Actinide Analysis from Large- Volume Seawater Samples Bill Burnett & Guebuem Kim Department of Oceanography Florida State University and Phil Horwitz PG.

Slides:

Advertisements

Similar presentations

Ra in Water using MnO2 Resin: New Developments

Advertisements

Analysis of Actinide Elements from Large Environmental Samples

Measurements of Ra Isotopes via MnO2 Resin

Rapid Actinide Analysis for Large Soil Samples

Analysis of Actinide Elements from Large Samples Henrieta Dulaiova Guebuem Kim Bill Burnett Florida State University and E. Philip Horwitz PG Research.

SURVEY OF CHEMISTRY LABORATORY I

Technical Updates on UTEVA, TEVA and TRU Resins

Optimizing Radiochemical Methods at SRS

1 Gravimetric Analysis 1.Dissolve unknown substance in water 2.React unknown with known substance to form a precipitate 3.Filter and dry precipitate 4.Weigh.

Separation and Identification of the Group II Hydroxides in an Unknown

1 Solution Stoichiometry The concentration of a solution is the amount of solute present in a given quantity of solvent or solution. M = molarity = moles.

Rapid Separation Methods for Bioassay Samples S. L. Maxwell, III and D. J. Fauth Westinghouse Savannah River Site.

Titration Chemistry: The Molecular Nature of Matter, 6 th edition By Jesperson, Brady, & Hyslop acid–base, 198–199, 811–819 redox reactions, 239–240.

MnO 2 Resin: Concentration of Radium Isotopes Deok-Soo Moon Bill Burnett Department of Oceanography Florida State University Tallahassee, Florida.

The Determination of 226 Ra in Water Samples Anil H. Thakkar Eichrom Technologies, Inc. eichrom TECHNOLOGIES INC.

Applications of Extraction Chromatography in Marine Geochemistry

Molar Concentration. Measuring Concentration Molarity (M): the number of moles of solute in 1 liter solution. Example: 0.5 moles of NaCl dissolved in.

Analysis of Actinide Elements from Large Samples Henrieta Dulaiova Guebuem Kim Bill Burnett Florida State University and E. Philip Horwitz PG Research.

Volumetric Acid Determination Week 1 - Standardize NaOH w/ pure KHP Determine Unknown %KHP Week 2 – Continue Unknown % KHP pH meter titration of an unknown.

Rapid Actinide Analysis for Large Soil Samples-Update Sherrod L. Maxwell, III Westinghouse Savannah River Company.

Principles & Modern Applications

MnO 2 Resin: Concentration of Radium Isotopes Deok-Soo Moon Bill Burnett Department of Oceanography Florida State University Tallahassee, Florida.

The Education and Research Office of Biochemistry and Molecular Biology Yeast RNA extraction and component identification (strong salt method)

Exp. 16: Volumetric Analysis: Redox Titration Normality = eq wt of solute L solution Acid/bases: #eq = # H + or OH - ionized Redox reactions – transfer.

General Engineering Laboratories Use of Eichrom Resins for Bioassay Pa-231 Bob Timm - GEL Tim Chandler - GEL Bill Burnett - FSU Mike Schultz - PerkinElmer.

Developments in Environmental Radiochemistry* Environmental Radioactivity Measurement Facility Department of Oceanography Florida State University Tallahassee,

Distribution of radionuclides in soils in surroundings of Bratislava, capital of the Slovak Republic. II. Man-made radionuclides Mátel Ľ., Rosskopfová.

The Determination of 226Ra in Water Samples

Updates from Eichrom’s Tech Support Lab Anil Thakkar May 4 th 2004 Charleston, SC.

New Extraction Methods for Actinides in Urine at SRS Sherrod L. Maxwell III and David Fauth Savannah River Site.

Qualitative Analysis: Group I

Recent Improvements in Rapid Column Separation Methods at SRS S. L. Maxwell, III, D. J. Fauth, R. C. Henderson, J. J. Smiley, S. R. Johnson Westinghouse.

Th, Pu & U Separation Using TEVA and UTEVA Resin

Recent Improvements in Rapid Column Separation Methods at SRS

New Extraction Chromatographic Resins or New Tools for the Tool Box E. Philip Horwitz and Daniel R. McAlister PG Research Foundation, Inc South Cass.

EIChroM I N D U S T R I E S, I N C. Introduction of Eichrom TEVA Disc: Tc-99 Analysis Anil H. Thakkar, Lawrence Jassin, Michael Fern Eichrom Industries,

New Fecal Method for Plutonium and Americium at SRS Sherrod L. Maxwell III and David Fauth Savannah River Site.

 Extraction of OM  Rock-Eval (Pyrolysis)  Elemental analysis  GC, HPLC & MS  SIRMS.

Lab 4 Chemical reactions. A.Signs of a Chemical Reaction Evolution of heat and light Formation of a gas Formation of a precipitate Color change.

Rapid actinide measurements in environmental samples Dr Phil Warwick Geosciences Advisory Unit Southampton Oceanography Centre.

Determination of 210 Pb in mineral waters using Eichrom Resin Alžbeta Ďurecová, Dagmar Bursová, František Ďurec, Daniela Borošová State Institute of Public.

New Fecal Method for Plutonium and Americium at SRS Sherrod L. Maxwell III and David Fauth Savannah River Site.

One-Column Separation and Analysis of Isotopic Am and Pu in Soil Samples Nidal M. Jadalla, Eberline Services, Albuquerque, NM Anil Thakkar, Eichrom Technologies,

MnO 2 Resin and Automated Measurements of Ra Isotopes Bill Burnett Dept. Oceanography Florida State University.

WARM UP 1. Write the equation for the neutralization reaction between sulfuric acid (H 2 SO 4 ) and ammonium hydroxide (NH 4 OH).

Problem 4.22 (b) Write ionic and net ionic equations for: K 3 PO 4 (aq) + Sr(NO 3 ) 2 (aq) 

An Improved Method for Determination of Ra-228 * Jamie Christoff & Bill Burnett Department of Oceanography Florida State University “The Double-Pass Approach”

Teknologi dan Rekayasa Objectives After this session, the students are expected to be able : 1.to explain the steps of determination of iron and manganese.

Determination of Fe SMK Negeri 13 Bandung.

Marine Biotechnology Lab

Anil H.Thakkar Eichrom Industries, Inc.. Darien, IL

Separation of Metal and Metal Oxides using Ethyl Acetate & Bromine

The Determination of 226Ra in Water Samples

Fe3+, Al3+, Cr3+, Ni2+, Co2+, Mn2+, Zn2+

Marine Biotechnology Lab

Technical Sales & Support Chemist

Radioactive Waste Processing at the Savannah River Site

Calculate the solubility of PbSO4 whose Ksp = 2.0 x 10-14:

Extraction of “clay fraction”.

Ra in Water using MnO2 Resin: Update

Unit 5: Acid-Base Calculations Lesson 4: Mixing Strong Acids + Bases

Drill: Calculate the solubility of PbSO4 Ksp = 2.0 x 10-14

Rapid Emergency Methods for Actinides and Sr-89/90

Al(OH)3, Cr(OH)3, Fe(OH)3, NiS, CoS, MnS, ZnS

Exp. Iron in Vitamin Tablet

Analysis of an Acid Base Titration Curve the Gran Plot

National Air and Radiation Environmental Lab

Analysis of an Acid Base Titration Curve the Gran Plot

EXP.NO.5 Redox Titration ( Oxidation Reduction Titration) A-preparation and standardization of KMnO4 soln. B- determination of [Fe2+] in unknown sample.

Presentation transcript:

Actinide Analysis from Large- Volume Seawater Samples Bill Burnett & Guebuem Kim Department of Oceanography Florida State University and Phil Horwitz PG Research Foundation

Acknowledgments Pavel Povinic, Jerry LaRosa IAEA Marine Environment Laboratory, Monaco PG Research Foundation

3 Marine Environment Laboratory Monaco

Need for Large Volumes zActivities of fallout Pu in the open sea very low — on order of 0.01 mBq/kg! zTo obtain good precision with reasonable count times (~1 week) requires volumes on the order of liters! zHow can we preconcentrate/separate actinides efficiently from such a large volume?

MnO 2 Co-precipitation Seawater, liters Acidify to pH 2, add Pu/Am tracers, stir/hold For 100L sample, add 35 mL sat KMnO 4 (~2.1g); Pu-->Pu(VI), org oxid, purple color Adjust pH to 8-9 with NaOH Add 0.5M MnCl 2 (2x vol of KMnO 4 ); --> MnO 2 ppt, dark brown 2MnO Mn H 2 O = 5MnO 2 + 4H + Re-adjust pH to 8-9 as necessary Stir occasionally to keep MnO 2 suspended for few hours Allow Mn0 2 (Pu, Am) ppt to settle overnight Pump supernatant into clean tank for Cs, Sr processing Drain MnO 2 slurry from bottom tap Seawater MnO 2 Suspension MnO 2 ppt (Pu, Am) ~4400 mg! supernatant Cs, Sr centrifuge/ filter

Transferring Water and MnO 2 Supernatant seawater transferred from one plastic tank to another via pumping — this will be used for 90 Sr and 137 Cs. MnO 2 suspension withdrawn from bottom of conical-shaped plastic tanks — processed for Am and Pu.

Fe(OH) 3 ppt Dissolve MnO 2 w (~2L) 2M HCl + (~20-40 mL) NH 2 OH. HCl (0.1g/mL) Add 50 mg Fe 3+ as FeCl 3 --> yellow Add (~1.5L) 2M NaOH to decrease acid conc. Add ~2mL NH 2 OH. HCl to reduce Fe 3+ --> Fe 2+ Pu*-->Pu 3+ ; colorless soln Add 20 mL NaNO 2 (0.1g/mL); Fe 2+ --> Fe 3+ ; Pu 3+ --> Pu 4+ Add 2M NH 4 OH to pH = 8-9; ppt Fe(OH) 3 Boil ~5 min to improve coagulation of Fe(OH) 3 ppt Adjust pH to 6-7 w 1M HCl to hold Mn in soln Let cool, settle, centifuge Fe(OH) 3 suspension, filter supernatant, dissolve ppt in acid for separation MnO 2 ppt (Pu, Am) Mn 2+ soln (Pu, Am) Mn 2+, Fe 2+ soln (Pu 3+, Am 3+ ) Fe(OH) 3 ppt (Pu, Am) Chemical separations

Collection of Fe(OH) 3 ppt Fe(OH) 3 is ppt and allowed to settle in 10-liter glass beakers Supernatant from Fe(OH) 3 suspension filtered through a 0.45  m filter

2-Column Separation: Part 1 U/TEVA TRU Resin® Resin® [Discard or to SrResin] 12 U, Th, Np Am, Pu

Actinide Separation: Part 2 U/TEVA Resin® Np, Th U M HCl 3 5N HCl H2C2O4 0.01M HCl 2.5M HNO3 2.5M HNO M NaNO2 2.5M HNO M HCl 3 4 4M HCl 0.1M NH4HC2O4 or 4M HCL + 0.1M H2Q TRU Resin® 4 3 Discard Am Pu 3 4

Results: Irish Sea Water * IAEA Intercomparison (Povinic, pers. comm.)

Am Spectrum

Pu Spectrum

Summary & Future Plans zMnO 2 /Fe(OH) 3 ppt effectively concentrates actinides from large volumes. zUTEVA/TRU effectively and easily separates Pu/Am from Fe(OH) 3 matrix. zInvestigate use of Diphonix for actinide preconcentration from large volumes.