LectureWeeks8and9 - Seawater-SAAfaculty.sites.uci.edu/.../LectureWeeks8and9-Seawater-SAA.pdffrom...

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  • Kf = 10‐16.5

  • Kf = 10‐16.5

    This is key, because not only does NH3 prevent precipitation but it also complexes some Zn2+. Cool!

  • We use an ammonia buffer solutionfor a reason...

    αY4- = 0.355 at pH =10.

  • Marcel Pourbaix(1904–1998)

    http://corrosion‐doctors.org/Biographies/PourbaixBio.htm

    Recall:Pourbaix Diagrams

    from Pourbaix, Atlas of electrochemical equilibria in aqueous solutions, 1974

  • Solubility product Ksp = 3.0×10−17

    Zn2+ + 2OH- → Zn(OH)2(s)

    Ksp = [Zn2+][OH -]2

    At pH=10, [Zn2+] = ??

    Zinc Hydroxide

  • Solubility product Ksp = 3.0×10−17

    Zn2+ + 2OH- → Zn(OH)2(s)

    Ksp = [Zn2+][OH -]2

    At pH=10, [Zn2+] = Ksp /[OH -]2

    Zinc Hydroxide

  • Solubility product Ksp = 3.0×10−17

    Zn2+ + 2OH- → Zn(OH)2(s)

    Ksp = [Zn2+][OH -]2

    At pH=10, [Zn2+] = Ksp /[OH -]2

    Zinc Hydroxide

    = (3.0×10−17) /(1.0×10−4)2

    = 3.0×10−9 M

    This is the maximum free Zinc concentration.

  • Ammonia Buffer Solution

    At pH=10, [NH3] = ??

    [NH3]total = 0.100M

    NH3 + H2O NH4+ + OH - pKb = 4.74

  • Ammonia Buffer Solution

    At pH=10:

    [NH3]total = 0.100M

    NH3 + H2O NH4+ + OH -

    [NH3] = 0.0846 M

    pKb = 4.74

  • And recall, we think we have:[Y4–] = 3.55 x 10‐5 M[Zn2+]max = 3.0 x 10‐9 M

  • Zinc - Ammonia Complexation

    At [NH3] = 0.0846M, αZn2+ = 1.61 x 10-5

  • Zinc - Ammonia Complexation

    At a TOTAL Zinc concentration of 1.00 x 10-4 M:

    [Zn2+] = αZn2+ [Zn2+]tot

    [Zn2+] = (1.61 x 10-5)(1.00 x 10-4)

    [Zn2+] = 1.61 x 10-9 M

    Therefore: no precipitation!

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    What is pZn at the equivalence point?

    Log Kf for the ZnY2- complex is 16.5. Both solutions are buffered to a pH of 10.0 using a 0.100M ammonia buffer.

    The alpha fraction for Y4- is 0.355 at a pH of 10.0.The alpha fraction for Zn2+ is 1.61 x 10-5.

    Once more, with feeling:

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    Total moles of Zinc = ??

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    Total moles of Zinc = (1.00 x 10-4 M)(0.050L)

    = 5.0 x 10-6 moles

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    Total moles of Zinc = 5.0 x 10-6 moles

    Equivalence point volume = ??

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    Total moles of Zinc = 5.0 x 10-6 moles

    Equivalence point volume = 0.100L

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    Total moles of Zinc = 5.0 x 10-6 moles

    Equivalence point volume = 0.100L

    [ ZnY2- ] = ??

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    Total moles of Zinc = 5.0 x 10-6 moles

    Equivalence point volume = 0.100L

    [ ZnY2- ] = 5.0 x 10-5 M

    We assume a stoichiometric reaction.

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    Total moles of Zinc = 5.0 x 10-6 moles

    Equivalence point volume = 0.100L

    [ ZnY2- ] = 5.0 x 10-5 M

    [ Zn2+ ] = ??

  • [ ZnY2- ] = 5.0 x 10-5 M

    We assumed a stoichiometric reaction. But actually, there is a little bit of free (uncomplexed) EDTA and free (uncomplexed) Zinc in solution.

    αZn2+ = 1.61 x 10-5

    Log Kf = 16.5. αY4- = 0.355

  • [ ZnY2- ] = 5.0 x 10-5 M

    We assumed a stoichiometric reaction. But actually, there is a little bit of free (uncomplexed) EDTA and free (uncomplexed) Zinc in solution.

    1.66 x 10-8 M

  • EDTA Titration

    You would like to perform a titration of 50.00 mL of a 1.00 x 10-4 M Zn2+ solution with a 1.00 x 10-4 M EDTA solution.

    Total moles of zinc = 5.0 x 10-6 moles

    Equivalence point volume = 0.100L

    [ ZnY2- ] = 5.0 x 10-5 M 1.66 x 10-8 M

  • Feature 17.5 in Skoog, et al., goes over a similar problem, but via a slightly different method.

  • from Pourbaix, Atlas of electrochemical equilibria in aqueous solutions, 1974

    Marcel Pourbaix(1904–1998)

    http://corrosion‐doctors.org/Biographies/PourbaixBio.htm

    Recall:Pourbaix Diagrams

    Because Zn(OH)2 can (twice) deprotonate too!

    ? ?

    Because Ksp = 3.0 x 10‐17

    [Zn2+][ZnO22–]

  • Announcements• Remaining Classes Including today, just five (or four) left! (M5/19, W5/21, 

    W5/28, M6/2, W6/4) Your “final” quiz will be on the Weeks 4 – 7 

    information, and tentatively will be given via Sapling over Wed., 6/4 – Sun., 6/8 (Week 10)

    • No more new textbook reading• For lab help, read papers and procedures from the course website, the Internet, etc.

    • 5 extra credit points from Dr. Edwards (by Thurs.)

    Course websitehttp://faculty.sites.uci.edu/chem2l/chem-h2lcm3lc/

  • Weeks 8 – 10 Objectives

    By the end of the course, you will be able to:

    • Explain the speciation of molecules in seawater

    • Explain hydrothermal vents and the origin of some elements in seawater

    • Describe how one can, and does, measure elements in seawater

    • Tell people why you like Chemistry, and specifically Analytical Chemistry

  • “Arbitrary definition" of a trace metal:  10 µmol kg‐1 ≈ 1 ppm (by weight)

    Fe, Ba, Mn are all trace metals;There are many others!

    Mg2+:  53 mmol kg‐1

    K+:  10.2 mmol kg‐1

    Ca2+:  10.3 mmol kg‐1

    Cl‐:  546 mmol kg‐1

    SO42‐:  28 mmol kg‐1

    Our measurements:

    IUPAC says:A trace element is one having 

  • “Arbitrary definition" of a trace metal:  10 µmol kg‐1 ≈ 1 ppm (by weight)

    Mg2+:  53 mmol kg‐1

    K+:  10.2 mmol kg‐1

    Ca2+:  10.3 mmol kg‐1

    Cl‐:  546 mmol kg‐1

    SO42‐:  28 mmol kg‐1

    Our measurements:

    IUPAC says:A trace element is one having 

  • 10 µmol kg‐1 ≈ 1 ppm (by weight)

    Mg2+

    Ca2+

    Cl-SO42-

    K+

    Our measurements!

  • 10 µmol kg‐1 ≈ 1 ppm (by weight)

    Al(OH)4-and

    Al(OH)3

    How would we measure this?

  • Zn2+

    Cu2+

    How would we measure these?

  • Cd2+

    Toxic chemicals need to be measured!

  • Hg2+

    Pb2+

    Toxic chemicals need to be measured!

  • Hg2+

    Pb2+

    Toxic chemicals need to be measured!

    … but how?

  • Anodic Stripping Voltammetry (ASV)

    Electrochemical Methods for Trace Metals in Seawater

    (1) First deposit a metal(like Cu on a metal strip)

    (2) Then, remove the metal(oxidize it by ASV)

    Oftentimes, the metal strip is a metal droplet (Hg). This is becausemercury forms a solid amalgam with most metals which then have very well-defined and sharp redox potentials, thus allowing for the detection of various metals at once

    Iron does not form an amalgam with Hg.

  • (in units of Ångstoms)

    AtomicEmission

    Spectroscopy

    Each elementhas a unique

    emission spectrum

    SpectroscopicMethods

    for Trace Metalsin Seawater

  • Inductively Coupled Plasma-Atomic Emission Spectroscopy

    ICP–AES

    Sharp narrow band spectra allow forsimultaneous multi-element measurements

  • (http://www.elementalanalysis.com/services/inductively-coupled-plasma-icp/)

    (http://wwwp.cord.edu/dept/chemistry/analyticallabmanual/experiments/icpaes/intro.html)

    * Here, Ar plasma is ~7000 K (Sun is ~5800 K)

    * Whitish light, like blackbody radiation

    * Strong colors due to main emission lines

    * Ar Plasma Coagulation for Cancer Treatment

    Inductively Coupled Plasma-Atomic Emission Spectroscopy

    ICP–AES

  • “Abs

    orpt

    ance

    Blackbody spectra

    Data compiled by the Intergovernmental Panel

    on Climate Change (IPCC)

    Recall: Blackbody spectra

  • Photoluminescence Spectroscopy

    Photoluminescence

    Jablonski diagram

    Kasha’s rule

    (image from answers.com)

    Recall: Photoluminescence Spectroscopy (Jablonski Diagrams)vibrationalrelaxation

  • Why are there not transitionsbetween all energy levels?

    Recall:

  • The Vernier System

    Similar to what is found in digital cameras

    Recall: The Vernier Fluorescence System

  • Mass Spectrometry is another method for analyzing both trace metals and organics in seawater.

    Molecular MS:

    Methane (m/z = 15)H2S (34)CO2 (44)Toluene (91)

    ICP-MS: Atomic MS

    *m/z is mass to charge ratioLimit of Detection (LOD)

  • (http://people.whitman.edu/~dunnivfm/FAASICPMS_Ebook/CH4/4_2.html)

    (http://en.wikipedia.org/wiki/Mass_spectrometry)

    Inductively Coupled Plasma-Mass Spectrometry

    ICP–MS

  • Mass Spectrometry in Seawater Environments

    Oxygen and CO2 depth profiles

  • MolybdenumAluminumZincIronCopper

    Different trace metals exhibit different types of Distributionswith depth and location in the oceans.

    • Conservative-type Distributions• Nutrient-type Distributions• Scavenged-type Distributions• Hybrid and Mixed Distributions

    Let’s look at some trace metals:

  • Mo is found in the oceans at an average concentration of 105 nmol kg‐1 as the oxyanion molybdate, MoO42‐.

    Molybdenum is a good illustration of a trace metal with a conservative-type distribution in the oceans.

    Conservative-type trace metals interact only weakly with particles, have oceanic residence times greater than 10,000 years (much greater than the mixing time of the oceans), and have concentrations that maintain a relatively constant ratio to salinity. Mo has an oceanic residence time of 80,000 years. It exhibits an almost uniform distribution in the oceans with only a slight depletion at the surface.

    Trace Molybdenum in Seawater

  • The concentration of trace Al in sea water varies with depth and location from 0.5 to 150 nmol kg‐1

    Aluminum is the best illustration of a trace metal with a scavenged-type distribution in the oceans.

    Trace metals with scavenged-type distributions have strong interactions with particles and short oceanic residence times (ca. 100 to 1,000 yrs). These residence times that are less than the ventilation or mixing time of the oceans. Theirconcentrations tend to be maximal near major sources such as rivers, atmospheric dust, bottom sediments, and hydro-thermal vents. Concentrations decrease with distance from the sources.

    Trace Aluminum in Seawater

  • The major external input of aluminum is from the partial dissolution of atmospheric dust delivered to the surface oceanespecially in the Mediterranean Sea.

    Total Dissolved Aluminium:

    Depth Profiles

    Trace Aluminum in Seawater

  • The concentration of trace Zn in sea water varies with depth and location from 0.5 to 10 nmol kg‐1

    Zinc is a striking example of a trace metal with a nutrient-type distribution in the oceans.

    Trace metals with nutrient-type distributions are dominated by the internal cycle of assimilation by plankton in surface waters. Consequently, their concentrations are lowest in surface waters where they are assimilated by phytoplankton and/or adsorbed by biogenic particles, and increase in the subsurface waters as sinking particles undergo decomposition or dissolution, followed by oxidation and remineralization in deeper waters. Oceanic residence times of nutrient-type, recycled elements are intermediate (a few thousand to one hundred thousand years).

    Trace Zinc in Seawater

  • Dissolved Zinc

    DepthProfile

    Zinc concentrations are lowest in surface waters where it is assimilated by phyto-plankton and/or adsorbed by biogenic particles, and increase in the subsurface waters as sinking particles undergo decomposition or dissolution.

    Trace Zinc in Seawater

  • Total Dissolved Zinc: Worldwide Distribution

  • ZincZn2+ vs. Total

    The majority of Znin the ocean is complexed with various ligands(biological?)

    Trace Zinc in Seawater

    Zinc has a nutrient-type distribution in the oceans.

  • Hybrid Distributions

    Some trace metals, such as iron and copper, have distributions that are strongly influenced by both recycling and relatively intense scavenging processes.

    Iron

    Trace Iron in Seawater

  • Copper: free and complexed

    Hybrid Distributions

    Some trace metals, such as iron and copper, have distributions that are strongly influenced by both recycling and relatively intense scavenging processes.

    Copper provides an interesting example of a trace metal that is an essential, required element, but that can be toxic at relatively low concentrations. It can be considered the “Goldilocks” metal.

    Trace Copper in Seawater

  • Hydrothermal Vents

    http://www.ocean.udel.edu/deepsea/level-2/geology/vents.html http://www.resa.net/nasa/images/ocean/smoker.jpg

  • Some History• First discovered in 1977.• Average depth ~7000 ft.• Temperature as high as 400oC; water doesn’t boil

    due to high pressure (~300 atm).• “Smokers” formed when super-hot vent water

    meets the cold deep ocean water (~2oC).• Metals: Fe, Mn, Cl, Ca,K, Li, Cu,Zn, and Pb.

  • Some Worldwide Locations of Hydrothermal Vents

  • A Black Smoker Hydrothermal Vent

  • 1. Cold sea water (2oC) seeps down through cracks into the ocean floor.2. Seawater continues to seep; the water’s temperature is raised to 350 – 400oC for black smokers; reacts

    with rocks in the ocean crust; chemical reactions change the water by: a) Oxygen is removed, b) it becomes acidic (pH~2.8), c) picks-up dissolved metals (Fe, Cu, and Zn) and H2S.

    3. The hot liquid rises because it’s density is less than that of cold liquids. The hot liquid carries the dissolved metals and sulfide with it.

    4. Hot fluid exits the chimney. Rxn triggered by cold temperature and oxygen present in seawater. White smokers (250 – 300oC) – this Rxn happens before exiting the chimney.

    http://www.divediscover.whoi.edu/vents/vent-infomod.html#

  • Hydrothermal Vent Chemistry

  • Black Smoker with Worms!

  • Some Worms

  • Sulfur Speciation in Hydrothermal Vents S2O32-

    SO32-

    S8SO2H2S

    SH-

    S2-

    SO42-

    HSO4-

    H2SO4

  • Sulfur Speciation in Hydrothermal Vents

  • pH measurements withthe Shinkai 6500 at a depthof 4000 m.

  • The Identification of Redox Species from Hydrothermal Vents by in situ Raman Spectroscopy: Instrumental analysis

    of DORISSDeep Sea Raman In Situ Spectrometer,

    developed by MBARIRaman scattering = inelasticRaman active species in hydrothermal

    fluid. ex/CH4, CO2, CO, H2S, H2, CO3 2-, and SO4 2-a typical in situ analysis parameters:

    -10-25 mW laser power-1-15 scans of 1-15 seconds duration are averaged-spectral resolution is 6-8 cm-1 when no slit is used, but 3-4 cm-1 when a 50mm slit is used.

  • DORISS and PUP on tool sled of ROV

    ROV tethered by copper wiring (electrical) and fiber-optic bundles(communication) to the research vessel

    The probe head is held by the robotic arm and is moved to the sampling site.

    Schematic of DORISS and picture of PUP (precision underwater positioner)

    Two types of probes: stand-off and immersion

    Images taken from:http://www.mbari.org/raman/hydrothermal.htm

    http://carbon.cudenver.edu/public/chemistry/classes/chem4538/raman.htm

  • Carbonate Speciation in Ocean Waters

  • Carbonate Speciation in Ocean Waters

  • Carbonate Speciation in Ocean Waters

  • Carbonate Speciation in Ocean Waters

  • CO2 on the Ocean Floor?

    Sea sediment storage proposed for carbon dioxide

    It may be possible to fight global warming by burying carbon dioxide in reservoirs hundreds of meters below the ocean floor.

    The developers of the concept contend that the global deep sea storage capacity of CO2 is virtually unlimited, and that the area within the 200-mile economic zone of the US coastline is capable of storing thousands of years of current US CO2 emissions. Carbon dioxide could be stored in reservoirs hundreds of meters below the ocean floor. Kurt Zenz House, a geoscientist at Harvard University, and his colleagues propose injecting CO2 into sea floor sediments at depths of at least 3,000 meters, where the cool temperature and high water pressure would transform CO2 into a dense liquid. At such high pressures, liquefied CO2 could eventually turn into solid crystals at temperatures of 8-10°C.

    Kurt Zenz House, Daniel P. Schrag, Charles F. Harvey, and Klaus S. Lackner; Permanent carbon dioxide storage in deep-sea sediments PNAS, August 7, 2006.

    Trapping Carbon Dioxide In An Icy Cage: Researchers Explore The Ocean Floor With Rare Instrument

    In collaboration with oceanographers from the Monterrey Bay Aquarium Research Institute (MBARI), a team of geologists at Washington University in St. Louis is using a rare instrument on the ocean floor just west of California. One of their earliest projects was to see if it's possible to capture carbon dioxide from the atmosphere and store it on the ocean floor. The geologists, headed by Jill Pasteris, Ph.D., professor of earth and planetary sciences in Arts & Sciences, and their MBARI colleagues are the first to deploy a Raman spectrometer on the ocean floor. The instrument combines a portable focusing lens with a potent laser to examine minerals, gases and liquids –even seawater itself. Pasteris' group and their MBARI colleagues are using Raman spectroscopy to see what carbon dioxide in either a pure liquid or a complex solid phase will do on the sea floor. They also are examining the feasibility of synthetically trapping carbon dioxide in solids called clathrate hydrates, ice-like solids that form a cage around gas molecules, such as methane, trapping them and storing them. Such solids occur naturally on the ocean floor. The hope is that someday carbon dioxide can be trapped in a similar way.

  • http://www.youtube.com/watch?v=huTJlHMR_LE

    Black Smoker and Hot Vent Creatures

    http://ocean.si.edu/ocean-videos/hydrothermal-vent-creatures

  • Weeks 8 – 10 Objectives

    By the end of the course, you will be able to:

    • Explain the speciation of molecules in seawater

    • Explain hydrothermal vents and the origin of some elements in seawater

    • Describe how one can, and does, measure elements in seawater

    • Tell people why you like Chemistry, and specifically Analytical Chemistry

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