Sampling - XRD/XRF Course preparation

Participants name :
Dinesh Purohit
(Manager QA)
Lakheri Cement Works
Venue Maddukarrai Cement Works
Date -

Holcim Group Support Ltd 2010

XRF situation in Lakheri

Equipment Details
Equipment

Range

Existing
Parameter

XRF KV

0-30 (+/- 0.1)

30

XRF MA

0-40(+/- 0.1)

40

MDP Speed

10000-28000

27000

MDP Temp

15-60 deg C

20-30 deg C

0-8 Pa

2-6.5 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

XRF situation in Lakheri (Cont)

Equipment maintenance/Lab conditions

Internal- When soft maintenance like cartridge change and other smaller
job
External When Major s break down due to hardware & software
problem .
We control and monitor XRF KV, XRF MA, MDP Speed , Spectrometer
pressure ,Sec Water receptivity, 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 - Drift Correction Method
Almost they are System sample with wide rage but some standard sample
like HOT Meal is synthetic.

Holcim Group Support Ltd 2010

10-03-08
Preparation XRD

XRF situation in Lakheri (cont.)

Supplier support

Service contract

service contract include only AMC twice in year and guarantee spares replacement(if required )
01 year service contract
Cost - 2,65,000 INR.

The supplier rate for service is good.

Specific issues for discussion with the supplier

Minimize break down time.

Critical spares availability in Indian counterpart.

One Maintance engg HQ should be at Jaipur/ Bhopal.

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.

Make more easy calibration procedure.

Water cartridge replacement alarm should give sufficient for replacement.

The serious and/or frequent problems are Hardware related problem generated XRF shut down
min. 1 month per year.

We faced many Hardware failures Related To Power supply system , and vacuum system,
Gonio Amplifier break down no any problem related to source, crystals & detectors.
Two times Software related problem Stopped XRF functions for 07 days .
Water pump failure , more noise and no new warrantee pump receive.
Instrument remain stopped for 07 week

Holcim Group Support Ltd 2010

10-03-08
Preparation XRD

XRD situation in Lakheri (Cont)

Preparation of Samples

Using same press pallet for XRD and XRF.

Before preparation of press pallet we ensure that powder should Below 63 microns size.
And results obtained of such press pallet again confirmed by our calibration standard
powder ,which was already analyzed at Techport, Thane.

Free lime analysis

free lime determined by calibration method only

free lime determined by XRD, cross checked by acid alkali titration once per shift
and some time much difference observed between them.

We need training of XRD to know

clinker phase with minimum and regular variation with bouge calculation.

XRD give absolute Free lime because some time wide variation observed
XRD and wet analysis.

XRD should give Quartz concentration.

XRD should explain portlandite, gypsum phase in clinker.

XRD should give information of alkali sulphate.

XRD should give important mineral present in Limestone.

Holcim Group Support Ltd 2010

between

10-03-08
Preparation XRD

XRF breakdown details

From (Date)

To (Date)

No. Of
days

Reason

25.04.2008

Tripp with alarms 8195,8237& 8222 than

change De Ionized cartage

28.07.08

30.07.2008

18.08.2008

21.08.2008

XRF tripped & automatically restart

Card of x ray generator Is faulty

Continuous
25.09.2008

02.10.2008

Need to change GENEX

Continuous
23.10.2008

25.10.2008

GENEX (S703683T) 1.2 KW, 60 KV

replaced

26.07.2009

28.07.2009

03

General Maintenance

23.08.2009

29.08.2009

07

De Ionized cartage Change

Holcim Group Support Ltd 2010

03

KV too high or too low

10-03-08
Preparation XRD

XRF breakdown details

8

02.09.2009

04.09.2009

Cassette is not coming, stuck in side the tank

09.09.2009

15.09.2009

Concentration analysis program not working

10

21.09.2009

23.09.2009

Cassette is not coming, stuck in side the tank

12

1.12.2009

03.12.2010

Free CaO note analyzed (XRD System not

configured , Found Results abnormal

13

09.07.2010

12.07.2010

Mg,Na,Ba & Ti Found Results abnormal

(found F FIFO - full alarm) change S
703424 MUX Pre amplifier card)

14

31.07.2010

11.08.2010

12

Water pump found jam, change water pump

,Replacement of Preamplifier (MUX) for
Goniometer , Si mono channel is not working

15

08.10.2010

15.10.2010

Sample Not analyzed, molecular Pump frequently

tripped, than increase temp. of pump

Holcim Group Support Ltd 2010

10-03-08
Preparation XRD

Specific problems or success stories

Almost we are not so comfort because of

5 time break down of hardware like- Genex, mono 2 failure, MDP Pump,
water Pump replaced after one and half year of reporting.

Some time service engg. reach at site after 7-10 day of information.

Software for calibration is not user friendly because during task same entry
were fill in three time .

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

Thank You

Holcim Group Support Ltd 2010

10-03-08
Preparation XRD