Investigating different physical and/or chemical forms of materials

Abstract

Apparatus and a method are described for investigating polymorphs of a material, isomers of a material which allow different isomeric forms to be resolved, different hydrates/solvates and/or different salts of a material. The apparatus comprises an assembly ( 2 ) of reactor devices ( 6 ) arranged within a reactor body ( 8 ) which incorporates a heating/cooling block ( 10 ) and a stirrer block ( 12 ). A vessel support block ( 14 ) supports respective sample vessels ( 15 ) below each reactor device ( 6 ) for receiving material from the reactor devices. The apparatus includes a control unit ( 4 ) which includes a computer ( 16 ) which controls a robot for delivering materials to the reactor devices; a heating/cooling unit ( 18 ); a stirrer control unit ( 20 ); and a pressure unit ( 22 ) which controls the passage of material from the reactor devices ( 6 ) to the sample vessels ( 15 ).

1 . A method of investigating the crystal habit of a selected material, comprising: 
 (A) providing a plurality of receptacles;    (B) depositing a selected quantity of a selected initial material into each said receptacle,    (C) subjecting said initial material to a first series of selected treatments, having selected first treatment variables, to form a resultant material in each of said receptacles wherein said treatments are controlled by a computer; and    (D) analyzing said resultant material to determine the crystal habit thereof and generating crystal habit data related thereto.    
   
   
       2 . A method according to  claim 1  including associating said crystal habit data of each said resultant material with said treatment variables.  
   
   
       3 . A method according to  claim 2  including storing said associated crystal habit data and said treatment in said computer.  
   
   
       4 . A method according to  claim 1  wherein said computer is programmed to select said treatment.  
   
   
       5 . A method according to  claim 1  including subjecting said resultant material to a second series of selected treatments.  
   
   
       6 . A method according to  claim 5  wherein said second series of selected treatments is selected by said computer depending upon the crystal habit data of said resultant material.  
   
   
       7 . A method according to  claim 1 , wherein said first treatment variables include solvent variables.  
   
   
       8 . A method according to  claim 7 , wherein said solvent variables are selected from one or more of the following: 
 (A) a first solvent variable relating to the number of solvents used for preparing said resultant material from said initial material;    (B) a second solvent variable relating to the timing of the addition of the solvent or solvents into said receptacle;    (C) a third solvent variable relating to the amount of a solvent or solvents used in a treatment; and    (D) a fourth solvent variable relating to the identity of a solvent or solvents used.    
   
   
       9 . A method according to  claim 8 , wherein at least two of said solvent variables are varied in a single series of experiments and/or in multiple series of experiments.  
   
   
       10 . A method according to  claim 8 , wherein the implementation of said solvent variables is under the control of said computer.  
   
   
       11 . A method according to  claim 1 , wherein said first treatment variables includes a duration variable wherein said initial material is treated for a selected duration.  
   
   
       12 . A method according to  claim 1 , wherein said first treatment variables includes a heating variable wherein said initial material is subjected to a heating means.  
   
   
       13 . A method according to  claim 12 , wherein said heating variable is selected from one or more of the following: 
 (A) a first heating variable relating to the time of operation of said heating means;    (B) a second heating variable relating to the duration of operation of said heating means; and    (C) a third heating variable relating to whether operation of said heating means is continuous or in stages.    
   
   
       14 . A method according to  claim 1 , wherein said first treatment variables includes a cooling variable wherein said initial material is subjected to a cooling means.  
   
   
       15 . A method according to  claim 1 , wherein said first treatment variables includes an agitation variable wherein said initial material is subjected to agitation.  
   
   
       16 . A method according to  claim 15 , wherein said agitation variable is selected from one or more of the following: 
 (A) a first agitation variable relating to the time of operation of an agitation means for agitating material;    (B) a second agitation variable relating to the duration of operation of said agitation means;    (C) a third agitation variable relating to whether operation of said agitation means is continuous or in stages; and    (D) a fourth agitation variable relating to the rate of operation of said agitation means.    
   
   
       17 . A method according to  claim 1 , wherein a temperature profile is defined for each said receptacle and wherein temperature profile data relating thereto is stored in said computer.  
   
   
       18 . A method according to  claim 1  wherein said receptacles include a porous member that is porous to fluids but not to said initial material.  
   
   
       19 . A method according to  claim 1  including the application of pressure to said receptacles during said first series of selected treatments.  
   
   
       20 . A method according to  claim 19  wherein application of said pressure is controlled by said computer.  
   
   
       21 . A method according to  claim 1  wherein said first series of selected treatments includes the addition of liquid to at least one of said receptacles and wherein said liquid is removed from said receptacles and analyzed.  
   
   
       22 . A method according to  claim 1  including analyzing said crystal habit data to identify 
 (A) polymorphs of said initial material;    (B) hydrates/solvates of said initial material; or    (C) salts of said initial material.    
   
   
       23 . A method according to  claim 1  wherein said initial material is subjected to a range of potential salt forming materials and wherein said resultant material formed thereby is a salt of said initial material.  
   
   
       24 . A method according to  claim 24  wherein said resultant material is in a crystalline form.  
   
   
       25 . A method to determine the crystal habit of a selected material thereby to investigate polymorphs, hydrates/solvates, or salts of said selected material, comprising: 
 (A) providing a plurality of receptacles;    (B) depositing a selected quantity of a selected initial material into each said receptacle,    (C) subjecting said initial material to a first series of selected treatments, having selected first treatment variables, to form a first resultant material in each of said receptacles wherein said treatments are controlled by a computer; and    (D) analyzing said first resultant material to determine the crystal habit thereof; and    (E) generating first crystal habit data from said analysis of said first resultant material.    
   
   
       26 . A method according to  claim 25  including subjecting said first resultant material to a second series of selected treatments, having selected second treatment variables, to form a second resultant material.  
   
   
       27 . A method according to  claim 26  wherein said second treatment variables are selected by means of a computer.  
   
   
       28 . A method according to  claim 26  wherein said second treatment variables are different from said first treatment variables.  
   
   
       29 . An investigation apparatus for investigating the crystal habit of an initial material wherein said initial material is subjected to selected treatment conditions thereby to investigate polymorphs, hydrates/solvates, or salts of said initial material, said investigation apparatus comprising 
 (A) a reactor assembly including 
 (1) a reactor body having an internal region; and  
 (2) an array of receptacles disposed in the internal region adapted for receiving a selected quantify of the initial material to be investigated; and  
   (B) a control unit in communication with said reactor assembly and including a computer operative to control said selected treatment conditions.    
   
   
       30 . An investigation apparatus according to  claim 29  wherein said reactor assembly includes a heating/cooling block operative to subject a selected temperature to said initial material in said receptacles.  
   
   
       31 . An investigation apparatus according to  claim 29  wherein said reactor assembly includes a stirrer block operative to agitate said initial material in said receptacles.  
   
   
       32 . An investigation apparatus according to  claim 29  wherein said reactor assembly includes 
 (A) a plurality of collection vessels located in the interior region of said reactor assembly, each said collection vessel being in fluid communication with one of said receptacles; and    (B) a collection vessel support block adapted to support said plurality of collection vessels.    
   
   
       33 . An investigation apparatus according to  claim 29  wherein said control unit operative to selectively vary the temperature during treatment of said initial material.  
   
   
       34 . An investigation apparatus according to  claim 29  wherein said control unit includes a stirrer control unit operative to selectively agitate said initial material during treatment thereof.  
   
   
       35 . An investigation apparatus according to  29  wherein said control unit includes a pressure unit operative to control a selected pressure during treatment of said initial material.  
   
   
       36 . An investigation apparatus according to  claim 29  where said receptacles are associated with means for condensing vapour for reducing loss of material therefrom by evaporation.  
   
   
       37 . An investigation apparatus according to  claim 36  wherein said receptacles include a porous member adapted to support said initial material when deposited therein, said porous member being porous to fluids but not to said initial material.  
   
   
       38 . An investigation apparatus according to  claim 37  including a pressure means operative to apply pressure within the internal region thereby to restrict the passage of fluids from said receptacles under gravity.  
   
   
       39 . An investigation apparatus according to  claim 38  wherein said pressure means is controlled by said computer.  
   
   
       40 . An investigation apparatus according to  claim 29  including 
 (A) a material supply means adapted to contain selected materials to be deposited into said receptacles; and    (B) a delivery means for transporting said selected materials from said supply means to a selected one of said receptacles.    
   
   
       41 . An investigation apparatus according to  claim 29  including an input means for inputting analytical data relating to material produced after treatment of said initial material into said computer, wherein said computer is programmed to analyse data input into it and determine variables to be used in a subsequent investigation on the same initial material, using said apparatus.  
   
   
       42 . An investigation apparatus according to  claim 29  for making a library of products.  
   
   
       43 . An investigation apparatus according to  claim 29  for effecting automatically a multiplicity of treatments of an initial material which treatments differ in at least one experimental variable.