic dyes, including but not limited to this, Nile Red.

The amount of water in facing systems drilling fluid can be measured using dyes for flow monitoring. Suitable dyes include, but are not limited to, fluorescein.

Information on the distribution of (part of) the products can be obtained by measuring traces of such elements as sulfur, Nickel and vanadium, with appropriate dyes.

Water hardness can be estimated as the total content of calcium and magnesium. It is advisable to use dyes, including fluorescent Ca+2 indicators, excited by UV light or visible light spectrum. As examples, but not limited to, derivatives, related Rhod-2, and the indicator Calcium Green, and the halide-specific fluorescent dye, 6-methoxy-N-(3-sulfopropyl)chinoline (SPQ). Bromide-ion (in the form of traces in systems reverse flow) can be measured by turning into hypobromite-ion and reaction type dyes Rhodamine 6G (Rhodamine 6G).

Heavy metals, including zinc, barium and cadmium, can be measured using the fluorescent indicator-based PE is agodnego metal, such as Phen-Green, or indicator-based compound that binds zinc chelate compound and a heavy metal, such as 5-nitrobenzothiazole coumarin (BTC 5N). Very high concentrations of chlorides in excess of biologically acceptable levels can be measured using, for example, acridine orange (Akridine Orange), one of the dyes series of acridine.

The pH value above 8 or below 5 can be determined using pH indicators, including but not limited to, SNARF-1 and BCECE. The levels of sodium and potassium can be measured using, for example, Sodium Green, SBFI and PBFI (bestfurniturestore connected with simple crown ether)supplied by the company Molecular Probes. Sulfides can be determined using, for example, chromogenic papadopulo substrate L-BAPNA (4-nitroanilide α-N-benzoyl-L-arginine). Derivatives of bimana (bimane), such as, for example, monobromobimane, firms Calbiochem, can be used to determine the sulphides, H2S, which is very toxic, and thiosulfate, which is used as a corrosion inhibitor in liquids for completion (trademark of Calbiochem).

Inorganic phosphate can be determined using a kit for the study of the drilling fluid on phosphate sample, such as PiPer Phosphate and EnzChek supplied by Molecular Probes (brand EnzChek). About what the definition of microbes to optimize the concentration of biocides can be carried out with the use of penetrating into the cell dye, such as MitoTacker supplied by Molecular Probes (Mitotracker is a trade mark). To determine the effectiveness of biocides in drilling fluids, water-based, glycosilated amidine and dihydrouridine can be used for staining living and dead cells. Measurement of iron content, it is important to optimize the concentrations of acceptors H2S and corrosion and can be implemented using calcein. Compatibility of the acid solution for well completion and brines with crude oil (including asphaltene precipitation) can be determined by measuring the relative changes of flow in microfluidic channels.

Compatible fluids with a solution for completion can be determined by measuring the relative changes of flow in microfluidic channels.

Data for use at the location of the well can be obtained by measuring the composition of the hydrocarbon compounds liquid chromatography.

Resistance or viscosity can be measured to hydrate inhibitors, such as ethylene glycol and methanol.

Buffers are used to maintain the pH during the reaction. The type of the buffer depends on the interval of pH values required for a specific use, and detailed chemical composition of the dye. Some dyes can withstand high importance is placed pH, when this expedient borate, or carbonate buffers (pH about 9), but for other dyes require a lower pH values, therefore, would be more appropriate such buffers like TRIS or MOPS, or even phosphate (pH of about 7-7,5). For other dyes may require even lower pH or other buffers. In examples 1 and 2, the buffer used to explain the method, represents 10 mm Tris pH 7.5.

The invention can be used for a number of different test fluids and fluids for wells, as indicated above, however, the examples given in the description, provide an analysis of the measurement fluid production wells on the resistance and the concentration of chlorides. The resistivity of the mud filtrate measured in example 1. In the analysis of the filtrate saline/RNRA preferably be diluted. Appropriate interval dilutions ranging from 1:1 to 1:100, preferably 1:10. The filtrate, consisting of fresh water/RNRA, analyze undiluted.

Fluorescence measured in example 2. Available fluorescent dye, Lucigenin (Lucigenin) was used to determine the concentrations of chlorides and got acceptable results. Lucigenin is usually advisable to apply the indicator Cl-in liposomes and reconstructed membrane vesico is Oh, therefore was used for testing.

In the measurement of some parameters such as resistance, the samples were subjected to electric current.

In samples where the measuring principle is based on fluorescence, samples were irradiated with light at a wavelength in the range of from 360 to 700 nm. The wavelength was determined by the spectrum of the excitation used fluorescent dye. For example, the preferred wavelengths of excitation for lucigenin sensitive to chloride ions of the dye, is 368 and 455 nm.

The following examples will clarify disclosed in the present description the invention. Examples are given only as a means of explanation and should not be construed as limiting the scope of the claims of the invention. Numerous changes can be made without disturbing creatures and scope of the claims of the present invention.

Experimental part

Conducted research on the measurement of the total resistance and chloride concentration in the filtrates of the two drilling fluids using microfluidic devices. Standard curves were obtained, which were converted to total resistance and the concentration of chlorides in solution. This study also showed that some parameters, such as the accurate calibration curves of standard solutions, the Protocol changes the response and the choice of the fluorescent agent, important from the point of view of obtaining results.

The chips used in the examples are standard multi-purpose chips that can be used for chemical samples, and are supplied Caliper Technologies, Aclara, and Micronics that specialize in microfluidic technology.

In addition to the control chip and the chemical composition of the monitoring costs, dilutions and measurements during the experiment was used the software.

To test liquids were used for the standard solutions of sodium chloride and mud filtrate. The composition of the drilling fluid are presented in table 1. The drilling fluid was prepared and spun at a temperature of 150°F for 16 hours. The solution was filtered in a standard API filter chamber with the use of filter paper increased hardness (FANN) for 3 hours, collecting a few cubic centimeters of filtrate.

Table 1
The composition of the drilling fluid: unweighted NaCl/RNRA
NaCl/PHPAFresh water/PHPA
Water (deionized)[bbl]0,910,91
Bentonite [mln]8,008,00
NaOH [mln]0,100,10
NaCl [mln]39,50--
The agent control the loss of fluid I [mln]1,001,00
The agent control the loss of fluid II [mln]1,501,50
PHPA1,01,0
Xanthan gum0,500,50

Example 1

Measure the resistance or conductivity of the filtrate of the drilling fluid: fresh water/RNRA and sodium chloride/RNRA. The fluid was a 2M NaCl in buffer, 10 ml Tris pH 7.5. The original solution was diluted with water to working solutions of 50, 100, 250 and 500 mm. The filtrate is fresh water/RNR - used undiluted, whereas the filtrate saline/RNA was diluted in ratio 1:10.

Microfluidized the device used to measure resistance, contained at least three cavities for holding solutions: sample fluid standard fluid and spent the downhole fluid. Cavities are connected to each other and all with a cavity for waste downhole solution.

Before using the chip was washed for 1 normal NaOH solution and was rinsed with buffer before introduction of the sample and the standard fluid. The cross section of the cavities has put strain is 100, 200, 300 and 400 In and measured the resulting current, the calculation of resistance was carried out on the above equation 1. To estimate conductances used software.

Preliminary results of measuring the resistance of the mud filtrate fresh water/RNRA, solutions of sodium chloride/RNRA and standard solutions are presented in figure 1 and 2. Figure 1 shows the step response when the voltage from 100 to 400 Volts. Each experiment is carried out once. The signal quality measurement is very good with only a little noise.

The data was re-laid in the form of the dependence of the current from the equivalent concentration of sodium chloride. You should note that although sodium chloride is the dominant substance emitting ion in the filtrate, some ions are ionic polymers and bentonite in the drilling fluid. Obviously, the response is not linear (figure 2), the steep initial increase should asymptotic approximation to the limiting current values.

Based on the composition of the drilling fluid (mass of sodium chloride in solution) the calculated molar concentration of the solution was 186,8 mm. The average measured molar concentration was 176,6 mm. The measured average concentration of a sample of fresh water was 16.7 mm. The summarized results are presented in table 2.

Table 2
The average measured concentration of drilling mud filtrate based on the measurement of the resistivity of
The average of 2 experimentsFresh water/RNR

[mm]
NaCl/PHPA

[mm]
10-20 seconds16,8798188,0051
20-30 sec16,65734172,5479
30-40 seconds16,52543172,8534
40-50 sec16,82557173,0319
The average concentration [mm]16,72204176,6096

Example 2

Measured concentrations of chloride. In the basis of measurement in this experiment is the fluorescence. Microfluidic device that is used for measuring the concentration of chloride, contains at least five chambers for holding fluids: sample fluid standard fluid, buffer, dye, and the spent solution. The chambers are connected with each other and all with the camera for the spent solution. As a standard source of fluid used 100 mm NaCl buffer, 10 mm borate buffer with a pH of 9.2. As a working solution used 100 mm diluted with 10 mm borate buffer with a pH of 9.2. As the dye used 40 μm of Lucigenin in 10 mm borate is the buffer with a pH of 9.2. As the samples used fresh water and 10%NaCl drilling mud. A sample of fresh water used undiluted, whereas the filtrate containing NaCl mud was diluted in the ratio of 1:17. Carried out the following sequence of operations.

(1) Washed chip 1 normal NaOH solution and was rinsed chip water purity HPLC.

(2) Then the water was removed from the cavities and the cavity was filled with the sample (fluid), a standard fluid, buffer and dye. Software used for monitoring expenses, dilutions and measurements during the experiment. The software also gives the standard curve and the curve for the sample. The program provides a measurement of the fluorescence of the outstanding dye and dye, repaid in three concentrations of chloride. The program allows dilution on the chip. In the first stage formed a "baseline" with the subsequent passage of 100% buffer solution through the point of detection, and measured the intensity of the background. In the second stage, 100% dye flowed through point detection to measure the maximum intensity. At the next stage was measured damping (i.e. decreasing intensity) of the dye in the presence of chloride ions. Stage dilution, which are presented in figure 3 represent the following: 1:16; 1:8; 1:4 for containing NaCl. The stage of dilution, which is shown in figure 4, are: 1:8; 1:4; 1:2 for mud filtrate in fresh water.

Results: the raw measurements of chloride are presented in figure 3 and 4 for fresh water and mud filtrate at 10%wage NaCl solution, respectively. The baseline and the line 100% of the dye shown in the first two stages of the curve in figure 3 and 4. Since Lucigenin is a dye that is subject to repayment, if any addition of chloride to the sample solution will be reflected on the curve as a reduction in the intensity of the dye. After establishing the baseline and the line 100% of the dye was added fluorescent dye (Lucigenin (Lucigenin)) to the standard solution was measured intensity of the fluorescence received speed curve for some extra points when measuring, representing 1:16, 1:8 and 1:4 (containing NaCl filtrate) and 1:8, 1:4 and 1:2 (sample of the filtrate, containing fresh water) dilution of sample buffer. The dye was added to the sample filtrate and measured the fluorescence intensity. The fluorescence of this dye was extinguished in the presence of the chloride ion, which resulted in a decrease in fluorescence intensity. Figure 3 shows the calibration standard and the test sample of the filtrate in the form of two sets of cascaded stages. In the first stage, each GSS is upnote device monitors the fluorescence of the dye in the absence of chlorides.

The generalization of the results of tests to determine the concentration of chlorides shown in table 3. The calculated results for a 10% solution of NaCl are in very good agreement with the actual values.

Table 3
Average measured concentrations of drilling mud filtrate based on measurements of fluorescence
DilutionThe concentration of the standard

[mm]
The concentration of the sample in the chip [mm]
1:15048
1:32522
1:712,512,3
DilutionThe concentration of the standard [mm]The concentration of the sample in the chip [mm]Actual concentration (NaCl in the composition of the mud)
1:15049,546,5
1:32528,523,25
1:712,5of 17.511,63

Example 3

Carried out the measurement of the concentration of calcium in microfluidic chip. The principle of measurement HV the method is fluorescence, but here we have used the fluorescent dye Fluo-5N. This dye increases its intensity by adding calcium ions. You should note that a similar response can be obtained by using the dye Oregon Green (antakarana salt BAPTA-2, patented and supplied by Molecular Probes). Sample preparation consists of the following: five micromol Fluo-5N was diluted in MOPS buffer. The initial calcium concentration in the standard solution was 60 mm. The result is shown in figure 5. The first two speed stages represent the baseline buffer and line 100% dye, the subsequent stages are 1:16, 1:8 and 1:4 dilution of 60 mm calcium buffer solution. The second speed stage, the use of buffer solution and 60 mm calcium solution (representing the test solution) in a separate cameras are identical to the steps of the first step of the curve.

1. Method of chemical analysis of downhole fluids, namely, that (a) collect samples of well fluids from two given points of the fluid, where the downhole fluid flow or stored, (b) impose those samples in microfluidic system for chemical measurements, including at least one microfluidic device containing a chip having at least one inlet for introduction of the test samples is SCA, at least one microfluidic channel and at least three of the cavity, c) perform one or more selected tests on the specified microfluidic device, (d) use the tool for the detection of test results and generate the data characterizing the results.

2. The method according to claim 1, characterized in that the sample collection implement of the locations selected from the group consisting of pipelines to the wells, pipelines from wells, downhole nodes near the bit, under the vibrating screen for drill cuttings and specialized station sampling on the production line.

3. The method according to claim 1, characterized in that it further implementing regulation (clarification) characteristics of the downhole fluid in response to data received as a result of the tests.

4. The method according to claim 1, characterized in that the sample of the downhole fluid is placed on microfluidic device by application of forces selected from the group consisting of application of electrokinetic forces, the application of pressure gradient over the cross section of the channels or use Mikroelektronika pumps.

5. The method according to claim 4, characterized in that it further carry out the selective application of pressure, vacuum, voltage or current to the inputs of the chip in various combinations to provide moves, adds, see the solution, dilution and separation of the downhole fluid.

6. The method according to claim 5, characterized in that additionally they use computer software to monitor speeds, adding, mixing, dilution and separation of these samples and the specified measurements.

7. The method according to claim 1, characterized in that for the implementation of the selected test using the method of fluorescence by comparing the intensity of the selected fluorescent dye that interacts with a standard fluid, with the intensity of a selected fluorescent dye that interacts with the sample of the downhole fluid.

8. The method according to claim 7, characterized in that the fluorescence method is used for testing the properties selected from the group of indicators consisting of reactivity of shale and Zeta-potential, ion concentration, inhibitors slate amine type and enzymes, the presence of biopolymers, the presence of acceptors oxygen, crude oil and emulsions, the presence of water in facing systems drilling fluid, the presence of traces of elements selected from sulfur, Nickel and vanadium, water hardness as a function of the total content of calcium and magnesium, bromide ions on the transformation in hypobromite, heavy metals, concentrations of chloride, sodium and potassium sulphides and compounds sulfides, bacteria, iron content.

. The method according to claim 1, characterized in that by means of the selected test and measure relative changes in consumption in microfluidic channels to determine the compatibility of the acid to close the productive formation and brine from the crude oil.

10. The method according to claim 1, characterized in that by means of the selected test and measure relative changes in consumption in microfluidic channels to determine the compatibility of formation brines from the solution to complete the reservoir.

11. The method according to claim 1, characterized in that when testing provide measurements of content of hydrocarbon compounds by liquid chromatography.

12. The method according to claim 1, characterized in that when testing provide measurements of the resistivity of a sample of the downhole fluid.



 

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Sample taker // 2299983

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EFFECT: higher reliability.

6 cl, 14 dwg

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