X-ray fluorescence analyzer with a plurality of measurement channels, and a method for performing x-ray fluorescence analysis

Patent metadata

Field	Value
Publication number	US-11199513-B2
Application number	US-201817049257-A
Country	US
Kind code	B2
Filing date	Apr 20, 2018
Priority date	Apr 20, 2018
Publication date	Dec 14, 2021
Grant date	Dec 14, 2021

Abstract

An X-ray fluorescence analyzer including an X-ray tube for emitting incident X-rays in the direction of a first optical axis. A slurry handling unit is configured to maintain a constant distance between a sample of slurry and the X-ray tube. A first crystal diffractor is located in a first direction from the slurry handling unit. The first crystal diffractor includes a first crystal and a first radiation detector configured to detect fluorescent X-rays diffracted by the first crystal at a first energy resolution. A second crystal diffractor is located in a second direction from the slurry handling unit. The second crystal diffractor includes a second crystal and a second radiation detector configured to detect fluorescent X-rays diffracted by the second crystal at a second energy resolution. The first crystal is a pyrolytic graphite crystal, the second crystal is of a material other than pyrolytic graphite, and the first and second crystal diffractors are configured to direct to their respective radiation detectors characteristic fluorescent radiation of a same element.

First claim

The invention claimed is:

1. An X-ray fluorescence analyzer, 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 comprising a first crystal,
a first radiation detector configured to detect fluorescent X-rays diffracted by said first crystal at a first energy resolution,
a second crystal diffractor located in a second direction from said slurry handling unit, said second crystal diffractor comprising a second crystal,
a second radiation detector configured to detect fluorescent X-rays diffracted by said second crystal at a second energy resolution,

characterized in that:
said first crystal is a pyrolytic graphite crystal,
said second crystal is of a material other than pyrolytic graphite, and
said first and second crystal diffractors are con-figured to direct to their respective radiation detectors characteristic fluorescent radiation of a same element.

2. The X-ray fluorescence analyzer according to claim 1 , 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.

3. The X-ray fluorescence analyzer according to claim 1 , wherein said first energy resolution is better than 300 eV at a reference energy of 5.9 keV.

4. The X-ray fluorescence analyzer according to claim 1 , wherein said first radiation detector is one of: a PIN diode detector, a silicon drift detector, a germanium detector, a germanium drift detector.

5. The X-ray fluorescence analyzer according to claim 1 , wherein said second radiation detector is a gas-filled proportional counter.

6. The X-ray fluorescence analyzer according to claim 1 , wherein said element is gold.

7. The X-ray fluorescence analyzer 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,
said first optical axis is at an oblique angle against said planar surface,
said first crystal diffractor is located at that rotational angle around said first optical axis at which said planar surface of said sample covers the largest portion of a field of view of the first crystal diffractor, and
said second crystal diffractor is located at another rotational angle around said first optical axis.

8. The X-ray fluorescence analyzer 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.

9. The X-ray fluorescence analyzer according to claim 1 , wherein the input power rating of said X-ray tube is at least 400 watts.

10. The X-ray fluorescence analyzer according to claim 9 , wherein the input power rating of said X-ray tube is at least 1 kilowatt, preferably at least 2 kilowatts, and more preferably at least 4 kilowatts.

11. The X-ray fluorescence analyzer according to claim 1 , wherein the optical path between said X-ray tube and said slurry handling unit is direct with no diffractor therebetween.

12. The X-ray fluorescence analyzer 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, preferably shorter than 40 mm, and more preferably shorter than 30 mm between said sample of slurry and said anode.

13. The X-ray fluorescence analyzer according to claim 12 , wherein said X-ray tube is an X-ray tube of the end window type.

14. The X-ray fluorescence analyzer 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.

15. The X-ray fluorescence analyzer according to claim 1 , further 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.

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

17. The X-ray fluorescence analyzer according to claim 1 , comprising a filter plate on the optical path between said X-ray tube and said slurry handling unit.

18. The X-ray fluorescence analyzer according to claim 17 , wherein said filter plate is located closer to said X-ray tube than to said slurry handling unit.

19. The X-ray fluorescence analyzer 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.

20. A method for performing X-ray fluorescence analysis, comprising:
irradiating a sample of slurry with incident X-rays and receiving fluorescent X-rays from the irradiated sample,
separating first and second predefined wavelength ranges from respective first and second portions of said received fluorescent X-rays with respective first and second crystal diffractors, wherein said first wavelength range and said second wavelength range both include characteristic fluorescent radiation of a same element, and wherein said first wavelength range is at least twice as wide as said second wavelength range,
detecting the fluorescent X-rays in said first and second separated wavelength ranges with respective first and second radiation detectors, wherein the energy resolution of said first radiation detector is better than 300 eV at a reference energy of 5.9 keV, thus producing respective first and second detection results, and
calculating a concentration of said element in said sample from at least one of said first and second detection results.

21. The method according to claim 20 , wherein said calculating comprises:
calculating a combined intensity of background radiation and fluorescent X-rays from others than said element using at least one of the first and second detection results,
subtracting, from the total intensity detected in a wavelength range containing said characteristic peak of fluorescent X-rays of an element to be measured in said sample, the calculated combined intensity of background radiation and fluorescent X-rays from other elements than said element of interest in said sample, and
providing the result of said subtracting as the calculated intensity of said characteristic fluorescent X-ray peak.

22. The method according to claim 20 , wherein said calculating comprises:
analyzing from said first and second detection results whether the influence of a characteristic peak from another element on the first detection result is larger than a predetermined threshold,
if said analyzing shows that the influence of said characteristic peak from said other element on the first det

Assignees

• Outotec Finland Oy

Inventors

• Koskinen Tommi
• Pelli Antti
• Sipilä Heikki

Classifications

• G01N23/223 Primary

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

• G01T1/1603

  with a combination of at least two different types of detectors · CPC title

• G01N2223/616

  earth materials · CPC title

• G01N2223/076

  X-ray fluorescence · CPC title

• G21K1/067

  using surface reflection, e.g. grazing incidence mirrors, gratings (multilayer mirrors G21K1/062) · CPC title