|Title of Invention||
A VISUAL MELTING RANGE APPARATUS
|Abstract||A Visual melting Range Apparatus is a micro controller based instrument comprising of a box type enclosed furnace with flat top surface for placing the sample; a fan is provided at the base of furnace for cooling the same, A CCD camera is vertically placed on the top of the furnace; a reflector lamp is provided angularly at 45º on the sample with controlled brightness; a video moniter is also provided to view the clear image of the sample; the entire operations are controlled by the central processing unit and the printer provides the necessary prints of calibration and accurate, precision and repeatable results.|
|Full Text||FORM 2
THE PATENTS ACT, 197® (39 of 1970)
COMPLETE SPECIFICATION (See Section 10)
A VISUAL MELTING RANGE APPARATUS
LABINDIA INSTRUMENTS PVT. LTD. of 201, NAND CHAMBERS, L. B. §. MARG, NEAR VANDANA CINEMA, THANE -400 602 MAHARASHTRA, India, INDIAN Company
The following specification particularly describes the
nature of the invention and the manner in which it is to be
performed s - A ^."^ ±S*
A VISUAL MELTING RANGE APPARATUS Field of Invention:
The invention relates to a micro processor based melting range apparatus for accurately measuring the physical appearance of the sample with reference to temperature.
Determination of melting point of a chemical is a routine requirement of chemical industry. Identification and purity of the product can be determined by the studying the melting point oi the substance and hence meJting point determination becomes a method of prime importance to the chemical industry.
The following conventional methods and respective instrumentation are being used:-
(1) Silicon Bath Method: Capillary Tube in Liquid Bath.
Traditionally the melting point is determined by suspending the capillary filled with sample in an oil bath. The oil is taken in a bath or Thiel"s Tube. The choice of the liquid depends on the range of melting temperature. Paraffin oil or silicon oils are normally used for this purpose. A dry substance is finely powdered and put into a capillary tube fused at one end so that the filing level is approximately 3mm. The thermometer along with the capillary tied with it is suspended in the oil bath.
The bath is gradually heated so that the temperature rise is approximately 2°C per minute. The oil is stirred with the help of stirrer and the sample is observed as the temperature rises. During the determination of the melting point, the temperatures are recorded at the beginning of the liquification and after complete liquification of the sample. Starting and ending temperatures of this process give the melting range of the substance.
(2) Kofler Hot Bench method: Kofler Hot Bench is a melting point apparatus built into
a bench form a stainless steel plate of 40 mm width and 360 mm long. The plate encloses
composite materials, which are in contact with the bottom surface. The materials are
heated from one end with controlled constant voltage heaters. The heat is transferred uniformly and longitudinally. Temperature gradient is achieved on the plate from 250°C to 50"C
Sample is sprinkled on the top surface along the length of the plate. A sharp line defines the molten and unmolten state of the sample.
A marker runs along one side of the plate with a calibrated scale and can pinpoint the melting point with an accuracy of + 2°C.
(3) Capillary method with optical sensing : Though this method gives very accurate results, it has limitations. In this method the samples, which become transparent on melting could only be detected. It is not possible to take the melting point of coloured substance and the substances, which decomposes on heating.
All the above methods and the instruments used have their own limitations for accuracy, repeatability and precision. These instruments do not have documentation facilities. They also create lot of environmental problems.
The instrument under patent has a number of unique features and also fulfills the following objectives:-
1. Melting range determination with sample prepared by slide system or capillary method.
2. High standard of accuracy, precision and repeatability.
3. Automatic detection rules out the human error.
4. Flexibility (versatility) for all types of samples (coloured powders, plastics, threads, etc.)
5. Calibration facilities with authentic traceable samples (assurance of results) (fig. No.5)
6. Magnified view of the melting process on a screen.
7. Graphical presentation and report printing for Good Laboratory Practices (GLP) requirement.
8. Easy to handle, safe and non-hazardous.
9. No pollution (no environmental hazards).
VISUAL MELTING RANGE APPARATUS - The new instrument is a micro-controller based unit comprises of following main parts:-
1. Heating Furnace
2. Flat Surface for placing the sample
3. Cooling Fan
4. Reflector Lamp
5. CCD Camera
6. Video Monitor
7. Electronic Control Unit
Figure 1 is a schematic diagram of the New Visual Melting Range Apparatus.
Figure 2 is a block diagram of the New Visual Melting Range Apparatus.
Figure 3 is an electronic circuit diagram of the New Visual Melting Range Apparatus.
The invention will now be described with reference to Fig. 1 to 6 in accompanying drawing.
Referring to Fig.l, basic unit of the instrument consists of a newly designed furnace (1) which has flat surface (2) for placing the sample. A cooling fan (3) is provided at the base for cooling the furnace. A sample (4) can be mounted on the flat surface of furnace. A CCD Camera (5) is vertically mounted on the top of the furnace. A reflector lamp (6) is adjusted angularly at 45° on the sample. A reflector lamp and camera are housed in camera housing (7). A video monitor (8) is also provided to see the clear image (9) of the sample on the screen. A central processing unit (10) controls the entire operation of the
instrument. A CPU has digital LCD display and keyboard for operation. A printer is connected to controller for result printouts and graphs.
Referring to Fig. 2, the Block Diagram of circuitry shows the temperature sensor and photo sensor with their amplifiers, which are monitored by CPU board, CPU Board is connected with power supply, LCD display, keyboard. CPU provides brightness control output to lamp driver for correct brightness of lamp. CPU also provides output to heater driver for temperature control of furnace through heater. CPU controls CCD Camera to provide for clear view of sample on the video monitor. A printer output is provided for printer connection.
Referring to Fig. 3, the electronic circuit diagram shows the connectivity of various electronic components used in new Visual Melting Range Apparatus.
Run No, : 1 Sample Hams i VANILLIN Sample Mo, si
X Axis Scale 22.0 L.units/div
Y Axis Scales 0,519 0C/div
Start Temp ; 81,90C
Start Temp. : 81.9"C End Temp. : 83.0°C
M.P. : 82.1 °C .
Inst. Calibrated on 13/06/2001
Report printed -14:43:21 16/06/2001 Analysis done on LABINDIA MR-Vis.
Visual Melting range apparatus is the latest state of the art micro-controller based instrument for determining Melting Range of white as well as coloured samples in powdered form.
Around 5mg of sample is uniformly spread on a glass slide and covered with a coverslip. The slide is then placed on a specially designed uniformly heated round furnace and subjected to heat as per the heating rate specified by the user.
A magnified image of the sample can be observed on a video monitor screen via a CCD camera. The effect of heat on the sample can be clearly seen. The change in physical appearance of the sample with reference to temperature is recorded and the start of melting and end of melting are determined automatically. This automatic detection of start and end of melting can be easily verified by observing the melting process on the video screen.
A representation of the entire melting process in the forms of a graphics printout is available for authentication as shown. This instrument also has a manual operation facility to lock the start of melting and end of melting. In Heat and Cool mode the start temperature of melting as well as solidification temperature of sample can be locked manually.
The apparatus also can be used for the conventional capillary method by simply attaching capillary conversion accessory.
BENEFITS OF INVENTION OVER CONVENTIONAL
FEATURES CONVENTIONAL INVENTION
1) Clarity in observation of melting process Vision is not clear Very high quality of clarity in vision Resolution can be enhanced with colour monitor
2) Automatic detection of start and end of melting. Not possible Detection is with human eye, human error possible Automatic detection hence no human error
3) Conventional (Glass capillary method) Possible
4) Requirement of calibrated thermometer Must Not required
5) Accuracy, precision & repeatability Poor, depends upon the judgement of operator Since detection is automatic very high standard of accuracy, precision & repeatability
6) Report printing & Graphical presentation of melting process for documentation Not possible Possible, (Unique feature)
7) Calibration with authentic sample for system suitability Not possible Possible (unique feature) fulfill GLP requirements
8) Safety, Hazard Not safe, Hazardous, use of oil is vulnerable for fire and accidents No oil bath hence very safe No hazards
9) Working process & environment Messy, Cumbersome, Evolution of oil fumes during heating process. pollute environment Easy to work, no oil hence no fumes, clean environ
10) Flexibility of sample M.P. of mainly solids in powder form is possible No restriction on samples besides normal samples, samples like fibers, plastics waxes can also can be done.
11) Thermo photometric analysis Not possible Can be enhanced for thermo photometric analysis
SPECIFICATION COMPARSION BETWEEN NEW AND CONVENTIONAL
1) Temperature control
Micro-controller based Precise control
Automatic and manual
3) Temperature range
4) Visual Image
5) Heating Rates
7) Cooling time
8) Accuracy &
Ambient to 300°C
Simple magnifier lens
Mercury Thermometer lesser resolution
Poor accuracy User dependent
One end sealed capillary
Ambient + 5°C to 350°C Extended range
10X Magnified Image on to the Video Monitor via CCD Camera
Program selective-precise 0.2, 0.5, 1, 2, 3, 6, 12°C /
LCD Digital display -high resolution (0.1 °C)
Faster cooling- More sample analysis
Reproducibility Automatic and of high standard. Slide & Cover slip as well as one end sealed capillary - versatile - USP/BP reqd.
10) Temperature sensor
11) Data storage
12) Sample Test Program
Not possible Not Possible
Solid state sensor - RTD PT 100.
Non Volatile Memory 20-test program
13) Report generation
14) Heating system
Oil bath with immersion heater - fragile, delicate and unsafe.
Through printer - GLP compliance
Round heat conductive metal block with built-in heating element and sensor - rugged and safe.
|Indian Patent Application Number||607/MUM/2001|
|PG Journal Number||13/2008|
|Date of Filing||28-Jun-2001|
|Name of Patentee||LABINDIA INSTRUMENTS PVT. LTD.|
|Applicant Address||201, NAND CHAMBERS, L. B. S. MARG, NEAR VANDANA CINEMA, THANE-400 602,|
|PCT International Classification Number||G01N25/04|
|PCT International Application Number||N/A|
|PCT International Filing date|