Abstract:
The invention is an automated robotic system for the production and testing of formulations at a very high throughput. It is an integrated system of hardware and software capable of preparing and evaluating hundreds of emulsions per day. The system can formulate aqueous solutions (SL), oil in water emulsions (EW), suspo-emulsions (SE), micro capsule suspensions (CS), micro-emulsions (ME), and suspension concentrates (SC) at the 1 ml to 25 ml scale. The system can process emulsions rapidly in an automated way and enable very flexible formulation recipes to be introduced. The system allows chemists to generate experimental samples of varying recipe and method to be conducted in parallel with projected throughput of up to 1200 formulations processed and characterized per day. Materials and consumables can be distributed from storage storage systems to the work stations where dispensing of ingredients in various states can be performed, including solids, liquids, gels, pastes, suspensions and waxes. The emulsions formed can be characterized using methods including phase diagnosis, turbidity analysis, viscosity and particle sizing using automated test equipment. An integrated module can also perform Tank Mix Compatibility testing in high throughput mode. The modular system allows future processes and tests to be added, either to a station, or as a new station. The software capability includes tracking of processes from start to finish and the integration of analytical data with the as-designed and as-formulated experimental results.

Description:
FIELD OF THE INVENTION  
       [0001]     This invention relates generally to an automated robotic system for the production and testing of formulations at a very high throughput. More specifically, it is an integrated system of hardware and software capable of preparing and evaluating hundreds of dispersed multi-phase solutions per day. The system can process formulations rapidly in an automated way and enable very flexible formulation recipes to be introduced. Up to 1200 formulations on the 1 to 20 mL scale can be made per day. This includes tracking of processes from start to finish and the integration of analytical data with the as-designed and as-formulated experimental results. Materials and consumables can be distributed from storage systems to the work stations where dispensing of ingredients in various states can be performed, including solids, liquids, gels, pastes, suspensions and waxes. The emulsions, dispersions, and/or solutions formed can be characterized using methods including phase diagnosis, turbidity analysis, viscosity and particle sizing. The modular system allows future processes and tests to be added, either to a station, or as a new station.  
       BACKGROUND OF THE INVENTION  
       [0002]     Formulation chemists in the Surface Actives Ingredients (surfactants) and agrochemical markets realize the potential for applying Design of Experiments (DOE) methods to assess the impact of many variables on the performance, shelf-life, delivery characteristics, contamination susceptibility, and customer satisfaction of their products. Due to the complexity of the formulation recipes and the number of variables to be evaluated, DOE techniques generate matrices of tens of thousands of experiments that must be conducted to explore and refine the experimental space for these products. The shear number of experiments required renders typical bench chemistry techniques ineffective. The invention described herein provides the formulation chemist with a means of tackling these large DOE matrices in an automated fashion.  
         [0003]     The Summary of the Invention is followed by a Detailed Description of the system. Finally, a Process Description provides step-by-step preparation and testing methodologies for a typical Solution in Water (SL) recipe and a Suspension Concentrate (SC) formulation recipe that is prepared and tested on the invention.  
       SUMMARY OF THE INVENTION  
       [0004]     The invention is an automated robotic system for the production and testing of formulations at a very high throughput. It is an integrated system of hardware and software capable of preparing and evaluating hundreds of dispersed multi-phase solutions per day. The system can formulate aqueous solutions (SL), oil in water emulsions (EW), suspo-emulsions (SE), micro capsule suspensions (CS), micro-emulsions (ME), and suspension concentrates (SC) at the 1 ml to 25 ml scale. The system can process emulsions rapidly in an automated way and enable very flexible formulation recipes to be introduced.  
         [0005]     The system allows chemists to generate experimental samples of varying recipe and method to be conducted in parallel with projected throughput of up to 1200 formulations processed and characterized per day. Materials and consumables can be distributed from storage systems to the work stations where dispensing of ingredients in various states can be performed, including solids, liquids, gels, pastes, suspensions and waxes. The emulsions formed can be characterized using methods including phase diagnosis, turbidity analysis, viscosity and particle sizing using automated test equipment. An integrated module can also perform Tank Mix Compatibility testing in high throughput mode. The modular system allows future processes and tests to be added, either to a station, or as a new station. The software capability includes tracking of processes from start to finish and the integration of analytical data with the as-designed and as-formulated experimental results.  
         [0006]     It is an object of the present invention to provide an automated robotic system for the production and testing of formulations.  
         [0007]     It is a further object of the present invention to provide a system for the research, development, manufacture, and sale of products for use in agriculture, horticulture, forestry and protection during transport or storage or use of the harvested products of agriculture, horticulture or forestry and the treatment of the environment to combat infestations of pests harmful to public health, safety or convenience.  
         [0008]     It is a further object of the present invention to provide such a system for the discovery and development of crop protection or crop enhancement products and products for the treatment of the environment to combat infestation of pests harmful to public health, safety or convenience.  
         [0009]     It is a further object of the present invention to provide such a system for the research, development, manufacture and/or sale of surfactants, fatty acids and rheology control agents in formulations for fabric care, personal care, textile, mining, mineral coating, asphalt, petroleum, fuels, viscose, cleaning, building, coatings, paper processing and manufacture and in all applications of nitrogen derived surfactants. 
     
    
     BRIEF DESCRIPTION OF THE DRAWINGS  
       [0010]      FIG. 1  illustrates rack and vial storage system  100 .  
         [0011]      FIG. 2  illustrates consumables store  200 .  
         [0012]      FIG. 3  illustrates robotic arm  300 .  
         [0013]      FIG. 4  illustrates solid dispensing station  400 .  
         [0014]      FIG. 5  illustrates an embodiment of liquids, suspensions, gels and meltables dispense station  500 .  
         [0015]      FIG. 6  illustrates normal liquids dispensing and pipetting, and characterization station  600 .  
         [0016]      FIG. 7  illustrates mixing or homogenizing station  700 .  
         [0017]      FIG. 8  illustrates flexible arm station  800  used in alternative embodiment.  
         [0018]      FIG. 9  illustrates comminutor station used in an alternative embodiment  900 .  
         [0019]      FIG. 10  illustrates phase stability and cloud point station  1000 .  
         [0020]      FIG. 11  illustrates buffers  1100 .  
         [0021]      FIG. 12  illustrates dispensing, pipetting, and characterization station  1200 , included in alternative embodiments.  
         [0022]      FIG. 13  illustrates an exemplary flow diagram for system set-up.  
         [0023]      FIG. 14  illustrates flow diagram of experiment for preparing and testing Solution in Water (SL) formulation.  
         [0024]      FIG. 15  illustrates flow diagram of experiment for preparing and testing Suspension Concentrate (SC) emulsion formulation.  
         [0025]      FIG. 16  illustrates an embodiment of the present invention comprising rack and vial storage system  100 , consumables store  200 , robotic arm  300 , mixing or homogenizing station  700 , phase stability and cloud point station  1000 , buffers  1100 , and dispensing, pipetting, and characterization station  1200 .  
         [0026]      FIG. 17  illustrates an embodiment of the present invention comprising rack and vial storage system  100 , consumables store  200 , robotic arm  300 , solid dispensing station  400 , liquids, suspensions, gels and meltables dispense station  500 , liquids dispensing and pipetting and characterization station  600 , mixing or homogenizing stations  700 , flexible arm station  800 , comminutor station  900 , phase stability and cloud point station  1000 , and buffers  1100 . 
     
    
     DETAILED DESCRIPTION OF THE INVENTION  
       [0027]     An automated robotic system is disclosed herein for the production and testing of formulations at a very high throughput. In a preferred embodiment, a run is considered to be the operation of the system over a 24 hour period, including an approximately 20 hour operation period and an approximately four hour set-up period. Further, the disclosed, preferred embodiment is based upon the use of a 25 mL vial to hold about 10 mL of test formulation. The embodiment disclosed herein is disclosed for illustrative purposes only, alternative embodiments are envisioned.  
         [0028]      FIG. 1  illustrates rack and vial storage system  100 , comprising rack  102  and vial  104 . Vials are of the order of 25 mL, and 24 mm diameter, 73 mm high. They are racked in racks with a ‘well-plate’ foot-print containing 6 vials per rack. Each vial is bar coded and each rack is bar-coded. As these are custom racks, there is likely no cost differential between having plastic racks molded or machined from metal. In fact, metal racks can provide a simpler and faster means to heat the vials, because placing a rack of vials on a hot-plate is faster than transferring vials from a rack to a heating block. In this instance too, less space is needed on a robot deck, as empty racks are not generated, diminishing the need for storage.  
         [0029]      FIG. 2  illustrates consumables station  200 . These are used to supply the materials needed for a run including vials, pipette tips and, optionally, materials to be dispensed. The number and size of the storage systems will depend on the manufacturer, vial size and functions as above, selected by the customer.  
         [0030]     There are many manufacturers of these storage systems or stations (for example, Zymark, CRS, TomTek, STRobotics, etc.,) and custom versions can be obtained. Standard models work with the ubiquitous ‘Well-Plates’ and it is intended that the system disclosed herein will rack materials in the same format, be it vials, pipette tips or even solids for dispensing. These racks can also be referred to as ‘plates’ but their height will not be a standard well plate height.  
         [0031]     These stations are designed to store and present to an arm or gantry robot, individual plates in a defined position. At the beginning of a run they are loaded appropriately and at the end of a run, they contain finished formulations, grouped as needed (pass, fail, etc.,), along with empty racks and used source vessels, ready for unloading.  
         [0032]     Capacity requirements are dependent upon the desired application. For example in one embodiment 2000 positions are provided to hold 1500 vials (leaving 500 empty) and in a second embodiment 1000 positions are provided with 600 vials (leaving 400 empty). Additionally, space is provided for consumables (for example 5000 pipette tips) and for compound supply.  
         [0033]      FIG. 3  illustrates robotic arm  300  showing arm  302  and rail  304 . There are many robotic arm manufacturers and the most suitable arm and manufacturer are selected during the design phase for each application. The robotic arm provides the transport connection between all the stations for making and characterizing the emulsions, by moving the racked vials between the stations as required. In some embodiments the system is augmented by a second arm. Where the system is not augmented by a second arm, the sole arm also has the task of loading individual vials into the mixing systems; this requires either a gripper tool change, or the design of a dual function gripper for both vial and rack handling.  
         [0034]     Operation of the robotic arm can be considered to be divided into three parts: set-up, where materials and racks are dispersed about the system; run, where samples and supplies are transported during making of emulsions and; clean-up, where at the end of a run, dispersed material and samples are restored to their proper location. The use of such an arm enables ‘random access’ type of ordering of processes supplied by the stations around the rail. In a preferred embodiment, the robotic arm has the ability to read rack identity by bar codes.  
         [0035]      FIG. 4  illustrates solid dispensing station  400 . Such a station can be obtained from multiple manufacturers, including Chemspeed, Autodose and Flexiweigh. The platform is adapted to suit individual requirements. The dispense accuracy of each system is dependant on the material to be dispensed. Additionally, a representative sample must be dispensed from the container in terms of particle size and chemical composition. If required, sample conditioning such as grinding and sieving can be used to prepare the powders. Dispenses of 1 mg can easily be achieved and pre-treatment of the powders will increase both accuracy and precision.  
         [0036]     The solid dispensing station  400  can accept racks of empty vials, or vials from other dispense stations in racks and can either be preloaded with materials for a run, or accept racks of materials to be dispensed. The station picks up either whole racks of vials or individual vials, places them on mass balance  402 , dispenses by weight, solids obtained from solid source hoppers  404  into each vial, returning the vials to the rack before placing the rack at the delivery/collection point. It also moves racks of materials to be dispensed from the delivery/collection point to the distribution point on the deck. The station also includes bar code reader  406 .  
         [0037]      FIG. 5  illustrates an embodiment of liquids, suspensions, gels and meltables dispense station  500 . This station is based upon a gantry or Cartesian laboratory robot. Again, there are many manufacturers of such systems for example the Gilson “Cyberlab” 230/240/400 type platforms. These robot systems allow up to six tools to be mounted on the tool head above the deck, and the deck can be fitted with custom equipment including sub-stations with other integral tools. In a preferred embodiment the tool head is fitted with devices such as, but not limited to: rack/plate gripper, vial and cap gripper, gel dispenser gripper if required, pipettor for small plastic disposable pipette tips, optional pipettor for glass disposable pipette tips, and vacuum canula for dispensing grinding beads.  
         [0038]     Some tools can require more than one tool position. Some of these devices are multifunctional. For example, the vial gripper can also function as the gel dispenser gripper. Additionally, in varying embodiments, more than one size of pipette can be required for precision and accuracy in dispensing. It is envisioned that both 5 mL and 500 μL tips are used.  
         [0039]     The deck is mounted with associated devices such as, but not limited to: movable gel dispensers  502 ; rack or dispensing locations  504 ; comminuting bead source  506 , pre-loaded with beads; bar code reader/decapper  508 ; orbital shaker  510 ; one or more heated blocks  512 ; heated glass pipette tips  514 ; second mass balance  516 ; pipette-tip rack space  518 ; liquid vial deck space to enable other sources of normal liquids to be placed on the deck; enough space to contain the racks (likely stacked) that have been emptied into other deck units; and trash collection chute  520  for pipette tips and vial caps. Bar code reader/decapper  508  is used for identifying and opening vessels that arrive capped. Mixtures requiring agitation, such as unstable suspensions, are delivered to orbital shaker  510  after decapping. Orbital shaker  510  is also used for mild mixing such as dissolution and with careful selection of the shaker, even more aggressive agitation can be achieved. Where needed, materials are placed to melt upon/within the one or more heated blocks  512 , the materials are then readied for dispensing. Heated glass pipette tips  514  can be preloaded to be heated for dispensing small quantities of meltables. Second mass balance  516  is used for confirming the dispense by weighing.  
         [0040]     Because of the distribution of the tools on the head of such robots (where fixed tools are in fixed positions on the head), not all the deck space is accessible by all tools. Specifically, for example, in certain instances the right hand tool cannot reach the left hand side of the deck and visa versa. This limits the position and access for each tool to the bed. Alternatively, the gel, paste and high viscosity fluid dispensing or the meltables dispensing can require a separate station or sub station, especially when combined with mixing or when the quantities that should be dispensed, exceed 2 mL. When mixing is not required, the dispense volume can be confirmed using a balance. However, since order of addition and mixing do not allow the tip of any dispenser to contact the mixed formulation, the dispensing must be conducted without touch-off.  
         [0041]     When a mixer is used with dispensing, the station includes a dedicated wash station in which the mixers are cleaned, along with a wash fluid reservoir, pumps, drainage and valves as required (specified during the design phase) mL and 500 μL tips are used.  
         [0042]      FIG. 6  illustrates normal liquids dispensing and pipetting, and characterization station  600 , which can be included in alternative embodiments. This station provides a pair of waste stations where two separated types of fluid can be pumped to waste, and can be preferred when fluids are incompatible. The tool head can be fitted with items such as: rack/plate gripper; vial, filter and cap gripper; pipettor for plastic disposable pipette tips; dispense needle attached to the off-deck dispensing pumps, valves and manifold; and dispense needle for dispensing a common wash fluid.  
         [0043]     Again, some tools can require more than one tool position and in a preferred embodiment, some devices are multifunctional. As before, more than one size of pipette is required for precision and accuracy in dispensing. It is envisioned that both 5 mL and 500 μL tips would be used. Additionally, a pipettor suitable for more viscous samples can require a separate tool or replace those in the 5 mL tip rack.  
         [0044]     The deck is mounted with devices, the number and position of which are dependent upon the application. The devices include but are not limited to the following: bar code reader/capper/decapper  602 ; caps source; second pipette-tip rack space  604 ; liquid vial deck space; second orbital shaker  606 ; tank mix testing unit  608 ; particle-sized injection port  610 ; dilution port  611 ; viscometry injection port(s)  612 ; filtration device; filter elements source  614 ; particle size detector  618 ; viscometry detector(s)  620 ; cap supply  622 ; wash station  628 ; bead collection  630 ; trash  632 ; photography system  624 , and particle microscopy system  638 .  
         [0045]     The bar code reader/capper/decapper  602  is used for identifying and opening vessels that arrive capped and for closing vials before they are sent to storage. In a preferred embodiment, a source for about 2000 caps is provided. In a preferred embodiment, pipette-tip rack space  604  comprises a source of special slotted tips for aspirating the comminuted mixture from the beads.  
         [0046]     Liquid vial deck space enables other sources of normal liquids to be placed on the deck. Similarly, in a preferred embodiment, enough space is provided to contain the racks and to provide space for sorting sample vials into classes (e.g. once pass/fail criteria are applied). Orbital shaker  606  provides general mild to moderate mixing but is also used for Tank Mix Testing  608 . Samples are pipetted into the particle-size injection port  610 , the actual particle size detector  618  being mounted off deck. Dilution port  611  allows dilution of the formulation for particle photography. Viscometry injection port(s)  612  allow for measurement of viscosity at different shear rates. Filtration devices allow for timing the filtration of tank mix test samples. Filter elements obtained from filter elements source  614  are used for the tank mix test. Photography system  624  is used for photographing the tank mix test filter surface.  
         [0047]     Off the robot deck are mounted large components of processing or measuring devices, including but not limited to: particle size detector  618 , photography system  624 , viscometer measurement electronics  620 , valve and pump system  626  for dispensing small (10&#39;s of micro liters) volumes of samples with a ‘majority solvent’ flush to the dispense needle, and pump and source of common wash fluid  616  connected to its needle.  
         [0048]      FIG. 7  illustrates mixer/homogenizer station  700  with liquid addition. These station(s) have the ability to mix in both high and low shear mode in parallel. Stations  702  include a two axis (one vertical and one horizontal axes) Cartesian robotic system that can move up to six mixer/homogenizers  704  mounted in-line on an arm, between several rows of up to six (n×6) vessels and to an ultrasonic wash station  706  and a rinse station  708 . Additionally, the vessels in which mixing is occurring can be heated or cooled via a temperature-controlled fluid jacket and a chiller/heater/circulator  710 . The mixers include hardware to mount 3 probes of ⅛″ diameter with their working ends at the mixer blade. These probes can be for measuring pH or tubes for dispensing fluids into the mixture connected to a liquid addition unit  712  as determined by application requirements.  
         [0049]     The mixer/homogenizer  704  preferred capabilities include: the ability to mix in high and low shear modes; the ability to determine some measure of torque such as current vs. speed to allow a crude measure of viscosity; and a head diameter of no more than 15 mm.  
         [0050]     The liquid addition units  712  allow specific liquid(s) to be dispensed while mixing. The liquid addition units are built from common components available from companies such as Hamilton, Cavro, Rheodyne and Valco. The numbers of designs of such devices are infinite, and those described here should be thought of as proposals to meet defined needs with the understanding that other component combinations can provide the appropriate functionality.  
         [0051]     In a first embodiment of a liquid addition unit, each of the mixer heads is provided with one supply tube, each supplied from a separate pump  714  and source bottle  716 . This allows the addition of up to six different liquids chosen by the mixer row position where the target vial is loaded. These pumps are able to quantitatively dispense moderate and low viscosity materials (flow at room temperature).  
         [0052]     In a second embodiment of a liquid addition unit, the mixer system is provided with two tubes along with a combination pH electrode. In a preferred embodiment an electrode of ⅛′ diameter which includes the temperature probe, is used. Fluid is supplied to each mixer/homogenizer head, one at a time, from valves  718 . As described, it can be used for pH adjustment; however, it can also be used for dispensing other normal liquids if pH adjustment is not needed.  
         [0053]     Additionally, off deck can be a pH multimeter  720  such as that available from NICO2000. Versions are available that accept up to 24 pH probes and 24 temperature probes.  
         [0054]      FIG. 8  illustrates flexible arm station  800  used in an alternative embodiment. Flexible arm  802  accepts racks of vials from the robot arm  302  delivery point and provides individual vials to capping/decapping/bar code reading/cap supply station  804 . For mixing, if caps are present, they are removed and discarded in trash bin  806  and the vials placed in the appropriate mixer location  704 . Alternatively, caps can be put on the vial before it is placed in comminutor  902  by flexible arm  802 . After processing, flexible arm  802  moves the vials to the capping/decapping/bar code reading/cap supply station  804  as needed and returns them to the appropriate racks.  
         [0055]     Systems within reach of flexible arm  802  can include but are not limited to: transfer area for delivery and receipt of racks of vials  808 ; rack storage space for emptied racks  810 ; capping/decapping/bar code reading/cap supply station  804  (vials only—not racks); if flexible arm  802  is used during the de-capping, trash chute  806 ; off mixer station(s); and comminutor loading receptacle  904 . The reach of the robot chosen is dependent upon the dimensions of the system, specifically the rack storage space and the comminutor.  
         [0056]      FIG. 9  illustrates comminution station  900  used in an alternative embodiment. In this embodiment, planetary ball mill  902  is modified and small vials of about 25 mL are placed around the periphery of vial holders  906  to provide the comminution action required for up to 32 vials in parallel. Capped vials are delivered to the mill containing solids liquids and beads. The planetary action causes the beads to roll and ‘fly’ in the vial, causing grinding of the solid particles. After a prescribed time, the mill returns to defined stop position  908  and the vials are extracted and racked by arm  802 . Before racking, the vials can be de-capped. Whether to de-cap depends on the future of the vial. Further, vials can be stored in the space provided and de-capping delayed to allow material to settle off the lid.  
         [0057]      FIG. 10  illustrates phase stability and cloud point station  1000 . Apart from torque feed-back from the mixing stations, phase stability and cloud point station  1000  is the first station visited by most samples where characterization takes place. It is based on Cartesian robotic system  1002  such as provided by Gilson. In a preferred embodiment, the only tool on the head  1004  is gripper  1006 . This gripper has the ability to invert the vials if needed. Mounted on the deck are turbidity analysis instrument(s)  1008  such as Turbiscan (from Formulaction) or similar systems, bar code reader  1010 , heated/cooled zones  1012  and space for at least 3 racks. Samples are delivered in racks by arm  302 , and vials withdrawn and either placed in the heated/cooled zones and subsequently into the turbidity analysis instrument systems, or immediately into the turbidity analysis instrument systems where they are characterized for such properties as turbidity, phase separated, homogeneous, sedimentation, creaming, foaming etc. The ability to invert the vial just before measurement, also allows foaming and sedimentation to be studied. The vials are then removed and either placed back into the original rack, or sorted into ‘pass’ and ‘fail’ racks as determined by the selection criteria. Arm  302  then removes the racks of vials.  
         [0058]      FIG. 11  illustrates temperature buffers  1100 . Typically, such complex automated systems need space to buffer the stations to allow processes occurring at different times and speeds, to be synchronized. Each of solid dispensing station  400 ; liquids, suspensions, gels and meltables station  500 ; normal liquids dispensing and pipetting and characterization station  600 ; flexible arm station  800 , phase stability and cloud point station  10000 ; and alternate dispensing, pipetting, and characterization station  1200  naturally provides some buffer capacity and space in storage systems  100  that can also be available during an experimental campaign. However, additional space can be required. For example, two embodiments could include ambient and temperature controlled buffers  1102  and  1104 , respectively. Additionally, arm  302  is then the only service that the buffers would require as these buffers would be ‘dumb’.  
         [0059]      FIG. 12  illustrates alternate dispensing, pipetting, and characterization station  1200 , which can be included in alternative embodiments. This station is based upon a gantry or Cartesian Laboratory Robot. Again, there are many manufacturers of such systems such as the Gilson “Cyberlab” 230/240/400 type platforms. These robot systems allow up to six tools to be mounted on the tool head above the deck, and the deck can be fitted with custom equipment including sub-stations with other integral tools.  
         [0060]     The tool head can be fitted with items such as: rack/plate gripper; vial and cap gripper; gel dispenser gripper; pipettor for plastic disposable pipette tips; pipettor for glass disposable pipette tips; dispense needle attached to the off-deck dispensing pumps, valves and manifold; and dispense needle for dispensing a common wash fluid  
         [0061]     Again, some tools can require more than one tool position and in a preferred embodiment, some devices are multifunctional. As before, more than one size of pipette can be required for precision and accuracy in dispensing. It is envisioned that both 5 mL and 500 μL tips would be used. Additionally, a pipettor suitable for more viscous samples can require a separate tool or replace those in the 5 mL tip rack.  
         [0062]     The deck can be mounted with the following associated devices, the number and position dependent upon the application: bar code reader/capper/decapper  1202 ; caps source  1232 ; pipette-tip rack space  1204 ; balance  1206 ; liquid vial deck space; particle-sized injection port  1208 ; viscometry injection port(s)  1210 ; drain wash station(s)  1212 ; gel dispensers  1220 ; orbital shaker  1214 ; heated block(s)  1216  and heated pipette tips  1218 .  
         [0063]     Bar code reader/capper/decapper  1202  is used for identifying and opening vessels that are capped and closing vials before they are sent to storage. In a preferred embodiment cap source  1232  provides a source for about 2000 caps. Balance  1206  is used for confirming the dispense by weight. Liquid vial deck space enables other sources of normal liquids to be placed on the deck. Similarly, in a preferred embodiment, enough space is provided to contain the racks and to re-order the vials into classes. Samples are pipetted into particle-sized injection port  1208 . Viscometry injection port(s)  1210  allow for measurement of viscosity at different shear rates. Orbital shaker with heating and cooling capability  1214  is where mixtures requiring agitation, such as unstable suspensions, are delivered after decapping. Orbital shaker  1214  can also be used for mild mixing such as dissolution. With careful selection of the shaker, even more aggressive agitation can be achieved. Materials are placed upon/within heated block(s)  1216  for melting. The materials are then readied for dispensing. Heated pipette tips  1218  can be preloaded and heated for dispensing small quantities of meltables.  
         [0064]     The off deck is mounted with devices, including but not limited to: second particle size detector  1222  and flush system; second viscometer electronics  1224 ; second valve and pump system  1226  for dispensing small (10&#39;s of micro liter) volumes of samples with a ‘majority solvent’ flush to the dispense needle; trash receptacle  1234 ; dilution port  1236 ; second particle microscopy system  1238 , and pump and source of common wash fluid connected to its needle  1228 .  
         [0065]     In this embodiment, the gel, paste and high viscosity fluid dispensing or the meltables dispensing (See  FIG. 5 ) can require separate mixing station  1230 . When mixing is not required, the dispense volume is confirmed using balance  1206 . However, as order of addition and mixing do not allow the tip of any dispenser to contact the mixed formulation, the dispensing must be conducted without touch-off.  
       Process Description  
       [0066]     The automated robotic system is designed to operate without manual interference for a minimum duration of, but not limited to, one day after it is initialized and loaded with relevant components (raw materials, consumables, vials and racks) in the set up phase. Each vial  104  in any given rack  102  represents a unique experiment and has its own set of parameters such as, but not limited to, number of components, type and quantity of each component, mixing time, comminution time, etc. The tool heads on solid dispensing station  400 , liquids, suspensions, gels and meltables dispense station  500 , normal liquids dispensing, and pipetting, and characterization station  600  and flexible arm station  800  are capable of handling both racks  102  and single vials  104 . However, arm  302 , used for transfer between stations in one embodiment, can handle only racks  102 . Hence, the vials  104  are always grouped together in racks  102  when being transferred between stations. Once on a station, vials  104  can be picked up by the tool head and taken to the required locations for processing.  
         [0067]     The actual working of the system is described in this section with the help of two examples: 1/experiment for preparing and testing Solution in Water (SL) emulsion formulation; and 2/experiment for preparing and testing Suspension Concentrate (SC) emulsion formulation.  
         [0068]     In the first example, the initialization and set up phase have also been elaborated upon to illustrate the steps involved in preparing the system for a batch of experiments.  
       EXAMPLE 1  
     Experiment for Preparing and Testing Solution in Water (SL) Emulsion Formulation  
       [0069]     The objective of this experiment is to prepare a clear formulation, within a certain pH range, containing one active ingredient and three different additives. Successful formulations are then further tested for their chemical and/or biological activity. The steps involved in this experiment are as follows: 
        1) Add additives in the vial     2) Add active ingredients in the vial     3) Add water in the vial     4) Mix at low shear for 30 seconds     5) Heat the mixture for 10 minutes at 60° C.     6) Mix at high shear for 2 minutes     7) Conduct phase analysis     8) Store the clear samples for 24 hours and reject others     9) After 24 hours, conduct phase analysis on stored samples     10) Store the clear samples for further analysis and reject others        
 
         [0080]     In the current example, the component properties and quantities in one particular experiment are assumed to be as those described in the Table below.  
                                                     Component   Type   Quantity (mL or g)                                Additive 1   Low viscosity liquid   0.6       Additive 2   High viscosity liquid   0.6       Additive 3   Solid   0.6       Active ingredient   Low viscosity liquid   7.6       Water   Low viscosity liquid   1                  
 
         [0081]     Before the experimentation can begin, the system undergoes a set-up phase comprising of the following steps:  
         [0082]     1) Load racks and vials in the rack and vial storage system 100  
         [0083]     2) Load consumables in consumables station 200  
         [0084]     3) Load components on appropriate stations  
         [0085]     4) Transfer consumables to appropriate stations  
         [0086]     The entire set-up procedure for the current experiment is represented in  FIG. 13  in the form of a work-flow diagram and is further elaborated herein.  
         [0087]      FIG. 13  illustrates the steps involved in the set-up phase of the system before experimentation can begin for preparing and testing Solution in Water (SL) emulsion formulation. The various steps involved in executing each block of the flow diagram are described below in detail, we note that this description is for illustration purposes only, various embodiments will necessitate various steps in various orders as will be readily seen by the experienced practitioner.  
         [0088]     Start system initialization step  1302 , is the first step of initialization. Here, the entire system is switched on and a primary system check is conducted by the operator.  
         [0089]     The next step is loading racks and vials step  1304 , where the required number of racks  102  and vials  104  are loaded in rack and vial storage system  100 .  
         [0090]     In loading consumables step  1306  all consumables such as but not limiting to pipette tips are loaded in consumables storage system  200 .  
         [0091]     In load active ingredient step  1308 , active ingredient(s) are loaded on liquid dispensing, pipetting, characterization station  600 . In a preferred embodiment, the active ingredients are loaded through the bottles connected to valve and pump system  626 .  
         [0092]     In load additive one, step  1310 , additive one is loaded on liquids, suspensions, gels, and meltables dispensing station  500 . In a preferred embodiment loading occurs at rack or dispensing locations  504 .  
         [0093]     In load additive two, step  1312 , additive two being high viscosity liquid, can be dispensed by movable gel dispensers  502  on liquids, suspensions, gels and meltables dispense station  500  and hence are loaded in one of gel dispensers  502 .  
         [0094]     In load additive three, step  1314 , additive three being a solid, is dispensed at solid dispensing station  400 . It is loaded in one of solid source hoppers  404  and can be placed either directly on solid dispensing station  400  or in rack  102  in consumables storage system  200 . From consumables storage system  200 , rack  102  containing hopper  404 , can then be picked up by robotic arm  302  and transported on rail  304  to solid dispensing station  400 .  
         [0095]     In load water step  1316 , water is loaded on liquid dispensing, pipetting, characterization station  600  through a bottle(s) connected to valve and pump system  626 .  
         [0096]     In transfer consumables step  1318 , consumables such as but not limited to pipette tips, are picked up from consumables storage system  200  by robotic arm  302  and transferred on rail  304  to liquids, suspensions, gels, meltables dispense station  500  and normal dispensing, pipetting, characterization station  600 .  
         [0097]     Finally, in system initialization complete step  1320 , after all components are loaded and consumables transferred, the system is ready to start the experiments.  
         [0098]      FIG. 14  illustrates the flow diagram of the experiment for preparing and testing Solution in Water (SL) formulation. The various steps involved in executing each block of the flow diagram are described below in detail. As before, we note that this description is for illustration purposes only, various embodiments will necessitate various steps in various orders as will be readily seen by the experienced practitioner.  
         [0099]     At start of experiment step  1402 , rack  102  containing as many as, but not limited to, six empty vials  104  is picked up by arm  302  and transferred to rack  102  entry point on liquids, suspensions, gels, meltables dispense station  500 . From here, it is moved to rack or dispensing locations  504  by the tool head on liquids, suspensions, gels and meltables dispense station  500 .  
         [0100]     In add additive one, step  1404 , the tool head picks up vial  104  from rack  102 , takes it to barcode reader/decapper  508  for barcode scanning and puts it back in rack  102 . Based on the barcode, the control software determines the component, in this case additive one, to be dispensed in vial  104 . For the current experiment, the tool head picks up a disposable pipette from pipette-tip rack space  518 , aspirates 0.6 mL of additive 1 and dispenses it in the appropriate vial  104  in rack  102 . The tool head then moves above the trash collection chute  520  to dispose of the pipette tip.  
         [0101]     In add additive two, step  1406 , additive two being a high viscosity liquid, is dispensed gravimetrically. The tool head transfers vial  104  from its rack  102  to mass balance  516 , which is then initialized and tare weight determined by the control software. The tool head then picks up movable gel dispenser  502  containing additive two, brings it over vial  104  and dispenses the additive two in discreet shots of 0.1 g until the balance registers 0.6 g. It then takes movable gel dispenser  502  back to its location and transfers vial  104  back in rack  102 . When all the dispense tasks of the liquids, suspensions, gels, meltables dispense station 500 are completed, rack  102  with all its vials  104  is transferred to rack  102  exit point on liquids, suspensions, gels and meltables dispense station  500 .  
         [0102]     In add additive three, step  1408 , rack  102  is picked up from rack  102  exit point on liquids, suspensions, gels and meltables dispense station  500  by arm  302  and transferred to the rack  102  entry point of solid dispensing station  400  for dispensing additive three. From there, vial  104  is first taken to barcode reader  406  for barcode scanning and then placed on mass balance  402  by the tool head on solid dispensing station  400 . From the barcode, the control software confirms the solid to be dispensed, in this case additive three, which needs to be dispensed in vial  104 . In the current example, hopper  404  containing additive three is picked up by the tool head and 0.6 g of additive three is added in vial  104  on mass balance  402 . When all solid dispensing tasks are completed, rack  102  is transferred to rack  102  exit point on solid dispensing station  400 .  
         [0103]     In add active ingredient step  1410 , arm  302  picks up rack  102  from the exit point on solid dispensing station  400  and transfers it to rack  102  entry point on normal liquids dispensing and pipetting, and characterization station  600 . The tool head picks up rack  102  from entry point and transfers it to rack  102  buffer zone. There, 7.6 mL of active ingredient is added volumetrically in the vial  104  by the needle on tool head from the active ingredient reservoir connected to valve and pump system  626 .  
         [0104]     In add water step  1412 , after adding active ingredient, the needle on tool head is rinsed in wash station  628  and then 1 mL of water is dispensed from the water reservoir connected to valve and pump system  626 . Rack  102  is then moved to rack  102  exit point on normal liquids dispensing and pipetting, and characterization station  600 .  
         [0105]     In mix vial step  1414 , arm  302  transfers rack  102  from exit point on normal liquids dispensing and pipetting, and characterization station  600  to rack  102  entry point  808  next to flexible arm  802 . Flexible arm  802  moves rack  102  from there to the rack storage space for emptied rack  810 . Vial  104  is picked up by flexible arm  802 , taken to barcode reading station  804  for identification and then placed on mixer/homogenizer station  704  on mixer/homogenizer station  700 . Parallel mixing stations  702  moves over up to six vials  104  placed on six parallel mixer/homogenizer stations  704 , moves vertically down till mixers are in vials  104 , and then starts mixing at low shear for 30 seconds. When the mixing time is complete, six parallel mixer/homogenizer stations  704  move vertically up till they are out of vials  104 , move to the ultrasonic bath  706  to get washed and then move to the rinse station  708  to get rinsed. The vials are moved back from mixer/homogenizer stations  704  to rack  102  in the rack storage space for emptied rack  810 . Rack  102  is then moved to rack  102  exit point.  
         [0106]     In heat vial step  1416 , arm  302  transfers rack  102  from rack  102  exit point on flexible arm station  800  to the temperature buffers  1100  where it is kept at 60° C. for 10 minutes.  
         [0107]     In adjust pH step  1418 , after 10 minutes, rack  102  is again transferred to rack  102  entry point  808  next to flexible arm  802 . Flexible arm  802  moves rack  102  from there to the rack storage space for emptied rack  810 . Vial  104  is picked up by flexible arm  802 , taken to barcode reading station  804  for identification and then placed on mixer/homogenizer station  700  for pH adjustment. Mixer/homogenizer  704  shaft has on it a pH probe connected to pH multimeter  720 , which measures the pH of mixture in vial  104  and controls the addition of acid/base via two valves  718  to reach the set-point value.  
         [0108]     In mix vial step  1420 , when the pH of mixture is within the desired range, the mixture in vial  104  is mixed at high shear for two minutes by the mixer/homogenizer  704 . After mixing, the mixer/homogenizers  704  move vertically up till they are out of the vials  104 , move to ultrasonic bath  706  to get washed and then moved to rinse station  708  to get rinsed. Vial  104  is moved back to rack  102  on the rack storage space for emptied rack  810  by flexible arm  802 . The rack  102  is then moved to rack  102  exit point by the flexible arm  802 .  
         [0109]     In phase analysis step  1422 , arm  302  transfers rack  102  from rack  102  exit point by flexible arm  802  to rack  102  entry point on phase stability and cloud point station  1000 . Tool head  1004  on this station picks up the  104  from rack  102  with gripper  1006 , takes it to barcode reader  1010  for identification and then puts it on turbidity analysis instrument  1008  for phase analysis.  
         [0110]     In determination step  1424 , the analysis results are analyzed by the software and the mixture is classified into categories such as, but not limited to, “Transparent”, “Turbid”, “Foamy”, “Two-phase” etc.  
         [0111]     If the mixture in vial  104  is not identified as “Transparent”, in rejection step  1426 , it is flagged as “rejected”, and moved to rack  102 , reserved for rejected samples, by tool head  1004 . This rack  102 , when filled, is moved to rack  102  exit point by tool head  1004 , picked up by arm  302  and transferred back to the rack and vial storage system  100 .  
         [0112]     This brings the system to end point  1438 , the experimental run is considered to be finished in the system.  
         [0113]     However, if the mixture in vial  104  is identified as “Transparent” by the instrument  1008 , in storage step  1428 , it is flagged as “passed”, and moved to rack  102 , reserved for “passed” samples, by tool head  1004 . This rack  102 , when filled, is moved to rack  102  exit point by tool head  1004 , picked up by arm  302  and transferred back to rack and vial storage system  100  in a space reserved for “passed” samples and stored for 24 hours. In phase analysis step  1430 , after 24 hours, arm  302  picks up rack  102  containing “passed” samples again from rack and vial storage system  100  and transfers them to rack  102  entry point on phase stability and cloud point station  1000 . Tool head  1004  on this station picks up vial  104  from rack  102  with gripper  1006 , takes it to barcode reader  1010  for identification and then puts it on turbidity analysis instrument  1008  for phase analysis.  
         [0114]     In second determination step  1432 , the analysis results are again analyzed by the software and the mixture is classified into categories such as, but not limited to “Transparent”, “Turbid”, “Foamy”, “Two-phase” etc.  
         [0115]     As before, in second in rejection step  1434 , if the mixture in vial  104  is not identified as “Transparent”, then it is flagged as “rejected”, and moved to rack  102 , reserved for rejected samples, by tool head  1004 . This rack  102 , when filled, is moved to rack  102  exit point by tool head  1004 , picked up by arm  302  and transferred back to the rack and vial storage system  100 .  
         [0116]     This brings the system to end point  1438 , the experimental run is considered to be finished in the system.  
         [0117]     However, if the mixture in vial  104  is identified as “Transparent” by the instrument  1008 , in storage step  1428 , it is flagged as “passed”, and moved to rack  102 , reserved for “passed” samples, by tool head  1004 . This rack  102 , when filled, is moved to rack  102  exit point by tool head  1004 , picked up by arm  302  and transferred back to rack and vial storage system  100  in a space reserved for “passed” samples and stored for future analysis.  
         [0118]     This brings the system to end point  1438 , the experimental run is considered to be finished in the system  
       EXAMPLE TWO  
     Experiment for Preparing and Testing Suspension Concentrate (SC) Emulsion Formulations  
       [0119]     The objective of this experiment is to prepare a suspension concentrate emulsion formulation, within a certain particle size distribution and viscosity range, containing one active ingredient and two different additives. Successful formulations are then further tested for their chemical and/or biological activity. The steps involved in this experiment are as follows:  
         [0120]     1) Add additives in the vial  
         [0121]     2) Add active ingredients in the vial  
         [0122]     3) Add water in the vial  
         [0123]     4) Comminute mixture for 60 minutes  
         [0124]     5) Measure particle size distribution  
         [0125]     6) If sample is within the desired particle size range, then measure viscosity. Else, reject the sample.  
         [0126]     7) If sample is within the desired viscosity range, then the sample is stored for further analysis. Else, the sample is rejected.  
         [0127]     In this experiment, the component properties and quantities are assumed to be as those described in the Table below.  
                                                     Component   Type   Quantity (mL or g)                                Additive 1   Low viscosity liquid   1.0       Additive 2   High viscosity liquid   1.0       Active ingredient   Solid   4.0       Water   Low viscosity liquid   4.0                  
 
         [0128]     Before starting the experiment, the automated robotic system undergoes the initialization and set-up phase, as was described in the earlier example.  
         [0129]      FIG. 15  illustrates the flow diagram of the experiment for preparing and testing Suspension Concentrate (SC) emulsion formulation. The various steps involved in executing each block of the flow diagram are described below in detail. We again we note that this description is for illustration purposes only, various embodiments will necessitate various steps in various orders as will be readily seen by the experienced practitioner.  
         [0130]     At start of experiment step  1502 , rack  102  containing as many as, but not limited to, six empty vials  104  is picked up by arm  302  and transferred to rack  102  entry point on liquids, suspensions, gels, meltables dispense station  500 . From here, it is moved to rack or dispensing locations  504  by the tool head on liquids, suspensions, gels and meltables dispense station  500 .  
         [0131]     In add additive one, step  1504 , the tool head picks up vial  104  from rack  102 , takes it to barcode reader/decapper  508  for barcode scanning and puts it back in rack  102 . Based on the barcode, the control software determines the component, in this case additive one, to be dispensed in vial  104 . For the current experiment, the tool head picks up a disposable pipette from pipette-tip rack space  518 , aspirates 1.0 mL of additive 1 and dispenses it in the appropriate vial  104  in rack  102 . The tool head then moves above trash collection chute  520  to dispose of the pipette tip.  
         [0132]     In add additive two, step  1506 , additive two being a high viscosity liquid, is dispensed gravimetrically. The tool head transfers vial  104  from rack  102  to mass balance  516 , which is then initialized and the tare weight determined by the control software. The tool head then picks up movable gel dispenser  502  containing additive two, brings it over vial  104  and dispenses the additive two in discreet shots of 0.1 g until the balance registers 1.0 g. It then takes movable gel dispenser  502  back to its location and transfers vial  104  back in rack  102 . When all the dispense tasks of liquids, suspensions, gels, meltables dispense station  500  are completed, rack  102  with all vials  104  is transferred to rack  102  exit point on liquids, suspensions, gels and meltables dispense station  500 .  
         [0133]     In add active ingredient step  1508 , rack  102  is picked up from rack  102  exit point on liquids, suspensions, gels and meltables dispense station  500  by arm  302  and transferred to rack  102  entry point of solid dispensing station  400  for dispensing active ingredient. From there, vial  104  is first taken to barcode reader  406  for barcode scanning and then placed on mass balance  402  by tool head on solid dispensing station  400 . From the barcode, the control software determines the solid, in this case active ingredient, which is to be dispensed in vial  104 . In the current example, hopper  404  containing active ingredient is picked up by the tool head and 4.0 g of active ingredient is added in appropriate vial  104 . When all solid dispensing tasks are completed, rack  102  is transferred to rack  102  exit point on solid dispensing station  400 .  
         [0134]     In add water step  1510 , arm  302  picks up rack  102  from exit point on solid dispensing station  400  and transfers it to rack  102  entry point on normal liquids dispensing and pipetting, and characterization station  600 . The tool head picks up the rack from entry point and transfers it to rack  102  buffer zone. Here, 4.0 mL of water is added volumetrically in vial  104  by the needle on tool head from the active ingredient reservoir connected to the valve and pump system  626 . After adding water, the needle on tool head is rinsed in wash station  628  and rack  102  is then moved to rack  102  exit point on normal liquids dispensing and pipetting, and characterization station  600 .  
         [0135]     In comminution step  1512 , beads are first added in vial  104  using a solids canula on the liquids, suspensions, gels, meltables dispense station  500 . Arm  302  transfers rack  102  from exit point on normal liquids dispensing and pipetting, and characterization station  600  to rack  102  entry point on liquids, suspensions, gels and meltables dispense station  500 , from where it is moved to the rack or dispensing locations  504 . The canula on the tool head of liquids, suspensions, gels and meltables dispense station  500  aspirates the required quantity of beads from the comminuting bead source  506  and dispenses them volumetrically into vial  104 . The rack is then moved to rack  102  exit point on liquids, suspensions, gels and meltables dispense station  500  by the tool head and transferred by arm  302  to rack  102  entry point  808  next to flexible arm  802 . Flexible arm  802  then moves rack  102  to the rack storage space for empty racks  810 . Vial  104  is picked up by flexible arm  802 , taken to capping/decapping/barcode reading/cap supply station  804  for identification and capping. In the capping/decapping/barcode reading/cap supply station  804 , when capping vial  104  in one embodiment, a cap is dispensed from the cap supply and held on the mouth of vial  104  by the tool head. Vial  104  is capped by rotating it around its central vertical axis and then placed in one of comminution locations  904  at defined stop position  908  on vial holder  906  of comminution station  900  by flexible arm  802 . The lid on comminution station  900  is closed and vial holders  906  are then rotated in planetary motion for 60 minutes. At the end of the comminution time, vial holder  906  stops at defined stop position  908 , and vial  104 , is picked up by flexible arm  802  and transferred back to rack  102  in the rack storage space for emptied rack  810 . Rack  102 , when filled, is moved by flexible arm  802  to rack  102  exit point  808 , from where it is transferred by arm  302  to rack  102  entry point on normal liquids dispensing, pipetting, characterization station  600  for bead removal. Vial  104  is moved to barcode reader/capper/decapper  602  by tool head on normal liquids dispensing and pipetting, and characterization station  600 . In one embodiment, the cap on vial  104  is gripped by the barcode reader/capper/decapper  602  tool head and vial  104  is rotated to be de-capped. The cap is disposed of in trash  632  and vial  104  is moved to back to rack  102 . Using special pipettes from the pipette-tip rack space  604 , only the suspension in vial  102  is aspirated and dispensed into new vial  104  in a different rack  102  in the rack buffer space. The barcode of new vial  104  containing the suspension is read at the barcode reader/capper/decapper  602 . The original vial  104  and rack  102  can then be sent to the rack and vial storage system  100  using arm  302  or remain on the station for characterization.  
         [0136]     In particle size distribution measuring step  1514 , for measuring the particle size distribution, the tool head picks up a pipette from pipette-tip rack space  604 , aspirates between 0.5 and 1.0 mL of suspension from vial  104  and injects it in the particle-size detector injection port  610 . This port allows dilution of the sample before measuring.  
         [0137]     In determination step  1516 , the injected sample is analyzed in the off-deck mounted particle analyzer  618  and the particle size distribution profile is generated. This profile is then compared by the software with the desired profile and based on the comparison; the samples are classified as “failed” or “passed”.  
         [0138]     In rejection step  1518 , if the measured particle size distribution of the sample from vial  104  is out of the desired range, then the formulation in that vial  104  is classified as “failed” and is not tested further. It can be transferred in another rack  102 , reserved for “failed” formulation and transferred to rack and vial storage system  100  when it is filled with vials  104 .  
         [0139]     This brings the system to end point  1530 , the experimental run is considered to be finished in the system.  
         [0140]     If the measured particle size distribution of the sample from vial  104  is within the desired range, then the formulation in that vial  104  is classified as “passed” and its viscosity is measured at both high-shear and low-shear. In high shear viscosity measurement step  1520  and in low sheer viscosity measurement step  1522  the tool head picks up a pipette from pipette-tip rack space  604 , aspirates between 0.5 and 1.0 mL of suspension from vial  104  and injects it in the viscometry injection port(s)  612 . The high shear and low shear measurements are conducted in two different viscometer detectors  620 . After the measurement is complete, viscometry injection port(s)  612  and off deck viscometer detectors  620  are automatically washed and cleaned.  
         [0141]     In viscosity determination step  1524 , the measured viscosities are compared with the desired values. If the measurements are within the desired range, then the samples are classified as “passed”. If not, they are classified as “failed”.  
         [0142]     In viscosity rejection step  1526 , samples classified as “failed” are not tested further and can be transferred to another rack  102 , reserved for “failed” formulations. This rack is moved to vial storage system  100  when filled with vials  104 .  
         [0143]     This brings the system to end point  1530 , the experimental run is considered to be finished in the system.  
         [0144]     If the formulation in vial  104  is classified as “passed”, then in storage step  1528  the formulation is moved by the tool head to rack  102 , reserved for “passed” samples. This rack  102 , when filled, is moved to rack  102  exit point by the tool head, picked up by arm  302  and transferred back to rack and vial storage system  100  in a space reserved for “passed” samples and stored for further analysis.  
         [0145]     This brings the system to end point  1530 , the experimental run is considered to be finished in the system.  
         [0146]     Although the apparatus and process of the present invention has been described in detail for purpose of illustration, it is understood that such detail is solely for that purpose, and variations can be made therein by those skilled in the art without departing from the scope of the invention. The apparatus and operation of the present invention is defined by the following claims.