Friday, May 2, 2014

Operation and calibration of Vankel dissolution tester, Model VK7000 with automatic sampling station model VK8000

       To lay down procedure for operation and calibration of Vankel Dissolution
  tester, Model VK 7000 with automatic sampling station, Model VK 8000.
2.1 Quality Control / Analytical Development Officer, whoever is operating the 
2.2 Quality Control Manager to ensure compliance.  
3.1 Operating Instructions   
3.1.1 Turn ON the main AC power supply to VK 7000 Dissolution testing station
3.1.2        Turn the power switch ON provided on the left hand side of the VK 7000 drive
  unit. The red LEDs on the system control will light and the system monitor will
  display start up screen.  
  PROGRAM REV 1.27  
  After a few seconds the previously set values will be displayed on the monitor
3.1.3         Remove  the  lids  on  the  vessels. Press  the 'LIFT  D'   key  twice   and  release     
  immediately. The   drive   unit  will  move  to  the  highest  position  and  stops 
  automatically .  
  Note:  To stop the drive unit, press  "LIFT  Ñ  or  D " at any position .
3.1.4    Remove  one  of  the  aligned  vessels  from  the  first  row  and keep it  safely.
  Fill  the water bath with purified  water till the water level comes just above the 
  outlet  valve from heater / circulator on the left side of the  bath. Check  for  any  
  leaks, tighten the screws on the bulkhead fittings on bath /heater inlet or outlet, 
  if any leak is there.  
3.1.5        Replace the vessel in original position.  
3.1.6 Switch  on  the  AC  power  supply to the VK750D Heater/Circulator and ON 
  the power switch on the backside of the unit. Ensure that the monitor display
  ---------- and the heater on indicator glows.  
3.1.7 Switch on the power supply to VK 8000 sampling station by keeping the ON/
  OFF  switch  provided  at  the right hand side in ON position. After initializing 
  display, "READY" will be displayed.  
3.1.8 If profile is to be performed, follow the following steps. Press 'MENU' key on VK 8000, Main menu shall be displayed. Press '7' key, '4' key and then  '9' key, Sampling head shall move to row no. 9. Remove the tube connections to replacement media/rinse reservoir and
  remove reservoir, wash with purified water and rinse with media. After
  washing keep it in original position. Connect the appropriate tubes as marked on the tubes to inlet and outlet of
  replacement media/rinse reservoir. Fill the replacement media/rinse reservoir with medium. Connect the replace-
  ment media chamber to replacement media pump with the tube marked 'to
  replacement media/rinse reservoir'. Press 'H' key, sampling head shall move to home position. Press 'ESC' key
  thrice. 'READY' shall be displayed on the VK 8000. Remove the media tray of media replacement pump and wash it with purified
  water and then rinse with media. Fix it in pump. Fill it with media and keep the
  heater tube in media and close with lid. Immerse the tube marked 'into media tray' in media tray and stick it with 
  cellophane tape on lid of media tray.  
3.1.9 Switch on the power supply to peristaltic pump. Put the pump in the forward
  direction  by  keeping  the  FWD/REV  switch  provided at rear side in FWD 
3.1.10 Fill purified water in cleaning reservoir upto 1 inch level (approx. 2.5 ltrs) and 
  keep  the  reservoir on  the dissolution vessel table of VK 7000. Fix the filters 
  of required porosity to the cannulas of sampling manifold.  
3.1.11 Press 'Ñ LIFT' key and slowly down the drive unit such that the sampling manifold
  is about 6 inches above the level of media in reservoir.  
3.1.12 Press ' Ñ Probes' key and adjust the probes by using Ñ lift key such that the 
  filters fixed to the cannulas are completely immersed in the media. Keep the
  levers on the peristaltic pump towards left side.  
3.1.13 Press the 'MENU' key on VK 8000. 'MAIN MENU' will appear. Press '4' key 
  'ENTER  PRIME  TIME' will appear. ENTER 99 seconds as prime time using
  numerical keys and press 'ENTER'.  
3.1.14 Press '5' key. 'ENTER  PURGE  TIME' will appear. ENTER 99 seconds as purge
   time using numerical keys and press 'ENTER'. Press 'ESC' key. 
3.1.15 Check all the cannulas on sampling manifold are properly connected with
  color coded Teflon tubes.  
3.1.16 Press 'CLEAN  SYSTEM' key on VK 8000. Press '1' to start cleaning.
3.1.17 After completion of cleaning, 'READY' will be displayed on VK 8000 and 
  Peristaltic pump will off.  
3.1.18 Perform the Volume calibration either by manual mode or by Automatic mode. Perform the Volume calibration by Automatic mode as follows.  
  Note : Ensure that the autocalibration fixture is perfectly dry. Press 'CAL' key when the system monitor on VK 8000 showing ready. Ensure
  that  the  auto  calibration fixture is in place and top of the calibration fixture is
  connected to the rear panel connector marked 'calibration'. Also ensure that
  pump is ON, in forward direction and levers are towards left. Press '2' for auto calibration and system starts calibration. After calibration is over, VK8000 displays with blinking 'Calibration completed' with
  alarm. Press any key to stop the alarm . Press  ESC TO EXIT will be displayed.
  Remove the autocalibration fixture, empty it, allow it to dry and fix it in original
  position and Press 'ESC' key. Verify the calibration by giving a dummy run as follows. Press PROG key, and write a programme for ROW  '0' with sample time points at 
  02 minutes and R-M Option in DISABLE condition. Keep six 10 ml calibrated test tubes in '0' Row in 1 to 6 columns. Press 'START
  PROG' key and enter the program number. Press '1' key three times. System gives calibrated volume in to the test tubes kept in '0' row. Then the system
  goes for purging. After purging the system comes to READY position. Perform the Volume calibration by manual mode as follows. Ensure that the peristaltic pump is ON, in forward direction and levers are 
  towards left. Press 'CAL' key when the system monitor on VK 8000 showing ready.
  Remove the autocalibration fixture, Media/Rinse reservoir and sample tray. Press '1' for Manual calibration and system starts calibration.  
  After priming is completed, the sampling valves comes down. Place a Calibrated 10 ml test tube or volumetric flask below the valve number 1.
  Press OPEN VALVES key and the valve start releasing the water. Press OPEN VALVES key again when exactly 10 ml of water is collected.
  Similarly perform the calibration for other valves from 2 to 6.  
  Then valves moves up and the system starts purging. After purging, Sampling station moves forward. VK8000 displays with blinking 
  Calibration completed' with alarm. Keep the Auto calibration fixture and 
  media/rinse reservoir  in place. Press any key except ESC key to stop the alarm. 'PRESS  ESC  TO  EXIT' is 
  displayed on the screen. Press 'ESC' key. System goes back to home position.
  Keep the sample tray in place. Repeat operation mentioned in point no. to  
3.1.19 Remove the cleaning reservoir from the table carefully by raising up the drive 
  unit,empty it and fill the tray with media upto 1 inch level(approx. .2.5 ltrs.) and
  follow point nos.3.1.10 to 3.1.15.  
3.1.20 After completion of cleaning, 'READY' will be displayed on VK 8000 and 
  Peristaltic pump will off.  
3.1.21 Remove the cleaning reservoir from the table carefully by raising up the drive 
  unit and keep it aside. Fill the specified quantity of medium in vessels 
  mentioned in the individual  monograph.  
3.1.22 Press "MENU" key on VK 7000 to get into the main menu.  
3.1.23 Press "2" to set clock. 'ENTER  DATE'  will be displayed with the current date.
  Press "ENTER" to accept it, otherwise key in the  new date using 0-9 numeric
  keys in mm/dd/yy  format. Press 'ENTER' key.  
3.1.24 Now 'ENTER  TIME :'  with current time of the day will be displayed in 24Hr. format
  Press "ENTER" to accept the displayed time otherwise key in the new time in
  24 Hr. format.  Press 'ENTER' key.  
3.1.25  Press "3" to set temperature  '** * SELECT TEMPERATURE SET MODE * * *
                will be displayed.  
3.1.26 Press "1" , the previously set bath temperature will be displayed. Press 
                 'ENTER' to accept it, otherwise enter, the exact temperature required (37.5°C) 
                 and press 'ENTER'.  
                 Note : If a mistake is made, press "CLEAR" the previous entry will be displayed again.
3.1.27 Press '4'. '*** REPORT  CENTER  CONTROL  ***' will be displayed. 
3.1.28 Press '1' to keep printer ON. Press '4' to again get into Report center control.
  Press '4' to ENTER print out frequency. ENTER print out frequency in minutes using
  0 to 9 keys. Press 'ENTER' key.
3.1.29 Press '5' to set print out ID. ENTER the numerical of the instrument ID No. and 
  press 'ENTER' (for example 080 for QAE080).  
3.1.30 Press 'MENU' key on VK 7000 to get into Main menu. Press '5' to write the 
  program. '*** SELECT  BASKET  OR  PADDLE' will appear.  
3.1.31 Select baskets by pressing '1'  or paddles by pressing '2' which ever is 
  mentioned in the monograph and then press MENU key.  
3.1.32 Fix the selected ones as described below. Glide each shaft up into the spindle so that all the uncoated part of the paddle 
  shaft   goes  into  the  spindle clutch or  insert   the  basket  holder  shaft  with 
  basket into the clutch spindle until the shaft is seen from clutch opening. Tighten the clutch screw on the spindle. Loosen the thumb screw on stop ring and remove the paddle/ basket height
  gauge  from the left second leg and slide the stop ring down completely and
  tight the thumb screw. Press  'LIFT  Ñ' and hold to lower the drive head, hold the key until the drive 
  head stops automatically. Loose  the  clamp  on  each  spindle  and  carefully  lower  each shaft until the 
  paddle  blade  or  basket  is  resting  on  the  bottom of the vessel. Tight each 
  clamp. Press and hold the 'LIFT  D' key and release the key after the drive unit raises 3 
  or 4  inches  up. Loose  the thumb screw on stop ring. Slide it up and clip the 
  paddle/basket  height  gauge  on  the  leg  between  the stop ring and safety 
  stop. Slide the gauge down so that it rests on the safety stop. Then slide the 
  stop ring  down until it rests on the top of the gauge. Tight the stop ring thumb 
  screw. Ensure that appropriate depth spacer (height gauge) is used for basket / 
  paddle whichever is fixed Press and hold the 'LIFT  Ñ  key until the drive unit stops automatically.
3.1.33 Keep the lids on each vessel.  
3.1.34 Press 'MENU' key on VK 7000 and then press '5' key and ensure the * mark is
  on selected option in select basket or paddle menu. Press 'ENTER' key.
3.1.35 'ENTER  RPM' will be displayed. ENTER the RPM value specified in the monograph
  using 0-9 keys and press 'ENTER' key.  
3.1.36 'ENTER  SET  BATCH  TEMPERATURE' will be displayed. ENTER 37.5°C as bath 
  temperature and press 'ENTER' key.  
3.1.37 'ENTER  TEST  LENGTH :' shall  be  displayed. Enter  test  length  2 minutes more 
  than the mentioned time in individual monograph using 0-9 numerical keys in 
  HH:MM format and press 'ENTER' key.   
  Ex.: Enter 32 minutes test length for 30 minutes.  
3.1.38 Final spin at 250 RPM will be displayed. ENTER the final spin time to be at 250
  RPM in mm:ss format as per monograph, if required. Press 'ENTER' key.
  1. Yes          2. No.                                          Will be displayed. Press 2 key. 
  1. Yes          2. No.                                          Will be displayed. Press 2 key. 
3.1.41 'SAMPLE  MANIFOLD  AUTO  CONTROL' will be displayed. Press '2' to disable.
3.1.42 Ensure that remote interface cable is connected to start input of VK8000
  and start output of VK 7000.  
3.1.44 Press 'PROG' key on VK 8000. ENTER Prog#(1-30):_____ will be displayed with
  cursor flashing at entry space.  
3.1.45 Enter the program number (from 1-30 only) and press 'ENTER' key.
3.1.46 Program variables menu will be displayed on VK 8000.  
3.1.47 Press '1' *** Set VK 7000 Parameters *** will be displayed.  
  1. Set COM Port ID. 4. Final Spin length.  
  2. Set spindle RPM. 5. Set Printer.  
  3. Set Bath temperature. 6. Set  DDM or Basket. Press 1 to set com port ID No. Keep 01 always. And press ENTER key. Press 2 key two times to set RPM as specified in individual monograph. And press 
  ENTER key. Press 3 key and 2 key to set VK7000 temperature (Bath temperature). Use 0-9 keys 
  to feed the bath temperature and press ENTER key. Press 4 to set final spin length in minutes : Seconds format and press ENTER key. Press 5 to set printer frequency at VK7000 in minutes and press ENTER key.
  1. Enable             2. Disable                         will be displayed. Press '1' key. Press 6 to select Basket or paddle.  
  1. Sequential        2. Simultaneous              will be displayed. Press '1' key. Press 'ESC' key to download set parameters to VK7000? "Y/N" appears, press "Y".
  ***PROGRAMME VARIABLES*** will be displayed.  
3.1.50 Press '2' sample time point will be displayed.  
3.1.51 Enter  the  sampling  time  as  per  monograph in hh:mm format. E.g.. to take 
  sample  after  45  min  enter 000:45. Press  'ENTER'. Row number will change to
  '1'. Enter 000:00. Press 'ENTER' to abort sampling after given time.
3.1.52 To perform dissolution profile with particular time interval gap in sampling
  enter the next sampling point also.  
  e.g.: To draw samples at an interval of 5 min upto 30 min, Enter sampling time 
  as 000:05 at row '0'. Press Enter and 000:10 at row '1'. Press Enter key and
  000:15 at row '2'. Press Enter and 000:20 at row '3'. Press Enter key and
  000:25 at row '4'. Press Enter and 000:30 at row '5'. Press Enter. Row number will
  change to '6'. Enter 000:00. Press 'ENTER' twice to abort sampling after given time.
3.1.53 Again program variables will appear. Press '3' to enter sample volume. Enter
  sample volume in ml (upto 14 ml only). Press 'ENTER' key.  
3.1.54 Press  '4'  to  ENTER  batch  selection. Press  '1'  to  enter  operator  name  (10 
  characters only). Press  'ENTER'. Press '2' to enter product name (10 characters
  only). Press 'ENTER'. Press '3' to enter Batch number (10 characters only). Press 
  'ENTER'. Press  '4'  to  enter  lot number (10 characters only). Press 'ENTER'. Press
  '5'  to enter group number  (10 characters only). Press 'ENTER'. Press '6' to enter
  notation (10 characters only). Press 'ENTER' key.  
3.1.55 Press 'ESC' to enter into program variables. Press '5' to enter the prime time
  (enter from 00 to 99 seconds only). Press 'ENTER'.  
3.1.56 Press '6'  to enter purge time. Enter upto 99 seconds only. Press 'ENTER' key.
3.1.57 Press '7' and press '1' to disable media replacement option or '2' to enable
  media replacement. It will ask R-M percentage, enter 100 & enter for 100%
3.1.58 Ensure that the levers on peristaltic pump are towards left side. The test tubes
  in sample tray are cleaned and dried.  
3.1.59 Press 'ESC' key.  READY will be displayed.  
3.1.60 Ensure that remote interface cable is connected to start input of VK8000
  and start output of VK 7000.  
3.1.61 Ensure that required number of clean & dry test tubes are placed in sample 
  tray of  VK8000.  
3.1.62 Ensure that the temperature in all vessels is 37 ± 0.5°C by keeping Thermometer
  or Sensor of digital thermometer or sensor of QA station in each vessel. Record 
  the initial temperature of each vessel in record of analysis.  
3.1.63 Drop tablets/capsules in each vessel and immediately press 'Start Program' on 
  VK8000 for  apparatus -2. For  apparatus -1, place  1 tablet/capsule  in  each  
  basket, fix baskets to shafts and down the drive unit until it stops automatically. 
  Press Start program on VK8000, It will ask "Enter Prog (1-30)", Enter the program 
  which you want to run "Press Enter". "Select Start Mode" submenu will be displayed,
  press 1 to select "Start Now" option. VK7000 options submenu will be displayed,
  press 1 to select "Load" and "Run" VK7000. Select VK7000 Program start mode,
  Press 1 to select "Instant", then the run starts.  
3.1.63 When the particular row sampling is completed the instrument gives a beep
  sound, and flashes the message 'Current row sampling is completed'. Press
  any key (except ESC) to proceed with further sampling.  
  Note : If you want to abort the running program press 'ESC' and 'Y'.
3.1.64 After the execution of complete program 'printing....... please wait......' will be
  displayed with a current row sampling completed alarm. Press any key after
  printing is over. Ready will be displayed.  
3.1.65 Analyse the samples as mentioned in individual monograph.  
3.1.66 Remove  the  lids  over  vessels, press  'lift  D'  twice in a second to raise up the
  drive units. Clean the dissolution apparatus by following SOP "Cleaning of Dissolution
3.1.67 ENTER the usage details in "Instrument/Equipment user log book" (Annexure -4)
3.2 Calibration of RPM, Wobble, Shaft alignment, PT 100 Sensor and
  Temperature distribution.  
3.2.1 Calibrate by following the SOP on "Operation and Calibration of Dissolution
  QA Station".  
3.2.2 Acceptance Criteria  
  Parameter Criteria  
  RPM   Should not vary by ±1 of the set value.  
  Wobble   Should not be more than 1 mm  
  Shaft alignment Deviation should be not more than 1.5° on both  
      x-axis and y-axis.    
  Temperature The temperature shown by all the eight   
      vessels shall be 37± 0.5°C.    
3.2.3 Record the observations in the calibration record (Annexure 1).  
3.2.4 Calibration schedule : Once in 3 months or after each major maintenance job.
3.3 Calibration of Timer :  
3.3.1 Operate the equipment as mentioned in point No. 3.1.1 to 3.1.4, and 3.1.32 
  to 3.1.39 by Entering test length as 30 min.    
3.3.2 Press 'RUN' key and start the calibrated stopwatch simultaneously.
3.3.3 At the end of 30 minutes, immediately stop the stopwatch.  
3.3.4 Record the set time and the time shown by calibrated stopwatch in the
  "Dissolution apparatus calibration record" (Annexure -2).  
3.3.5 Acceptance Criteria : The difference between set time and the time shown
  by calibrated stopwatch shall not be more than 36 seconds.  
3.3.6 Calibration schedule : Once in 3 months or after each major maintenance job.
3.4 Dissolution Apparatus Suitability test by using Prednisone tablets RS 
  and salicylic acid tablets RS :  
3.4.1 Proceed as directed in the General Test Procedures "Dissolution Apparatus-
  suitability test by using Prednisone  tablets RS  " and "Dissolution Apparatus-
  suitability test by using Salicylic acid tablets RS ". Record the data in "Worksheet -
  Calibration Record". For Prednisone tablets in "Suitability test with USP "Prednisone
  tablets" (Annexure-5). For Salicylic acid tablets in "Suitability test with USP
  Salicylic acid tablets" (Annexure-6). Get these "Worksheet - Calibration Records"
  from documentation cell.  
3.4.2 Record  the  results  in  format "Dissolution  Apparatus - Suitability  test"  
  separately. (Annexure -3)  
3.4.3 Acceptance Criteria : The  results  shall  conform   with  the  specifications
  provided  by  USP  Convention Inc., for the particular Lot No. of Prednisone
  tablets RS and Salicylic acid tablets RS.  
3.4.4 Calibration Schedule : Once in 6 months or after each major maintenance job.
3.5 Calibration of media sampled  and replaced :  
3.5.1 Perform the volume calibration by following point no. to 3.1.20.
3.5.2 Clean the system for three times by priming and purging for 99 secs with purified
3.5.3 Put off the heater and ensure that the instrument is at ambient temperature.
3.5.4 Take about 80 mL of purified water into six LOD bottles and weigh them (W1)
  Keep them below the probes.  
3.5.5 Weigh six test tubes and keep in '0' row of sampling collection tray (W2).
3.5.6 Perform a dummy run with a run time of 2 mins by keeping media replacement 
  option in 'enable' mode and sampling volume 10 mL.  
3.5.7 After completion of the run, weigh sample collected in the test tubes (W3) and
  weigh the LOD bottles with water (W4).  
  Calculate the media replaced by using the following formula :  
  Media replaced (L2) : (W4-W1) + (W3-W2) g  
  Media replaced (L2) : (W4-W1)  + (W3-W2)  x 1.00396 mL  
  Media sampled (L1) : (W3- W2) g  
  Media sampled (L1) : (W3- W2) x 1.00396 mL  
  Record them in calibration record for media replacement (Annexure-7).
3.5.8 Calculate the difference between media replaced and media sampled for all the six
3.5.9 Acceptance Criteria : The difference between media sampled and replaced should
  be not more than 0.7 mL and the media sampled should be 10 ± 0.7 mL.
3.5.10 Calibration schedule : Once in 3 months and after any major maintenance job.
4.1 Specimen format of "Calibration record" for Calibration of RPM, Wobble, 
  Shaft  alignment, temperature  Sensors  and  temperature  distribution - Annexure 1. 
4.2 Specimen format of "Calibration record" for calibration of Timer  - Annexure 2. 
4.3 Specimen format of "Dissolution apparatus - suitability test " - Annexure 3.
4.4 File the calibration records in Dissolution calibration record file, kept near the 
  Dissolution apparatus.  
4.5 Specimen format of "Instrument/Equipment user log book" - Annexure 4.
4.6 Specimen format of "Dissolution Apparatus - Suitability test with USP Prednisone
  tablets" worksheet - Annexure - 5.  
4.7 Specimen format of "Dissolution Apparatus - Suitability test with USP Salicylic Acid
  Tablets" worksheet - Annexure - 6.  
4.8 Specimen format of "Calibration record for media replacement" - Annexure 7