JP2662357B2 - Fully automated system for petroleum product analysis testing - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fully automated system for analyzing and testing petroleum products (hereinafter abbreviated as a fully automated system).

[0002]

2. Description of the Related Art Conventionally, analysis and testing of petroleum products (hereinafter referred to as "testing") among analysis and testing operations at a refinery have been conducted.
Density (JIS K2249), sulfur content (JIS K2541), flash point (JI
S K2265), kinematic viscosity (JIS K2283), cloud point / pour point (JI
JIS that specifies the scope of application, types of test methods and analytical test equipment, test procedures, etc., as seen in S K2269), aniline point (JIS K2256), bromine value / bromine index (JIS K2421), etc. Implemented according to standards. In addition, test methods based on product tests are applied to receiving raw materials, intermediate products, samples for plant operation management, and the like.

[0003] On the other hand, samples handled in a test operation in a refinery include naphtha / gasoline samples containing highly volatile components, light oil samples such as kerosene and gas oil which are fluid at normal temperature, and those having high viscosity or flow at room temperature. It consists of a number of samples (hereinafter referred to as primary samples) having a wide range of physical properties, such as heavy oil-based samples having no physical properties, heavy-pressure residual oils, and vacuum residual oils (hereinafter referred to as primary samples). Test items are required to be tested. For reference, Table 1 shows an example of the difference in the degree of demand in the test items for each oil system.

[0004]

[Table 1]

[0005] Incidentally, the above-mentioned test work in a refinery is performed by introducing a quality control system for centrally managing sample information, test information and test results, or an automatic analysis test apparatus for automatically analyzing an analysis test specified in JIS. The efficiency of the analysis and the accuracy of the analysis test (hereinafter referred to as the test accuracy) are improved by the introduction of the system. In recent years, there has been a growing demand for a fully automated system in which almost all operations related to analysis tests on samples of petroleum products are automated in order to improve efficiency.

[0006]

However, in the above-mentioned fully automatic system, a measurement operation or a measurement data of a series of test operations required in an analysis test performed using an individual automatic analysis test apparatus is required. Only a semi-automated system in which only collection, organization, and printing are automated is provided. For example, storage of an appropriate primary sample according to physical property values, and transfer of the primary sample to a test container (2 (Subsequent sample container), subdividing (collecting) a sample that requires pretreatment (hereinafter referred to as a secondary sample fractionating operation), a pretreatment operation according to the type or state of the sample, At present, the disposal of the sample after the completion of the measurement, etc. is still performed depending on human labor.

The inventors of the present invention have studied the factors that do not achieve the realization of the above-mentioned fully automatic system, and as a result, of the above-mentioned operations that are currently performed manually, the operation of separating the secondary sample and the type of sample or The inability to automate appropriate pre-processing operations according to the state was found to be the biggest factor. To be more specific, in order to automate the sorting operation of a secondary sample, a sorting device that can perform the sorting operation satisfactorily for samples having all physical property values is required. When using gasoline and naphtha samples,
Even if the sample is cooled to prevent evaporation of the light-boiling components, when the sample is sucked into the dispensing tip, the inside of the dispensing tip will be depressurized, which will cause the light-boiling components to evaporate. There were problems such as causing the value to vary. Furthermore, in the dispensing step, since the temperature of the sample in the dispensing tip rises and the light-boiling components evaporate, there is also a problem that the internal pressure in the dispensing tip increases and dripping of the dispensed sample occurs. Was. Accordingly, in the case of a sorting apparatus having only the sorting method using the above-described dispensing tip, the sample to be applied to the sorting apparatus is necessarily limited (to a sample having limited physical properties). It could not be used as a fractionation device for automation, which is required to be able to handle samples of the type described above.

[0008] In order to automate an appropriate pretreatment operation according to the type or state of the sample, at least a so-called dehydration operation for removing water in the sample is required for samples having various physical properties. It must be able to perform well. However, the conventional pretreatment apparatus employs a method in which a dehydrating agent is added at room temperature and a shaking machine is used to perform a dehydrating operation of the heavy oil-based sample. Unfavorable for the system sample, and even if the sample is heated to increase its fluidity, the sample temperature drops again during the shaking process with a shaker, causing the sample to solidify or decrease its fluidity. As a result, there was a disadvantage that the dehydration efficiency was reduced, and it could not be used as a pretreatment device for automation, which was also required to be able to handle various types of samples.

In the above-described conventional semi-automated system, when pre-processing is performed on a sample for plant operation management, the above-mentioned pre-processing operation is not fully automated, so that the semi-automatic operation is inevitable. There has been a problem that the number of samples that can be analyzed using the automation system is limited.

[0010]

Means for Solving the Problems Accordingly, the present inventors have:
Eliminating the factors that hinder the above-mentioned automation, as a result of intensive research aimed at realizing a fully automated system, as a result, it has a plurality of sorting units that employ different sorting methods, and from among the plurality of sorting units, Select a sorting unit that employs a sorting method suitable for the physical properties of the sample, and transfer the sample in the primary sample container to the secondary sample container dedicated to the analytical test device by the selected sorting unit. Using a sorting apparatus for sorting, and having a plurality of processing units each employing a different processing method, among the plurality of processing units, a processing unit employing a processing method adapted to the physical properties of the sample. By using a pre-processing device that performs pre-processing of a sample, if necessary, by using the selected processing unit, it is possible to eliminate the above-mentioned hindrance factor of the fully automated system, thereby maximizing the realization of the fully automated system. The second trial was a bottleneck It found that it is possible automated operation preparative minute and pre-processing operations, and have completed the present invention.

That is, according to the present invention, a code providing device for providing a code for identifying a sample to a primary sample container containing a sample and a primary sample container provided with a code by the code providing device are provided at least in a desired form. A primary sample container storage device to be stored under the temperature conditions, a capping device for opening or closing the primary sample container, and a primary sample container opened by the capping device, at least,
A primary sample container standby device for temporarily storing the desired temperature condition, and a plurality of sorting units each employing a different sorting method, and a sorting unit adapted to the physical properties of the sample among the plurality of sorting units. The sample in the primary sample container of the primary sample container standby device is transferred to the secondary sample container dedicated to the analytical test device by a selected amount by the selected sorting unit employing the sampling method. A sorting apparatus for sorting, having a plurality of processing units each employing a different processing method, selecting a processing unit adopting a processing method suitable for the physical properties of the sample from the plurality of processing units. A pre-processing device for pre-processing the sample, if necessary, by the selected processing unit, at least one or more automatic analysis test devices for analyzing the sample in the secondary sample container, and each of the above devices Between the primary and secondary sample containers. A container transporting device, connected to each of the above devices, and at least storing analysis test conditions preset for each sample corresponding to each code, and operating conditions of each device preset for each type of sample. A control system having a function of automatically controlling each of the above-mentioned devices based on these conditions, storing and / or recording test results, and performing arithmetic processing, and automatically automatically perform a plurality of samples sequentially. It is a fully automated system characterized by analyzing.

[0012]

An embodiment of the present invention will be described below with reference to the drawings. However, the present invention is not limited to the following embodiment.

FIG. 1 is a schematic diagram showing an embodiment of a fully automated system for analyzing and testing petroleum products according to the present invention. The fully automated system of the present embodiment shown in FIG. 1 includes a code attaching device 1 for attaching a code for sample identification to a primary sample container containing a sample of a petroleum product, Primary sample container storage device 2 provided
And a capping device 3 disposed at the subsequent stage of the primary sample container storage device 2 and a primary sample container disposed at the subsequent stage of the capping device 3 and opened by the capping device 3 for temporary storage. Primary sample container standby device 4
Is disposed on the subsequent stage side of the primary sample container standby device 4,
A preparatory device 5 for preparating a sample in the primary sample container into a secondary sample container dedicated to the analytical test device in a specified amount, and a pretreatment device 6 for performing pretreatment of the sample as necessary when collecting the sample. A primary sample container or a secondary sample container disposed between the sorting device 5 and the pretreatment device 6 for analyzing a sample in the secondary sample container; A robot hand 8 as a sample container transfer device for transferring a sample,
It comprises a management system 9 which is a computer connected to each of the above devices and controlling each of the devices.

The code providing apparatus 1 comprises a primary sample receiving section 21 for receiving a primary sample container in which a sample is contained and capped in advance, and a code corresponding to the type of the sample in each primary sample container. A label issuing machine 22 for issuing and affixing a label (for example, a bar code label or the like) to which a label is attached, and a label reader 23 for reading a code attached to the label affixed to the primary sample container. The above-mentioned code giving device may be of a type in which numerals, characters, and barcodes are printed directly on the primary sample container.

A primary sample container storage device 2 provided at the subsequent stage of the code providing device 1 is a device for setting conditions such as a temperature and an inert gas seal for each type of sample and individually storing them. As a primary sample container storage device suitable for use in this embodiment, for example, a device as shown in FIG. 2 is exemplified. The primary sample container storage device 2 shown in FIG. 2 includes a storage room 2A for storing a primary sample container containing a gasoline / naphtha-based sample, and a storage room 2B for storing a primary sample container containing a light oil-based sample. And a storage room 2C for storing a primary sample container containing a heavy oil-based sample. The storage room 2A is a storage room including a box covered with a heat insulating material 24, a refrigerator 25, a stirring fan 26, and an automatic door 27,
The inside of this storage room 2A is controlled by the refrigerator 25 and the stirring fan 26 under the control of the management system 9 by -10.
The temperature is adjusted from + 5 ° C. to + 5 ° C., and the optimum temperature condition for storing a primary sample container containing a sample containing light-boiling components such as gasoline and naphtha can be obtained. The storage room 2B also has a box covered with the heat insulating material 24, like the storage room 2A.
A storage room equipped with a stirring fan 26 and an automatic opening / closing door 27. The interior of the storage room 2B is kept at room temperature, and the optimal temperature conditions for storing a primary sample container such as kerosene or light oil that can be handled at room temperature. It can be. Further, the storage room 2C is also provided with a box covered with a heat insulating material 24, a stirring fan 26, an automatic opening / closing door 27 and a heater 28 in the same manner as the storage rooms 2A and 2B. The temperature inside the 2C is controlled from + 60 ° C. to + 80 ° C. by a heater 28 and a stirring fan 26 which are operated while being controlled by the management system 9, and the pour point of C heavy oil, normal pressure residual oil and the like is 60 ° C. or less. Alternatively, the temperature condition can be set to be optimal for storing a highly viscous primary sample. The capping device 3 disposed on the subsequent stage of the primary sample container storage device 2 opens the primary sample container from the primary sample container storage device 2 or closes the primary sample container after the completion of the sorting operation. Device.

As shown in FIG. 3, the primary sample container standby device 4 provided at the subsequent stage of the capping device 3 has three temperature-controlled thermostats, ie, gasoline
A constant temperature bath 4A for holding a primary sample container X containing a naphtha-based sample, a constant temperature bath 4B for holding a primary sample container Y containing a light oil-based sample, and a primary sample container Z containing a heavy oil-based sample. The primary sample container, which is constituted by a constant temperature bath 4C to be on standby and opened by the capping device 3, is kept on standby under conditions suitable for each sample type until it is conveyed to the sorting device 5. That is, the temperature of the thermostatic bath 4A is adjusted from -10 ° C to + 5 ° C under the control of the management system 9, and the temperature condition can be set to an optimal temperature for waiting for the primary sample containing the gasoline / naphtha-based light-boiling component.
Further, the temperature of the thermostatic bath 4B is adjusted to room temperature under the control of the management system 9, and can be set to an optimal temperature condition for waiting for a primary sample containing components that can be handled at room temperature, such as kerosene and light oil. Further, the temperature of the constant temperature bath 4C is controlled from + 60 ° C. to + 80 ° C. under the control of the management system 9, and the primary sample having a pour point of 60 ° C. or less such as C heavy oil and normal pressure residual oil or containing a highly viscous component is kept on standby. Temperature conditions can be optimal. As an alternative to the constant temperature bath 4C, for example, a commercially available explosion-proof hot plate may be used.

As shown in FIG. 4, the sorting apparatus 5 includes a sorting section 5A for sorting a gasoline / naphtha-based primary sample,
And a fractionation unit 5B for fractionating a heavy oil-based primary sample. The sorting section 5A of the present embodiment takes a predetermined amount of sample from the primary sample container X containing the gasoline / naphtha-based sample in the thermostat 4A of the primary sample container standby device 4, and separates it according to the test item. An electronic balance 29 which is dispensed into containers for various analytical test devices having different shapes (hereinafter, referred to as secondary sample containers) and used to determine whether or not a predetermined amount has been dispensed after the dispensing operation. A weighing unit including a jig 29A for stably placing the secondary sample container M on the electronic balance 29; and a device part for actually dispensing a sample. It is composed of a discharge tube 31, a gas introduction tube 32 for sample pressure feed, a fluid supply / discharge tube 33, a sample supply / discharge tube 35, a stop valve 36 interposed in the sample supply / discharge tube 35, and a waste sample receiver 37. I have.

As shown in FIG. 5, the sealing device 30 has a short columnar head portion 40 having a through hole penetrating from the upper surface to the lower surface, and is inserted into the through hole of the head portion 40 to be integrated. A balloon 41 provided with an elastic bag in a ring shape is provided on the outer peripheral surface of the lower end side of the cylindrical body 42 and further protruding downward from the lower surface of the head portion 40. I have it. As shown in FIG. 4, one end of the sample supply / discharge tube 31 communicates with the sample supply / discharge tube 35, and the other end passes through the inside of the cylindrical body 42 of the sealing device 30 as shown in FIG. It communicates with the lower surface of the body 42. Moreover, when the balloon 41 is inserted into the opening of the primary sample container X and sealed, the other end extends downward until the other end of the sample supply / discharge tube 31 is sufficiently immersed in the sample in the primary sample container X. ing. One end of the sample introduction gas introducing tube 32 is connected to a sample supply gas supply device (not shown), and the other end passes through the inside of the cylinder 42 of the sealing device 30 and communicates with the lower surface side of the cylinder 42. ing.

On the other hand, one end of the fluid supply / discharge tube 33 is connected to the inside of the balloon 41 through the inside of the cylindrical body 42, and the other end is connected to the fluid supply / discharge for supplying / discharging a fluid for inflating / deflating the balloon 41. Means (not shown).
Therefore, utilizing the inflation and deflation of the balloon 41 caused by putting a predetermined fluid into and out of the balloon 41,
The balloon 41 is airtightly fixed to the opening of the primary sample container X,
It can also be detached.

In order to sort the gasoline / naphtha-based primary sample in the primary sample container X into the secondary sample container by the sorting unit 5A, first, the robot hand 8 operates the secondary sample container storage (not shown). Out of the secondary sample container from the electronic balance 29
Put on. Then, the tare weight of the electronic balance 29 is automatically set to zero under the control of the management system 9. Next, the opening of the sample supply / drain pipe 35 is set in accordance with the opening position of the secondary sample container, and the robot hand 8 grasps the sealing device 30 and inserts the balloon 41 into the opening of the primary sample container X. 41 is expanded and sealed, and the other end of the sample supply / discharge tube 31 is sufficiently immersed in the sample in the primary sample container X. Next, in this state, a gas such as air is pressure-fed into the sample pressure gas introduction tube 32 by a sample pressure gas supply device (not shown) to pressurize the void portion in the primary sample container X and stop valve. Open 36. Thus, the sample in the primary sample container X is supplied into the secondary sample container via the sample supply / discharge tube 31. further,
Under the control of the management system 9, it is confirmed by the electronic balance 29 that the predetermined amount has been supplied. At the same time, the air supply from the sample supply gas supply device is stopped, the stop valve 36 is closed, and the primary sample container is connected. The sorting operation for the next sample container ends.

The sorting section 5B of this embodiment takes a predetermined amount of sample from the primary sample containers 1B and 1C containing the light and heavy oil systems of the constant temperature baths 4B and 4C of the primary sample container standby device 4, This is dispensed into a secondary sample container, and as shown in FIG. 4, a dispensing tip 50, a dispensing tip storage unit 51, a dispensing tip transfer tool 52, a dispensing probe 53, a dispensing tip attaching device 54, It comprises a waste chip receiver 55 and a dispenser 56. The dispensing tip 50 is preferably one that can be replaced for each sample in order to prevent contamination between samples. For example, an outer cylinder of a commercially available disposable polypropylene syringe may be used. The dispensing tip storage unit 51 is a kind of container that literally stores a plurality of dispensing tips 50. The dispensing tip transfer tool 52 uses the same method as the above-described sealing by the balloon 41 of the sealing device 30 used in the dispensing section 5A, and inserts the dispensing tip transfer tool 52 into the dispensing tip 50, A balloon (not shown) is inflated to fix the dispensing tip 50 to the dispensing tip transfer tool 52, and is used to transport the dispensing tip 50 to a predetermined position. Also,
The dispensing probe 53 is configured such that when the dispensing tip 50 is attached as shown in FIG. 6, the inner wall of the dispensing tip 50 is sealed with an O-ring 53A. The robot hand 8 grasps the head 53B and transports it to a predetermined position. The dispensing tip mounter 54 is used as a temporary stand for the dispensing probe 53 to which the dispensing tip 50 is mounted, in addition to performing the operation of attaching and detaching the dispensing tip 50 to and from the dispensing probe 53. The waste chip receiver 55 is a container for receiving a used chip detached from the dispensing probe 53 after the end of the dispensing. The dispenser 56 is connected to the dispensing probe 53 by a Teflon tube, and operates to suck a sample into the dispensing tip 50 attached to the dispensing probe 53 or discharge the sample from the dispensing tip 50. This is a device for supplying and discharging gas, and the control of the sample suction amount is performed by the management system 9.

In the dispensing section 5B of this embodiment, a dispensing probe 53 of a sealing type using an O-ring is used as a suction type device. However, the present invention is not limited to this.
It is more preferable to use a sealing method using a balloon which is used in the aforementioned Japanese Patent Application No. 5-111244 “Liquid sample dispensing apparatus” because the sealing performance is improved. Further, when the heavy oil-based sample is to be collected by the above-mentioned dispensing section 5B, it is preferable that the dispensing tip 50 is also heated to 60 ° C. in advance and used. More preferably, a device for preheating the chip 50 is provided.

As shown in FIG. 7, the pretreatment device 6 comprises a treatment section 6A for pretreating a light oil sample and a treatment section 6B for pretreating a heavy oil sample. The processing unit 6A includes a funnel 61, a filter paper 62 set in the funnel 61, a funnel holding base 63 for holding the funnel 61, and a secondary sample container holding base for setting a secondary container M for receiving a pre-processed sample. 64 and a plurality of desiccant hoppers 65 for storing desiccants. A plurality of funnels 61 on which filter papers 62 are set in advance are held on the funnel holding base 63. As the desiccant, for example, anhydrous sodium sulfate is used for the pretreatment of the density / aniline point test, and anhydrous calcium chloride is used for the pretreatment of the sulfur content test. The funnel holder 63 is provided with a plurality of funnels 6 on a turntable.
Has a structure to hold 1 and a new funnel 6 for each pretreatment.
1 and the filter paper 62 are supplied. Further, on the secondary sample container holding table 64, various secondary sample containers having different shapes can be set.
The secondary sample container set on the secondary sample container holding table 64 to receive the filtrate can be moved up and down. The funnel 61 and the filter paper 62
Is not particularly limited, but in each case, a commercially available polypropylene funnel or the like and a commercially available paper filter paper are sufficient. Further, the desiccant hopper 65 keeps the temperature of the desiccant in the desiccant hopper 65 at 60 ° C. so that the desiccant inside the hopper does not absorb moisture in the air, Into the air to block the contact between the desiccant and the outside air. Further, the feeding of the desiccant into the desiccant hopper 65 is controlled by the management system 9, and the desiccant corresponding to the test item of the sample to be subjected to the pretreatment is set in advance.

On the other hand, the processing section 6B comprises a stirring table 66 with a heating mechanism and a plurality of desiccant hoppers 65 for storing desiccants. As the desiccant, the same desiccant used in the processing section 6A described above is used. Also,
The stirrer 66 with a heating mechanism is provided with a heating mechanism for maintaining the sample temperature at 60 ° C. for the purpose of lowering the viscosity of the sample during the pretreatment operation and maintaining fluidity, and a stirring function for rotating a stirrer in the pretreatment container. have. Note that a commercially available magnetic stirrer with a heating mechanism may be used for the stirring. The desiccant hopper 65 is the same as the desiccant hopper of the processing section 6A described above.

As the automatic analysis test device 7 provided at the subsequent stage of the above-mentioned fractionating device 5 and pretreatment device 6, a device usually used in analysis and test work in a refinery or the like can be used. For example, density (JIS K2249), sulfur content (JIS K
2541), flash point (JIS K2265), kinematic viscosity (JIS K2283),
Cloud point / pour point (JIS K2269), aniline point (JIS K225
6), It is composed of a device that automatically and exclusively analyzes and tests individual petroleum products such as bromine number and bromine index (JIS K2421).
Usually, it is composed of a plurality of dedicated automatic analysis test devices according to the items of the analysis test.

The management system 9 is a so-called computer connected to each device described above, and a storage device is installed inside or outside the management system 9. Further, in this storage device, analysis test conditions set for each sample to be analyzed and operating conditions of each device set for each type of sample corresponding to each code are registered in advance. Examples of the analysis test conditions include, but are not limited to, the presence and method of pretreatment, the type of dehydrating desiccant used for pretreatment, and the measurement conditions of the automatic analysis test device 7, but are not limited thereto. By setting other conditions according to the above, more precise control can be performed. The operating conditions include, for example, the set temperatures of the primary sample container storage device and the standby device, the type of the sorting device to be used, and the like. However, the operating conditions are not limited thereto, and other conditions may be set as necessary. However, more devices can be controlled. The management system 9 of the present embodiment not only has a function of automatically controlling each device based on the analysis test conditions and the operating conditions of each device, but also stores the test results obtained by the automatic analysis test device 7, It also has the function of recording and further processing. In addition, the management system 9 pre-registers the operation time of each device. In particular, when performing a large number of analysis tests, the management system 9 performs each analysis test more efficiently, for example, so that all the analysis tests are completed in a short time. It also has an optimization processing function to determine the order.

Next, the operation of the above-described fully automatic system of this embodiment will be described. (1) Assignment and Storage of Label First, the received primary sample containers are manually input into the primary sample input port 21 in the order registered in the management system 9. The loaded primary sample container is moved to the label issuing machine 22 by the robot hand 8 and is provided with a label.
Next, the primary sample container is moved to the label reader 23 by the robot hand 8 to read the code attached to the label by the label reader 23, and then the predetermined position of the primary sample container storage device 2 (specifically, For example, the primary sample container containing the gasoline / naphtha-based sample is in the storage room 2A, the primary sample container containing the light oil-based sample is in the storage room 2B, and the primary sample container containing the heavy oil-based sample is in the storage room 2C. ). The storage location is stored in the storage device of the management system 9.

(2) In the case of a gasoline / naphtha sample In the case of a gasoline / naphtha sample which does not require pretreatment and whose test item is only density, first, the robot hand 8
After taking out the primary sample container containing the sample from the storage room 2A and moving it to the capping device 3, the capping device 3 opens the primary sample container. Next, the opened primary sample container is moved to the constant temperature bath 4A of the primary sample container standby device 4 by the robot hand 8.

Next, the robot hand 8 takes out a density measurement container, which is one of the secondary sample containers, from a secondary sample container storage (not shown) and places it on the electronic balance 29 of the sorting section 5A. Place. Then, the management system 9 sends a signal indicating zero tare to the electronic balance 29 to complete the weighing preparation. Subsequently, in the dispensing unit 5A of the dispensing device 5, a predetermined amount of the sample is dispensed from the primary sample container waiting in the constant temperature bath 4A of the primary sample container standby device 4, and the dispensed sample immediately has the above density. Discharged into the measuring container.

Next, the container for density measurement, in which the sample is contained, is moved from the electronic balance 29 to a predetermined position of the density meter (one of the automatic analysis test devices 7) by the robot hand 8. Subsequently, a measurement start signal is sent from the management system 9 to the density meter, and the density meter performs measurement based on the measurement condition of the sample stored in the management system in advance.

During the above measurement, the primary sample container whose collection has been completed is taken out of the thermostatic bath 4A of the primary sample container standby device 4 by the robot hand 8, moved to the capping device 3, and closed. , And temporarily return to the storage room 2A of the primary sample container storage device 2. In addition, storage room 2A
After all the tests related to the above sample have been completed and the measurement results have been sent from each automatic analyzer such as a density meter to the management system 9, the primary sample container is returned from the storage room 2 </ b> A by the robot hand 8. While being returned to the mouth 21, the storage position of the primary sample container previously stored in the storage device of the management system 9 is deleted from the storage device.

The container for density measurement, which has been measured, is also used by the robot hand 8 for storing used containers (not shown).
Or discarded outside the fully automated system. (3) Operation of heavy oil-based sample If a heavy oil-based sample requires pre-treatment and the test items are density and sulfur content, first, the primary sample container containing the sample is set by the robot hand 8. Is taken out of the storage room 2C and further moved to the capping device 3, where the capping device 3
Then, the primary sample container is opened. Next, the opened primary sample container is moved to the constant temperature bath 4C of the primary sample container standby device 4 by the robot hand 8.

Next, a pretreatment container containing a stirrer, which is one of the secondary sample containers, is taken out of a secondary sample container storage (not shown) by the robot hand 8, and a desiccant for density / aniline point is removed. The port of the pre-treatment container is applied to the desiccant supply port of the desiccant hopper 66 in which the desiccant is supplied, and a predetermined amount of desiccant is charged into the pre-treatment container. Then, the robot hand 8 removes the pretreatment container containing the desiccant from the electronic balance 2 of the sorting unit 5B.
Place it on 9. Further, the management system 9 sends a signal of zero tare to the electronic balance 29 to complete the preparation for weighing.

Next, the robot hand 8 takes out the dispensing tip transfer tool 52, takes out the dispensing tip 50 from the dispensing tip storage unit 51 by this dispensing tip transfer tool 52, and transfers it to the dispensing tip mounting device 54. I do. Thereafter, the dispensing tip transfer tool 52 is returned to the original position by the robot hand 8.

Next, the dispensing probe 5 is
3 is taken out and attached to the dispensing tip 50 being transferred to the dispensing tip attaching device 54. Subsequently, the dispensing probe 53 on which the dispensing tip 50 is mounted is taken out of the dispensing tip attaching device 54 by the robot hand 8, and the sample in the primary sample container of the thermostat 4C is placed in the pretreatment container where the preparation for weighing is completed. To a predetermined amount. After the sorting,
The dispensing probe 53 is returned to the dispensing tip mounter 54 once.

Next, the pretreatment container containing the sampled sample is placed on the stirring table 66 having a heating mechanism of the processing section 6B by the robot hand 8. Further, the sample in the pretreatment container is stirred while being heated for a predetermined time, and the sample is dehydrated by allowing the desiccant to settle after being stirred and left standing. During the pretreatment (dehydration) operation, the robot hand 8 takes out a density measurement container, which is one of the secondary sample containers, from the secondary sample container storage (not shown), and removes the container from the sorting unit 5B. It is placed on the electronic balance 29, and a signal of zero tare is sent from the management system 9 to the electronic balance 29 to complete the preparation for weighing.

Next, the dispensing probe 53 with the dispensing tip 50 mounted thereon, which was previously placed on the dispensing tip mounting device 54, is taken out by the robot hand 8, and the sample (after the desiccant is settled) in the pretreatment container is taken out. Supernatant) is collected in a density measuring container on the electronic balance 29 until a predetermined amount is reached.

After completion of the fractionation, the above-mentioned container for density measurement containing the sample therein is moved from the electronic balance 29 to a predetermined position of the density meter by the robot hand 8. Subsequently, a measurement start signal is sent from the management system 9 to the density meter, and the density meter performs measurement based on the measurement condition of the sample stored in the management system in advance. Further, the measured density measurement container and the pre-treated container after the sorting are sequentially placed in the robot hand 8.
To start the next sulfur pretreatment operation.

Next, the pretreatment container containing the stirrer, which is one of the secondary sample containers, is taken out of the secondary sample container storage by the robot hand 8, and the desiccant for sulfur content in the processing section 6B is placed. The port of the pretreatment container is applied to the desiccant supply port of the desiccant hopper 66, and a predetermined amount of desiccant is charged into the pretreatment container. Then, the pretreatment container containing the desiccant is placed on the electronic balance 29 of the sorting unit 5B by the robot hand 8. Further, the management system 9 sends a signal of zero tare to the electronic balance 29 to complete the preparation for weighing. Next, the same pretreatment operation and fractionation operation as described above are performed to fractionate the sample into a sulfur content measurement cell, which is one of the secondary sample containers. After the completion of the fractionation, the above-mentioned cell for measuring the sulfur content containing the sample is moved from the electronic balance 29 of the fractionation unit 5B to a predetermined position of the sulfur content meter by the robot hand 8. Subsequently, a measurement start signal is sent from the management system 9 to the sulfur analyzer, and the sulfur analyzer measures based on the measurement conditions of the sample stored in the management system in advance. Furthermore, during this measurement operation,
The above operation is repeated to prepare a second sulfur content measurement cell containing the pretreated sample.

Next, after the sulfur content measurement of the first sulfur content measurement cell is completed, the measured sulfur content cell is
While being transported to the used container case by the robot hand 8, the second sulfur measurement cell containing the pre-processed sample is similarly moved by the robot hand 8 from the electronic balance 29 of the sorting unit 5 </ b> B to the sulfur meter. Move to a predetermined position. Subsequently, a measurement start signal is sent from the management system 9 to the density meter, and measurement is performed in the same manner as described above. The used pretreatment container is transported to the used container case by the robot hand 8 during this measurement. Also, during the above-mentioned sulfur content measurement operation, the primary sample container whose sorting has been completed is taken out of the thermostatic bath 4C of the primary sample container standby device 4 by the robot hand 8, moved to the capping device 3, and closed. , And temporarily return to the storage room 2C of the primary sample container storage device 2. Further, after all the tests related to the above-mentioned sample have been completed and the measurement results have been transmitted from the respective automatic analyzers such as the densitometer to the management system 9 for the primary sample container returned to the storage room 2C, the robot hand 8 stores the primary sample container in the storage room. The storage position of the primary sample container previously stored in the storage device of the management system 9 is deleted from the storage device while being returned to the primary sample inlet 21 from 2C. The measured secondary sample container is transported by the robot hand 8 to the used container case.

As described above, in the fully-automated system of this embodiment, as the primary sample container storage device, the optimal temperature conditions for storing the primary sample containing light-boiling components such as gasoline and naphtha ( A storage room 2A whose temperature has been adjusted to -10 ° C to + 5 ° C), a storage room 2B whose temperature has been adjusted to an optimum temperature condition for storing a primary sample such as kerosene and light oil which can be handled at room temperature, and heavy oil C, Pour point of pressure residue oil etc. is 6
A primary sample container storage device 2 provided with a storage room 2C whose temperature is adjusted to an optimum temperature condition (+ 60 ° C. to + 80 ° C.) for storing a primary sample of 0 ° C. or lower,
Moreover, since the temperature of each storage room is controlled by the management system 9, each sample can always be stored under favorable temperature conditions regardless of the type (physical properties) of the sample.

In the fully automated system according to the present embodiment, as the primary sample container standby device, the optimum temperature condition (from -10 ° C. to 10 ° C.) for standby of the primary sample containing light-boiling components such as gasoline and naphtha. + 5 ° C), a constant temperature bath 4B whose temperature has been adjusted to the optimal temperature condition for waiting for a primary sample such as kerosene or light oil that can be handled at room temperature, heavy oil C, residual oil at normal pressure, etc. The primary sample container standby device 4 is provided with a constant temperature bath 2C whose temperature is adjusted to the optimum temperature condition (+ 60 ° C. to + 80 ° C.) for the pour point of 60 ° C. or lower or the high viscosity primary sample to wait. Moreover, since the temperature of each storage room is controlled by the management system 9, each sample can always be kept on standby under favorable temperature conditions regardless of the type (physical properties) of the sample.

Further, in the fully automatic system of this embodiment, a dispensing section 5B employing a suction type dispensing method using a conventional dispensing tip and a dispensing method employing a pressurized pressure type are employed. Since the dispensing apparatus 5 having the dispensing unit 5A is provided, in the dispensing operation of the secondary sample, the dispensing operation of the gasoline / naphtha-based sample is performed by the dispensing unit 5A, whereby the conventional dispensing is performed. Eliminates problems such as variations in analytical values due to evaporation of light-boiling components and dripping during the fractionation process, which were observed when fractionating gasoline / naphtha-based samples using the tip-type suction fractionation method Was done.

Further, in the fully automated system of the present embodiment, in addition to the processing section 6A for pretreating the light oil-based sample, a stirring table 66 with a heating mechanism, and a plurality of desiccants for storing desiccants Since the pretreatment device 6 including the hopper 65 and the treatment unit 6B for performing the pretreatment of the heavy oil-based sample is provided, the sample temperature is set to 60 ° C.
By rotating the stirrer in the pretreatment container while maintaining the pressure, the viscosity of the heavy oil-based sample during the pre-operation can be reduced, and the fluidity can be maintained. Therefore, when performing the pretreatment of the heavy oil-based sample, a desiccant whose type and particle size are selected in advance is added, and the sample is stirred while keeping the liquid temperature of the sample during the process at 60 ° C., and further allowed to stand still. After the desiccant is allowed to settle, the supernatant is separated and the dewatering agent can be dewatered without lowering the fluidity of heavy oil as in the treatment method using a conventional dehydrating agent and a shaker. The dewatering efficiency maintains the same dewatering efficiency as the conventional pretreatment device.

(Experimental Example 1) In the case of density, sulfur content and aniline point tests, a gasoline / naphtha sample of regular gasoline, a light oil sample of solvent A intermediate product and a heavy oil sample were used. An analysis test was performed on three kinds of samples of a certain Minas type C heavy oil intermediate product using the fully automated petroleum product analysis test system of the above-described example under the test items and pretreatment conditions shown in Table 2.

[0046]

[Table 2]

Table 3 shows a comparison between the test results obtained in the above examples according to the present invention and the test results obtained by the conventional method. The results of the analysis test obtained by using the fully automated petroleum product analysis test system of the present example and the results of the analysis test obtained by the conventional method showed a very good agreement. Also,
In the analysis test using the fully automated system for analyzing petroleum products of this example, the same analysis operation was repeated three times, but no variation was found in the test results. In the fully automated petroleum product analysis test system of this example, the highly volatile components of the regular gasoline-based sample were not scattered, and the pretreatment and preparative operation was performed even for the Minas-based C heavy oil intermediate product sample. The fluidity of the sample could be maintained.

[0048]

[Table 3]

[0049]

As described above, according to the fully automated petroleum product analysis test system of the present invention, the test conditions and the operating conditions of the test apparatus preset for each sample are stored, and From sample collection to test operation based on conditions,
Since the collection and arrangement of test results and the disposal of samples are fully automated, the following effects are obtained.

(1) A completely automatic system for analysis tests, which was difficult with the prior art, can be realized regardless of the type (physical properties) of the sample.

(2) The efficiency of the analysis test can be further improved by integrating the complete system for the analysis test realized by the present invention with the conventional management system.

(3) Human errors due to complicated operations that are likely to occur in semi-automation are completely eliminated.

(4) A plurality of samples having different physical properties could be continuously tested with high test accuracy.

(5) There is no need for manual labor, and there is no variation in test results due to the skill of the analyst, and the accuracy of repeated tests is improved.

[Brief description of the drawings]

FIG. 1 is a conceptual diagram of a fully automated petroleum product analysis test system according to the present invention.

FIG. 2 is a perspective view showing an example of a primary sample container storage device indicated by reference numeral 2 in FIG.

FIG. 3 is a perspective view showing an example of a primary sample container standby device indicated by reference numeral 4 in FIG.

FIG. 4 is a schematic diagram showing an example of a fractionating device indicated by reference numeral 5 in FIG.

FIG. 5 is a sectional view showing an example of a sealing device indicated by reference numeral 30 in FIG.

FIG. 6 is a cross-sectional view showing an example of a dispensing probe indicated by reference numeral 53 in FIG.

FIG. 7 is a schematic diagram showing an example of a preprocessing device indicated by reference numeral 6 in FIG.

[Description of sign]

 DESCRIPTION OF SYMBOLS 1 ... Code attaching device 2 ... Primary sample container storage device 2A, 2B, 2C ... Storage room 3 ... Capping device 4 ... Primary sample container standby device 4A, 4B, 4C ... Constant temperature bath 5 ... Sorting device 5A, 5B ... Sorting Part 6: Pretreatment device 6A, 6B: Processing unit 7: Automatic analysis test device 8: Robot hand 9: Management system X, Y, Z: Primary sample container M: Secondary sample container 21: Primary sample container inlet 22 ... Label issuing machine 23… Label reader 24… Insulation material 25… Refrigerator 26… Stirring fan 27… Automatic open / close door 28… Heater 29… Electronic balance 29A… Jig 30… Seal device 31… Sample supply / discharge tube 32… Sample pressure feed Gas introduction tube 33 ... Fluid supply / discharge tube 35 ... Sample supply / discharge tube 36 ... Stop valve 37 ... Waste sample receiver 40 ... Head part 41 ... Balloon 42 ... Cylindrical body 50 ... Dispensing tip 51 ... Dispensing tip storage part 52 … Dispensing tip transfer tool 53… Dispensing tip Over Bed 53A ... O-ring 53B ... head unit 54 ... dispensing tip attachment 55 ... waste tip receiving 56 ... dispenser 61 ... funnel 62 ... filter paper 63 ... funnel holder 64 ... secondary sample container holding 65 ... desiccant hopper

Continuation of front page (72) Inventor Hirotaka Kusaka 2421 Hayano, Mobara-shi, Chiba (56) References JP-A-2-251755 (JP, A) JP-A-2-251,763 (JP, A) JP-A-4- 274765 (JP, A)

Claims (1)

(57) [Claims] 1. A code providing device for providing a code for identifying a sample to a primary sample container containing a sample, and a primary sample container provided with a code by the code providing device is provided at least in a desired temperature condition. A primary sample container storage device that stores the primary sample container, a capping device that opens or closes the primary sample container, and a primary device that temporarily stores the primary sample container opened by the capping device at least at a desired temperature condition. A sample container standby device, a plurality of sorting units each employing a different sorting system, and a sorting unit employing a sorting system suitable for the physical properties of the sample among the plurality of sorting units. A sampler in which the selected sampler in the primary sample container standby device separates a predetermined amount of the sample in the primary sample container into a secondary sample container dedicated to the analytical test device, Has a plurality of processing units that employ a processing method, and selects a processing unit that employs a processing method that matches the physical properties of the sample from among the plurality of processing units, and by the selected processing unit, If necessary, a pre-processing device for pre-processing the sample, at least one or more automatic analysis test devices for analyzing the sample in the secondary sample container, and a primary sample container or A sample container transport device for transporting the next sample container, and connected to each of the above devices, at least, analysis test conditions preset for each sample corresponding to each code, and each of the above-mentioned preset for each sample type A management system having a function of storing operating conditions of the device, automatically controlling the respective devices based on these conditions, storing and / or recording test results, and performing arithmetic processing; Automatically sequence multiple samples Fully automated system for petroleum products analytical test, characterized by analysis.