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(12) United States Patent (10) Patent No.: US 9,354.231 B1 Glover (45) Date of Patent: May 31, 2016

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(12) United States Patent (10) Patent No.: US 9,354.231 B1 Glover (45) Date of Patent: May 31, 2016 USOO9354231B1 (12) United States Patent (10) Patent No.: US 9,354.231 B1 Glover (45) Date of Patent: May 31, 2016 (54) REACTIVE SELF-INDICATING ABSORBENT Chemisorption of Cyanogen Chloride by Spinel Ferrite Magnetic Nanoparticles T. Grant Glover, Jared B. DeCoste, Daniel Sabo, and Z. MATERIALS, METHODS, AND SYSTEMS John Zhang Langmuir 2013, 29, 5500-5507.* Glover, T. Grant, et al., “Carbon-Silica Composite Adsorbent: Char (75) Inventor: Thomas Grant Glover, Bel Air, MD acterization and Adsorption of Light Gases.” Microporous and (US) Mesoporous Materials, 111, pp. 1-11, 2008. Peterson, Gregory W., et al., “Ammonia Vapor Removal by (73) Assignee: Leidos, Inc., Reston, VA (US) Cu(BTC) and Its Characterization by MAS NMR.” Journal of Physical Chemistry C, 113, pp. 13906-13917, 2009. Britt, David, et al., “Highly Efficient Separation of Carbon Dioxide (*) Notice: Subject to any disclaimer, the term of this by a Metal-Organic Framework Replete With Open Metal Sites.” patent is extended or adjusted under 35 Proceedings of the National Academy of Science, vol. 106, No. 49. U.S.C. 154(b) by 1165 days. pp. 20637-20640, Dec. 8, 2009. Britt, David, et al., “Metal-Organic Frameworks With High Capacity (21) Appl. No.: 13/189,736 and Selectivity for Harmful Gases.” Proceedings of the National Academy of Science, vol. 105, No. 33, pp. 11623-11627. Aug. 19, (22) Filed: Jul. 25, 2011 2008. * cited by examiner (51) Int. Cl. GOIN 27/2403 (2006.01) Primary Examiner — Krishnan S Menon GOIN33/543 (2006.01) Assistant Examiner — Dwan A Gerido (52) U.S. Cl. (74) Attorney, Agent, or Firm —Dawn-Marie Bey; Bey & CPC .......... G0IN33/5438 (2013.01); G0IN 27/403 Cotropia PLLC (2013.01) (57) ABSTRACT (58) Field of Classification Search The present disclosure relates, according to some embodi ments, reactive self-indicating adsorbent materials, methods, CPC. G01N 33/5438: G01N 27/403; G01N 27/06; and systems. A system may comprise, for example, a reactive G01N30/96; G01N 27/021; G01N 27/3271; self indicating adsorbent material, wherein the reactive self G01N 2030/965; G01N 27/126; G01N 27/12: indicating adsorbent material comprises at least one Super G01N 27/60; G01N33/0031: G01N 27/002: paramagnetic particle and a semi permeable Support, wherein B01J 19/0046; B01J 2219/00527; B01J the at least one Super paramagnetic particle is configured Such 2219/00585 that at least one magnetic property of the at least one Super USPC .......................................... 436/149, 150, 151 paramagnetic particle changes upon contact with an adsor bate; and/or at least one detector configured and arranged to See application file for complete search history. detect the at least one magnetic property. In some embodi ments, a method for assessing the performance and/or (56) References Cited remaining life of an adsorbent material may comprise (a) U.S. PATENT DOCUMENTS contacting a fluid comprising an adsorbate with the adsorbent material under conditions that permit the adsorbate to contact 4,254,616 A * 3/1981 Siminski et al. ............. 60/39.12 the at least one Superparamagnetic particle, whereina change 6,202,471 B1* 3/2001 Yadav et al. ................. T3/31.05 in a magnetic property of the at least one Super paramagnetic particle occurs upon contact with the adsorbate; (b) detecting OTHER PUBLICATIONS the magnetic property of the at least one Super paramagnetic Adsorption of Sulfur Dioxide by CoFe2O4 Spinel Ferrite particle; and/or (c) comparing the detected magnetic property Nanoparticles and Corresponding Changes in Magnetism T. Grant to a reference to produce an assessment of the performance Glover, Daniel Sabo, Lisa A. Vaughn, Joseph A. Rossin, and Z. John and/or remaining life of the adsorbent material. Zhang Langmuir 2012, 28, 5695-5702.* 16 Claims, 22 Drawing Sheets INLET FILTER OUTLET U.S. Patent May 31, 2016 Sheet 1 of 22 US 9,354.231 B1 FIG. I. U.S. Patent May 31, 2016 Sheet 2 of 22 US 9,354.231 B1 210 FIG 2 U.S. Patent May 31, 2016 Sheet 3 of 22 US 9,354.231 B1 s s U.S. Patent May 31, 2016 Sheet 4 of 22 US 9,354.231 B1 exer ..., xx x x x x x x x Mr.x r >O OO QQ COO. M - {XX O <>< U.S. Patent May 31, 2016 Sheet 5 of 22 US 9,354.231 B1 066 6{DIH 096 096 U.S. Patent May 31, 2016 Sheet 6 of 22 US 9,354.231 B1 U.S. Patent May 31, 2016 Sheet 7 of 22 US 9,354.231 B1 s U.S. Patent May 31, 2016 Sheet 8 of 22 US 9,354.231 B1 re in a a 4. -- \ O 1 2 3 4 5 6 7 8 9 10x10 time (min/g) FIG. I.4 U.S. Patent May 31, 2016 Sheet 9 of 22 US 9,354.231 B1 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 20 (degrees) FIG. I5 U.S. Patent May 31, 2016 Sheet 10 of 22 US 9,354.231 B1 FIG. I.6A U.S. Patent May 31, 2016 Sheet 11 of 22 US 9,354.231 B1 FIG. I.6B U.S. Patent May 31, 2016 Sheet 12 of 22 US 9,354.231 B1 1 OO 8O al e f S.E 60 9. " c S c o es c 40 > O O.O O.2 O.4 O.6 O.8 1.O PIP FIG. 1 7 U.S. Patent May 31, 2016 Sheet 13 of 22 US 9,354.231 B1 1.1 -T-I-T-I-T Saturation Poin 1.O a as: H test 1 are - a - are - rare - up test 2 --------- . test 3 g Sl C C X 9 s s - 10 11 12x10 time (ming) FIG. 18 U.S. Patent May 31, 2016 Sheet 14 of 22 US 9,354.231 B1 O.40 O.35 O.30 O.25 O.20 | 0.15 O. 10 OO5 4000 3600 32OO 2800 2400 2000 1600 12OO 800 Wavenumber (cm) FIG. I9 U.S. Patent May 31, 2016 Sheet 15 of 22 US 9,354.231 B1 o cN o co ve 174 172 170 168 166 164 162 160 158. 156 154 binding energy (eV) FIG. 20 U.S. Patent May 31, 2016 Sheet 16 of 22 US 9,354.231 B1 SO exposed Native MNPS i 820 810 800 790 780 770 760 binding enegy (eV) FIG 21 U.S. Patent May 31, 2016 Sheet 17 of 22 US 9,354.231 B1 SO exposed Native MNPS i 545 540 535 530 525 52O 515 binding enegy (eV) FIG. 22 U.S. Patent May 31, 2016 Sheet 18 of 22 US 9,354.231 B1 SO exposed Native MNPS 740 730 720 710 700 690 binding enegy (eV) FIG. 23 U.S. Patent May 31, 2016 Sheet 19 of 22 US 9,354.231 B1 - Exposed to SO - Unexposed Particles 10 20 30 40 50 60 70 8O 90 2-theta degrees FIG. 24 U.S. Patent May 31, 2016 Sheet 20 of 22 US 9,354.231 B1 100 8O CoFeO - - - - - - - CoFe2O4 60 exposed to SO an 40 Sp O i 20 E O2 O s .9 d -20 (s s -100 -50x1O -40 -30 -20 - 10 0 1 O 20 30 40 50 Magnetic Field (G) FIG. 25 U.S. Patent May 31, 2016 Sheet 22 of 22 US 9,354.231 B1 *HNÅRHC-- .„…* 00’000900000;00'000€00’000Z GEZITWW.HONuuelfi/u?u.BWIL '91-7ZZ C d 00Z| 000|| d 009 007 US 9,354.231 B1 1. 2 REACTIVE SELF-INDICATING ABSORBENT embodiments, may be non-invasive. In some embodiments, a MATERIALS, METHODS, AND SYSTEMS magnetic property to be detected may be selected from rem nant magnetization, coercivity, Saturation magnetization, FIELD OF THE DISCLOSURE and/or combinations thereof. In some embodiments, a Super paramagnetic particle may The present disclosure relates, in Some embodiments, reac comprise a crystalline face centered cubic structure. A Super tive self-indicating adsorbent materials, methods, and sys paramagnetic particle may comprise a spinel ferrite accord temS. ing to Some embodiments. A Superparamagnetic particle may have, in some embodiments, a chemical formula MFeO. BACKGROUND OF THE DISCLOSURE 10 where M represents a transition metal (e.g., cobalt, copper, iron, magnesium, manganese, nickel, Zinc, and/or combina Frequently filters are simply changed on a set schedule tions thereof). Cobalt, iron, oxygen, and/or combinations regardless of their ongoing performance and/or remaining thereofmay be desirable components of a Super paramagnetic capacity. For example, the filters that are used in research particle in Some embodiments. A Superparamagnetic particle buildings to filterhood exhausts are typically changed on a 15 may have, according to Some embodiments, a generally schedule regardless of remaining filter capacity. This spherical shape or a generally cuboidal shape. approach may be inefficient in that filters may be changed According to some embodiments, MNPs and/or adsorbent prior to exhaustion and/or ineffective in that filters may be left materials may be contacted with and/or bind one or more of a in use beyond their actual ability to perform. wide variety of adsorbates. Examples of adsorbates may Determining the remaining life of a carbonair filter may be include, without limitation, Agent 15 (BZ), ammonia, an encumbered by a need to remove it from service. For arsine, arsenic pentafluoride, bis(trifluoromethyl)peroxide, example, upon removal of a filter from service, a carbon boron tribromide, boron trichloride, boron trifluoride, bro sample may be taken from the filter and properties of the mine, bromine chloride, bromomethane, carbon monoxide, carbon may be assessed in a lab.
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