On-line X-ray fluorescence spectrometer for accurate monitoring

and improving blending sharpness in liquid production processes

The Epsilon Xflow

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Michel Zoontjes, May 2017

Content

Background of XRF

The Epsilon Xflow

Applications

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X-ray fluorescence

XRF is a widely used technique for elemental analysis of elements from Be up to Am

Concentration ranges are from a few ppm up to 100%

Non destructive technique

Minimal sample preparation required

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X-ray fluorescence for laboratories

Wavelength Dispersive XRF

+ Mature Technology

+ Best light element performance

+ Fast

- High Power (1 – 4 kW)

- Long optical path

Energy Dispersive XRF

+ Simultaneous multi-element analysis.

+ Low power (5 – 50 W)

+ Compact technology (no crystals, collimators)

+ Steep improved performance

- Lower resolution (~140 eV)

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Move to on-line analysis

Continues sampling

High frequent analysis of process

Fast feedback loop

More efficient process control

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Sample

cup

Developing the Epsilon Xflow

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Flowcell

In Out

Flowcell

In Out

Leak protection foil

Leak detector

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The analytical heart of the spectrometer

Analytical performance based on: Epsilon 3XLE

– Low drift and robust 15 W X-ray tube, produced

in PANalytical facility

– Latest Detector technology

– Tunable tube for optimal excitation per element

(4 – 50 kV)

Leakage protection

– Extra protection foil

– Leak detector between optical path and flowcell

Flexible and easy accessible flow cell

– Executed in process compatible materials

→Analytical requirements, pH, temperature

Analyse from sodium onwards

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Why is that difficult?

Lighter elements (Na, Mg) are more challenging for XRF due to physics

--> lower energy photons have shorter penetration depths

Emitted X-ray photons have to pass two foils

Measurement is done in air

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The Epsilon Xflow

1. Epsilon 3XLE

technology with a low maintenance flowcell

– Automated drift correction for stable, long-term operation

2. Built-in computer, operated with touch-screen

– Remote communication options

3. Multiple direct outputs, for stand-alone operation

– Used for direct valve activation

4. Purge option (for operation in ATEX-regulated zones)

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Part of a fully integrated solution

From sampling up to data integration

– Flow selection

– Sample conditioning

– Waste management

– Automatic calibration validation

– Adapted to process conditions

Petrochemicals

Accurate blending of ultra low sulfur fuels

Control real-time desulfurization processes to

optimize margins

Enable pro-active reaction to catalyst killers

(Fe, Ni, V) to extend catalysts life-time

Control the blending and production of lubrication oils

Polymer production

Accurate dosing of additives

Monitor homogenous catalysts in polymerization

processes

Control PTA production processes

Environmental

Monitor hazardous compounds in waste- and

process streams

Control the use of chemicals in wood preservation

processes

Mining

Monitor and react on changes in situ leaching

processes

Check mine wastewater compositions

Real-time analysis of liquors and reagents during

ore processing

Metals

Monitor yield in precious metal recovery

Analysis the depletion of plating baths and powder coatings

Food

Accurate dosing of nutrients in food and feed

streams

Control the salt concentration in food streams

Applicable for a wide range of industries

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Blending

Refinery processing

Accurate blending of ultra low sulfur fuels

Accurate blending of

ultra low sulfur fuels

IN: S in crude oil

(0.5 - 5%)

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Cl, Ni, V, Fe, Si,…

OUT: S in fuels

< 10 ppm

(Euro VI, Tier 3)

Control real-time desulfurization

processes to optimize margins

Enable pro-active reaction to catalyst killers

(Fe, Ni, V) to extend catalysts life-time

Feed

control

Sulfur blending sharpness for Euro VI, Tier 3

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5 mg/kg

9 mg/kg

50 mg/kg

~7 mg/kg 8 mg/kg

Blend ULS fuels accurately and efficiently to meet Euro VI,

Tier 3

Commercial fuel

7-days continuous flow and analysis

Data is drift corrected

Process monitoring - Refinement of nickel concentrates

Refinery processes

Environmental regulations /

waste check

Ore mining

Nickel concentrates

(Ni, Cu, Co, …)

Copper cake

Ni cathodes

Ni briquettes

Ni salts Co solution

Real-time analysis of acid nickel solutions

H2SO4 solution is used to extract nickel from ore concentrates

Acid solution

Measured at elevated temperatures (45°C) to homogenize solution

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Real-time analysis of acidic nickel

solutions

Dynamic measurement

Repeated for 71 times at 45°C

Total measurement time 4 minutes

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Element (wt%)

S 7.4 +/- 0.03

Ni 10.8 +/- 0.04

Real-time analysis of liquors and reagents

Optimize nickel recovery in leaching processes

Realize the highest product quality

– Verify extraction of all Cu and Co in the process

Seeing the unexpected

– Cu, Zn, Pb, As, Cd, Hg in Ni solutions

→ Emissions of waste water

to environment need to be reported

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Summary

Technical innovations over the past 20 years made XRF available for on-line analysis

The Epsilon Xflow is adaptable to meet process requirements

First applications shows the analytical capability of the Epsilon Xflow

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For more information please visit our booth