Tap Density Apparatus Calibration, Purpose :
Tap Density Apparatus Calibration, The purpose of this SOP is to describe the operation, calibration and cleaning of Bulk density apparatus (Model: Electrolab ETD-1020) used for the Bulk density test of raw materials in the quality control laboratory at XX Pharmaceuticals Limited.
Tap Density Apparatus Calibration, Scope :
This procedure is applicable for Bulk density apparatus (Model: Electrolab ETD-1020), installed in the quality control laboratory of XX Pharmaceuticals Limited.
Definitions / Abbreviation:
[][]SOP: Standard Operating Procedure.
[][]QC: Quality Control.
[][]USP: United State Pharmacopoeia
Responsibility
Executive, QC
[][]To ensure that this procedure is followed.
[][]To maintain the records properly as per SOP.
Manager, Quality Control
[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.
[][]Schedule calibration of the instrument at the defined intervals.
Head of Quality Assurance
[][]Approval of the SOP.
[][]To ensure the overall implementation of the SOP.
Procedure:
Precaution(s):
[][]The equipment should not be set near to room heating equipment or direct sunlight.
[][]Use mask, gloves and safety goggles during handling the instrument.
[][]Disconnect the power supply before cleaning of the instrument.
[][]Prior to use, user must ensure that equipment is calibrated.
[][]Avoid any dust gathering on the bearings.
[][]Do not lubricate the bearings.
[][]Keep the shaft of the cylinder holder and the tip of the cylinder holder clean.
[][]Do not press the cylinder holder when the tapping base of cylinder holder is not touching the anvil.
[][]Place the cylinder in the holder only when the holder is placed on the anvil.
Operation:
[][]Ensure that working area is clean.
[][]Connect power cord of the instrument to mains and switch ‘ON’ the instrument.
[][]Instrument will initialize itself and the display will flash and show the start up screen.
[ELECTROLAB TAP DENSITY
ETD-1020 VER 3.0
[][]Set the mode of operation as USP or USER using the ‘DIGIT SCROLL’ key on the front panel.
[][]In USP mode, instrument will stop after every program and validation; report is available at the end of test.
[][]In USER mode, instrument will stop after the set tap value and no validation and result screen will be available. This method is used only when no. of taps are specified in the method.
[][]Press the ‘METHOD’ key to toggle between USP-I and USP-II method and select the required method.
[][]Press ‘SET’ key to set the test parameter.
[][]Display reads
[TAP COUNT 1: # # # # ▲▼◄
SET : EXIT / Enter : SCROLL
[][]Set the TAP COUNT 1.
[][]Enter the Tap count 1 within 1 to 9999 using the ‘UP/DOWN’ & ‘DIGIT SCROLL’ key.
[][]Press ‘ENTER’ key to go next parameter.
[][]Similarly set TAP COUNT 2 and TAP COUNT 3.
[][]In USP method, set TAP COUNT 1 as 250 taps, TAP COUNT 2 as 500 taps and TAP COUNT 3 as 500 taps.
[][]Set the date and time using the ‘UP/DOWN’ & ‘DIGIT SCROLL’ key.
[][]Select the print option & press ‘SET’ key to scroll back to main menu.
[][]Pass a quantity of material sufficient to perform the test through 20-mesh screen to break up any agglomerates.
[][]Transfer about 100 g sample into a dry 250 ml graduated cylinder with 2 ml accuracy.\
[][]Alternatively transfer a small quantity (less than 100 g) of sample into a 100 ml cylinder with 1ml accuracy to minimize the sample quantity.
[][]Press the ‘START’ key.
[][]Weigh the test sample and enter the weight of test sample.
[][]Press the ‘ENTER’ key to register the weight.
[][]Level the sample without tapping or compacting.
[][]Read the unsettled apparent volume to the nearest graduated unit and enter the volume using the ‘UP/DOWN’ & ‘DIGIT SCROLL’ key.
[][]Press the ‘ENTER’ key to register the volume.
[][]Fix the measuring cylinder into the holder provided for holding the measuring cylinder on the instrument.
[][]Lock the holder assembly.
[][]Press the ‘START’ key again to run the test.
[][]Display will show the elapsed taps and drops per minute.
ELAPSED TAP: # # #
Drops / Min. : # # #
[][]After programmed TAP COUNT 1 is over, measure the tapped volume to its nearest graduated unit.
[][]Enter the measured tapped volume using ‘UP / DOWN’ & ‘DIGIT SCROLL’ Keys.
[][]Press ‘ENTER’ key to register the value.
[][]Press ‘START’ key to continue TAP COUNT 2 program.
[][]Measure the tapped volume at the end of TAP COUNT 2 program and enter the value using ‘UP / DOWN’ & ‘DIGIT SCROLL’ Keys.
[][]The difference between the two counts will be displayed as a result.
[][]If the result after the completion of TAP COUNT 2 is less than 2.0%, press ‘STOP’ key to end the operation and to get the results.
[][]If the result is more than 2.0%, then press ‘START’ key again to start the TAP COUNT 3 program to get a new value.
[][]Repeat the operation till the difference between two succeeding measurements is less than 2.0%.
[][]Press ‘STOP’ key once the desired difference is obtained instrument will display the results.
[][]The results of Bulk density or initial density, tapped density and Hausner ratio and compressibility index will be displayed one after another by using ‘DOWN’ key.
[][]The results shall be recorded separately or taken as a print out.
[][]After operation enter usage details in Operation Logbook of Bulk Density Apparatus as per Annexure – II.
Calibration:
[][]Calibration of Drop distance
[][]Calibrate the instrument once in a year or whenever there is a major maintenance.
[][]Disconnect the instrument from mains.
[][]Gently disassemble the sample holder assembly.
[][]Remove the top cover by unscrewing the holding screws given on the bottom of the instrument i.e. the screws given on the four sides and one screw given on the backside near the power switch. The places are marked for convenience.
[][]Place the sample holder in the slot of USP I and manually rotate the cam wheel so that the holder is at the highest position.
[][]The stem of the holder is now on the top of the highest position of the cam (which is marked as a groove on the wheel.
[][]Measure the distance from base to the bottom of the holder (h1) using a suitable vernier caliper.
[][]Rotate the wheel to get the lowest position, the position from which it started to raise again.
[][]Measure the distance from base to the bottom of the holder (h2) using a suitable vernier caliper.
[][]The difference between the h1 and h2 gives the drop distance.
[][]Record the observations in the calibration information sheet (Annexure –I).
[][]Repeat the same procedure on the USP-II slot.
[][]Record the observations in the calibration information sheet (Annexure –I).
[][]When the distance is not within the prescribed limit, change the teflon bottom of the stem to get the required height.
[][]Carefully replace the top cover and close.
[][]Calibration of Drop rate
[][]Connect the instruments for main and proceed for the calibrations for drops rate.
[][]Switch ‘ON’ the mains.
[][]Select USP-I or USP-II method using ‘METHOD’ key
[][]The indicator light glows in USP-I or USP-II on the front panel
[][]Using ‘SCROLL BAR’ keys, select the USER method and press ‘SET’ key.
[][]Enter the number of taps to 100
[][]Press ‘START’ key and simultaneously start the stopwatch.
[][]Record the time at which the tapping stops in the calibration information sheet (Annexure –I).
[][]Similarly perform the test using 250, 750 and 1250 taps and note the timings
[][]Calculate the drops per minute in both USP-I and USP-II method.
[][]Record the drops per minute in the calibration information sheet (Annexure –I)
[][]If the instrument is out of calibration, inform the Manager, Quality Control.
Cleaning Procedure:
[][]Clean the instrument after every use.
[][]Switch ‘OFF’ the instrument and switch ‘OFF’ the mains.
[][]Remove the cylinders from the apparatus and clean the cylinder.
[][]Clean the apparatus with cotton cloth.
[][]Clean the surrounding areas of instrument with a cloth dampen in water.
Annexure:
Annexure-I: Calibration Information Sheet for Tap Density Apparatus.
Annexure-II: Operation Logbook of Tap Density Apparatus