# US 9,435,757 B2 · Sample viscosity and flow control for heavy samples, and X-ray analysis applications thereof

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- Number: US 9,435,757 B2
- Document ID: US9435757B2
- Status: Granted
- Kind: B2
- Application number: 14/739,433
- Filed: 2015-06-15
- Published: 2016-02-04
- Granted: 2016-09-06
- Earliest claimed: 2011-08-15
- Assignees: X-Ray Optical Systems, Inc.
- Applicants: X-Ray Optical Systems, Inc.
- Inventors: George Allen; Stuart Shakshover; Sony Cheryian
- Web page: https://patentgrep.com/patent/US9435757B2

## CPC

- G01N 23/223: by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
- G01N 1/28: Preparing specimens for investigation {including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q}(mounting specimens on microscopic slides G02B21/34; means for supporting the objects or the materials to be analysed in electron microscopes H01J37/20 {; laboratory gas handling apparatus B01L5/00})
- G01N 33/2823: {Raw oil, drilling fluid or polyphasic mixtures}
- H01J 35/16: Vessels; Containers; Shields associated therewith
- G01N 2223/076: X-ray fluorescence
- H01J 2235/18: Windows, e.g. for X-ray transmission
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)

## Abstract

An x-ray analysis system having an x-ray engine with an x-ray source for producing an x-ray excitation beam directed toward an x-ray analysis focal area; a sample chamber for presenting a sample stream to the x-ray analysis focal area, the analysis focal area disposed within a sample analysis area defined within the chamber; an x-ray detection path for collecting secondary x-rays and directing the x-rays toward a detector; an x-ray transparent barrier on a wall of the chamber through which the x-rays pass; and a blocking structure partially blocking the sample analysis area, for creating sample stream turbulence in the sample analysis area and over the barrier. The blocking structure may be disposed asymmetrically about a central axis of the x-ray analysis focal area and/or the sample analysis area; and may be a rounded pin. A heating element may be used to heat the sample stream for improving flow.

## Claims

### Claim 1

An x-ray analysis sample handling apparatus, comprising:
a sample chamber defining a sample analysis area within which a sample stream flows about an x-ray analysis focal area of an x-ray engine;
an x-ray transparent barrier in a wall of said chamber for allowing x-rays to/from the sample analysis area;
a blocking structure disposed asymmetrically about a central axis of the x-ray analysis focal area and/or the sample analysis area and partially blocking the sample analysis area, for creating sample stream turbulence in the sample analysis area and over the barrier.

### Claim 2 (depends on 1)

The apparatus of claim 1, wherein the blocking structure provides a flushing mechanism to inhibit precipitate and/or other contamination of the barrier.

### Claim 3 (depends on 2)

The apparatus of claim 2, wherein the blocking structure comprises a rounded pin.

### Claim 4 (depends on 1)

The apparatus of claim 1 in combination with an x-ray analysis system, the x-ray analysis system comprising the x-ray engine including:
an x-ray excitation path; and
an x-ray detection path;
wherein the x-ray excitation and/or the x-ray detection paths define the x-ray analysis focal area in said chamber.

### Claim 5 (depends on 4)

The combination of claim 4, wherein the focal area is a focal point.

### Claim 6 (depends on 5)

The combination of claim 5, wherein the focal point is defined by focused x-rays to/from at least one focusing optic in the x-ray excitation path and/or the x-ray detection path.

### Claim 7 (depends on 6)

The combination of claim 6, wherein the at least one focusing optic is at least one curved diffracting optic or polycapillary optic.

### Claim 8 (depends on 6)

The combination of claim 6, wherein the at least one focusing optic is at least one focusing monochromatic optic.

### Claim 9 (depends on 8)

The combination of claim 8, wherein the at least one focusing monochromatic optic is a curved crystal optic or curved multi-layer optic.

### Claim 10 (depends on 5)

The combination of claim 5, wherein at least one focusing optic in the x-ray detection path is positioned such that an input focal point thereof is at the x-ray focal point, and corresponds to an output focal point of at least one focusing optic in the x-ray excitation path.

### Claim 11 (depends on 4)

The combination of claim 4, wherein the x-ray analysis system comprises a monochromatic wavelength-enabled XRF analyzer.

### Claim 12 (depends on 11)

The combination of claim 11, wherein the analyzer is an MWDXRF or ME-EDXRF analyzer.

### Claim 13 (depends on 1)

The apparatus of claim 1, further comprising a heating element to heat the sample stream for improving flow of the sample stream.

### Claim 14 (depends on 1)

The apparatus of claim 1, wherein the sample comprises a petroleum-based product requiring the measurement of an analyte therein.

### Claim 15

The apparatus of 1, wherein an analyte measured is at least one element chosen from the following list: S, Cl, P, K, Ca, V, Mn, Fe, Co, Ni, Cu, Zn, Hg, As, Pb, and Se.

### Claim 16 (depends on 1)

The apparatus of claim 1, wherein the stream is crude oil, and an analyte measured is chlorine.

### Claim 17

An x-ray analysis system comprising:
an x-ray engine having an x-ray source for producing an x-ray excitation beam, the x-ray excitation beam directed toward an x-ray analysis focal area;
a sample chamber for presenting a sample to the x-ray analysis focal area, the x-ray analysis focal area disposed within a sample analysis area defined within the chamber;
an x-ray detection path for collecting secondary x-rays from the focal area and directing the secondary x-rays toward a detector;
an x-ray transparent barrier on a wall of the chamber through which the x-ray excitation beam and the secondary x-rays pass; and
a blocking structure disposed asymmetrically about a central axis of the x-ray analysis focal area and/or the sample analysis area and partially blocking the sample analysis area, for creating sample stream turbulence in the sample analysis area and over the barrier.

### Claim 18 (depends on 17)

The system of claim 17, wherein the analyzer comprises a monochromatic wavelength-enabled XRF analyzer.

### Claim 19 (depends on 18)

The system of claim 18, wherein the system is an MWDXRF or ME-EDXRF analyzer.

### Claim 20 (depends on 17)

The system of claim 17, wherein an analyte measured is at least one element chosen from the following list: S, Cl, P, K, Ca, V, Mn, Fe, Co, Ni, Cu, Zn, Hg, As, Pb, and Se.

### Claim 21 (depends on 17)

The system of claim 17, wherein the stream is crude, and an analyte measured is chlorine.
