US4592082A
Expired / Lapsed
US
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Quantitative determination of mineral composition by powder X-ray diffraction
Assignee: United States Department of Energy
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Filing: 1984-08-10
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Granted: 1986-05-27
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Expires: 2004-08-10
Abstract
Abstract An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.
Inventors
- 👤 Gayle A. Pawloski
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 18:29
CPC Classifications
G; G01; G01N; G01N23/00; G01N23/20; G01N23/207; G01N33/00; G01N33/24
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
266 words
A method of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, wherein n=13, where m≦n, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K j =(X j /X l )(I l /I j ) for each mineral (j=2 . . . n) in the group of known minerals (j=2 . . . n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample; indentifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X j /X l for each mineral (j=2 . . . m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I j of each mineral in the test sample to the measured highest integrated intensity peak I l of the reference mineral in the test sample, and from the previously determined standard coefficients, X j /X l =K j (I j /I l ); and calculating the weight fraction of the reference mineral X l , and the weight fractions X j of each mineral (j=2 . . . m) from the condition that the sum of the weight fractions is 1, ΣX i =1 (i=1 . . . m).
Claim 2
Independent Claim
266 words
A method of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, wherein n=13, where m≦n, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K j =(X j /X l )(I l /I j ) for each mineral (j=2 . . . n) in the group of known minerals (j=2 . . . n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample; indentifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X j /X l for each mineral (j=2 . . . m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I j of each mineral in the test sample to the measured highest integrated intensity peak I l of the reference mineral in the test sample, and from the previously determined standard coefficients, X j /X l =K j (I j /I l ); and calculating the weight fraction of the reference mineral X l , and the weight fractions X j of each mineral (j=2 . . . m) from the condition that the sum of the weight fractions is 1, ΣX i =1 (i=1 . . . m).
Claim 3
Dependent Claim
50 words
The method of claim 1 wherein the test sample does not contain the reference mineral, further comprising the steps of: adding a known amount of the reference mineral to the test sample; and normalizing the calculated weight fractions of the minerals to correct for the amount of reference mineral added.
Claim 4
Dependent Claim
11 words
The method of claim 1 wherein the reference mineral is quartz.
Claim 5
Dependent Claim
11 words
The method of claim 2 wherein the reference mineral is quartz.
Claim 6
Dependent Claim
40 words
The method of claim 1 wherein the step of obtaining the x-ray diffraction pattern of the test sample is performed using a goniometer having a theta compensating slit to keep a constant area of the sample irradiated during a scan.
Claim 7
Dependent Claim
12 words
The method for claim 5 wherein the scan covers the range 2°-45°2θ.
Claim 8
Dependent Claim
17 words
The method of claim 6 wherein the scan is performed in steps of 0.04°2θ every 4 seconds.
Claim 9
Dependent Claim
24 words
The method of claim 1 wherein the standard coefficients are determined from a measured calibration curve of each mineral relative to the reference mineral.
Claim 10
Dependent Claim
27 words
The method of claim 8 wherein the standard coefficients are determined by a least squares fit of the measured values for a number of different weight ratios.
Claim 11
Independent Claim
303 words
A method of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, where m≦n, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K j =(X j /X l )(I l /I j ) for each mineral (j=2 . . . n) in the group of known minerals (j=2 . . . n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample using a goniometer having a theta compensating slit to keep a constant area of the sample irradiated during a scan, wherein the scan covers the range 2°-45° 2θ and is performed in steps of 0.04° 2θ every 4 seconds; indentifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X j /X l for each mineral (j=2 . . . m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I j of each mineral in the test sample to the measured highest integrated intensity peak I l of the reference mineral in the test sample, and from the previously determined standard coefficients, X j /X l =K j (I j /I l ); and calculating the weight fraction of the reference mineral X l , and the weight fractions X j of each mineral (j=2 . . . m) from the condition that the sum of the weight fractions is 1, ΣX i =1 (i=1 . . . m).
Claim 12
Independent Claim
303 words
A method of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, where m≦n, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K j =(X j /X l )(I l /I j ) for each mineral (j=2 . . . n) in the group of known minerals (j=2 . . . n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample using a goniometer having a theta compensating slit to keep a constant area of the sample irradiated during a scan, wherein the scan covers the range 2°-45° 2θ and is performed in steps of 0.04° 2θ every 4 seconds; indentifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X j /X l for each mineral (j=2 . . . m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I j of each mineral in the test sample to the measured highest integrated intensity peak I l of the reference mineral in the test sample, and from the previously determined standard coefficients, X j /X l =K j (I j /I l ); and calculating the weight fraction of the reference mineral X l , and the weight fractions X j of each mineral (j=2 . . . m) from the condition that the sum of the weight fractions is 1, ΣX i =1 (i=1 . . . m).
References Cited (Backward Citations)
US3102952A
Cited
US3027086A
Cited
US2897367A
Cited
US3079499A
Cited
US3260845A
Cited
US3322948A
Cited
US3428802A
Cited
US3855470A
Cited
JPS55158545A
Cited
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