X-ray fluorescence analyzer system and a method for performing X-ray fluorescence analysis of an element of interest in slurry

Patent metadata

Field	Value
Publication number	US-11680913-B2
Application number	US-201917049261-A
Country	US
Kind code	B2
Filing date	Feb 18, 2019
Priority date	Apr 20, 2018
Publication date	Jun 20, 2023
Grant date	Jun 20, 2023

Abstract

An X-ray fluorescence analyzer system including an X-ray tube, a slurry handling unit, and a crystal diffractor located in a first direction from the slurry handling unit. The crystal diffractor separates a predefined wavelength range from fluorescent X-rays that propagate into the first direction, and directs the fluorescent X-rays in the separated predefined wavelength range to a radiation detector. The crystal diffractor includes a pyrolytic graphite crystal. The predefined wavelength range includes characteristic fluorescent radiation of a pre-defined element of interest with its atomic number Z between 41 and 60, the ends included. An energy resolution of the radiation detector is better than 600 eV at the energy of the characteristic fluorescent radiation.

First claim

The invention claimed is:

1. An X-ray fluorescence analyzer system, comprising:
an X-ray tube for emitting incident X-rays in the direction of a first optical axis,
a slurry handling unit configured to maintain a constant distance between a sample of slurry and said X-ray tube,
a first crystal diffractor located in a first direction from said slurry handling unit, said first crystal diffractor being configured to separate a predefined first wavelength range from fluorescent X-rays that said incident X-rays generate in said sample of slurry and that propagate into said first direction, and configured to direct the fluorescent X-rays in the separated predefined first wavelength range to a first radiation detector,
a processing part configured to receive and process output signals produced by said first radiation detector, wherein said processing part is configured to estimate a proportion of background radiation using at least a first proportion of said output signals indicative of detected X-rays that are within said first wavelength range but apart from the wavelength of said characteristic fluorescent radiation of said element of interest wherein:
the first crystal diffractor comprises a pyrolytic graphite crystal,
said predefined first wavelength range comprises characteristic fluorescent radiation of a predefined element of interest with its atomic number Z between 41 and 60 the ends included,
an energy resolution of said first radiation detector is better than 600 eV at the energy of said characteristic fluorescent radiation, and
said processing part is configured to calculate a detected amount of said characteristic fluorescent radiation of said element of interest by subtracting from output signals at wavelengths of said characteristic fluorescent radiation said estimated proportion of background radiation.

2. The X-ray fluorescence analyzer system according to claim 1 , wherein said processing part is configured to estimate said proportion of background radiation using at least said first proportion of said output signals indicative of detected X-rays that are within said first wavelength range but shorter than the wavelength of said characteristic fluorescent radiation of said element of interest, and a second proportion of said output signals indicative of detected X-rays that are within said first wavelength range but longer than the wavelength of said characteristic fluorescent radiation of said element of interest.

3. The X-ray fluorescence analyzer system according to claim 1 , wherein said energy resolution of said first radiation detector is better than 300 eV at the energy of said characteristic fluorescent radiation, and said first radiation detector is a solid-state semiconductor detector.

4. The X-ray fluorescence analyzer system according to claim 1 , wherein the input power rating of said X-ray tube is at least 1 kilowatt.

5. The X-ray fluorescence analyzer system according to claim 4 , comprising primary filter material in the form of a layer across said first optical axis between said X-ray tube and said slurry handling unit.

6. The X-ray fluorescence analyzer system according to claim 5 , wherein a transmission of said layer of primary filter material is more than 5% for photons with energies larger than 15 keV.

7. The X-ray fluorescence analyzer system according to claim 1 , wherein
the X-ray tube comprises an anode for generating said incident X-rays, and
said slurry handling unit is configured to maintain a shortest linear distance that is shorter than 50 mm between said sample of slurry and said anode.

8. The X-ray fluorescence analyzer system according to claim 1 , wherein the diffractive surface of said pyrolytic graphite crystal is one of the following: a simply connected surface curved in one direction; a simply connected surface curved in two directions; a rotationally symmetric surface that is not simply connected.

9. The X-ray fluorescence analyzer system according to claim 1 , wherein:
said slurry handling unit is configured to maintain a planar surface of said sample of slurry on a side facing said X-ray tube, and
said first optical axis is perpendicular against said planar surface.

10. The X-ray fluorescence analyzer system according to claim 1 , wherein:
said slurry handling unit is configured to maintain a planar surface of said sample of slurry on a side facing said X-ray tube, and
said first optical axis is at an oblique angle against said planar surface.

11. The X-ray fluorescence analyzer system according to claim 1 , further comprising a plurality of other crystal diffractors in addition to said first crystal diffractor, each of said first and other crystal diffractors being located at a respective rotation angle around said first optical axis and each of said crystal diffractors being configured to separate a predefined wavelength range from fluorescent X-rays that propagate into the respective direction, and configured to direct the fluorescent X-rays in the respective separated predefined first wavelength range to a respective radiation detector.

12. The X-ray fluorescence analyzer system according to claim 11 , wherein:
said plurality of other crystal diffractors comprises a second crystal diffractor comprising a second crystal, configured to direct the fluorescent X-rays in the respective separated second predefined wavelength range to a respective second radiation detector, and
said second crystal is of a material other than pyrolytic graphite.

13. The X-ray fluorescence analyzer system according to claim 12 , wherein said second crystal is one of: a silicon dioxide crystal, a lithium fluoride crystal, an ammonium dihydrogen phosphate crystal, a potassium hydrogen phthalate crystal; and wherein said second radiation detector is a gas-filled proportional counter.

14. The X-ray fluorescence analyzer system according to claim 1 , comprising:
an analyzer body,
a front wall of said analyzer body,
an opening in said front wall, and
a holder for removably holding said slurry handling unit against an outer side of said front wall and aligned with said opening in said front wall.

15. The X-ray fluorescence analyzer system according to claim 14 , wherein said X-ray tube and said first crystal diffractor are both inside said analyzer body, on the same side of said front wall.

16. The X-ray fluorescence analyzer system according to claim 1 , comprising a calibrator plate and an actuator configured to controllably move said calibrator plate between at least two positions, of which a first position is not on the path of the incident X-rays and a second position is on the path of the incident X-rays and in a field of view of the first crystal diffractor.

17. The X-ray fluorescence analyzer system according to claim 1 , wherein said predefined element of interest is silver.

18. A method for performing X-ray fluorescence analysis of a predefined element of interest in slurry, wherein said predefined element of interest has its atomic number Z between 41 and 60 the ends included and the method comprises:
emitting incident X-rays in the direction of a first optical axis towards a sample of said slurry,
using a first crystal diffractor with a pyrolytic graphite crystal to separate a predefined first wavelength range from fluorescent X-rays that said incident X-rays generate in said sample of slurry, wherein said predefined first wavelength range comprises characteristic fluorescent radiation of said predefined element of interest,
directing the fluorescent X-rays in the separated predefined first waveleng

Assignees

• Outotec Finland Oy

Inventors

• Sipilä Heikki
• Pelli Antti
• Koskinen Tommi

Classifications

• G01N23/223 Primary

  by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence · CPC title

• G01N2223/616

  earth materials · CPC title

• G21K2201/062

  the element being a crystal · CPC title

• G01T1/16

  Measuring radiation intensity (G01T1/29 takes precedence {; self-powered detectors G01T3/006; using an ionisation chamber filled with a liquid or solid, e.g. frozen liquid, dielectric G01T3/008}) · CPC title

• C22B3/02

  Apparatus therefor · CPC title