TE TECH CHNICAL AD L ADVAN ANCES S IN HA HALLMAR ARKING - - PowerPoint PPT Presentation

TE TECH CHNICAL AD L ADVAN ANCES S IN HA HALLMAR ARKING

Rakesh Bhan – Managing Director Fischer Measurement Technologies (India) Pvt. Ltd. 03.08.2019

Gold ld S Stages a and A Analy lysis is

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• Various analytical methods
• OES
• X-ray Fluorescence Analysis (XRF)
• Fire Assaying
• Etc.
• Methods giving macro structural information
• Ultrasonic Transmission and Resonant

Ultrasound Spectroscopy (RUS)

• Eddy-current analysis (EC)
• Etc.

OES/XRF/Fire Assay Ultrasonic Eddy-current

Analytical integrity, composition

Gold Inspection

Bene nefits o

• f EDXR

XRF T F Techn hniqu que

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• Fast, Quick, Accurate and Non Destructive
• Requires no or very less sample preperation
• Measurement is done directly on solid sample and does not rely on

acid digestion

• Quantitative Analysis of gold alloys including Platinum Group Metals

(Pt, Pd, Rh, Ru, Ir, Os)

• Easy to use and practically feasible
• Quantification of all metals of interest in one single measurement.
• Advances in detection sensitivity has improved precision and accuracy
• f the measurement comparable to fire assay method.

Major C Components o

• f an E

EDXRF

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Pr Prim imary Fi Filt lter: Fixed or Multiple Changeable Filters like Nickel, Aluminum , Mylar etc. SDD D Detec ector / S Si P PIN N Detec ector/PC : Resolutions : 140eV/ 180eV/ 800eV X-Ra Ray t tube ube: Micro Focus tube with Beryllium Window Colli llimator: Fixed or Motorised Changeable Collimators like - Ø 0.2 mm (7.9 mils), Ø 0,6 mm (23.6 mils), Ø 1 mm (39.4 mils), Ø 3 mm (118 mils) others on request Camer era: High Resolution CCD Camera

Mea easurem emen ent – Effec ects a and nd Inter erferenc nces es

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Fact ctors Af Affect cting Ac g Accuracy cy and Reproduci cibility of

• f

XRF M Mea easurem emen ents

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Instrument Factors:

• Resolution of the Detector
• Collimator
• Measuring distance
• Measuring time
• Calibration

External Factors:

• Sample Homogeneity
• Environmental Conditions
• Positioning of the Sample
• Focusing
• Operator Skill
• Measurement Approach

Sp Spec ectrum – Prop

• portional C

al Cou

• unter T

Tube

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Counts per second as detected by the detector Measurement time for which the sample was exposed to X-Ray Measuring Parameters Material Composition as detected by the XRF Instrument Wider spectrums with

• verlaps due to High

Energy Resolution

Sp Spec ectrum – Si PIN / / SDD De DD Detec ector

• r

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Material Composition as detected by the XRF Instrument Measuring Parameters Measurement time for which the sample was exposed to X- Ray Counts per second as detected by the detector Time for which a detector is unable to detect another photon when a photon is being detected Unique spectrums for individual elements due to low Energy Resolution

SDD De DD Detec ector

• r

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• Better sensitivity at low energies

Al peak for PIN (blue) and SDD (grey)

New I Impr provemen ents i in n Detec ector T Techno hnology

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Function Existing Setup 20/30 mm2 SDD +

• ld DPP electronics

New Setup (SuperSense) SDD + DPP: DPP+

• Max. energy

resolution Fe55 < 165 eV < 140 eV Time to peak 1.6 µs 0.4 µs Top width 0.4 µs 0.125 µs Count rate in cps up to 100.000 up to 500.000 Diagnostic features Bus Errors

• Tracking power

supply

• voltages and

currents

• BIAS voltage
• cooler current
• detector

temperature

• HT operation

350.000 300.000 200.000 250.000 150.000 100.000 50.000

Recorded count rate [cps]

1.000.000 2.000.000 3.000.000 4.000.000 5.000.000

True count rate [cps]

Measu asurement S Spot

• t S

Size

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/ 1 / ) 1 ( d d s d d d c M ⋅ + + ⋅ =

The size of the measurement spot depends on

• size of collimator c,
• focal spot of the anode s0
• ratio d0/d1.

X-ray tube Sample

• Small Measurement spot allows for the best determination of

inhomogeneity's

• Large Measurement spot allows for low influence of

inhomogeneity

Adv dvanc nced O ed Optical Co Collimati tion S n Systems

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mono capillary poly capillary mirror optics 100 – 300 ~ 10 - 60 20 x 50 spot size [µm] ~ 10 ~ 500 ~ 10 amplification

Measu asuring D Distan ance ce - Md Md

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• Automatic correction of the reading
• Any md in the valid calibrated range

can be chosen

• Signal (count rate) ~ 1 / (measuring distance)2

repeatability ~ √count rate

• → keep measuring distance small!

Measu asuring T Time

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• Repeatability: s ~ √measuring time
• Four times longer measuring time will improve the repeatability by

a factor of 2.

• Sometimes very long measuring time will not further improve the

standard deviation. It is better to utilise the mean value of several measurements

• With advances in signal processing electronics, very accaurate

results can be obtained with a measuring time of 30 mins.

Calib libratio tion

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• To ensure valid results, measuring equipment shall be calibrated

against measurement standards traceable to international or national measurement standards.

• Ensures Traceability of measurement results
• Helps to minimize the Systematic Error
• Integrity of the calibration standards is

very important

Automatio tion a and D Data Integrity ity

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MES Level Field Level Operator Level Controller Level

Enterprise Level

PLC

ERP

SCADA MES

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Thank You for Your Attention!

Rakesh Bhan Fischer Measurement Tech. India Pvt. Ltd. Plot No.138/1, City Centre, Hinjewadi Phase 1, Pune +91 9766309851 rakesh@fischerindia.com