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Instrumental Methods of Analysis1. Introduction
1. Writing Intensive1. Rewrites are Required2. Large Amount of Excel Data Management
2. Work1. Individual
1. Work Log2. Own Sample3. Exams4. Lab Book pages
2. Group1. Division and Attribution of Labor (Accountability)2. Reports3. Calibration Curves
3. Single Analyte (Skill Development and Cross Comparison Methods)1. Overlapping Themes
1. Statistics/Sampling2. Solution Chemistry3. EDTA4. Isotopes5. Phase Separations
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1. Writing Intensive2. Work3. Single Analyte4. Problem Based
• What is best method for lead analysis?• What is best method for This particular sample?
5. Ethics and Service Learning1. How do we know?2. Critical Thinking
Instrumental Methods of Analysis1. Introduction
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Electronics, Spectroscopy, Electrochemistry, Chromatography
Confusion Confusion
“Too much from instructor” information
IodideElectrolysis
Chromium &permanganate
UV-Vis
FluorideIon Selective
Electrode
Quinine Fluorescence
Cu GraphiteFurnaceAtomic
Absorption
DMSO Infrared
Spectroscopy
Methanol GasChromatography
7 different analytes7 different methods
How do we selectOr compare methods/Instruments?
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Figures of Merit Theme Knowledge
Pb AnodicStripping
Voltammetry
Pb DithizoneUV-Vis
Tetraethyl 207Pb MS
Pb Ion Selective Electrode
Pb EDTA InfraredSpectroscopy
EDTA Pb HPLC
207Pb in EDTA by proton NMR
Pb Atomic Absorption
Calcein BluePb Fluorescence
Quenching
Choose Method: Cross Compare/measure LOD
Role of solution pH important
Pb Limit of detection?Pb Linear range?Pb Selectivity?Pb Signal/Noise?
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Week Topic “Lab” Concept Stat Chem Isotope
Ethics
1 Pb & Society; Statistics and Ethics Pototo populations x x
2 Signals & Noise; LOD Analog & Digital filters x
3 Relevant Chemistry; Exam I ISE & Pb(OH)2 x
4 Intro Spectroscopy IR & UV-Vis x
5 Molecular Spectroscopy IR & UV-Vis x
6 Fluorescence and AA Fluorescence and FAA x x
7 AA and Vibrational, Exam II Fluorescence and FAA x x
8 Break, NMR Break
9 NMR, Off campus sampling NMR, ASV x x x
10 MS, NMR, ASV x x x
11 Intro Electrochem., Select Method sample prep x x x
12 Potentiometry, sample analysis x x
13 ASV, Take home exam III ICP-MS, GC x x
14 Separations ICP-MS, GC x x
15 Separations How do we know? Ethics x x
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Why Lead?
Health
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Same size,Shape, chemistryDifferentOrbitals,Different total Number of electrons
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Warren et al, TIBS, 1998, 23, 217
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Current measurementsno longer rely on zincprotoporphyrinas PbB effectson fetal developmentcan be detectedat values of PbB<5 ug/dL
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ALAD dehydratase with lead binding site
An estimated 40% of lead in blood plasma bound to ALAD
Wetmur, 1994
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Enhanced ALA concentration leadsto tautomers which easily formradicals which may attack the cellwall - leading to early cell death. Heme dies about 20% earlier
Hammond and Dietrich, 1990
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Because lead affected ALADresulting in overproduction of ALAALA may also affect the functionof GABA but a close similarityin molecular structure
GABA controls leaf tip growth, and brain development. Functionchanges with time, so growing tips and infants differentially affected from adults
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Herlenius and Lagercrantz, 2001Ben-Ari1, 2001
Certain portions of the brain more greatly affected: prefrontal cortex: problem solvinghippocampus (memory)cerebellum (motor coordination, body movement, posture and balance)
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Why Lead?
Everywhere
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Lead as anore in the earthrelatively benign
Human activitydistributeslead into theenvironment
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Modern major uses
1. Pigments2. Leaded Gasoline3. Munitions
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Eliminating Childhood Lead Poisoning:A Federal Strategy Targeting Lead Pain Hazards, Feb. 2000
Decade ThousandTonswhite lead
ThousandTons red lead(litharge)
MillionsOccupiedUnits
White leadper unit(pounds)
Remainingleadthousandstons
1914-23 1340 0 24.35 110 413
1920-29 1307 356 29.91 87 184
1930-39 737 421 34.86 42 104
1940-49 476 1189 42.83 22 72
1950-59 196 816 43.02 7 37
1960-69 82 781 63.45 3 20
1970-79 29 625 80.39 1 841
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Cement block
ash
Sewagesludge
landfill
incinerate
Mine
reclaim
fertilizer
groundwater
Depositlocally
Bottom sludge
Depositelsewhere
Fishing sinkers& shot
Plant uptake
Flow to groundwater
To air
Other Ecosytem Impacts of Lead
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2009 Class Project
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Loyola Chem Sr.
S. 1994Growing Scientists20 5th graders map park soil lead
F 1994Northwest IncineratorAustin homes: Yard Soil Lead
F 1995Northwest IncineratorGrid map
House DustUptown 5th graders sample and tourlabs
F 1996
F 1997House DustLittle village Boys and Girls Club(failed) F 1998Northwest Incinerator
Tight grid and isotopes
F. 1999Bethel New Life: BrownfieldSoil sampling
F 2000Orozco School: House Dust
F 2001Pullman: White Lead Factory
House DustWest Pullman White Lead factory
F 2002
Alanah Fitch [email protected]
S 2008Lead in ToysEvanston Childcare
NationalAward forThe Class
ACSMtgposter
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Homes Municipal Waste Incinerator
Incinerator 1994, 1995, 1998
Lead Elimination Action DriveWest-side Alliance for a Safe Environment (WASTE)Center for Neighborhood TechnologyAustin Neighborhood Council
Pb?
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Wind
BackgroundSoil lead “Shadow” depends on
Stack heightLargest depositionIs here
Decreasing amts
Incinerator 1994, 1995, 1998
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Incinerator 1994, 1995, 1998
Students meet withelderly ladies who letthem sample soils.The ladies discuss theirconcerns.
sampling
Control
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4915 W. Kamerling
440
1040
2311431
4822 W. Potomac
187
150 250
1850 1385
4833 W. Crystal
garage
372
1800
Incinerator 1994, 1995, 1998
Front
Back
Soil Lead in parts per million (ppm)
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439
2620
3067
700
2808
BRICK
2900
1133
6613 N. Ashland
1538
FRAME
6729 N. Ashland
Incinerator 1994, 1995, 1998
Comparison homes, 17 mile away
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Second year: Resample with respect tothe wind; also allowing for up and down windcomparisons. Wins a National Award.
Luke later goes to CroatiaOn UN project onLead dispersion bygasoline
Incinerator 1994, 1995, 1998
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North
Chicago
Washington
Demolished lot
Wind Pattern
Cic
ero
2312
8982
32
1231210546346
15
320
42
0
101
Pul
aski 644 mO
rr H
igh
Sch
ool
Incinerator 1994, 1995, 1998
This data presentedTo Mayor’s advisorycouncil
Class final: enterBusch National Env.Award competition –Place third
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0
2
4
6
8
10
12
14
PPM Soil Lead
Fre
qu
ency
< 0.5 mile from incinerator
> 0.5 mile from incinerator
Incinerator 1994, 1995, 1998
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Wind
BackgroundSoil lead “Shadow” depends on
Stack height Largest depositionIs here
Decreasing amts
Incinerator 1994, 1995, 1998
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0
1530
4661
-61
-46
-30
-15
0
15
30
46
61
NNNE
NE
ENE
E
SE
Incinerator 1994, 1995, 1998
Last time: we finally set up an experiment worthy of an An air pollution expert
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Across1 the system of pipes and other apparatus for conveying water,
liquid wastes, etc., as in a building3. the fluid that circulates and carries oxygen throughout the human
body4. being placed at risk8 the quality of degree of being toxic or harmful to plants or animal
life9. the introduction of harmful substances or products into the
environment10. a mixture of pigment and liquid12. food, eating healthy14. a pain located in the head15. the age group affected most by lead poisoning17. President on the $20 bill18. a transparent, odorless, tasteless liquid, a compound of hydrogen
and oxygen, H20, that constitutes rain, oceans, lakes, rivers, etc.19. . to take ill through eating
Down2. a heavy, comparatively soft, malleable, bluish‑gray metal. A
toxic metal, that has been widely used in paints, plumbing and fixtures, and in some water supply service lines
3. composer thought to have had lead poisoning5. the portion of the earth's surface consisting of dirt6. the air, water, minerals, organisms, and all other external factors
surrounding and affecting a given organism at any time7. dry particle of earth10. a table illustrating the periodic system, in which the chemical
elements are shown in related groups11. . the process of preparing the samples by breaking down the baby
wipes into a substance suitable testing13. a silver‑white divalent metal found in limestone, chalk, milk16. the science that deals with the composition and properties of
substances and various elementary forms of matter
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2009 – Brainstorm on Projects
Short list by next week
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Health Effects of Lead
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Inhalation depends uponthe particle size.
This data is for humans
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Dissolution of lead carbonate particles insimulated gastric juices as a function of particle size
For birds, the uptake will depend upon the pH and grinding action in the gizzard. For ruminants, the uptake will depend upon the lifetime in the digestive organs
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94-99% of lead attached toexternal surfaces of erythrocytes
1-6% lead in plasma,of which 99% attached toproteins
~0.1 to 0.6 % of lead isas the free cation
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Ca BaActive uptake ofcalcium,apparentlyto lesser extent other divalent similarsized cations,including lead.
Recognition will be similar for various species
Calcium uptake is controlled by Vitamin D and growth regulators parathyroid hormone (PTH)
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Calcium is stored to the endoplasmic reticulum, lead will alsogo there
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Basophilic Stippling of Dog Blood caused by nucleation ofribonucleoproteins in presence of lead
High lead causes deformation of blood cells and shorter lifetime ofthe red blood cell.Double whammy - production is also affected
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Current measurementsno longer rely on zincprotoporphyrinas PbB effectson fetal developmentcan be detectedat values of PbB<5 ug/dL
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Renal biopsy of a 28 year old shipwrecker. Dense intranuclear inclusion body is characterized by a fibrillary outer margin; Cramer, Goyer et al. Brit. J. Indust. Med., 1984
1 hour after exposurelead isfoundwithin the kidneys,becausekidneysare monitoringbloodcalciumlevels viathe glomerular filtration rate
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Renal biopsy of a 28 year old shipwrecker. Interstitial fibrosis with atrophy of some tubular lining cells; Cramer, Goyer et al. Brit. J. Indust. Med., 1984
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Damage to kidney results in hypertension gout
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Thomas Rowlandson’s The King’s Bath
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Cruikshank’s gout
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Calcium is closely monitored by kidney because it plays a largerole in various signalling processes
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Calcium bound to calmodulinC. Yang, G. S. Jas, K. Kuczera, J. Biomolecular Structural Dynamics,2001, 19,257-271
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Lead double whammy1. Low lead turns on triggers2. Hi lead turns off triggers
Calcium serves as a trigger for musclecontractions: troponin C
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Colic is a form of muscle spasmingSo are the “shakes”
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Lead, like calcium, is deposited to the hard tissuesImplications for the Trophic level of lead in the environment
Osteocalcin (bone Gla protein (BGP)) controls calcium depositionand is affected by lead: weaker bones for affected individuals
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Longitudinal Section & Cross Section of Bone
TrabecularBone
Compact Bone
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Seizures can result from lead due to Ca triggers of the synapses
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Other Irrelevant Information thatIs mildly amusing/interesting on Lead
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886oC
-0.2oC (Au)230oC (Ag)
Purity of Pb: 99.9% achieved
~5,000 years ago Cuppellation Begins
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