Auto Density Measurement System - Ray
Contents
1. 7 Using the Columns Automatic Measuring System 8 e Column Calibration 8 e Sample Density 6 9 Check a Calibrated 9 Errors dueto Air 10 Use and Care of Density Floats 10 Correction 10 Care of the Density Column 1 11 Solutions and Densities 2 2 12 Densities of Aqueous Organic Solutions Table 13 pO 1 Fs Ts 11 14 e Wiring Diagram 240 00 14 Density Gradient Column e Wiring Diagram 110 Volts wecsctdcnsccntoatoentccntvnstesabinctientucetmessianticnmectwastnaiie 15 8 e 16 dines cede diesem nema 17 Density Gradient Column User Manual Thank you for purchasing the Ray Ran Au2. 800 1700 1600 1990 1990 2190 2180 2890 1600 2890 12 Density Gradient Column Densities of Aqueous Organic Solutions Ethyl Alcohol C2H3 13 Density Gradient Column 48 593 211 91823 429 028 621 207 98 399 79975 547 117 684 247 77806 49 379 91995 604 208 90805 396 89979 99 094 670 243 78814 382 77946 507 100 79784 368 78934 506 075 641 203 14 Approved warp 2 4 i IONN EE pa MATERIAL Annodise Electro Plate COMMENTS Live ciruit Neutral circuit 12V circuit Elsctronic amp PRT circiut FOR TOLERANCES AND SYMBOLS SEE DRAWING OFFICE CODE OF PRACTICE ert Column DO NOT SCALE We TEST EQUIPMENT LTD wiring Diagram DRAWN BY PR ISSUE No 3 DATE DWG No 10 05 2006 DEA WD 240V Density Gradient Column Drawing Approved O 19 i UL MATERIAL PROCESSES Spray Heat Treat Chem Black Annodise Electro Piate COMMENTS Live ciruit Neutral circuit DESCIPTION MM Density Column unless stated DO NOT SCALE wiring Diagram 2 10 05 2006 DGA WD 110v D
3. e Repeat the procedure to read sample densities from another column Check a calibrated column The apparatus has the capability to check a calibrated column for errors which may cause the gradient to break down and become un reliable This may be due to a change in atmospheric conditions or simply the amount of time that the column has been in use To check a calibrated column e Display reads lt Main Menu gt lt Calibration gt Press lt Select gt Display reads lt Which Column gt lt Column gt Rotate the dial on the front display to select the column B C or Abort Press lt Select gt Display reads lt Calibration Menu gt lt Calibrate Columns Rotate the dial on the front display until the display reads lt Check Calibration gt Press lt Select gt If the wrong column has been selected or you wish to exit the procedure rotate the dial until lt Abort gt is displayed e Display reads lt Calibration Check gt lt Float No gt and lt Density gt Move the microscope viewer to float 1 When the microscope is in range of the floats density the apparatus Density Gradient Column will Beep The display will read lt Float 1 gt followed by the float density Check the position of the float to see if its position is still relative to the density reading on the display If the float has moved then re calibration of the gradient will be required e return to the main menu select lt Exit gt Errors due to
4. the ambient temperature exceeds 20 C it is advisable to cool the water bath by connecting either a tap water supply or preferably a chiller system an option which can be supplied by Ray Ran to the cooling coil This will allow the temperature controller to work more effectively ensuring temperature accuracy within the column Reduce the ambient temperature of the bath to below 20 C using the chiller system and leave to stabilise Set the temperature controller to 23 C set point which will then go into control mode and keep the water bath at 23 C Low cost Chiller Units can be purchased from Ray Ran please contact for details amp quotations Filling Equipment The Pumped Filling Equipment is used to build a density gradient column over a required range by connecting 2 conical flasks which are secured to the apparatus by a Polycarbonate plate A screwed pinchcock is fitted for controlling the flow of liquid through silicone rubber tubes Density Gradient Column The filing system and the flask stirrer are turned on off using the switches located on the front of the electronics cabinet If the standard pumped filling system is to be used please follow the instructions in this manual If the microprocessor filling equipment is to be used instead of the pumped filling equipment please consult its own technical manual Filling a Gradient Column Mixing Liquids To build a density gradient column two solutions of suitable miscible liquids
5. Air A major source of errors in columns containing water is air absorbed in the solution forming bubbles on the floats and samples which can be very small and difficult to detect A cyclic movement of the floats or samples usually indicates the presence of small bubbles These air bubbles can be prevented by de gassing the two solutions before filling the column e Ethanol solutions should be de gassed by using a vacuum e Salt solutions should be de gassed by boiling If air bubbles form on the floats remove the float from the column This can be done using a long thin piece of wire with a ring at the end bent at right angles Once the float has been removed dip it in distilled water containing a few drops of liquid soap then return the float to the column Caution This must be done carefully so the gradient is not disturbed If the bubbles persist after re wetting the samples or floats the column should be built again taking the recommended precautions Use and Care of density Floats Calibrated Density Floats are manufactured from coloured soda lime glass No appreciable change in density has been recorded after several years use in water ethanol or hydrocarbon solutions If the floats are to be used in strong alkaline solutions it is advisable to periodically check one float by comparison with a float not used in a alkaline solution Alternatively Ray Ran can offer a re calibration service Although the floats come with a complete ca
6. RAHAN POLYTEST Product User Manual Advanced Auto Density Gradient Column Copyright C 1998 All Rights Reserved Issue 2 v1 05 Revised July 2007 RAY RAN TEST EQUIPMENT LTD Kelsey Close e Attleborough Fields Industrial Estate Nuneaton e Warwickshire e CV11 6RS e United Kingdom Tel 44 0 24 7634 2002 e Fax 44 0 24 7664 1670 E Mail polytest ray ran com Web Site http www ray ran com 1809001 S WCs E Certificate No 4915 www ray ran com POLYMER TEST EQUIPMENT FOR WORLD WIDE QUALITY CONTROL Density Gradient Column CONTENTS User 4 Description of the Apparatus 222 4 Lifting amp 2 2 4 11 4 8 5 lt 5 Setting the 5 5 5 Filling the Gradient Column 2 2 22 0202 4 1 6 e Mixing 6 e Filling the Column see ceive 6 Column Clearing
7. are needed 860cc of each liquid will be required Solution A should be a low density and solution B should be high density To calculate the densities needed to build a successful column first take into account the density range to be covered e Reduce the range from the lowest density required from solution A by 20 e Increase the range to the highest density of solution by 30 Example e Range required 0 90 1 00 e Solution A 0 90 20 0 88 e Solution B 1 00 30 1 03 The density of the solutions can be estimated with hydrometers standard dilution tables or with density floats the lowest float should sink steadily in solution A and the highest float should rise steadily in solution B A Table of suitable liquid systems and an Ethanol Water standard dilution table are include with this manual If a water based system is to be used it is advisable to de aerate the solutions after mixing by vacuum or gentle heating If the heating method is used it is important to note the suppliers recommendations and comments on fumes given off by the solutions Each solution must be mixed thoroughly PLEASE CONSULT THE MANUFACTURERS MATERIAL SAFETY DATA SHEETS MSDS WHEN USING CHEMICALS AND COSHH REQUIREMENTS Filling the Column Please ensure that the sweep baskets are placed into the test tubes before filling the glass tubes with your gradient liquid and that the cord is safely secured Empty the tube and rinse with alcoho
8. drop them into the column starting with the lowest density first then replace the rubber cap Leave the floats to reach equilibrium Once this has been achieved the gradient column can be calibrated Column Clearing Device The automatic column clearing device or sweep clears the density column of test samples and density floats without disturbing the gradient The device consists of a swivelled beam that is positioned over the glass test tubes with the basket line attached to the main line using a screw connector To operate the device attach a sweep basket to the main cord at the top of the swivel beam and turn on the switch located on Density Gradient Column the front panel of the electronics cabinet Use the up down switch to activate the sweep in the direction required The motor is automatically switched off when the mesh basket reaches the top and bottom of the tube To change from one basket to another the line will need to be unscrewed and secured to the top of the column tube so other baskets can be raised from the remaining tubes Please note that the baskets can only be changed between columns when they are at rest in the bottom of the test tube When a column is to be cleared attach the basket cord of the appropriate column to the clearing device and press the switch into the up raise position The device will rise slowly so the gradient is not disturbed When the basket reaches the top of the column it will automatically s
9. ensity Gradient Column ANGLE PROJECTION 60 RAVE RAIN TEST EQUIPMENT LTD DESCIPTION Pumped Filling System ick ISSUE No DWG No RR IBGA PFS Ray Ran Products and Services Raw Material Evaluation Code Product RR 5MBA Model 5MBA Melt Flow Indexer RR 5SA Model 5SA Melt Flow Indexer Model 5MPCA Melt Flow Indexer RR DGA 3 Column Density Gradient Apparatus RR BDA Apparent Bulk Density Apparatus RR ADV Adventurer Balance Readability 0 1mg 110 260g Capacity RR VOY Voyager Balance Readability 0 1mg 62 410 100g Capacity RR DIS Discovery Balance Readability 0 1mg 110 310g Capacity RR MB Moisture Balance Readability 0 1 0 05 0 01 110 35 45g Cap Sample Preparation Code Product RR TSMP2 Model 2 Test Sample Injection Moulding Apparatus RR HCP Hand Operated Test Sample Cutting Press RR PCP Pneumatically Operated Test Sample Cutting Press Auto Cycle Test sample Notching Cutter RR CNC Test Sample Profile Cutter RR CNC 2 Test Sample Profile Cutter Larger TSC Standard Test Sample Cutters Sample Testing Code Product RR HDV2 2 Station HDT Vicat Softening Point Apparatus RR HDV4 4 Station HDT Vicat Softening Point Apparatus RR HDV6 6 Station HDT Vicat Softening Point Apparatus RR TAA Th
10. ermal Ageing Apparatus RR LTB Low Temperature Brittleness Tester RR ESC Environmental Stress Cracking Apparatus RR FSL Unrestrained Linear Thermal Film Shrinkage Apparatus RR FSHP Hot Plate Film Shrinkage Apparatus RR IMT Universal Pendulum Impact Tester RR FWT Falling Weight Impact Tester RR FD Falling Dart Impact Tester RR ETT Advanced Elmendorf Tear Tester RR FT Static And Dynamic Friction Tester RR M Universal Tensile Tester Various Capacity D202 Digital Handheld Durometer B202 Analogue Handheld Durometer WS777 Analogue amp Digital Durometer Workstations 17
11. fore being placed in the column To aid identification samples from sheet material should be cut with a sharp blade into various shapes The time required for the samples to reach equilibrium vary with the type of sample Granules usually reach maximum density within one hour of immersion whereas thin films may require longer Several height sightings should be taken until the sample is stable The density can then be measured Display reads lt Main gt lt Calibration gt Rotate the dial until lt Test Samples gt is displayed then press lt Select gt Display reads lt Column gt Rotate the dial on the front display to select the active column you wish to read the sample densities from When the column has been chosen press lt Select gt e Display reads lt Sample 1 gt Move the microscope sight to the centre of the first sample and take the density reading from the display then select lt Next gt If the thermal printer has been activated the display will read lt Print gt instead of lt Next gt e Display reads lt Sample 2 gt Move the microscope sight to the centre of the second sample and take the density reading from the display then select lt Next gt e Repeat the procedure for all the samples you wish to measure e When you have finished taking your readings rotate the dial on the front panel until lt Exit gt is displayed Press the green button Display reads lt Main Menu gt lt Calibration gt
12. l and allow too dry Return the tube back into the water jacket and fit the plastic cap to the top of the tube and secure the tube in place with the tube clamp Insert the PTFE tube through the plastic cap and ensure the PTFE filling tube is at the bottom of the test tube Density Gradient Column Carefully place the PTFE stirrer bar into conical flask A the flask with 2 outlet holes and place the connected flasks onto the filling platform Connect the outlet of flask A to the inlet of the pump using the tubing supplied Connect the flared end of the PTFE filling tube to the longest length of tubing then connect the other end to the tubing to the outlet of the pump Close the nylon screwed pinchcock on the tube connecting the two flasks and the outlet tube of flask A Pour the low density solution A into flask A and the high density solution B into flask B Fit the retaining plate over the flasks to keep the flask secure before stirring the liquid Open the nylon pinchcock which connects the two flasks When hydrostatic equilibrium has been reached the stirrer should be switched on for a short period to allow the two solutions to mix in flask A before pumping begins Ensure all valves are in the open position and that the PTFE filling tube is situated within the test tube before the pump is switched on The filling rate depends on the density range of the column Wider ranges will require longer filling times The columns test tube wi
13. libration certificate it is advisable to record the colour markings diameter and density of each float in a register or log book to ease the identification process Do not use metallic measuring devices such as micrometers or vernier callipers to measure the floats unless of the plastic type Before the floats are put into the gradient column they should be wetted in the residue from the filling device or similar solution to prevent air bubbles Finger marks can make wetting the floats difficult If this is the case the floats should be cleaned with a suitable detergent solution After long periods of use the floats may become covered in a thin film of material from the samples This film can be removed by immersing the float in a diluted solution of nitric acid The floats should not be cleaned with paper towels or laboratory wipes as repeated rubbing can alter the floats density Correction Factor If the floats are used at temperatures other than 23 C a correction should be applied to obtain maximum accuracy The correction is obtained with the following equation Correction for 1 difference in temperature Float density at 23 C 0 000028 This equation is then applied as follows 10 Density Gradient Column Below 23 C Stated density of Float Correction for each C difference in temperature Above 23 C Stated density of Float Correction for each C difference in temperature Care of the Density Column Some
14. ll fill at a constant rate The mixture of fluids in flask A will become progressively more dense as the liquid enters from flask B It is important to leave the pump on until nearly all of the liquid has been pumped from flask A Once the graduated tube is full remove the plastic cap and the PTFE tube from the column Caution Turn the pump and stirrer off immediately as the flasks empty This will prevent air being pump into the column and destroying the gradient It is recommended that after use the filling equipment is flushed through with water to prevent hardening of the tubes The rate of mixing the fluid from Flask A to Flask B can be controlled by using the pinchcock located between the flasks The Rate of filling the test tube can be increase by turning the speed control switch located next to the filling pump Wide density ranges where there is a considerable difference between the two solutions will require a longer filling time to allow the solution to mix thoroughly in the stirrer flask The flow into the column is also affected by the density and viscosity of the solution If the ambient temperature is above or below 23 C and a supply of water is not available use the equation shown under the heading Use and Care of Density Floats to apply a correction factor to the density readings Once the test tubes have been filled with the correct density gradient wet the floats in de ionised water to remove air from the surface and
15. solutions can damage the Perspex water jacket and acrylic finishes It is therefore important that all spills are mopped up immediately The water jacket should not be cleaned with acetone or similar solvents which will cause stresses and cracking A mild detergent solution should be used for general cleaning More persistent stains and small scratches can be removed with an Aerosol Acrylic Polish After opening the pinchcock on the filling platform check the interconnecting tube for air bubbles these can be removed by momentarily lifting one flask After use disconnect the filling tube remove the flasks from the platform rinse them with water and allow to dry They should be stored in a safe place with the connecting tubes attached 11 Solutions and Densities Methanol Benzyl Alcohol Isopropanol water Isopropanol Diethylene Glycol Ethanol Carbon Tetrachloride Ethanol Water Toluene Carbon Tetrachloride Water Calcium Nitrate Water Potassium lodide Water Sodium Bromide Zinc Chloride Ethanol Water Carbon Tetrachloride 1 3 Dibrompropane 1 3 Dibrompropane Ethanol Bromide Ethylene Bromoform Carbon Tetrachloride Bromoform n octane Dimethylformahide Tetrachlorethane Ethyl lodide Methylene lodide Density Gradient Column 800 920 790 1000 790 1000 790 1590 790 1000 870 1590 1000 1450 1000 1600 1000 1600
16. ss hair select lt Add Float gt Caution Please ensure that the microscope has been moved to the appropriate float before selecting the lt Add Float gt button If this is not done the reading will not be stored and the calibration will have to be carried out again Enter the density of the float from the issued calibration certificate by rotating the dial on the front panel then select lt Enter gt e Display reads lt Float 2 gt lt Add Float gt To add another float move the microscope sight to the next float and select lt Add Float gt Rotate the dial on the front panel to the required density and select lt Enter gt e Repeat the procedure until all the used floats in the column have been entered into the microprocessor e When all of the floats have been entered rotate the dial on the front panel until the display reads lt End Cal gt then press the green button Density Gradient Column e Display reads lt Save Cal Data gt Press lt Select gt to save the calibration data to the microprocessor or rotate the dial the front panel to display lt Continue if more floats are to be added or lt Abort Cal gt to abort the calibration procedure e When lt Save Cal Data gt is selected the display will read lt Main Menu gt lt Calibration gt Repeat the procedure to calibrate the other columns if required Sample Density Readings When the column has been calibrated test samples should be thoroughly wetted be
17. to Density Gradient Apparatus Please read this manual before operation If you have any questions regarding the installation and operation of the equipment please contact Ray Ran for assistance Description of The Machine The Gradient Column Method accurately determines the density of small solid specimens in any form eg sheet film granule powder etc The glass test tube is filled with two miscible solutions The resulting mixture varies at a linear rate with the lowest density at the top of the tube and the highest density at the bottom Calibrated glass marker floats of precisely known densities are introduced into the column and sink to a point where the density matches that of the solution The apparatus uses a linear encoder to calibrate the gradient of the column This is achieved by focusing the optical microscope onto the centre of the calibrated float and entering the floats density value into the microprocessor A sample of unknown density is introduced to the column and allowed to reach equilibrium The linear encoder measures the samples position in the tube relative to the marker floats which is then displayed on the LCD its density Depending on the columns use or age the density distribution of the gradient can remain stable for up to 40 weeks For additional information refer to the test standard ISO 1183 Lifting amp Installation It is recommended The Density Column be lifted by two people and placed on a le
18. ube in place Caution Any graduated tubes left empty and not clamped will rise when the water jacket is filled and may cause a hazard Power Up When the machine is first turned on after filling the water jacket the display will read e lt Move sight to home position gt Move the microscope crosshead in an upward direction to the top rail until a beep can be heard When the beep sounds this means that the sight is in its home position Please note that this only has to be done when the power is first turned on The display will now read e lt gt lt Calibration gt See column calibration Thermal Printer If a Thermal Printer has been supplied with the Density Column simply connect the supplied RS232 data transfer cable from the printer to the RS232 socket located at the rear of the columns control box If the Thermal Printer has been supplied after initial installation of the apparatus you will need to configure the apparatus for printing mode To do this e When lt gt lt Calibration gt is displayed on the LCD press and hold the green button for 10 seconds lt Printer On gt will display briefly on the LCD Repeat the procedure to turn the printer off Setting the Temperature To set the required temperature of the jacket press the up down keys on the temperature controller Please allow 30 minutes for the temperature of the fluid inside the jacket to reach equilibrium Cooling Coil If
19. vel robust bench at a height that is suitable for the operator to take accurate measurements The apparatus should be shielded from direct sunlight to prevent algae growth within the column If the room temperature is above 23 C the column should be within reach of a mains water supply and waste or connected to a pumped cooling device Electrical Characteristics 240 50hz 110 60hz Please ensure that the mains cable plug is fitted into an electrical safety device before turning on the apparatus This Appliance Must Be Earthed Caution Please do not turn on apparatus until the water jacket has been filled with fluid as this may damage the water pump The water jacket may be filled from the top of the column through one of the test tube holes The use of de ionised water in addition to 100ml of ethylene glycol type antifreeze will keep the jacket clean and algae free The liquid should be Luke warm to reduce the risk of thermal shock and stress to the water jackets material Caution Please pay great attention to the water mark levels shown on the front of the main cabinet These levels are marked to show the water fill level of the jacket relative to the number of test tubes to be used Please do not fill above these levels as excess water may spill into the rear of the cabinet Density Gradient Column The test tube in which a gradient is to be built can be left in situ provided the tube clamp is holding the t
20. witch off Once the basket has reached the top remove the test samples and the density floats then return the basket to the bottom of the tube by pressing the switch into the down position Repeat the procedure to clear the remaining graduated tubes Using the Columns Automatic Measuring System Column calibration Caution Please do not attempt to calibrate the column until the water temperature has stabilised at 23 Deg C To use the column correctly you must calibrate the column by entering the float value reference into the microprocessor To do this ensure that the microscope sight is in the home position e Display reads lt Main Menu gt lt Calibration gt Press lt Select gt Display reads lt Which Column gt lt Column gt Rotate the dial on the front panel to select column B C or Abort If Abort is selected the display will default back to the main menu Once the column to be calibrated has been chosen press lt Select gt Display reads lt Calibration Menu gt lt Calibrate Column gt Press lt Select gt to calibrate the column or rotate the dial on the front panel to display lt Check Calibration gt or lt Abort gt Display reads lt Calibration Mode gt lt Float 1 gt lt Add Float gt Move the microscope sight to the centre of the first float The focus of the sight can be adjusted by rotating the knob at the side of the microscope When the centre of the float has been positioned against the microscope cro
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