Abstract:
Methods of analyzing processes for making catalysts and/or certain properties of catalysts using a plurality of reaction zones are provided. The methods of the present invention have the capability to define and execute, in rapid succession, a plurality of experiments under disparate reaction conditions. An operator may define and execute a plurality of experiments on user-defined quantities of disparate catalysts, using user-defined input feeds, residence times, and temperature profiles.

Description:
BACKGROUND OF THE INVENTION  
       [0001]     The present invention relates generally to the field of chemical evaluation systems, and more particularly, to systems for the high throughput analysis of chemical reactions and associated chemical properties.  
         [0002]     In the search for chemical compounds and for more efficient chemical reactions, automated systems for experimentally testing chemical reactions have been developed. Typically, these systems subject a known chemical composition or set of chemical compositions to a predefined set of reaction variables. If the test reaction or the output of the reaction exhibits desirable properties, further investigation of the particular reaction or composition may be warranted.  
         [0003]     Automated testing is frequently used in the area of catalyst development. Generally, catalyst screening systems involve confining a compound in a pressure vessel and contacting the compound with one or more fluid phase reactants at a controlled temperature, pressure, and flow rate. If the compound produces some minimal level of reactant conversion to a desired product, the compound undergoes more thorough characterization in later processes.  
         [0004]     One such automated system for screening catalysts is disclosed in U.S. Pat. No. 6,149,882. This document discloses a system for screening members of a combinatorial library by contacting library members with a test fluid. The system comprises a single volume of reactant fluid which is simultaneously applied to a combinatorial library of chemical compositions. The system is especially designed so that all members of the combinatorial library experience an identical fluid flow, under identical pressures and temperature. The system is said to provide the benefit of increasing the speed at which combinatorial libraries of chemical compositions can be screened for catalytic characteristics. In addition, this document discloses the use of multiple reactors and a sampling probe positioned to sample the vessel effluent.  
         [0005]     There are, however, numerous unsatisfied needs in the art. In particular there is a need for automated systems and methods for simultaneously analyzing chemical compositions under independent sets of reaction conditions. For example, there is a need for a system wherein a plurality of disparate chemical compositions can be simultaneously analyzed using different flow rates, under different pressures and temperatures. Such a system would provide much needed speed and flexibility in the analysis of chemical compounds, including catalyst analysis.  
         [0006]     The present invention meets these and other needs in the art. Generally, the invention is directed to a high throughput analysis system that provides the capability to define and execute in rapid succession a plurality of experiments under disparate reaction conditions. An operator may define and execute a plurality of experiments on user-defined quantities of disparate chemical compositions, using user-defined input feeds, residence times, and temperature profiles.  
       STATEMENT OF INVENTION  
       [0007]     In a first aspect of the present invention there is provided a method of analyzing any one or more of the following: at least one physical property of a reaction product, at least one chemical property of a reaction product, at least one performance property of composition used in producing a reaction product, at least one of the effects of any one or more reaction conditions on a reaction product, and at least one of the effects of any one or more reaction conditions on at least one performance property of any composition used in producing a reaction product, wherein said method comprises at least the following: 
        a. providing at least a first and a second reaction zone, wherein said first and said second reaction zones each have associated therewith a plurality of corresponding reaction conditions, and wherein at least one of the reaction conditions associated with the first reaction zone is capable of being modified independently of the corresponding reaction condition associated with the second reaction zone;     b. providing in said first reaction zone at least a first catalyst and a first reactant;     c. providing in said second reaction zone at least a second catalyst and a second reactant, said first catalyst can be the same or different from said second catalyst, and said first reactant can be the same or different from said second reactant;     d. subjecting at least one of said reaction zones to a set of reaction conditions to produce a reaction product; and     e. analyzing said reaction product to determine at least one of the following: at least one physical property of said reaction product, at least one chemical property of said reaction product, at least one performance property of said first catalyst, at least one performance property of said second catalyst, at least one performance property of said first reactant, at least one performance property of said second reactant, at least one of the effects of any one or more reaction conditions a physical or chemical property of the reaction product; at least one of the effects of any one or more reaction conditions a performance property of the first or second catalysts, and at least one of the effects of any one or more reaction conditions on a performance property of the first or second reactants.        
 
         [0013]     In a second aspect of the invention there is provided a system for analyzing any one or more of the following: at least one physical property of a reaction product, at least one chemical property of a reaction product, at least one performance property of a reactant used in producing a reaction product, at least one of the effects of any one or more reaction conditions on a reaction product, and at least one of the effects of any one or more reaction conditions on at least one performance property of any reactant used in producing a reaction product, wherein said system comprises at least the following: 
        a. at least a first and a second reaction zone, each having associated therewith an inlet through which at least one reactant is introduced and an outlet through which at least one reaction product produced therein is expelled,     b. a first controlling system for controlling at least one of the following reaction conditions for the first reaction zone: its temperature profile, the rate at which at least one reactant is introduced therein through its inlet, and the rate at which at least one reaction product is expelled therefrom through its outlet, and a second controlling system for controlling at least one of the following reaction conditions for the second reaction zone: its temperature profile, the rate at which at least one reactant is introduced therein through its inlet, and the rate at which at least one reaction product is expelled therefrom through its outlet, wherein at least one of said reaction conditions associated with the first reaction zone is capable of being controlled independently of the corresponding reaction condition associated with the second reaction zone; and     c. an analyzing system for analyzing at least one reaction product expelled from the first or second reaction zones to determine at least one of the following: at least one physical property of said reaction product, at least one chemical property of said reaction product, at least one performance property of a reactant used in producing a reaction product, at least one of the effects of any one or more reaction conditions on a reaction product, and at least one of the effects of any one or more reaction conditions on at least one performance property of any reactant used in producing a reaction product.        
 
         [0017]     In a third aspect of the present invention, there is provided a method for controlling the analysis of catalysts, comprising at least the following: 
        a. receiving reaction input data defining a plurality of chemical reactions to be performed under distinct reaction conditions in a plurality of reaction zones;     b. communicating with a heating element and at least one of a plurality of input controls to create the plurality of chemical reactions defined by the reaction input data in the plurality of reaction zones;     c. communicating with at least one valve to control an output flow out of one of the plurality of reaction zones; and     d. communicating with a detector to analyze the output flow out of one of the plurality of reaction zones.       
 
     
    
     BRIEF DESCRIPTION OF THE DRAWINGS  
       [0022]     Other features of the invention will be further apparent to those of ordinary skill in the art from the following detailed description of certain specific embodiments of the invention taken in conjunction with the accompanying drawings, of which:  
         [0023]      FIG. 1  is a schematic diagram of an exemplary embodiment of an analysis system in accordance with the present invention;  
         [0024]      FIG. 2  is a schematic diagram of a reactor block in accordance with an aspect of the present invention;  
         [0025]      FIG. 3  is an exploded view of a reactor core in accordance with an aspect of the present invention;  
         [0026]      FIG. 4  is top view of a reactor core in accordance with an aspect of the present invention;  
         [0027]      FIG. 5  is a sectional view of a reactor core in accordance with an aspect of the present invention;  
         [0028]      FIG. 6  is a block diagram of software components comprised in an exemplary embodiment of a system in accordance with the invention;  
         [0029]      FIG. 7  depicts an exemplary user interface screen for the input of data relating to test sample reaction conditions in accordance with an aspect of the invention;  
         [0030]      FIG. 8  depicts an exemplary user interface screen for the input of operator temperature settings in accordance with an aspect of the invention;  
         [0031]      FIG. 9  depicts an exemplary user interface screen for the input of data related to flow rate control in accordance with an aspect of the invention;  
         [0032]      FIG. 10  depicts an exemplary user interface screen related to test sample analysis data in accordance with an aspect of the invention;  
         [0033]      FIG. 11  depicts a flow diagram of the algorithm for queuing test sample experiments in accordance with an aspect of the invention. 
     
    
     DETAILED DESCRIPTION OF THE INVENTION  
       [0034]      FIG. 1  is a schematic diagram of an exemplary embodiment of an analysis system  110  in accordance with the invention. System  110  comprises a plurality of reaction blocks  112  that house a reactor core  114 . Reactor core  114  houses one or more reaction zones  116  that receive sample catalysts that are the subject of analysis.  
         [0035]     Each reaction zone  116  comprises an inlet through which at least one reactant is introduced and an outlet through which at least one reaction product produced therein is expelled. Each reaction zone  116  is in fluid communication with various input controls that include, for example, one or more reactant feed sources  118  and associated valving  119 , mass flow controllers  120 , and/or moisture saturators  122 . As shown in  FIG. 1 , the components of the analysis system are connected via feed lines  123  and other associated piping.  
         [0036]     Reaction product produced within reaction zones  116  flows to reaction zone selector valve  124  which is operable to selectively route the reaction product. Generally, reaction zone selector valve  124  routes the reaction product from one reaction zone  116  on to reaction core selector valve  128 , while routing the output flow from the remaining reaction zones  116  to waste. In embodiments comprising multiple reaction blocks  112  and reactor cores  114  as shown in  FIG. 1 , the system comprises a reactor core selector valve  128  that receives designated reaction product streams from each reactor core  114  and is capable of selectively routing the reaction products to a waste stream or to the detector  126  for analysis. Output flow line heating element  125  operates to heat reaction product flow lines  127  to prevent exhaust gases from condensing in lines  127 . Reactor core heating element operates to heat reactor core  114  to the desired experimental temperature.  
         [0037]     Analysis system  110  further comprises one or more control computers  130  that communicate with other components of the system to independently control the reaction conditions of each reaction zone  116  and selectively analyze the reaction products produced therein. As shown in  FIG. 1 , control computer  130  communicates with other system components over communication bus  131 . In embodiments having more than one reactor block  112 , each reactor block  112  may be associated with a separate control computer  130 . Alternatively, a single control computer  130  may control each of a plurality of reactor blocks  114 . Examples of reaction conditions controlled by control computer  130  include, for example, the temperature profile of reaction zones  116 , the rate at which at least one reactant is introduced to reaction zones  116 , and the rate at which at least one reaction product is expelled from reaction zones  116 . Control computer  130  also communicates with detector computer  132  to implement analysis requests. Furthermore, control computer  130  communicates with data archive computer  134  to maintain an archive of the analysis parameters and results.  
         [0038]      FIG. 2  is a schematic representation of a single reactor block  112 . Reactor block  112  comprises a plurality of reaction zones  116 , each of which may house a catalyst to be analyzed. Although the present invention may be discussed in terms of catalyst analysis, the catalyst may be any composition, liquid or solid, sought to be analyzed. These other uses will become evident to those skilled in the art after reading this specification.  
         [0039]     Typically, a solid chemical composition (e.g., a catalyst) is supplied to reaction zones  116  in the form of a fixed bed. The catalyst may be supported on solid particles or may itself be granular or a porous solid. Reaction zones  116  preferably comprise a reaction tube of specified dimensions that is capable of supporting a catalyst bed. Generally, the reaction zone may be any vessel or container capable of supporting a catalyst. Depending on the property or reaction condition being analyzed, each catalyst may be loaded into a different reaction zone  116  in the same or different amounts, at the same or different heights, and with the same or different particle sizes.  
         [0040]     In accordance with the specific embodiment of the invention illustrated in  FIG. 1 , one or more reactants is introduced to one or more reaction zones  116 . Each reaction zone  116  is in fluid communication with one or more input controls such as a reactant feed source  118 . In the exemplary embodiment, an individual reaction zone  116  may be in fluid communication with one or more reactant feed sources  118 . A selector valve  119  is used to select one or more reactants. In alternative embodiments, one reactant feed source  118  may be used to supply a reactant to each reaction zone  116  within an individual reactor core  114 . In addition, a different reactant feed source  118  may be associated with each individual reactor core  114 . The reactants may be liquids or gases and may include, for example, hydrocarbons compositions, such as those containing at least one of the following: methane, ethane, propane, butane, propylene, etc.  
         [0041]     Another input control in fluid communication with reaction zone  116  includes one or more mass flow controllers  120 . As depicted in  FIG. 2 , a mass flow controller  120  controls the flow rate of each reactant introduced into an individual reaction zone  116 . Accordingly, residence time may be varied from reaction zone to reaction zone by changing the flow rate of a reactant being introduced. For example, depending on the dimensions of the reaction zone, catalyst particle size, and catalyst bed height, flow rate may be varied over a range of rates that will correspond to a range of residence time. Residence time for this specific embodiment is defined as The time the reactant(s) is in contact with the catalyst(s) under a specific set of reaction conditions. In addition, control of the rate of flow rate into a reaction zone  116  also serves to control the rate at which a reaction product is expelled from a reaction zone  116 .  
         [0042]     Optionally, one or more reaction zones  116  may be in fluid communication with a moisture controller such as a moisture saturator  122 . In this specific embodiment, moisture saturator  122  can provide and/or regulate the moisture content of the reactant(s) and/or the reaction zones  116 .  
         [0043]     In the system illustrated in  FIG. 1 , each reaction zone  116  is housed in reactor core  114 . Specifically, in this exemplary embodiment, eight reactor zones  116  are housed in a single reactor core  114 . Of course, more or less reactor zones  116  may be associated with a single reactor core  114 .  
         [0044]     In one specific embodiment, the temperature of each reaction zone  116  can be controlled at the reactor core  114  level. Under such circumstances, each reactor core  114  can be in thermal communication with a heating element. With this specific configuration, the temperature of each reactor core  114  and its associated reaction zones  116  can be regulated by, for example, control computer  130 .  
         [0045]     Reaction zones  116  typically have the same temperature profile as their corresponding reactor core  114 . Reactor core temperature profiles are typically defined by their temperature ranges, their ramp rates and/or their dwell times. These parameters can be regulated by any suitable means. In the specific embodiment illustrated in  FIG. 1 , they are regulated by control computer  130 .  
         [0046]     Reactor core temperatures, ramp rates and dwell times for a specific system made in accordance with the present invention depend, in part, upon the product being made, the property being analyzed, and/or the materials from which the system&#39;s components are manufactured. When practicing this embodiment of the invention, those skilled in the art, after reading this disclosure, will be able to determine the core temperatures, ramp rates and dwell times that best suits their needs. All such configurations are deemed to be encompassed by the present invention. In addition to altering temperature profiles on a run by run basis, in embodiments comprising multiple reactor cores, it is also within the scope of this invention for the temperature profile of individual reaction zones to be simultaneously varied.  
         [0047]     As one example, if the system illustrated in  FIG. 1  is designed for the catalytic conversion of hydrocarbons (e.g., propane and/or propylene—containing reactants) to unsaturated aldehydes or acids, the reactor core temperature will typically range from 150° C. to 1000° C., and more typically from 250° C. to 750° C. Moreover, the ramp rate will typically range from 0.10°C./min to 25° C./min, and more typically from 1° C./min to 10° C./min.  
         [0048]     The design of reactor core  114  aids the overall throughput of the system. An exemplary embodiment of reactor core  114  is depicted in  FIGS. 3-5 . As shown, reactor core  114  comprises a cylindrical block  310  having a hollow center  312 .  
         [0049]     Block  310  can be made of any suitable material that can withstand the particular temperature profile and/or reaction conditions to which it is to be subjected. In the specific embodiment illustrated in  FIG. 1 , block  310  can be made out of a material such as, for example stainless steel.  
         [0050]     Reaction zones  116  are distributed symmetrically around block  310  at a uniform radius from the center of the cylinder. All configurations of reaction zones within block  310  are, however, encompassed by the present invention. If it is desired for reactor block  310  not to be affected by the addition of small masses associated with the reactants in reaction zones  116 , reactor block  310  will typically have a relatively large thermal mass.  
         [0051]     When used to make unsaturated aldehydes or acids from lower chain hydrocarbon compositions, temperatures within reactor block  310  typically can reach as high as 1000° C. At these temperatures, it is often desirable to uses insulators  314  positioned on opposite ends of reactor block  310  to isolate other system components from the intense heat. Insulator  314  may be manufactured from any suitable material that can provide sufficient insulation. In this specific embodiment, insulator  314  can be manufactured, for example, out of ceramic composite material.  
         [0052]     In the system illustrated in  FIG. 1 , input manifolds  316  are positioned adjacent insulators  314  and serve to further thermally isolate reactor block  310 . Generally, a cooling fluid can be circulated in input manifolds  316 , if desired. Input manifolds are manufactured from any suitable material. In this specific embodiment, input manifolds can be manufactured from stainless steel.  
         [0053]     Reactor core  114  also comprises sealing rings  318 . If used, sealing rings  318  operate to provide a tight seal around the inlets of the reaction zones without having to exert large amounts of pressure. This is especially useful when the reaction zones are made from a more fragile material such as glass or quartz, as opposed to a more rigid material such as stainless steel. However, it is within the scope of this invention to use sealing rings with the more rigid reaction zones such as those made out of steel. _.  
         [0054]     Referring back to  FIG. 2 , detector  126  is operable to analyze the reaction product expelled from the reaction zones  116  to determine at least one of the following: at least one physical property of said reaction product, at least one chemical property of said reaction product, at least one performance property of a reactant or catalyst used in producing a reaction product, at least one of the effects of any one or more reaction conditions on a reaction product, and at least one of the effects of any one or more reaction conditions on at least one performance property of any reactant or catalyst used in producing a reaction product.  
         [0055]     Depending on the analytical device being employed, the high throughput system disclosed herein can be used to analyze any number or physical, chemical or performance properties of reactants, catalysts or reaction products. The specific properties being analyzed will depend upon the specific goals and objectives of the end user.  
         [0056]     In the embodiment wherein the system is used to make unsaturated aldehydes or acids, an example of physical, chemical and performance properties that can be analyzed are as follows. Examples of physical properties that can be analyzed included thermal conductivity, adsorption, porosity, viscosity, specific gravity, heat capacity, dielectric constant, and the like. Examples of chemical properties include spectroscopic properties, compositional data, pH, molecular mass, molecular structure, and the like. Examples of performance properties of the reactant or catalyst include reactivity, conversion, percent yield, absorption, stability, selectivity, and the like.  
         [0057]     Detector  126  can be any suitable device. The specific type of device employed when practicing an embodiment of this invention will depend, in part, on the properties being analyzed. However, in the specific embodiment wherein the system is being used to make unsaturated aldehydes or acids, detector  126  is typically a spectroscopic or chromatographic device. In certain preferred embodiments, it is envisioned that an infrared spectrometer is used to generate an infrared spectrum of the reaction product; and Partial Least Squares (PLS) is used to mathematically separate and analyze individual analyze concentrations. Detector  126  may also be designed to provide low dead volume that requires short purge times to further aid in maintaining a high throughput for the system.  
         [0058]     Although the system depicted in  FIG. 1  shows a single detector  126 , it is within the scope of this invention that a number of detectors can be used. In addition, detector  126  may also comprise multiple channels to further expedite the analysis process.  
         [0059]      FIG. 6  is a block diagram of software components that may be employed in the exemplary embodiment of a system in accordance with the invention. As shown, the specific control computer  130  comprises the following software components: test sample control  610 , spectrometer control  612 ; and transfer lines temperature control  614 .  
         [0060]     It should be noted that, after reading this disclosure, those skilled in the art will learn how to make modifications to the block diagram. Such modifications are deemed to fall within the scope of this invention. For example, spectrometer control  612  can be any control for any analytical device. Similarly, transfer lines heater control  614  can be a moisture control, or the like. Set out below is a description of a fairly specific block diagram of software components encompassed by this invention.  
         [0061]     In this specific embodiment, test sample control module  610  provides a user interface and also communicates with reactor cores  114  and selector valves  124  and  128  of the system illustrated in  FIG. 1  to implement a plurality of reactions specified by the operator. In the exemplary embodiment, a single instance of sample control module  610  is responsible for the experiments implemented at a single reactor core. For each reactor core  114  that is used, a unique instance of test sample control module  610  is substantiated. Thus, while only a single instance of test sample control  610  is shown in  FIG. 6 , multiple instances may be operating on control computer  130 . Furthermore, each instance of test sample control  610  may operate on a separate computing device.  
         [0062]     In the specific block diagram illustrated in  FIG. 6 , test sample control module  610  comprises test sample input module  620 , reactor temperature control module  622 , flow control module  624 , and sample analysis monitor module  626 . Test sample input module  620  provides for defining new test sample experiments. Specifically, test sample input module  620  allows the operator to define the reaction conditions for a plurality of test sample experiments.  
         [0063]     After reading this disclosure, those skilled in the art would be able to configure data on a computer screen in an infinite number of ways depending upon their specific needs and objectives. One example of a user interface screen that can be associated with input module  620  for defining test sample reaction conditions is illustrated in  FIG. 7 . As shown therein, establishing a new test protocol involves identifying a sample, the sample&#39;s mass, the sample&#39;s height, and a residence time. For example, a user may define that sample X, having a mass of 2 grams and a height of 4 cm, is to undergo testing with a residence time of 5 seconds. The residence time is defined as the sample volume divided by the flow rate. In certain preferred embodiments, the sample volume is the cylindrical volume in the catalyst tube, which in the exemplary embodiment is equal to the sample height multiplied by Πr 2 , where r represents the radius of the catalyst tube. Using values for the residence time and the sample volume, a flow rate for the test sample is calculated.  
         [0064]     The exemplary user interface of  FIG. 7  also provides for identifying the name of the party submitting the sample, a description of the sample, and the contents of the sample. Although not shown in the exemplary screen, a system in accordance with the invention further provides the capability to specify the input feed that is to be used. For example, an operator of the system may specify that the input fluid is to be hydrogen as opposed to some other feed source gas.  
         [0065]     Thus, a system in accordance with this embodiment of the invention provides for entering a plurality of test samples, each of which may have different masses, heights, and residence times. Further, each test sample experiment may be specified to be conducted with a particular reactant feed source. Collecting this information, which defines the reaction conditions for a plurality of chemical reactions, allows for defining a plurality of unique experiments which can be run simultaneously. By comparison, existing systems operate to expose test samples, which have a common size and configuration, to a common test protocol under the same flow rate. Accordingly, a system in accordance with this embodiment of the present invention provides versatility that is not provided by existing systems.  
         [0066]     Test sample control module  610  of the specific block diagram illustrated in  FIG. 6  further comprises reactor temperature control module  622 . Generally, reactor core temperature control module  622  allows for the operator of the system to specify temperature conditions for reactor core  114 . This can also be used to specify temperature conditions of defined sections of the reactor core such that the temperature conditions of the defined sections can be controlled independently. These temperature conditions are implemented in reactor core  114 , or one or more defined sections, while the test sample experiments, which have been specified as explained above in connection with  FIG. 7 , are executed.  
         [0067]     One specific example of a screen that can be implemented by reactor temperature control module  622  for gathering operator temperature settings is illustrated in  FIG. 8 . After reading this disclosure, those skilled in the art would be able to configure this data on an interface screen in an infinite number of ways depending on their needs and objectives.  
         [0068]     As shown in the specific screen illustrated in  FIG. 8 , the operator can specify an initial temperature value and a period for which the initial temperature is to be held. Thereafter, the temperature may be increased by an operator defined gradient until reaching an operator defined plateau value. In this specific example, the operator can specify up to five such “ramps” which are executed sequentially. Once a set of temperature ramp settings have been defined, they may be saved and recalled for use in future tests.  
         [0069]     Test sample control module  610  of the specific block diagram illustrated in  FIG. 6  further comprises flow control module  624 . Flow control module  624  can provide an interface for displaying the present flow data as well as allowing the user to change those flows.  
         [0070]     One specific example of a user interface screen which can correspond with flow control module  624  is illustrated in  FIG. 9 . As shown, for each of the eight reaction zones  116  that are comprised in reactor core  114  of the exemplary test system, the actual flow rate and the desired flow rate are displayed. Values for the desired flow rates are calculated based upon the residence time defined by the operator as explained above in connection with  FIG. 7 . The operator can change the flow rate from that calculated by the system simply by introducing a new value in the appropriate location.  
         [0071]     Flow control module  624  can also be configured to control the queuing of tests within a reactor core  114  for analysis. Thus, flow control module  624  can be used to determine which experiment is to be implemented within a particular reactor core  114 .  
         [0072]     In one specific example, flow control module  624  queues test samples within a reactor core on a first-in-first-out basis. When a test sample is next in the queue, the flow control module can be configured to communicate with the various components of the test apparatus including feed source selector valves  119 , mass flow controls  120 , and saturators  122  to implement the flow settings associated with the particular test sequence. Thus, flow control module  624  can identify which test is to be analyzed and activate the various components of the apparatus to insure that the reaction conditions correspond to those specified by the operator. Once the reaction conditions have been established, flow control module  624  can be designed to communicate with reaction zone selector valve  124  to direct the output flow from the queued test reaction to reactor core selector valve  128 .  
         [0073]     Test sample control module  610  of the specific block diagram illustrated in  FIG. 6  further comprises sample analysis monitor module  626 . Sample analysis monitor module  626  can be configured to provide an interface to the test screening that is presently being analyzed at detector  126 .  
         [0074]     One specific example of a user interface screen which can correspond to sample analysis monitor module  626  is illustrated in  FIG. 10 . As shown, the test sample experiment presently being analyzed is identified along with the physical readings for that test sample.  
         [0075]     Referring back to the specific block diagram illustrated in  FIG. 6 , control computer  130  further comprises spectrometer control module  612 . Spectrometer control module  612  can be used to determine which test sample, from amongst those queued at each of the reaction cores  114 , is to be analyzed next. Spectrometer control module  612  can also be used to communicate with reactor core selector valve  124  to route the flow from the appropriate reactor core  114  to detector  126 , and to communicate with detector computer  132  as to when to begin operating on the reaction product flow stream.  
         [0076]     As explained above, for the plurality of reaction zones  116  associated with any one particular reactor core  114 , flow control module  624  is responsible for identifying which of the reactions is to be implemented at any particular time. Accordingly, flow control module  624  controls the operation of reaction zone valves  124  and thereby identifies which test sample within a reaction core  114  is to be analyzed.  
         [0077]     Spectrometer control module  612  can be configured to control reactor core selector valve  128  and thereby identify which test sample across the reactor cores is to be analyzed. Generally, in this specific embodiment, spectrometer control module  612  operates on a modified first-in-first-out algorithm. The basic rule of operation is typically that the test sample that has been waiting the longest across the reactor cores  114  is selected for evaluation next. However, if there is a long purge delay associated with that particular test sample, and another one of the queued experiments can be performed before the delay elapses, the other test experiment may be implemented first.  
         [0078]     Another embodiment of this invention pertains to an algorithm for queuing test sample experiments. One example of a flow diagram of such an algorithm is illustrated in  FIG. 11 .  
         [0079]     As shown, at step  1110  of the flow diagram illustrated in  FIG. 11 , spectrometer control module  612  calculates the length of time that each test sample has been waiting to be analyzed. At step  1112 , the sample that has been queued the longest is determined. At step  1114 , module  612  determines whether any of the test samples that are waiting to be analyzed can be implemented in less time than the delay associated with the test sample that has been queued the longest. If so, that sample is selected as the next test sample to be analyzed at step  1116 . If there is not another test sample that can be analyzed within the delay time associated with the test sample that has been queued the longest, the test sample that has been queued the longest is selected for testing at step  1118 . At step  1120 , reactor core selector valve  128  is set to route the reaction product from the appropriate reactor core. At step  1122 , spectrometer control module  612  determines if the appropriate delay time associated with purging gas feed lines  127  has elapsed. If so, at step  1124 , module  612  communicates to spectrometer interface server  630  to begin implementing the queued test experiment.  
         [0080]     Referring back to the specific block diagram illustrated in  FIG. 6 , control computer  130  further comprises transfer lines heater control module  614 . Transfer lines heater module  614  is responsible for controlling the heating of lines  127  leading out of the reaction zones to detector  126 . For certain uses, it may be desirable to maintain transfer lines  127  heated to at least a minimum temperature in order to prevent condensing of the reaction flow on its way from reaction zones  116  to detector  126 . Transfer lines heater control  614  can be configured to operate with heating element to bring the transfer lines up to, and/or maintain, a desired temperature or temperature profile.  
         [0081]     Again referring back to the specific block diagram illustrated in  FIG. 6 , detector computer  132  comprises spectrometer interface server  630 . Spectrometer interface server  630  is responsible for receiving requests to implement spectrometer screenings from spectrometer control module  612  and communicating with detector  126  to physically implement the request. Spectrometer interface server  612  can also be configured to relay the readings from detector  126  back to spectrometer control module  612 .  
         [0082]     Referring once again to  FIG. 6 , data archive computer  134  comprises archive database  640 . Archive database  640  is responsible for maintaining an archive of the screening tests that have been performed. Accordingly, as test samples are analyzed, the data is archived in archive database  640  for later retrieval and analysis.  
         [0083]     As stated above, the preferred configuration of the high throughput systems and analytical methods disclosed herein depends, in part, of the desired needs and objectives of the end user. Those skilled in the art will, however, be able to design such preferred systems and methods after reading this disclosure. Some examples of certain optional/preferred embodiments of the high throughput systems and analytical methods disclosed herein are set out below.  
         [0084]     Specifically, in certain preferred embodiments, the reaction product produced in the high throughput system is not injected into a mobile-phase detector. Instead, once the desired reaction product sample is selected, the entire amount of the sample passes directly through the detector. In this embodiment, no separate mobile phase is necessary or utilized.  
         [0085]     In other preferred embodiments of the high throughput systems disclosed herein, a sampling probe is not used to remove and transport a reaction product sample to a detector.  
         [0086]     In still other preferred embodiments, a selection valve is used to select a single stream of a reaction product sample to be sent to the detector. In this preferred process, a sampling valve which diverts a portion of the reaction product flow of the single stream to the detector and returns the non-diverted flow to a waste stream via a return line is not utilized. Instead, in this embodiment, the high throughput system directs the entire selected stream to the detector.  
         [0087]     In yet other preferred embodiments, the high throughput system utilizes a valve to select the desired reaction product stream. That valve, however, does not provide selective fluid communication between an inert fluid source and flow restrictors since an inert purge fluid is not used.  
       EXAMPLES  
       [0088]     Examples 1-3 demonstrate certain aspects of the flexibility of the present high throughput system. In each example, different, multiple catalyst compositions are evaluated in separate reactor block experiments under different reaction conditions.  
         [0089]     The catalyst samples were prepared by traditional methods to obtain granules of 10 to 20 mesh fraction. The granules are loaded to PYREX® reactor tubes (i.e. reaction zones) of specified dimension: length=11.6 cm, outer diameter=6.3 mm, and wall thickness=1.2 mm. The tubes contained a glass wool plug to support the catalyst bed. The reaction zones were loaded by height with nominal catalyst bed height being 4 cm.  
         [0090]     The analysis system consisted of three reactor cores, each containing a reactor core that has eight reaction zone positions. Position one in each reactor core was reserved for a blank tube used to obtain a background spectrum for effluent gas analysis of the remaining reaction zone samples. Accordingly, seven catalysts were analyzed in each reactor core run. Analysis of the effluent gas was by a single infrared spectrometer. Requests for analysis and rate of sampling was determined by the control computer in accordance with the present invention.  
         [0091]     Although it may be varied, the reactant feed composition was fixed at 1.0 mol % propane in air saturated with water at ambient conditions for each reactor core experiment. Residence time was varied from sample-to-sample by changing the reactant feed gas flow rate over the range of 5 ml/min to 20 ml/min. This corresponded to a range of residence time on a normal 4 cm sample of approximately 3 to 12 seconds. For purposes of the present examples, evaluation conditions were programmed for 3 seconds residence time.  
         [0092]     Temperature profiles were controlled at the reactor core and were defined by a designated ramp rate and dwell time. A total of 5 ramp and dwell segments could have been programmed for a given reactor core. Maximum reactor temperature was limited to 400° C. For purposes of the present examples, a ramp from 200° C. to 300° C. at 5° C./minute followed by a ramp from 300° C. to 400° C. at 1° C./minute with a 5 minute dwell between steps was performed for each sample. Each sample was analyzed at different temperatures.  
         [0093]     In the following examples, each catalyst was prepared individually. Catalyst samples of common composition are distinguished from one another by differences such as calcination temperatures and calcination atmospheres as indicated. The samples were evaluated concurrently as grouped in three separate reactor core runs. The results tabulated include the temperature at which the sample was analyzed, the percent of propane feed converted to any other product (Conv.), the percent of propane feed converted to carbon monoxide or carbon dioxide (COx Yield), percent of propane feed converted to acrylic acids (AA Yield), the percent of converted propane that form acrylic acids (AA Select), composition of the catalyst, and the calcination temperature and atmosphere used to prepare the catalyst.  
       Example 1  
       [0094]    
       
         
               
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
               
             
           
               
                   
                   
               
               
                   
                   
               
               
                   
                 Temp 
                   
                 COx 
                 AA 
                 AA 
                   
                   
               
               
                   
                 (° C.) 
                 Conv. 
                 Yield 
                 Yield 
                 Select 
                 Composition 
                 Calcination Process 
               
               
                   
                   
               
             
             
               
                   
               
             
          
           
               
                 A 
                 362 
                  9% 
                  5% 
                 1% 
                 11% 
                 Mo 1.0 V 0.3 Te 0.23 Nb 0.15   
                 550° C./Nitrogen 
               
               
                 B 
                 365 
                  7% 
                  4% 
                 1% 
                 14% 
                 Mo 1.0 V 0.3 Te 0.23 Nb 0.15   
                 575° C./Nitrogen 
               
               
                 C 
                 392 
                 25% 
                 21% 
                 0% 
                  0% 
                 Mo 1.0 V 0.3 Te 0.23 Nb 0.15   
                 600° C./Nitrogen 
               
               
                 D 
                 392 
                 22% 
                 15% 
                 4% 
                 18% 
                 Mo 1.0 V 0.3 Sb 0.25 Nb 0.10   
                 575° C./Nitrogen 
               
               
                 E 
                 370 
                 41% 
                 38% 
                 1% 
                  2% 
                 Mo 1.0 V 0.3 Sb 0.25 Nb 0.10   
                 600° C./Nitrogen 
               
               
                 F 
                 395 
                 39% 
                 37% 
                 0% 
                  0% 
                 Mo 1.0 V 0.3 Se 0.23 Nb 0.125   
                 500° C./Nitrogen 
               
               
                 G 
                 340 
                 36% 
                 34% 
                 1% 
                  3% 
                 Mo 1.0 V 0.3 Se 0.23 Nb 0.125   
                 500° C./Nitrogen 
               
               
                   
               
             
          
         
       
     
       Example 2  
       [0095]    
       
         
               
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
               
             
           
               
                   
                   
               
               
                   
                   
               
               
                   
                 Temp 
                   
                 COx 
                 AA 
                 AA 
                   
                   
               
               
                   
                 (° C.) 
                 Conv. 
                 Yield 
                 Yield 
                 Select 
                 Composition 
                 Calcination process 
               
               
                   
                   
               
             
             
               
                   
               
             
          
           
               
                 A 
                 382 
                 51% 
                 26% 
                 27% 
                 54% 
                 Mo 1.0 V 0.3 Te 0.23 Nb 0.125 In 0.01   
                 600° C./Nitrogen 
               
               
                 B 
                 382 
                 52% 
                 26% 
                 29% 
                 57% 
                 Mo 1.0 V 0.3 Te 0.23 Nb 0.125   
                 600° C./Nitrogen 
               
               
                 C 
                 362 
                 49% 
                 24% 
                 27% 
                 56% 
                 Mo 1.0 V 0.3 Te 0.23 Nb 0.125 In 0.005   
                 600° C./Nitrogen 
               
               
                 D 
                 402 
                 20% 
                 16% 
                  0% 
                  0% 
                 Mo 1.0 V 0.3 Sb 0.15 Ga 0.03 Nb 0.1   
                 575° C./Nitrogen 
               
               
                 E 
                 392 
                 25% 
                 14% 
                  9% 
                 36% 
                 Mo 1.0 V 0.3 Sb 0.15 Ga 0.03 Nb 0.051   
                 600° C./Nitrogen 
               
               
                 F 
                 369 
                 62% 
                 43% 
                 17% 
                 27% 
                 Mo 1.0 V 0.3 Te 0.23 Nb 0.11   
                 600° C./Argon 
               
               
                 G 
                 361 
                 49% 
                 25% 
                 28% 
                 58% 
                 Mo 1.0 V 0.3 Te 0.23 Nb 0.125   
                 575° C./Nitrogen 
               
               
                   
               
             
          
         
       
     
       Example 3  
       [0096]    
       
         
               
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
               
             
           
               
                   
                   
               
               
                   
                   
               
               
                   
                 Temp 
                   
                 COx 
                 AA 
                 AA 
                   
                   
               
               
                   
                 (° C.) 
                 Conv. 
                 Yield 
                 Yield 
                 Select 
                 Composition 
                 Calcination process 
               
               
                   
                   
               
             
             
               
                   
               
             
          
           
               
                 A 
                 400 
                 15% 
                 13% 
                 1% 
                 7% 
                 Mo 1.0 Sn 0.3 Sb 0.15 Nb 0.05   
                 600° C./Air 
               
               
                 B 
                 401 
                  2% 
                  2% 
                 0% 
                 0% 
                 Mo 1.0 Sn 0.3 Sb 0.15 Nb 0.05   
                 600° C./Argon 
               
               
                 C 
                 401 
                 95% 
                 88% 
                 1% 
                 1% 
                 V 1.0 Sb 1.4 Sn 0.2 Ti 0.1   
                 600° C./Argon 
               
               
                 D 
                 401 
                 26% 
                 26% 
                 0% 
                 0% 
                 V 1.0 Sb 1.4 Sn 0.2 Ti 0.1   
                 600° C./Nitrogen 
               
               
                 E 
                 401 
                 49% 
                 45% 
                 1% 
                 2% 
                 Mo 1.0 V 0.3 Sb 0.25 Nb 0.15   
                 600° C./Nitrogen 
               
               
                 F 
                 384 
                 34% 
                 24% 
                 9% 
                 26%  
                 Mo 1.0 V 0.3 Sb 0.15 Nb 0.05   
                 575° C./Nitrogen 
               
               
                 G 
                 401 
                 −1% 
                  0% 
                 0% 
                 0% 
                 Empty tube 
                 not applicable 
               
               
                   
                   
                   
                   
                   
                   
                 (blank position) 
               
               
                   
               
             
          
         
       
     
         [0097]     The above data provides those skilled in the art with a significant amount of valuable data. Once the optimal catalyst is selected, then the system can be employed to identify the optimal reaction conditions.  
         [0098]     Thus, the various embodiments of this invention provide methods and systems for high-throughput analysis of catalysts. According to an aspect of the invention, catalysts can be simultaneously analyzed using different reaction conditions. This provides for great flexibility and improved speed in the analysis process.  
         [0099]     While the invention has been described and illustrated with reference to specific embodiments, those skilled in the art will recognize that modification and variations may be made without departing from the principles of the invention as described above and set forth in the following claims. Accordingly, reference should be made to the appended claims as indicating the scope of the invention.