US3764805A
Expired / Lapsed
US
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Control of propellant compositions by x-ray fluorescence analysis
Assignee: United States Department of the Army
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Filing: 1967-07-06
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Granted: 1973-10-09
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Expires: 1987-07-06
Abstract
Abstract The use of multiple linear regression analysis in correlating the data obtained by the X-ray fluorescence analysis of propellant compositions. Ingredient concentrations and particle sizes are predicted by means of multiple regression equations which relate characteristic emission line intensities with particle sizes and ingredient concentrations. These equations give more accurate predictions than simple regression equations which are commonly used.
Inventors
- 👤 B Alley
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 08:30
CPC Classifications
G; G01; G01N; G01N23/00; G01N23/22; G01N23/223; G01N2223/00; G01N2223/07; G01N2223/076
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
752 words
The method of analyzing propellant compositions containing light elements by means of X-ray emission spectrography wherein K Alpha emission lines are transmitted through a thin film sample having a thickness lying in a range of film thickness variations, said method comprising the steps of: a. measuring with an X-ray spectrograph the K Alpha emission line intensity of an aluminum standard transmitted separately through each sample of a plurality of pairs of samples of said film, said plurality covering the range of film thickness variations in said film, recording the number of seconds for the aluminum K Alpha radiation for each sample of said plurality of pairs of samples of film to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; b. measuring with said spectrograph the K Alpha emission line intensity of a light element from a standard containing said light element, said K Alpha emission line from said light element being transmitted separately through each sample of said plurality of pairs of samples of film, recording the number of seconds required by each member of said plurality of pairs of samples of film to transmit sufficient K Alpha radiation from said light element to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample member of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; c. plotting on a graph all of the ratios derived from measuring the aluminum K Alpha radiation from one sample of each of said plurality of pairs of samples of film against the ratio derived from measuring the K Alpha radiation of said light element from said one sample of each of said plurality of pairs of samples of film and plotting on said graph the value of said reciprocal of all of the ratios derived from measuring the aluminum K Alpha radiation from said one sample of each of said plurality of pairs of samples of film against the value of said reciprocal of the ratio derived from measuring the K Alpha radiation from said light element from said one sample of each of said plurality of pairs of samples of film; d. measuring with said spectrograph the K Alpha emission line intensity in counts per second for the K Alpha radiation transmitted from said aluminum standard through each of the members of a pair of samples of said thin film to reach a predetermined fixed count, determining the aluminum K Alpha intensity ratio of the aluminum K Alpha intensity transmitted through one of said members to the aluminum K Alpha intensity transmitted through the other of said members, and selecting from said graph as a correction factor the ratio of said light element on said graph corresponding to said aluminum K Alpha intensity ratio; e. measuring with said spectrograph the K Alpha emission line intensity of said light element from said standard containing said light element in counts per second for the K Alpha radiation transmitted through said other member of said pair of samples of thin film to reach a predetermined fixed count, measuring the K Alpha emission line intensity of said light element in a sample of said composition in counts per second for the K Alpha radiation transmitted through said one of said other member of said pair of samples to reach a predetermined fixed counT, and determining the ratio of said K Alpha intensity from said light element in said composition to said K Alpha intensity from said light element in said standard; f. dividing said ratio of said K Alpha intensity from said light element in said composition to said K Alpha intensity from said light element in said standard by said correction factor to determine the corrected analytical intensity ratio of the K Alpha intensity of said light element in said composition to the K Alpha intensity of said light element in said standard containing said light element; and g. applying said corrected analytical intensity ratios to multiple regression means to determine the concentrations of ingredients, each containing a said light element, and the particle sizes of solid ingredients, each containing a said light element.
Claim 2
Independent Claim
752 words
The method of analyzing propellant compositions containing light elements by means of X-ray emission spectrography wherein K Alpha emission lines are transmitted through a thin film sample having a thickness lying in a range of film thickness variations, said method comprising the steps of: a. measuring with an X-ray spectrograph the K Alpha emission line intensity of an aluminum standard transmitted separately through each sample of a plurality of pairs of samples of said film, said plurality covering the range of film thickness variations in said film, recording the number of seconds for the aluminum K Alpha radiation for each sample of said plurality of pairs of samples of film to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; b. measuring with said spectrograph the K Alpha emission line intensity of a light element from a standard containing said light element, said K Alpha emission line from said light element being transmitted separately through each sample of said plurality of pairs of samples of film, recording the number of seconds required by each member of said plurality of pairs of samples of film to transmit sufficient K Alpha radiation from said light element to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample member of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; c. plotting on a graph all of the ratios derived from measuring the aluminum K Alpha radiation from one sample of each of said plurality of pairs of samples of film against the ratio derived from measuring the K Alpha radiation of said light element from said one sample of each of said plurality of pairs of samples of film and plotting on said graph the value of said reciprocal of all of the ratios derived from measuring the aluminum K Alpha radiation from said one sample of each of said plurality of pairs of samples of film against the value of said reciprocal of the ratio derived from measuring the K Alpha radiation from said light element from said one sample of each of said plurality of pairs of samples of film; d. measuring with said spectrograph the K Alpha emission line intensity in counts per second for the K Alpha radiation transmitted from said aluminum standard through each of the members of a pair of samples of said thin film to reach a predetermined fixed count, determining the aluminum K Alpha intensity ratio of the aluminum K Alpha intensity transmitted through one of said members to the aluminum K Alpha intensity transmitted through the other of said members, and selecting from said graph as a correction factor the ratio of said light element on said graph corresponding to said aluminum K Alpha intensity ratio; e. measuring with said spectrograph the K Alpha emission line intensity of said light element from said standard containing said light element in counts per second for the K Alpha radiation transmitted through said other member of said pair of samples of thin film to reach a predetermined fixed count, measuring the K Alpha emission line intensity of said light element in a sample of said composition in counts per second for the K Alpha radiation transmitted through said one of said other member of said pair of samples to reach a predetermined fixed counT, and determining the ratio of said K Alpha intensity from said light element in said composition to said K Alpha intensity from said light element in said standard; f. dividing said ratio of said K Alpha intensity from said light element in said composition to said K Alpha intensity from said light element in said standard by said correction factor to determine the corrected analytical intensity ratio of the K Alpha intensity of said light element in said composition to the K Alpha intensity of said light element in said standard containing said light element; and g. applying said corrected analytical intensity ratios to multiple regression means to determine the concentrations of ingredients, each containing a said light element, and the particle sizes of solid ingredients, each containing a said light element.
Claim 3
Dependent Claim
14 words
The method of claim 1 wherein said concentrations of said ingredients are held constant.
Claim 4
Dependent Claim
16 words
The method of claim 1 wherein said particle sizes of said solid ingredients are held constant.
Claim 5
Dependent Claim
22 words
The method of claim 1 wherein said particle sizes of said solid ingredients and said concentrations of said ingredients are held constant.
Claim 6
Dependent Claim
36 words
The method of claim 1 wherein said corrected analytical intensity ratios are determined from the same composition and are used to derive any combination of said ingredients concentrations and said particle sizes in the same composition.
Claim 7
Independent Claim
702 words
The method of analyzing compositions containing a light element to determine the corrected analytical ratio of said element in said composition by means of X-ray emission spectrography wherein the K Alpha lines are transmitted through a thin film sample having a thickness lying in a range of film thickness variations, said method comprising the steps of: a. Measuring with an X-ray spectrograph the K Alpha emission line intensity of an aluminum standard transmitted separately through each sample of a plurality of pairs of samples of said film, said plurality covering the range of film thickness variations in said film, recording the number of seconds for the aluminum K Alpha radiation for each sample of said plurality of pairs of samples of film to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample of each pair of said plurality of pairs of sample of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; b. Measuring with said spectrograph the K Alpha emission line intensity of a light element from a standard containing said light element, said K Alpha emission line from said light element being transmitted separately through each sample of said plurality of pairs of samples of film, recording the number of seconds required by each member of said plurality of pairs of samples of film to transmit sufficient K Alpha radiation from said element to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample member of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; c. Plotting on a graph all of the ratios derived from measuring the aluminum K Alpha radiation from one sample of each of said plurality of pairs of samples of film against the ratio derived from measuring the K Alpha radiation of said element from said one sample of each of said plurality of pairs of samples of film and plotting on said graph the value of said reciprocal of all of the ratios derived from measuring the aluminum K Alpha radiation from said one sample of each of said plurality of pairs of samples of film against the value of said reciprocal of the ratio derived from measuring the K Alpha radiation from said element from said one sample of each of said plurality of pairs of samples of film. d. Measuring with said spectrograph the K Alpha emission lIne intensity in counts per second for the K Alpha radiation transmitted from said aluminum standard through each of the members of a pair of samples of said thin film to reach a predetermined fixed count, determining the aluminum K Alpha intensity ratio of the aluminum K Alpha intensity transmitted through one of said members to the aluminum K Alpha intensity transmitted through the other of said members, and selecting from said graph as a correction factor the ratio of said element on said graph corresponding to said aluminum K Alpha ratio; e. Measuring with said spectrograph the K Alpha emission line intensity of said element from said standard containing said element in counts per second for the K Alpha radiation transmitted through said other member of said pair of samples of thin film to reach a predetermined fixed count, measuring the K Alpha emission line intensity of said element in a sample of said composition in counts per second for the K Alpha radiation transmitted through said one of said other member of said pair of samples to reach a predetermined fixed count, and determining the ratio of said K Alpha intensity from said element in said composition to said K Alpha intensity from said element in said standard; f. dividing said ratio of said K Alpha intensity from said element in said composition to said K Alpha intensity from said element in said standard by said correction factor to determine the corrected analytical ratio of the K Alpha intensity of said light element in said standard containing said light element.
Claim 8
Independent Claim
702 words
The method of analyzing compositions containing a light element to determine the corrected analytical ratio of said element in said composition by means of X-ray emission spectrography wherein the K Alpha lines are transmitted through a thin film sample having a thickness lying in a range of film thickness variations, said method comprising the steps of: a. Measuring with an X-ray spectrograph the K Alpha emission line intensity of an aluminum standard transmitted separately through each sample of a plurality of pairs of samples of said film, said plurality covering the range of film thickness variations in said film, recording the number of seconds for the aluminum K Alpha radiation for each sample of said plurality of pairs of samples of film to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample of each pair of said plurality of pairs of sample of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; b. Measuring with said spectrograph the K Alpha emission line intensity of a light element from a standard containing said light element, said K Alpha emission line from said light element being transmitted separately through each sample of said plurality of pairs of samples of film, recording the number of seconds required by each member of said plurality of pairs of samples of film to transmit sufficient K Alpha radiation from said element to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample member of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; c. Plotting on a graph all of the ratios derived from measuring the aluminum K Alpha radiation from one sample of each of said plurality of pairs of samples of film against the ratio derived from measuring the K Alpha radiation of said element from said one sample of each of said plurality of pairs of samples of film and plotting on said graph the value of said reciprocal of all of the ratios derived from measuring the aluminum K Alpha radiation from said one sample of each of said plurality of pairs of samples of film against the value of said reciprocal of the ratio derived from measuring the K Alpha radiation from said element from said one sample of each of said plurality of pairs of samples of film. d. Measuring with said spectrograph the K Alpha emission lIne intensity in counts per second for the K Alpha radiation transmitted from said aluminum standard through each of the members of a pair of samples of said thin film to reach a predetermined fixed count, determining the aluminum K Alpha intensity ratio of the aluminum K Alpha intensity transmitted through one of said members to the aluminum K Alpha intensity transmitted through the other of said members, and selecting from said graph as a correction factor the ratio of said element on said graph corresponding to said aluminum K Alpha ratio; e. Measuring with said spectrograph the K Alpha emission line intensity of said element from said standard containing said element in counts per second for the K Alpha radiation transmitted through said other member of said pair of samples of thin film to reach a predetermined fixed count, measuring the K Alpha emission line intensity of said element in a sample of said composition in counts per second for the K Alpha radiation transmitted through said one of said other member of said pair of samples to reach a predetermined fixed count, and determining the ratio of said K Alpha intensity from said element in said composition to said K Alpha intensity from said element in said standard; f. dividing said ratio of said K Alpha intensity from said element in said composition to said K Alpha intensity from said element in said standard by said correction factor to determine the corrected analytical ratio of the K Alpha intensity of said light element in said standard containing said light element.
Claim 9
Dependent Claim
33 words
The method of claim 6 wherein said composition comprises an uncured mixture of polybutadiene-acrylic acid copolymer, powdered aluminum, ammonium perchlorate, and a member selected from the group consisting of ferric oxide and ferrocene.
Claim 10
Dependent Claim
11 words
The method of claim 6 wherein said light element is chlorine.
Claim 11
Dependent Claim
13 words
The method of claim 8 wherein said thin film is polyethylene terephthalate resin.
Claim 12
Dependent Claim
50 words
The method of claim 9 wherein said standard containing said light element is a pellatized mixture comprising about 35 percent by weight sodium chloride, about 22 percent by weight aluminum powder, 41 percent by weight methyl cellulose, 0.8 percent by weight ferric oxide, and 1.2 percent by weight zinc sulfide.
Claim 13
Dependent Claim
11 words
The method of claim 6 wherein said light element is aluminum.
Claim 14
Dependent Claim
11 words
The method of claim 6 wherein said light element is sulfur.
Claim 15
Dependent Claim
434 words
In the process of analyzing compositions containing a light element by X-ray spectrography wherein the K Alpha emission lines are transmitted through a thin, transparent film sample having a thickness lying in a range of film thickness variations, the improvement which consists of a method for determining a correction factor for said film, said method comprising the steps of: a. Measuring with an X-ray spectrograph the K Alpha emission line intensity of an aluminum standard transmitted separately through each sample of a plurality of pairs of samples of said film, said plurality covering the range of film thickness variations in said film, recording the number of seconds for the aluminum K Alpha radiation for each sample of said plurality of pairs of samples of film to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ration; b. Measuring with said spectrograph the K Alpha emission line intensity of a light element from a standard containing said light element, said K Alpha emission line from said light element being transmitted separately through each sample of said plurality of pairs of samples of film, recording the number of seconds required by each member of said plurality of pairs of samples of film to transmit sufficient K Alpha radiation from said element to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample member of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; c. Plotting on a graph all of the ratios derived from measuring the aluminum K Alpha radiation from one sample of each of said plurality of pairs of samples of film against the ratio derived from measuring the K Alpha radiation of said element from said one sample of each of said plurality of pairs of samples of film and plotting on said graph the value of said reciprocal of all of the ratios derived from measuring the aluminum K Alpha radiation from said one sample of each of said plurality of pairs of samples of film against the value of said reciprocal of the ratio derived from measuring the K Alpha radiation from said element from said one sample of each of said plurality of pairs of samples of film.
Claim 16
Dependent Claim
434 words
In the process of analyzing compositions containing a light element by X-ray spectrography wherein the K Alpha emission lines are transmitted through a thin, transparent film sample having a thickness lying in a range of film thickness variations, the improvement which consists of a method for determining a correction factor for said film, said method comprising the steps of: a. Measuring with an X-ray spectrograph the K Alpha emission line intensity of an aluminum standard transmitted separately through each sample of a plurality of pairs of samples of said film, said plurality covering the range of film thickness variations in said film, recording the number of seconds for the aluminum K Alpha radiation for each sample of said plurality of pairs of samples of film to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ration; b. Measuring with said spectrograph the K Alpha emission line intensity of a light element from a standard containing said light element, said K Alpha emission line from said light element being transmitted separately through each sample of said plurality of pairs of samples of film, recording the number of seconds required by each member of said plurality of pairs of samples of film to transmit sufficient K Alpha radiation from said element to reach a predetermined fixed count, subsequently determining the ratio of the number of seconds of one sample member of each pair of said plurality of pairs of samples of film to the number of seconds of the other sample of said pair, and determining the value of the reciprocal of said ratio; c. Plotting on a graph all of the ratios derived from measuring the aluminum K Alpha radiation from one sample of each of said plurality of pairs of samples of film against the ratio derived from measuring the K Alpha radiation of said element from said one sample of each of said plurality of pairs of samples of film and plotting on said graph the value of said reciprocal of all of the ratios derived from measuring the aluminum K Alpha radiation from said one sample of each of said plurality of pairs of samples of film against the value of said reciprocal of the ratio derived from measuring the K Alpha radiation from said element from said one sample of each of said plurality of pairs of samples of film.
Claim 17
Dependent Claim
64 words
The improvement according to claim 13 wherein said standard containing said light element is a composition comprising 20 percent to 60 percent by weight alkali metal chloride, 0.5 percent to 5 percent by weight zinc sulfide, 0.5 percent to 5 percent by weight ferric oxide, 10 percent to 30 percent by weight powdered aluminum, and 25 percent to 45 percent by weight methyl cellulose.
Claim 18
Dependent Claim
12 words
The improvement according to claim 14 wherein said light element is chlorine.
Claim 19
Dependent Claim
12 words
The improvement according to claim 14 wherein said light element is aluminum.
Claim 20
Dependent Claim
12 words
The improvement according to claim 14 wherein said light element is sulfur.
References Cited (Backward Citations)
US3591803A
Cited
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