Automatic palynological filtration device and method of preparing samples for palynofacies studies

Abstract

The subject of the present invention is an automatic palynological filtration device comprising a base, constituting a supporting and stabilising element, on which at least two column covers are inseparably attached, in which filtration columns are placed, wherein on the base, preferably between the column covers, there is an engine chamber, which is attached to the vibrating plate, which vibrating plate is fixed to the base using supporting springs with rods, preferably attached in the four corners of the base, which enable adjustment of the vibration range and constitute a flexible attachment of the vibrating plate to the base. The subject of the invention is also a method of preparing samples for palynofacies studies using the automatic palynological filtration device.

Description

[0001] AUTOMATIC PALYNOLOGICAL FILTRATION DEVICE AND METHOD OF PREPARING SAMPLES FOR PALYNOFACIES STUDIES

[0002] The present invention relates to an automatic palynological filtration device for palynofacies studies and a method for preparing samples for palynofacies studies.

[0003] Organic microremains (OM) originate directly or indirectly from living organisms, both plant and animal. Initially, OM analysis using an optical microscope focused mainly on the analysis of morphology, taxonomy and biostratigraphic studies based on organic walled microfossils, e.g. sporomorphs or Dinoflagellata cysts. After many years of research, Combaz (1964) introduced the term "palynofacies" as a term for organic matter (kerogen) extracted from rock by chemical maceration using hydrochloric (HCI) and hydrofluoric (HF) acid. Palynofacies studies are based on the qualitative and quantitative analysis of kerogen components while observing their physical characteristics (size, shape, colour, as well as their state of preservation). Initially, this method received a lot of criticism. However, since the beginning of the 1980s it has been used on a large scale, both in scientific research and in the exploration industry for hydrocarbons and mineral resources.

[0004] Currently, palynofacies analysis is used in research works to reconstruct sedimentary environments, determine the nature of deposition, the source area of terrigenous material and the distance from alimentation zones, determine the source of organic matter, interpret transport directions, sea level changes, and even paleogeographic reconstructions. Both biostratigraphic analyses based on organic microfossils and palynofacies analysis have also found application in the petroleum industry. Recognition of individual components of palynological matter allows for determining the type of kerogen (inert, oil-forming, gas-forming) found in the rock. Furthermore, based on the colour of microremains (i.e., Fischer et al., 1980), it is possible to estimate the degree of chemical transformation and maturity of organic matter. Together, these analyses provide information on the oil-bearing potential of rocks, which is essential in hydrocarbon exploration (Tyson, 1993).

[0005] The standard procedure for preparing samples for palynofacies studies consist of following steps: the cleaned rock material is crushed and dried, the crushed rocks are flooded with a solution of hydrochloric acid to remove carbonates, silica is then is removed from the neutralised material using a 70% solution of hydrofluoric acid. After, the residue obtained is sieved manually in an aqueous environment on a nylon sieve with holes of 15 pm diameter to remove grains of a finer fraction (mainly clay minerals). Finally, the organic matter is separated from the remaining mineral components using a heavy liquid, an aqueous solution of zinc chloride (ZnCL) with a specific density of approximately 2 g / cm3.

[0006] The times taken by the individual steps of preparing one sample are as follows:

[0007]

[0008] The above table shows that when preparing one sample, a technician must be involved in 35 min to 1 h 15 min of work, of which 20 - 60 min is filtering.

[0009] The aim of the present invention was to develop a device that would allow a significant reduction in the time of sample preparation for palynofacies studies, limiting the effort and time of the technician’s work, as well as simplifying the activities performed by him, reducing or even eliminating the possibility of sample contamination, and decreasing time of work under aggressive conditions.

[0010] This objective has been achieved by the subject of this invention, which is an automatic palynological filtration device comprising a base, constituting a supporting and stabilising element, on which at least two column covers are inseparably attached, in which filtration columns are placed, wherein on the base, preferably between the column covers, there is an engine chamber, which is attached to the vibrating plate, which vibrating plate is fixed to the base using supporting springs with rods, preferably attached in the four corners of the base, which enable adjustment of the vibration range and constitute a flexible attachment of the vibrating plate to the base;

[0011] - wherein said vibrating plate has at least two holes for the filtration columns and adheres on the perimeters of these holes to the filtration columns transferring vibrations to the filtration columns during the operation of the filtration device; - the filtration columns are mounted in the vibrating plate by means of a mounting plate which is an integral part of the column, which mounting plate together with the column is placed in holes in the vibrating plate;

[0012] - from the top, the filtration column is plugged with a plug equipped with a nozzle with a quick connector to which the water system pipes are connected, in the central part the filtration column is equipped with the above-mentioned mounting plate enabling mounting to the vibrating plate, while in the lower part, the filtration column contains a clamp that tightens the filter, preferably nylon, to the bottom of the filtration column;

[0013] - in the engine chamber, a drive is placed, which sets the vibrating plate in motion, wherein the drive of the filtration device is an engine placed in a sealed housing, in the engine chamber, attached from the bottom to the vibrating plate, which engine contains a shaft extending from both sides of the engine, the shaft equipped with asymmetric weights that generate vibrations of the device during operation;

[0014] - wherein the filtration device is equipped with a water supply and water system valves and the water supply comprises a conduit supplying water to the switchboard, the switchboard fitted with at least two valves regulating the amount of water supplied to the individual filtration columns and the conduits supplying water to subsequent nozzles / columns;

[0015] - in the base there are at least two openings draining excess water together with filtration waste to the settling tank, wherein the draining openings are preferably located under the bottom of the filtration column;

[0016] - below said draining openings in the base there is a settling tank collecting solid material and draining water, preferably resting on settling tank guides attached from below to the base; and

[0017] - the filtration device is connected by wire to the control module. Preferably, the settling tank is connected to a conduit for draining water / filtered material.

[0018] Preferably, the drive for the filtration device is a 24-volt DC motor.

[0019] Preferably, the drive power supply is located outside the filtration device, preferably in the control module.

[0020] Preferably, the control module consists of a power supply, a start / stop switch, a potentiometer by means of which it is possible to control the vibration frequency, a socket for connecting the filtration device, and a 230 volt plug.

[0021] Preferably, the mounting plate together with the filtration column is placed in the holes in the vibrating plate and then is additionally immobilized, preferably using a locking system.

[0022] Preferably, the filtration columns are made of an acid-resistant material, such as PVC.

[0023] Preferably, the filtration device comprises six filtration columns and six column covers.

[0024] The subject of the present invention is also a method of preparing samples for palynofacies studies using an automatic palynological filtration device as defined above, comprising the steps of:

[0025] - crushing the material to be examined;

[0026] - the crushed material is subjected to maceration using HCI and / or HF;

[0027] - a nylon sieve is stretched onto the bottom of a filtration column, a clamp is put on the nylon sieve and the filtration column is secured from the top with a plug with a nozzle;

[0028] - the prepared filtration columns are installed in the holes of a vibrating plate;

[0029] - the crushed material after the maceration step with HCI and / or HF is placed in the individual filtration columns;

[0030] - the subsequent pipes supplying water to the columns are connected to the nozzles; - the filtration device is activated and the appropriate revolutions are set using the potentiometer;

[0031] - the vibrating plate which is vibrating, transfers vibrations to the filtration columns, forcing movement in the water with the sediment inside the columns;

[0032] - after filtration is completed, the filtration columns are dismantled, the nylon filters are removed and the filtered material is rinsed from them into the test tubes.

[0033] The solution proposed by the Inventors (Automatic Palynological Filtration Device) allows to reduce the time spent on filtration to 2 minutes of the technician's work per sample. This result is the effect of the development of the filtration device construction, automation of the filtration process and the possibility of filtering many, for example, six samples at the same time. The technician's work is limited at this stage to replacing and filling the filtration columns.

[0034] Based on the team's many years of experience, the proposed solution has been adapted to work in an aggressive chemical environment. The invention has been designed in a way that prevents contamination of samples filtered in the device, which is particularly important in the case of detailed palynological analyses. Due to the use of proven solutions in the design and the isolation of electronics from the harmful effects of chemicals, the invention is characterised by reliability. Reliability combined with the previously mentioned advantages of the invention makes this solution a particularly interesting proposition for laboratories in the field of hydrocarbon exploration, where the time of obtaining palynological information plays a significant role and translates directly into drilling costs.

[0035] Although vibrating tables and sieves have been widely used for a long time in many industries, until now no device intended for laboratory filtration of palynological material in an aquatic environment has appeared on the market. Brief description of the drawings

[0036] The subject of the present invention is shown in the drawings, where:

[0037] Fig. 1 shows a perspective view of an automatic palynological filtration device according to the present invention;

[0038] Fig. 2 shows a perspective view of the base of an automatic palynological filtration device according to the present invention;

[0039] Fig. 3 shows a diagram of a filtration column of an automatic palynological filtration device according to the present invention.

[0040] EMBODIMENT

[0041] Description of the filtration device

[0042] • Base (1)

[0043] • Column cover (2)

[0044] • Drive (3)

[0045] • Control module (not shown)

[0046] • Vibrating table (4)

[0047] • Filtration columns (5)

[0048] • Water supply (not shown).

[0049] Base ( 1 )

[0050] Fig. 2 shows the structure of the base (1): column cover (2), engine chamber (6) fixed to the vibrating plate (4), settling tank guides (7), water system valves (8), draining openings (9), support springs with rods (10).

[0051] The base (1) is a load-bearing element and stabilises the entire structure. In the central part of the base (1) there are six openings that drain excess water together with filtration waste. Below the previously described openings, there is a settling tank, whose task is to collect solid material and drain water to the discharge point. Water may be drained in two ways: through the installation to the settling tank and then through the discharge pipe to the drain, e.g. a sink, or by placing the filtration device directly above the sink, then the water flows directly through the opening in the settling tank. In the corners of the base (1) there are support springs with threaded rods (10) that allow for the adjustment of the vibration range. Both the springs and the rods provide a flexible mount for the vibrating plate (4).

[0052] Column cover (2)

[0053] The column cover (2) is permanently connected to the base (1). The purpose of the cover (2) is to prevent contamination of samples filtering in adjacent columns (5). Additionally, the walls of the cover (2) protect the engine chamber (6) from water and block direct access to the drive mechanism (3).

[0054] Drive (3)

[0055] Drive (3) for the filtration device (3) is a 24-volt DC motor with a shaft extending from both sides of the engine. Asymmetric weights have been attached to the shaft, which generate vibrations of the device during operation. The engine is located in a tight housing and is attached to the vibration plate from the bottom. The drive power supply has been led outside the filtration device and is located in the control module, thanks to which any flooding of the engine does not pose a threat to the filtration device operator.

[0056] Control module

[0057] The control module is a separate element of the set, communication with the filtration device is via a wire. Leading the electronics outside the filtration device ensures safety of use, because the operator is not exposed to chemical vapours, and also ensures a longer service life of the electronics. The control module consists of a power supply, a switch (start / stop), a potentiometer, which allows you to control the vibration frequency, a socket for connecting the filtration device, and a 230-volt plug.

[0058] Vibrating plate (4)

[0059] At the base of the vibrating plate (4) in the central part there is an engine chamber (6).

[0060] The engine (not shown) generates vibrations transferred via the vibrating plate (4) to the filtration columns (5). The columns (5) are mounted in the plate (4) via a mounting plate (11) which is an integral part of the column (5). The mounting plate (11) together with the column (5) is placed in holes in the vibrating plate (4) and then additionally immobilized through a locking system, which allows for better transfer of vibrations from the vibrating plate (4) to the columns (5). At the tops of the plate (4) there are four holes where the threaded rods of the base (1) are inserted. Contact between the vibrating plate (4) and the base (1) takes place via springs (10) on which the plate (4) rests.

[0061] Filtration column (5)

[0062] The filter column (5), shown in Fig. 3, is made of PVC pipe. This material was chosen mainly due to the acid resistance of the material and its mechanical strength. From the top, the column (5) is plugged with a plug (13) equipped with a nozzle (12) with a quick connector, to which the water system pipes are connected. In the central part, the column (5) "passes" through a square plate enabling assembly to the vibrating plate (4). In the lower part, there is a clamp that tightens the nylon filter to the bottom of the column (5).

[0063] Water system

[0064] The water system consists of: a hose supplying water to the switchboard, a switchboard equipped with six valves regulating the amount of water supplied to individual columns (5) and pipes supplying water to subsequent nozzles / columns.

[0065] Operation of the filtration device

[0066] Installation of the filtration columns (5)

[0067] First, filter columns have to be prepared (5), for this purpose a nylon sieve is stretched onto the bottom of the filtration column, then a clamp is put on the nylon sieve while the filtration column (5) is secured from the top with a plug (13) with a nozzle (12). The prepared filtration columns (5) are installed in the holes of a vibrating plate (4), mounting plates of the columns (5) are pressed with the flaps of the vibrating plate (4), and then the closed flaps are secured with a lock. The material, after the chemical treatment stage (maceration with HCI and HF), is placed in the individual filtration columns (5). Then the nozzles are connected to the subsequent pipes supplying water to the columns.

[0068] Filtration

[0069] After installing the columns (5), the device is turned on using the "start" button and then the appropriate speed is set using the potentiometer. When the engine is running, the rotating weights cause the vibrating plate (4) to vibrate. The vibrating plate (4) transfers the vibrations to the filtration columns (5), which force the water with sediment inside the columns to move. The turbulent movement of the water with the sediment causes grains with an undesirable fraction to be washed out through the sieve. The continuous water supply during filtration allows for faster removal of unwanted material and its more thorough cleaning.

[0070] After filtering the material, the filtration columns are dismantled, then the next nylon filters are removed and the filtered material is rinsed from them into test tubes. Both the filters and the columns are reusable. The columns, together with the plugs and clamps, can be washed in a dishwasher, while to clean the filters, they should be washed by hand in water with detergent and then rinsed with a large amount of water.

Claims

Claims1. An automatic palynological filtration device comprising a base (1), constituting a supporting and stabilising element, on which at least two column covers (2) are inseparably attached, in which filtration columns (5) are placed, wherein on the base (1), preferably between the column covers (2), there is an engine chamber (6), which is attached to the vibrating plate (4), which vibrating plate (4) is fixed to the base (1) using supporting springs with rods (10), preferably attached in the four corners of the base (1), which enable adjustment of the vibration range and constitute a flexible attachment of the vibrating plate (4) to the base (1);- wherein said vibrating plate (4) has at least two holes (51) for the filtration columns (5) and adheres on the perimeters of these holes (51) to the filtration columns (5) transferring vibrations to the filtration columns (5) during the operation of the filtration device;- the filtration columns (5) are mounted in the vibrating plate (4) by means of a mounting plate (11) which is an integral part of the column (5), which mounting plate (11) together with the column (5) is placed in holes in the vibrating plate (4);- from the top, the filtration column (5) is plugged with a plug (13) equipped with a nozzle (12) with a quick connector to which the water system pipes are connected, in the central part the filtration column (5) is equipped with the above-mentioned mounting plate (11) enabling mounting to the vibrating plate(4), while in the lower part, the filtration column (5) contains a clamp that tightens the filter, preferably nylon filter, to the bottom of the filtration column(5);- in the engine chamber (6), a drive (3) is placed, which sets the vibrating plate(4) in motion, wherein the drive (3) of the filtration device is an engine placed in a sealed housing, in the engine chamber (6), attached from the bottom to the vibrating plate (4), which engine contains a shaft extending from both sides of the engine, the shaft equipped with asymmetric weights that generate vibrations of the device during operation;- wherein the filtration device is equipped with a water supply and water system valves (8) and the water supply comprises a conduit supplying water to the switchboard, the switchboard fitted with at least two valves regulating the amount of water supplied to the individual filtration columns (5) and the conduits supplying water to subsequent nozzles (12) / columns (5);- in the base (1) there are at least two draining openings (9) which drain excess water together with filtration waste to the settling tank, wherein the draining openings (9) are preferably located under the bottom of the filtration column(5);- below said draining openings (9) in the base (1) there is a settling tank collecting solid material and draining water, preferably resting on settling tank guides (7) attached from below to the base (1); and- the filtration device is connected by wire to the control module.

2. The filtration device according to claim 1, characterised in that the settling tank is connected to a conduit for draining water / filtered material.

3. The filtration device according to claim 1 or 2, characterised in that the drive (3) for the filtration device is a 24-volt DC motor.

4. The filtration device according to any one of claims 1-3, characterised in that the drive power supply is located outside the filtration device, preferably in the control module.

5. The filtration device according to any one of claims 1-4, characterised in that the control module consists of a power supply, a start / stop switch, a potentiometer bymeans of which it is possible to control the vibration frequency, a socket for connecting the filtration device, and a 230 volt plug.

6. The filtration device according to any one of claims 1-5, characterised in that the mounting plate (11) together with the filtration column (5) is placed in the holes in the vibrating plate (4) and then is additionally immobilized, preferably using a locking system.

7. The filtration device according to any one of claims 1-6, characterised in that the filtration columns (5) are made of an acid-resistant material, such as PVC.

8. The filtration device according to any one of claims 1-7, characterised in that it comprises six filtration columns (5) and six column covers (2).

9. Method of preparing samples for palynofacies studies using an automatic palynological filtration device as defined in any one of claims 1-8, comprising the steps of:- crushing the material to be examined;- the crushed material is subjected to maceration using HCI and / or HF;- a nylon sieve is stretched onto the bottom of a filtration column (5), a clamp is put on the nylon sieve and the filtration column (5) is secured from the top with a plug (13) with a nozzle (12);- the prepared filtration columns (5) are installed in the holes of a vibrating plate (4);- the crushed material after the maceration step with HCI and / or HF is placed in the individual filtration columns (5);- the subsequent pipes supplying water to the columns (5) are connected to the nozzles (12);- the filtration device is activated and the appropriate revolutions are set using the potentiometer;- the vibrating plate (4) which is vibrating, transfers vibrations to the filtration columns (5), forcing movement in the water with the sediment inside the columns (5);- after filtration is completed, the filtration columns (5) are dismantled, the nylon filters are removed and the filtered material is rinsed from them into the test tubes.

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