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Analysis Results for Lunar Soil Simulant Using a Portable X-Ray Fluorescence Analyzer

R. E. Boothe · 2006

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NASA/TM—2006–214709 Analysis Results for Lunar Soil Simulant Using a Portable X-Ray Fluorescence Analyzer R.E. Boothe Marshall Space Flight Center, Marshall Space Flight Center, Alabama November 2006

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The NASA STI Program Office…in Profile Since its founding, NASA has been dedicated to the advancement of aeronautics and space science. The NASA Scientific and Technical Information (STI) Program Office plays a key part in helping NASA maintain this important role. The NASA STI Program Office is operated by Langley Research Center, the lead center for NASA’s scientific and technical information. The NASA STI Program Office provides access to the NASA STI Database, the largest collection of aeronautical and space science STI in the world. The Program Office is also NASA’s institutional mechanism for disseminating the results of its research and development activities. These results are published by NASA in the NASA STI Report Series, which includes the following report types: • TECHNICAL PUBLICATION. Reports of completed research or a major significant phase of research that present the results of NASA programs and include extensive data or theoretical analysis. Includes compilations of significant scientific and technical data and information deemed to be of continuing reference value. NASA’s counterpart of peerreviewed formal professional papers but has less stringent limitations on manuscript length and extent of graphic presentations. • TECHNICAL MEMORANDUM. Scientific and technical findings that are preliminary or of specialized interest, e.g., quick release reports, working papers, and bibliographies that contain minimal annotation. Does not contain extensive analysis. • CONTRACTOR REPORT. Scientific and technical findings by NASA-sponsored contractors and grantees. • CONFERENCE PUBLICATION. Collected papers from scientific and technical conferences, symposia, seminars, or other meetings sponsored or cosponsored by NASA. • SPECIAL PUBLICATION. Scientific, technical, or historical information from NASA programs, projects, and mission, often concerned with subjects having substantial public interest. • TECHNICAL TRANSLATION. English-language translations of foreign scientific and technical material pertinent to NASA’s mission. Specialized services that complement the STI Program Office’s diverse offerings include creating custom thesauri, building customized databases, organizing and publishing research results…even providing videos. For more information about the NASA STI Program Office, see the following: • Access the NASA STI Program Home Page at http://www.sti.nasa.gov • E-mail your question via the Internet to help@sti.nasa.gov • Fax your question to the NASA Access Help Desk at 301–621–0134 • Telephone the NASA Access Help Desk at 301–621–0390 • Write to: NASA Access Help Desk NASA Center for AeroSpace Information 7121 Standard Drive Hanover, MD 21076–1320 301–621–0390

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NASA/TM—2006–214709 Analysis Results for Lunar Soil Simulant Using a Portable X-Ray Fluorescence Analyzer R.E. Boothe Marshall Space Flight Center, Marshall Space Flight Center, Alabama Natonal Aeronautcs and Space Admnstraton Marshall Space Flght Center • MSFC, Alabama 35812 November 2006 

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Acknowledgments The author gratefully acknowledges the contrbutons of Therese Howe wth KeyMaster Technologes, Inc., Kennewck, WA. TRAdemARkS Trade names and trademarks are used in this report for identification only. This usage does not constitute an official endorsement, ether expressed or mpled, by the Natonal Aeronautcs and Space Admnstraton. Avalable from: NASA Center for AeroSpace Informaton 7121 Standard Drve Hanover, MD 21076–1320 301–621–0390  Natonal Techncal Informaton Servce 5285 Port Royal Road Springfield, VA 22161 703–487–4650

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TABLe OF CONTeNTS 1. INTRODUCTION ............................................................................................................................ 1 2. INSTRUMENT DESCRIPTION ..................................................................................................... 2 3. TEST DESCRIPTION ...................................................................................................................... 4 4. TEST RESULTS ............................................................................................................................... 6 5. CONCLUSIONS .............................................................................................................................. 8 REFERENCES ..................................................................................................................................... 9 

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LIST OF FIGUReS 1. TRACeR™ III–IV portable XRF analyzer ............................................................................ 2 2. Example of analyss results dsplayed on the PDA ................................................................ 3 3. Example XRF spectrum of JSC–1 ......................................................................................... 6 LIST OF TABLeS 1. JSC–1 chemistry ..................................................................................................................... 5 2. JSC–1 analysis results using the TRACeR III–IV ................................................................. 7 v

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LIST OF ACRONYmS ANd SYmBOLS Al alumnum Ca calcum Cr chromum Fe ron JSC–1 Johnson Space Center number one K potassum Mg magnesum Mn manganese MSFC Marshall Space Flght Center Na sodum N nckel O oxygen P phosphorous PDA personal dgtal assstant S slcon SPIN slcon P-type ntrnsc N-type detector T ttanum TRACeR taggant recognton and authentcaton code enabled reader XRF x-ray fluorescence v

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v

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TECHNICAL MEMORANDUM ANALYSIS ReSULTS FOR LUNAR SOIL SImULANT USING THe A PORTABLe X-RAY FLUOReSCeNCe ANALYZeR 1. INTROdUCTION Long-term habtaton mssons on the Moon wll requre that natural lunar resources be used to minimize the amount of material and supplies that must be transported from Earth. For example, lunar soil will potentially be used for oxygen generation, water generation, and as filler for building blocks. NASA’s n stu fabrcaton and repar program s evaluatng portable technologes that can assess the chemistry of lunar soil and lunar soil simulants. This Technical Memorandum summarizes the analysis results of Johnson Space Center number one (JSC–1) lunar soil simulant using the taggant recognition and authentication code enabled reader (TRACeR™) III–IV handheld x-ray fluorescence (XRF) analyzer manufactured by KeyMaster Technologes, Inc. The focus of the evaluaton was to determne how well the current instrument configuration would detect and quantify the components of JSC–1. 1

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  1. INSTRUmeNT deSCRIPTION The TRACeR III–IV XRF analyzer was selected for evaluation because it provided the capability to detect and quantify elements with relatively low atomic weights including aluminum (Al), titanium (Ti), and silicon (Si) that are significant components of JSC–1. TRACeR is able to analyze for these elements because it generates a vacuum pressure of approximately 1 torr between the detector and the analyzer head by employing a detachable vacuum accessory. Although handheld XRF analyzers were available from several addtonal manufacturers at the tme ths study was conducted, they dd not have the capablty to provide quantification data for Al, Ti, or Si, and therefore were not tested. In addition to elemental analysis, the TRACeR III–IV can identify and classify metal alloys. The nstrument s programmed wth a database of alloy spectra that are mathematcally compared to sample spectra to find the best match. Alloy database classifications include iron (Fe), nickel (Ni), and Al. This capability might also prove to be useful during lunar missions if alloy identification is requred pror to repar and fabrcaton operatons. Figure 1 is a photograph of the TRACeR III–IV. The analyzer weighs approximately 4 lb and the analyzer/vacuum pump combination weighs approximately 9 lb. It can be operated using a personal digital assistant (PDA), which is the most portable configuration, and a computer. The instrument uses an x-ray tube as the source and has a Si P-type intrinsic N-type (SiPIN) detector. Figure 1. TRACeR III–IV portable XRF analyzer. Figure 2 shows an example of the analysis results as viewed on the PDA screen. An XRF spectrum s provded, along wth a breakdown of elemental components and weght percentages. 2

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s results dsplayed on the PDA.1 Fgure 2. Example of analys 3

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  1. TeST deSCRIPTION JSC–1 powder was analyzed using a data collection time of 180 s per test and an instrument power level of 15 kV. The simulant was analyzed five times and the results were averaged. The vacuum accessory was employed to enhance detecton of Al, S, and T. The nstrument was operated usng a laptop computer rather than the PDA, because the laptop software provided the operator with more flexibility regarding the selecton of elements for quanttatve measurements. A calibration model had to be developed to obtain quantitative JSC–1 chemistry information. Feldspar, an alumnoslcate wth the general formula XAl(1–2)Si(2–3)O8, where X is sodium (Na), potassium (K), or calcium (Ca), was used to develop the model. Unfortunately, Feldspar was deficient as a calibration material for several reasons. As shown in table 1, it did not contain Ti, manganese (Mn), chromium (Cr), or phosphorous (P) which are all present in JSC–1. In addition, the Feldspar samples were in solid form while JSC–1 exists as a powder, and the XRF analysis can be impacted by a material’s physical characteristics. Even though these deficiencies were recognized, a more representative analog of JSC–1 could not be identified. 4

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Table 1. JSC–1 chemistry.* Major Components Oxide Concentration (wt%)** Standard Deviation (wt%) SiO2 47.71 0.1 TiO2 1.59 0.01 Al2O3 15.02 0.04 Fe2O3 3.44 0.03 FeO 7.35 0.05 MgO 9.01 0.09 CaO 10.42 0.03 Na2O 2.7 0.03 K2O 0.82 0.02 MnO 0.18 0 Cr2O3 0.04 0 P2O5 0.66 0.01 Total = 98.94 JSC–1 Trace Elements Element Concentration (ppm)** Standard Deviation (ppm) Scandium 29.2 0.5 Cobalt 47.7 1.6 Nickel 137 18 Rubidium 12.3 1.5 Cesium 0.339 0.01 Strontium 860 36 Barium 822 13 Lanthanum 48.2 0.9 Cerium 94.6 1.7 Neodymium 42 2 Samarium 7.44 0.13 Europium 2.18 0.04 Terbium 0.825 0.01 Ytterbium 1.99 0.04 Zirconium 125 3 Hafnium 3.55 0.08 Tantalum 1.96 0.04 Uranium 1.51 0.08 Thorium 5.65 0.07 Arsenic 18.7 8.9 Selenium <0.5 0 Antimony 0.564 0.57 Tungsten 36.1 2.6 Gold 40.7 29.4 Bromine 0.85 0.07 Lutetium 0.293 0.01 * Source — McKay, D.S.; Carter, J.L.; Boles, W.W.; Allen, C.C.; and Allton, J.H.: “JSC–1: A New Lunar Soil Simulant,” Engineering, Construction, and Operations in Space IV, American Society of Civil Engineers, pp. 857–866, 1994. ** Wt% and ppm data are the mean of three analyses. 5

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  1. TeST ReSULTS A representative XRF spectrum of JSC–1 obtained using the TRACeR III–IV is shown in figure 3, and table 2 summarizes the analysis results. Only the major elemental constituents including Na, Al, Si, K, Ca, Fe, and magnesium (Mg) could be detected and quantified. Mn and Ti were detected but could not be quantified since they were not included in the calibration model. Cr, P, and the numerous JSC–1 trace elements were below the nstrument’s detecton lmts. Standard devaton values for the measured weght percentages were low, whch ndcated that analysis results were consistent for multiple scans of JSC–1. The percentage error values for chemistry composition were very high, which was due in part to the nonoptimized calibration model. Figure 3. Example XRF spectrum of JSC–1. 6

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Table 2. JSC–1 analysis results using the TRACeR III–IV. Measured Wt% of Detected Elements (Present as Oxides) Test No. Na Mg Al 1 1.55 10.03 12.53 2 1.59 11.15 12.02 3 1.67 12.87 11.51 4 1.61 12.47 11.56 5 1.59 10.41 12.28 Average 1.6 11.38 11.98 Standard 0.04 1.25 0.44 Deviation Accepted Value 2.7 9 15 % Error 41% –26% 20% Si K Ca Fe 34.51 0.1 12.21 16.16 34.55 0.17 12.42 15.13 34.55 0.12 12.16 15.35 34.47 0.06 11 16.12 34.49 0.04 11.48 16.16 34.51 0.1 11.85 15.78 0.03 0.05 0.59 0.5 47 0.8 10.4 10.8 27% 88% –14% – 46% 7

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  1. CONCLUSIONS The TRACeR III–IV portable XRF analyzer was only able to detect and quantify constituents of JSC–1 that were present at weight levels of approximately 1–2 percent and higher. KeyMaster, the manufacturer, advised that quantification of Mn and Ti would likely be possible if they were included in the calbraton model. However, responses for Cr, P, and the trace elements would lkely reman below detection limits even with enhancement of the model. The instrument was stable in that repeated JSC–1 analysis provded consstent quanttatve chemstry values. Three significant efforts would be required to bring the TRACeR III–IV to a status more suitable for lunar missions: (1) PDA software modification to incorporate the JSC–1 analysis protocol, (2) development of an XRF standard, similar to JSC–1, and (3) refinement of the calibration model. 8

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ReFeReNCeS 1. “The Lab,” KeyMaster Technologes, Inc., http://www.keymastertech.com/lab.html, accessed October 31, 2006. 9

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Form Approved REPORT DOCUMENTATION PAGE OMB No. 0704-0188 Public reporting burden for this collection of information is estimated to average 1 hour per response, including the time for reviewing instructions, searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection of information. Send comments regarding this burden estimate or any other aspect of this collection of information, including suggestions for reducing this burden, to Washington Headquarters Services, Directorate for Information Operation and Reports, 1215 Jefferson Davis Highway, Suite 1204, Arlington, VA 22202-4302, and to the Office of Management and Budget, Paperwork Reduction Project (0704-0188), Washington, DC 20503 1. AGENCY USE ONLY (Leave Blank) 2. REPORT DATE November 2006 4. TITLE AND SUBTITLE 3. REPORT TYPE AND DATES COVERED Techncal Memorandum 5. FUNDING NUMBERS Analysis Results for Lunar Soil Simulant Using a Portable X-Ray Fluorescence Analyzer 6. AUTHORS R.E. Boothe 7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) George C. Marshall Space Flght Center Marshall Space Flght Center, AL 35812 9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES) Natonal Aeronautcs and Space Admnstraton Washngton, DC 20546–0001 11. SUPPLEMENTARY NOTES 8. PERFORMING ORGANIZATION REPORT NUMBER M–1176 10. SPONSORING/MONITORING AGENCY REPORT NUMBER NASA/TM—2006–214709 Prepared by the Engneerng Drectorate Materals Test Branch 12a. DISTRIBUTION/AVAILABILITY STATEMENT Unclassified-Unlimited Subject Category 35 Avalablty: NASA CASI 301–621–0390 13. ABSTRACT (Maximum 200 words) 12b. DISTRIBUTION CODE Lunar soil will potentially be used for oxygen generation, water generation, and as filler for building blocks durng habtaton mssons on the Moon. NASA’s n stu fabrcaton and repar program s evaluatng portable technologes that can assess the chemstry of lunar sol and lunar sol smulants. Ths Techncal Memorandum summarizes the results of the JSC–1 lunar soil simulant analysis using the TRACeR III–IV handheld x-ray fluorescence analyzer, manufactured by KeyMaster Technologies, Inc. The focus of the evaluation was to determine how well the current instrument configuration would detect and quantify the components of JSC–1. 14. SUBJECT TERMS Fluorescence, regolth, chemcal elements, analyss 17. SECURITY CLASSIFICATION 18. SECURITY CLASSIFICATION OF REPORT OF THIS PAGE Unclassified Unclassified NSN 7540-01-280-5500 10 15. NUMBER OF PAGES 16 16. PRICE CODE 19. SECURITY CLASSIFICATION 20. LIMITATION OF ABSTRACT OF ABSTRACT Unclassified Unlmted Standard Form 298 (Rev. 2-89) Prescribed by ANSI Std. 239-18 298-102

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National Aeronautics and Space Administration IS20 George C. Marshall Space Flight Center Marshall Space Flight Center, Alabama 35812

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