[Ifeffit] sample preparation for liquid samples

Matthew Marcus mamarcus at lbl.gov
Tue Jan 11 11:52:20 CST 2011


Charles Supper sells capillaries with 10um wall thickness and ID ranging from 0.3 to 2.5mm, in quartz, borosilicate or regular glass.  These make nice sample holders
if your beam is small enough.  You can either work in transmission, making the thickness and concentration such that the edge jump is ~1, or in fluorescence, making
the edge jump <<1 or the absorption by the Mn << that from the water.
    mam
  ----- Original Message ----- 
  From: "Dr. Dariusz A. Zając" 
  To: XAFS Analysis using Ifeffit 
  Sent: Tuesday, January 11, 2011 1:31 AM
  Subject: Re: [Ifeffit] sample preparation for liquid samples


  Hi,
  you can use the standard sample holder for liquids, or to use something similar I constructed/used in Hasylab.
  For Mn:K edge you can also think about transmition measurements (if sample holder allows). For the concentrations - similar to solids, IMVHO. However it is good to measure few concentrations to compare them. You should also think about the effect of radiolysis in aqueous solution. To eliminate this the sample holder for liquids working in continuous-flow mode can be used.
  greetings
  kicaj
  W dniu 11-01-11 10:12, Polzer, Frank pisze: 
    Dear all,



    I would like to measure manganese oxide nanoparticles at the Mn K edge.



    The nanoparticles are affixed to polystyrene latex carrier particles (PS) and the whole composite material (MnO2 at PS with ca. 5 m-% MnO2 in the composite) is dispersed in water.



    Therefore we consider measuring the composite material in the dried state as a powder as well as in the dispersed state in water. The sample preparation for powders to me is quite straight forward, but I would really appreciate if somebody could share his experience with sample preparation and measurements of liquid samples.



    I think that aqueous samples are best measured in the fluorescence mode. That’s why I am concerned of problems like self-absorption and so on. 



    Can anybody tell my what is a good concentration range to overcome effects like self-absorption and how to get good fluorescence data in general? And what kind of sampler holder or materials (cuvettes, etc.) are best suited for aqueous samples?





    I am looking forward to receiving some helpful replies!





    Cheers,



    Frank





    Dipl. Chem. Frank Polzer

    F-I2 - Soft Matter and Functional Materials

    Helmholtzzentrum Berlin für Materialien und Energie

    Lise-Meitner-Campus

    Hahn-Meitner-Platz 1

    14109 - Berlin



    Tel.: +49 30 8062-43830

    Fax:  +49 30 8062-42308



    frank.polzer at helmholtz-berlin.de





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    Forschungszentren e.V

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    Helmholtz-Zentrum Berlin für Materialien und Energie GmbH

    Mitglied der Hermann von Helmholtz-Gemeinschaft Deutscher Forschungszentren e.V

    Aufsichtsrat: Vorsitzender Prof. Dr. Dr. h.c. mult. Joachim Treusch, stv. Vorsitzende Dr. Beatrix Vierkorn- Rudolph
    Geschäftsführer: Prof. Dr. Anke Rita Kaysser-Pyzalla, Prof. Dr. Dr. h.c. Wolfgang Eberhardt, Dr. Ulrich Breuer

    Sitz Berlin, AG Charlottenburg, 89 HRB 5583

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