DESCRIPTION

[0017] The present invention is an automated chemistry system having the ability to record and automatically replay the actions of laboratory devices occurring during a laboratory experiment. With reference to FIG. 1 , the automated chemistry system 10 includes a controller 12 , input/output device 14 , control module 16 , and various laboratory instruments/devices 18 . The controller 12 is preferably a personal computer with an operating system such as WINDOWS® NT that allows for graphical program manipulation. The input/output device 14 is connected to the controller 12 and allows the user of the automated chemistry system 10 to interact with the controller 12 . The input/output device 14 typically includes a keyboard, monitor, mouse, speakers and/or other input/output devices used in association with computers such as microphones, touch screens, trackballs, etc. Also connected to the controller 12 is the control module 16 , which comprises a number of interface boards/cards that allow the controller to communicate with the laboratory devices. To this end, the boards of the control module 16 monitor the laboratory devices 18 and pass information about the laboratory devices on to the controller 12 . In addition, the boards of the control module 16 pass signals from the controller 12 on to the laboratory devices 18 to control the operation of the laboratory devices. The laboratory devices 18 may include pumps, stirrers, heaters, coolers, vacuum devices, temperature monitors, pressure monitors, and other sensors and laboratory instruments. Furthermore, the term “laboratory devices” as used herein may refer to any number of devices used in chemical processes, regardless of size, and regardless of whether the device is or can be used in a traditional “laboratory” setting.

[0018] Operation of the laboratory devices 18 generally results in an action directed to reaction materials within a reactor. Alternatively, operation of the laboratory devices 18 may provide information about the reaction materials in the reactor. The reactor may take a number of different forms, but an exemplary reactor used in many automated chemistry systems 10 is shown in FIG. 2 . As shown in FIG. 2 , the reactor 20 includes a glass reactor interior 22 for holding reaction materials/mixtures. The reactor interior 22 is contained within a glass reactor jacket/shell 24 . The reactor jacket 24 includes a jacket inlet 23 and a jacket outlet 25 . The jacket inlet 23 allows fluid to enter the space between the reactor interior 22 and the reactor jacket 24 and exit out the jacket outlet 25 . A glass reactor head 26 covers the top of the reactor interior 22 , and forms a seal between the reactor head 26 and the reactor interior 22 . The head 26 includes a number of ports 28 which provide passages between the reactor interior and the outside of the reactor.

[0019] The automated chemistry system utilizes software stored in either the control module 16 or the controller 12 to provide a graphical user desktop 32 for controlling the laboratory devices. The graphical user desktop 32 may be accessed by the user through the input/output device 14 . As shown in FIG. 3 , the graphical user desktop 32 includes an overview screen 34 that displays graphical representations of the reactor and associated laboratory devices used to carry out a desired experiment. The graphical user desktop may also include several other screens and pull down menus. Examples of such other screens and pull down menus are described herein and include, but are not limited to, the recipe editor screens and pull down menus described herein. In the embodiment shown in FIG. 3 , the overview screen 34 of the graphical user desktop 32 displays a reactor 20 , a pH control system 38 , a first chemical feed 40 , a second chemical feed 42 , a stirrer 44 , a temperature control system 46 , and a summary of reactor conditions box 48 . Of course, other laboratory instruments may be included on the overview screen if they are required for a particular experiment. The user has the ability to set up the graphical user desktop to properly represent all instruments used in a particular experiment.

[0020] The graphical user desktop 32 allows the user to easily see how the instruments 18 associated with the reactor 20 are arranged and monitor the progress of an experiment from the overview screen 34 . The graphical user desktop 32 also provides the user with the ability to control each of the laboratory devices 18 used in the experiment directly from the screen. Accordingly, the automated chemistry system 10 allows the user to conduct an experiment by commanding one instrument after another to take certain actions, thereby orchestrating the experiment step-by-step, in real-time, from the desktop 32 . Alternatively, as explained in more detail below, the user may program the system to run independent of human operation, and thereby leave the desktop while the experiment is automatically carried out unattended by a human operator.

[0021] Real Time Experiment Control

[0022] All laboratory devices depicted on the desktop may be controlled by clicking on the control “button” (i.e., selectable option) associated with that device (e.g., the “pH Control” button 39 , the “Feed 1 Control” button 41 , the “Feed 2 Control” button 43 , the “Stirrer Control” button 45 , or the “Temperature Control” button 47 ). A pointer 50 visible on the desktop 32 may be controlled with the mouse, thereby allowing the user to click on the desired device/buttons. For example, if the user clicks on the “Stirrer Control” button 45 , a dialog box will be displayed showing the stirrer parameters, as shown in FIG. 4 . Thus, if the user wants to change the stirrer speed from 50 rpm to 100 rpm, the user clicks the display of the stirrer setpoint rpm in the dialog box and, using the keyboard, inserts the number “100” in place of the number “50.” Next, the user clicks on the “Accept” button at the bottom of the dialog box, and the stirrer immediately starts spinning at the new rate of 100 rpm. Of course, any number of different means may be used to allow the user to enter operating parameters and the system to receive such parameters related to a particular laboratory device. For example, representative device control panels could be used to allow the user to enter the operational parameters or graphical parameter representations could be used to adjust parameters (e.g., clicking on a representative stirrer could adjust the stirrer spin speed). As a further example, operational parameters could be keyed into the system, adjusted by a click of the mouse, or entered vocally.

[0023] Similarly, the user may click on one of the “Feed Control” 41 or 43 (or “pH Control” 39 ) buttons to control the feed rate and amount of liquid product to be fed to the reactor. After clicking on the “Feed Control” buttons, a dialog box appears, similar to that shown in FIG. 7 , allowing the user to insert a desired feed rate (in weight or volume per minute) and a desired feed amount (in total weight or volume). Again, after clicking the “Accept” button at the bottom of the dialog box, the workstation will begin the desired feed.

[0024] The desktop also provides for temperature control of the reactor. After clicking on the “Temperature Control” button 47 , a dialog box appears, allowing the user to choose the desired temperature measurement to control. After choosing a desired temperature or temperature range, the user also provides a ramp rate which defines the rate at which the temperature will change (e.g., ° C./min). After completing the information in the dialog box, the user clicks the “Accept” button at the bottom of the dialog box and the workstation immediately begins to control the identified temperature based upon the users instructions. When the temperature control determines that the temperature is not in the preferred range, a pump will cause thermal control fluid to flow into the jacket inlet 23 , through the jacket 24 , and out the jacket outlet 25 , thereby pumping heated or cooled fluid in to the jacket and respectively heating or cooling the reactor contents surrounded by the jacket 24 .

[0025] With reference again to FIG. 3 , the information presented on the overview screen 34 continuously changes based upon actual experiment conditions. For example, the “Feed 1” data box 90 is periodically updated to show the actual amount of fluid that has been fed through the Feed 1 pump. Also, the “Reactor Contents” data box 98 keeps track of the total volume of fluid in the reactor while the “Reactor Conditions” box 48 keeps track of the reactor temperature, pressure and pH. If the condition of the reactor reaches a certain threshold, a warning will be sounded or displayed on the desktop. For example, if the volume of reactor contents becomes dangerously high, an alarm sounds or a message appears on the screen warning the user to avoid over-filling the reactor. Similarly, if the reactor contents reach a threshold temperature, making the reactor unstable, a warning will be sounded or displayed, warning the user to decrease the temperature of the reactor contents.

[0026] In addition to fully automated experimentation, the desktop also allows the user to note a manual action taken by the user, such as the addition of a compound manually added to the reactor during the experiment. In this situation, the user clicks on the “Log Comment” button 52 provided on the overview screen 34 . After clicking this button 52 , the user is provided with a dialog box that asks the user to insert information about some manual action, such as the name of the compound entered and the amount. This feature allows the system to completely log all steps taken by the user during any given experiment, whether controlled from the desktop or manually input by the user.

[0027] A report of data showing information logged by the system 10 during the experiment is available to the user by clicking one of the “Report” buttons 54 on the desktop. These “Report” buttons provide the user with various information, including a list of all actions taken during a particular experiment, tabulated or graphical data about various conditions at different times during the experiment, and information about instruments used during the particular experimental process.

[0028] Recipe Programming and Unattended Operation

[0029] If the user desires, the system 10 may be pre-programmed to complete all steps of an experiment automatically, thereby allowing the experiment to be conducted unattended. By clicking on the “Menu” button 56 , the user is presented with a “Recipe Editor” option (not shown). After clicking the “Recipe Editor” button, the user is presented with a recipe editor 58 . The recipe editor 58 is a tool for programming an experiment to be performed automatically by defining a “recipe” (i.e., a series of steps to be followed to accomplish a desired result). The recipe is saved as an executable computer program that can be played using the system software. A preferred embodiment of the recipe editor 58 is shown in FIG. 5 . As shown in FIG. 5 , the preferred embodiment of the recipe editor includes a “Stage Details” tab 62 , a “Stage Specials” tab 64 , and a “Stage Overview” tab 68 . Each tab provides different options to the user concerning the recipe.

[0030] Under the “Stage Details” tab 62 , the recipe editor 58 is designed to set up the automated experiment as a series of steps or stages. A stage indicator 60 is provided on each screen of the recipe editor on the top right of the screen. The stage indicator shows an indication of the stage as well as arrows for maneuvering between stages. The user programs each stage of the recipe under the “Stage Details” tab, and by using the stage indicator to maneuver between stages. Each screen under the “Stage Details” tab includes a variety of icons representative of various operations (e.g., temperature control 70 , addition of liquids 72 , pressure control 78 , pH control 74 , stirring 76 , etc.). The user identifies a desired action in each stage by inputting performance information in the boxes associated with each icon. For example, if the user wants to start the experiment by setting the reactor temperature to 25° C. for at least 20 minutes, the temperature set point of 25° C. is indicated in temperature mode box 70 and a hold time of 20 minutes is indicated in the hold time box 80 . After identifying this first stage, the user then moves to the next stage by pressing the “>” arrow in the stage indicator 60 . In the next stage, the user programs an additional step to be carried out, such as adding a new chemical through the “addition mode” box 72 or stirring the reaction through the “stirrer” box 76 . When additional stages are added, the total number of stages in the experiment are shown in the stage indicator 60 . For example, in FIG. 5, a seven stage experiment has been created and the first stage of the experiment is displayed in under the “Stage Details” tab. The user can move between stages by clicking the arrows to the right and left of the indicated stage in the stage indicator 60 . By moving through the experiment stage-by-stage, the user defines the complete experiment, breaking down the experiment to define how the equipment and laboratory devices should function in each stage.

[0031] In addition to automated stages, the user may program a manual stage. This is done by clicking the “enabled” button in the manual confirmation box 82 , and inserting instructions on the manual step to be taken by the user. This feature is especially useful when solids are to be added to the reactor during an experiment. For example, if 10 grams of NaCl is to be added to the reactor in a given stage, the user can note this as a stage in the recipe editor and note that manual confirmation is required before moving to the next stage. Thus, when the workstation automatically replays the recipe, a confirmation box will appear asking if 10 grams of NaCl has been added to the reactor. The confirmation box will include “yes” and “no” buttons the user may click in response. The workstation will not proceed with the experiment until the user makes a positive response that the NaCl has been added. Of course, the recipe programmer must recognize that manual confirmation steps can not be used if he/she desires to conduct a fully automated experiment with no user present to oversee the experiment.

[0032] The “Stage Specials” tab 64 allows the user to customize certain functions associated with different stages of the programmed experiment. For example, the “Stage Specials” tab provides for experiment termination conditions (e.g., excessive pressure, temperature, etc.), data logging rates (i.e., snapshot of experiment conditions taken at a periodic rate), and special alarm settings (e.g., excessive pressure, temperature, etc.).

[0033] The “Stages Overview” tab 68 allows the user to review the entire experiment in a single spreadsheet format, such as that shown in FIG. 6 . The “Stages Overview” tab 68 allows the user to see stages next to each other in tabular fashion, allowing the user to view the entire experiment on a single page, line-by-line. If the user sees any problems with the experiment set-up or desires changes in any particular stage, he or she can double click on the line showing the particular stage and be transferred to the “Stage Details” tab for that stage. At the “Stage Details” tab, the user may make any required modifications to the experimental set-up. Alternatively, the user may make modifications to different stages directly from the “Stages Overview” tab 68 by single clicking on an particular information item and changing the entry for that item. For example, if the user wants to change the hold time in step one from 20 to 25 minutes, the user can click on the “20” in line one and enter the new data in place of the old.

[0034] After all stages of a recipe are entered into the system, the recipe is saved by clicking the “Save” button 84 . Thereafter, the created recipe is saved and the user is returned to the overview screen 34 .

[0035] At the overview screen 34 , the user may execute the recipe by clicking on the menu button 35 . Clicking on the menu button 35 will provide the user with a number of options, one of which being an “Execute Recipe” button (not shown). Choosing this “Execute Recipe” button 66 will allow the user to choose from a list of recipes saved in the system. After the user chooses a recipe, the workstation will confirm that all laboratory devices required to execute the chosen recipe are connected to the system. If all required laboratory devices are not connected, the user will receive an error message informing the user that the required devices to execute the recipe are not properly connected. Also, before starting the experiment, the system will request confirmation that the reactor 20 has been filled with any required starting materials. Finally, before starting the experiment, the system will ask the user when he or she wants the experiment to begin. The user generally has the ability to start the experiment immediately or at a predefined time. For example, if the user wants an experiment to start in the middle of the night, the user can instruct the workstation to start the experiment at that time.

[0036] After an experiment is concluded using a recipe, several reports about the experiment are available for viewing. First, a recipe report showing each of the experimental steps taken during the experiment is available for viewing. Second, an experiment log, showing conditions as recorded at periodic times during the experiment is available. Also, trends reports are available that allow the user to view information in graph form, such as temperature vs. time and pH vs. time. Furthermore, an equipment report is available, listing all of the equipment that was used to perform an experiment pursuant to a particular recipe.

[0037] The overview screen 34 also provides the user with the ability to edit any recipes saved in the system. This option is available by clicking the menu button 35 , which presents the user with an “Edit Recipe” option (not shown). By clicking the “Edit Recipe” button, the user is presented with a list of recipes saved in the system. After the user chooses a recipe, the recipe information is presented in the recipe editor and the recipe may be edited in the recipe editor, as described above.

[0038] Automatic Recording Feature

[0039] Another option available to the user of the workstation is to record an experiment as it is conducted in real-time so that the experiment can be automatically replayed at a later time. This feature allows a user to program a recipe by actually going through a series of experimental actions as opposed to programming a recipe in advance using the “Recipe Editor.”

[0040] Referring to FIG. 3 , in order to record an experiment, the user activates the record option by simply clicking the “Record” button 100 provided on the overview screen 34 before starting an experimental process. Of course, any number of different means may be used to activate the record option, including voice activation, keyboard entry, activation of a related P/O device or some other activation method. Regardless of the means used to activate the record option, the record option is preferably provided through the graphical user desktop using a button on one of the screens, a pull down menu or on-screen instructions to the user describing how to activate the record option. After selecting the record option, the user then conducts an experiment from the overview screen by choosing various control buttons and instructing the laboratory devices to take certain actions, as described above under the heading “Real Time Experiment Control.” As the user conducts the experiment, each instruction given by the user is automatically recorded by the microprocessor in a recipe file and stored in the controller or controller module. The stored file is automatically named based on the date and time it was created. In addition to recording specific actions of the laboratory devices, other information about the experiment is also recorded. For example, times between instructions are recorded. If the user ends a process prematurely, that is also recorded and made part of the recipe. In short, the system 10 stores all information required to duplicate an experiment as conducted by the user. When the user has taken all desired experimental steps to be recorded, the “Record” button is clicked again to deactivate the record option and end the recorded session. At this time, the user has the choice of storing the file under a different file name than the name automatically assigned to the file.

[0041] A user/chemist will typically use the “Record” feature when there is a chance that he or she will want to repeat the experiment about to be conducted. The “Record” feature allows the user to actually program an experiment by conducting an ad hoc experiment, improvising each step of the experiment in an attempt to achieve a desired result. The user may then automatically replay the experiment without having to take additional steps to program the experiment into the system. For example, a chemist may want to take a certain chemical composition and change some property of the composition (e.g., boiling point, color, etc.) through some manipulative process involving various steps (e.g., the addition of other chemical agents, heat, pressure, etc.) to be determined extemporaneously. After achieving a desired result through such a process, the chemist may not remember every step taken to get to the desired result. However, if the chemist used the “Record” feature, a recipe has been automatically created, and the experiment can be automatically reproduced, without additional work by the chemist or a third party and without the chemist's presence to monitor replay of the experiment. This frees the chemist to do other important jobs and take other actions without having to try to reproduce past experiments or having to program a recipe for automatic reproduction. Thus, the “Record” feature of the system automatically records all experimental steps taken during a real-time experiment, and creates a recipe that may be run to automatically reproduce past experimental results.

[0042] As shown in FIG. 3, a “Pause” button 102 is provided next to the “Record” button 100 . The “Pause” button 102 will allow the user to take actions that are not recorded or omit long periods of inactivity from the recorded recipe. For example, the user may decide that he wishes to add a particular chemical to the reactor in the current experiment, but does not want the recorded recipe to show this step. To omit the step from the recorded experiment, the user clicks on the “Pause” button 102 , adds the chemical feed from the desktop, and then clicks the “Pause” button again to return to recording. Likewise, if the user wants to take a break and not have the period of inactivity recorded in the recipe, the user may click the “Pause” button 102 upon leaving for the break. Upon return, the user may click the “Pause” button 102 again, and the system will return to recording all actions taken during the experiment and related times for each action.

[0043] In addition to the ability to pause a recording so that certain actions or periods of inaction do not appear on the playback, the user of the system 10 has the ability to add a manual pause and associated comment into the recipe so that playback of the experiment is temporarily suspended until the user responds the recorded comment. A manual pause may be programmed in the playback of the experiment by using one of the laboratory device control buttons (e.g., 39 , 41 , 43 , 45 , 47 , etc.). For example, if the user clicks the “Feed 1 Control” button 41 , a dialog box 104 will be provided as shown in FIG. 7 . The dialog box not only allows the user to insert a desired feed rate and amount for the step, it also allows the user to enter a comment and note that a manual pause should be inserted before the step is carried out. Thus, if a particular experiment requires the user to add 25 grams of NaCl to the reactor and then start a feed from the Feed 1 device, the user can note this in the comment box 106 and indicate in the check box 108 that a manual pause should be included in playback before conducting the Feed 1 step. Of course other means than those described above may be used for entering comments and the manual pause, including, without limitation, voice activation and entry.

[0044] With a comment and manual pause entered, playback of the experiment will cause a dialog box to appear showing the comment and requesting a manual confirmation before continuing. Thus, if the recorded comment associated with the manual pause is “add 25 grams of NaCl before continuing,” playback of the experiment will include a dialog box that shows this comment and then asks the user to indicate by clicking a “yes” or “no” button whether the comment has been read and it is OK to continue the experiment. Manual pauses may also be programmed by clicking the “Log Comment” button 52 . Clicking the “Log Comment” button 52 results in a dialog box appearing along with a comment entry line and manual pause check box, similar to that shown in FIG. 7 , that allows the user to enter a comment and note that a manual pause should be inserted in playback of the experiment. Thus, the manual pause included with the automatic recording feature of the present invention allows the user of the system 10 to confirm that manual actions taken by the user during his or her experiment will also be included in the experiment when the experiment is replayed.

[0045] In operation, the user/chemist must decide whether to use the “Record” feature at the start of an experimental process. When using the “Record” feature, the user first connects the required laboratory equipment and prepares the required chemicals in appropriate containers, noting the initial set-up using the control software screen. Once set up is complete and noted in the computer, the chemist presses a “Record” button on the control software screen. Pressing the record button causes the system to note the initial set-up requirements and prepare to build a recipe based on the upcoming actions. Next, the chemist proceeds with the experiment using the graphical user desktop 32 , and the system automatically records every action made by the chemist. For example, if the chemist heats up the reactor during the experiment, the system will note the addition of heat and at what step and time to add the heat. If the chemist adds a chemical to the reactor, the system will note the addition of a chemical, along with the sequence and timing of adding the chemical. The complete experiment results are recorded in a recipe that can be automatically duplicated to reproduce previously achieved results. The record feature saves the user from having to manually program a recipe because the system automatically recorded every action taken in recipe format after the “Record” button 100 was pressed.

[0046] Once the experiment is complete and recorded by the system as a recipe, it is available for replay. To replay a recipe, the user simply selects the recipe from the list of recipes as described above under the heading “Recipe Programming and Unattended Operation.” During replay of the recipe, the system automatically duplicates the previously conducted experiment. The duplicated experiment is conducted by replaying the steps of the recorded experiment in the same order and with the same timing, with the exception that the system provides for removal or insertion of certain periods or steps. For example, manual pauses may be included in the replay involving steps that the system can not complete automatically (such as addition of a special chemical in granular form). In this situation, the user/chemist conducting the experiment is prompted to take the manual step. After the manual step is complete, the chemist then confirms that the step is complete by an appropriate response to the system. In this manner, the system provides a recipe-recorder that will record every step of an experiment by a chemist and allow that experiment to be automatically replayed without the need for additional manual programming by the chemist as traditionally accomplished through the use of a recipe builder/editor or similar programming device.

[0047] In addition to the above, recipes recorded through the system may be edited, just as any other recipe saved in the system. To do this the user selects the menu button 35 , which presents the user with an “Edit Recipe” option (not shown). By clicking the “Edit Recipe” button, the user is presented with a list of recipes saved in the system. After the user chooses the recorded recipe, the recipe information is presented in the recipe editor and the recorded recipe may be edited by the user.

[0048] Although the present invention has been described in considerable detail with reference to certain preferred versions thereof, other versions are possible. For example, various screens and dialog boxes described herein could be configured significantly different from the arrangement disclosed herein. Furthermore, the processes and steps required to record an experiment as disclosed herein could also be significantly altered without departing from the scope of the present invention. As another example, additional or different laboratory devices, reactors, and hardware configurations could be used instead of those disclosed herein. Therefore, the spirit and scope of the appended claims should not be limited to the description of the preferred versions contained herein.