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Sampling - XRD/XRF Course preparation

Participant’s name :
Dinesh Purohit
(Manager QA)
Lakheri Cement Works
Venue – Maddukarrai Cement Works
Date -

© Holcim Group Support Ltd 2010

0.5 Pa 400-4500 1900-2150 Spectrometer Pressure (Vacuum) Sec Water Resistively * Check up of equipments as per ICS Instrument Status © Holcim Group Support Ltd 2010 10-03-08 Preparation XRD 2 .1) 40 MDP Speed 10000-28000 27000 MDP Temp 15-60 deg C 20-30 deg C 0-8 Pa 2-6.0.1) 30 XRF MA 0-40(+/.XRF situation in Lakheri Equipment Details Equipment Range Existing Parameter XRF KV 0-30 (+/.

Spectrometer pressure .XRF situation in Lakheri (Cont…) • Equipment maintenance/Lab conditions      • Internal.Drift Correction Method Almost they are System sample with wide rage but some standard sample like HOT Meal is synthetic. XRF MA. P10 Gas cylinder pressure and flow No Environment problems related to laboratory conditions Room Temp maintained 20-22 deg C Analysis control    We use press pallet as well as calibration standard press pallet in drift correction When analysis became out of tolerance (permissible limit) or addition/ deletion of New calibration standard . © Holcim Group Support Ltd 2010 10-03-08 Preparation XRD 3 .Sec Water receptivity. We control and monitor XRF KV.When soft maintenance like cartridge change and other smaller job External – When Major s break down due to hardware & software problem . MDP Speed .

 Critical spares availability in Indian counterpart. Two times Software related problem – Stopped XRF functions for 07 days .  Water cartridge replacement alarm should give sufficient for replacement.  Supplier should trained at least Two instrument engg so that they can be able to follow the service engg on phone and able to resolve cassette stucked in transmission problem & can able to change FPC window and minimize XRF break down time. Instrument remain stopped for 07 week © Holcim Group Support Ltd 2010 10-03-08 Preparation XRD 4 .     We faced many Hardware failures Related To Power supply system .2. Specific issues for discussion with the supplier  Minimize break down time. The supplier rate for service is good.  One Maintance engg HQ should be at Jaipur/ Bhopal.XRF situation in Lakheri (cont.65.) • Supplier support  Service contract    service contract include only AMC twice in year and guarantee spares replacement(if required ) 01 year service contract Cost . Gonio Amplifier break down no any problem related to source. 1 month per year.000 INR.  • The serious and/or frequent problems are Hardware related problem generated XRF shut down min. and vacuum system. more noise and no new warrantee pump receive. crystals & detectors. Water pump failure .  Make more easy calibration procedure.

cross checked by acid alkali titration once per shift and some time much difference observed between them. • XRD give absolute Free lime because some time wide variation observed XRD and wet analysis. © Holcim Group Support Ltd 2010 between 10-03-08 Preparation XRD 5 . gypsum phase in clinker. And results obtained of such press pallet again confirmed by our calibration standard powder . • XRD should give important mineral present in Limestone.which was already analyzed at Techport. • XRD should give Quartz concentration. • XRD should explain portlandite. Thane.XRD situation in Lakheri (Cont…) Preparation of Samples   Using same press pallet for XRD and XRF. We need training of XRD to know • clinker phase with minimum and regular variation with bouge calculation. Free lime analysis   free lime determined by calibration method only free lime determined by XRD. Before preparation of press pallet we ensure that powder should Below 63 microns size. • XRD should give information of alkali sulphate.

08.2008 GENEX (S703683T) 1.10.8237& 8222 than change De – Ionized cartage 2 28.10.2008 02.08.2008 XRF tripped & automatically restart Card of x ray generator Is faulty 4 Continuous 25.2009 03 General Maintenance 7 23.07.04.2 KW. 60 KV replaced 6 26.2008 Tripp with alarms 8195.08.08.2008 25.09.08 30.10.2008 3 18.2008 Need to change GENEX 5 Continuous 23.07.2009 28.2009 29.07.XRF breakdown details From (Date) To (Date) No. Of days Reason 1 25.07.2008 21.2009 07 De – Ionized cartage Change © Holcim Group Support Ltd 2010 03 KV too high or too low 10-03-08 Preparation XRD 6 .

07.2009 23.2009 7 Concentration analysis program not working 10 21.12.2009 04.09. Si mono channel is not working 15 08.2010 12 Water pump found jam. stuck in side the tank 12 1.2009 03.09.09.10.2009 3 Cassette is not coming.08.2010 4 Mg.07.2009 15.full alarm) change S 703424 MUX Pre amplifier card) 14 31.2010 12.12.XRF breakdown details 8 02.Na.09.2010 11.2010 7 Sample Not analyzed.10.09. stuck in side the tank 9 09.09. of pump © Holcim Group Support Ltd 2010 10-03-08 Preparation XRD 7 . Found Results abnormal 13 09.07. molecular Pump frequently tripped. change water pump .2010 15.2010 3 Free CaO note analyzed (XRD System not configured .2009 3 Cassette is not coming.Replacement of Preamplifier (MUX) for Goniometer .Ba & Ti – Found Results abnormal (found F – FIFO . than increase temp.

MDP Pump. water Pump replaced after one and half year of reporting. • Some time service engg. mono 2 failure.Specific problems or success stories Almost we are not so comfort because of – • 5 time break down of hardware like. reach at site after 7-10 day of information. • There were no sufficient time Before alarm to replace de ionizing water cartridge and within half hour water cartridge became useless © Holcim Group Support Ltd 2010 10-03-08 Preparation XRD 8 .Genex. • Software for calibration is not user friendly because during task same entry were fill in three time .

Thank You © Holcim Group Support Ltd 2010 10-03-08 Preparation XRD 9 .