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Introduction
Mercury in the atmosphere can be from manmade sources (coal-fired power plants, municipal incinerators, industrial boilers) or from natural sources (forest fires, geologic formations, volcanoes) Precipitation is the primary mechanism for transporting airborne gaseous or particulate mercury from the atmosphere to surface water and land
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Mercury Analysis
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Method
Technique
Sample type
7470A
CV-AAS
Liquid waste
7471A
CV-AAS
7472
ASV
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CV-AAS
Cold Vapor-Atomic Absorption Spectroscopy
Samples are digested or dissolved Mercury is reduced to free atomic state by using tin (II) chloride or sodium boro-hydride in a closed reaction vessel Mercury is measured by atomic absorption
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CV-AAS
Step Description Hot plate Sample acid digestion Closed vessel microwave Interference removal Wet chemistry Mercury reduction Analysis AAS
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1 hour
Few minutes
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DMA-80 Advantages
Direct Hg determination at trace level on solid and liquid samples No sample digestion step No wet chemistry pre-treatment step Fast, approximately 6 minutes per sample Eliminates waste disposal Validated results (US EPA method 7473) for solid and liquid matrices
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DMA-80
Major components
Sample dosing system Thermal process furnaces Atomic absorption spectrophotometer System controller
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Sample Introduction
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Thermal process
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Thermal Process
Step Temperature range 20-300C Typical temperature 300C Time range Typical time
Drying
0-300 s
60 s
Decomposition
800-1.000C
Catalysis
550-650C
600C
Amalgam
850-950C
900C
0-30 s
12 s
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Oxygen
Function Carrier and decomposition gas 4 bar (60 psig)
Inlet pressure
Flow rate
Purity
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Working range(2)
Detection limit
0,02
0,2
(1)Sample
6 minutes
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System controller
Lab TERMINAL
Touch-screen Pentium-based controller, 266 MHz, 64 MB Ram, Windows 98, Color 12,1 TFT SVGA monitor, CD-ROM, FD, Smart Card Reader, 2 COM, 1 USB, LAN ports
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Terminal 1024
12 large high resolution color screen controller Touch control display Supplied with keyboard and mouse EasyControl software for a complete control of all reaction parameters Optional EasyDoc software for data export on external computer
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EasyControl Software
Evolution of previous Windows based DMA-80 software Selectable calibration algorithm Virtually unlimited memory for programs and actual data storage Built-in service and diagnosis functions CFR-21 part 11 compliant
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System Status
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Measurement/Graphic
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Balance Setup
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Mercury Trap
Optional mercury trap to be located at DMA-80 outlet Activated charcoal Safe operation Easy and ready to install
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Getting Started
Oxygen cylinder with gas regulator stable at 4 bar (60 psig) Power 115-230 V/50-60 Hz Analytical balance with serial interface Windows compatible printer Standard reference materials Aqueous standards Precision pipettes
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DMA-80 Calibration
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DMA-80 Calibration
Liquid standards
Different concentrations, same volume Same concentration, different volumes Use fresh standards, stabilized with HNO3 or HCl/K2Cr2O7
Solid standards
Certified mercury content Vary by weight
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0 ng
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10 ng
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20 ng
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30 ng
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100 ng
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200 ng
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500 ng
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100 ng
0,1546
2,2%
200 ng
0,3117
1,9%
500 ng
0,7285
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0,9%
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Calibration Curves
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DMA-80 Accuracy
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Hg content (g/kg) 5,8 0,5 34 4 93,8 3,7 141 19 1.400 80 6.250 190
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DMA-80 Precision
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Fresh Salmon
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Collecting Sample
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Weighing
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Loading Autosampler
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Loading Furnace
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After Analysis
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Fresh Salmon
Run 1 2 3 4 5 Weight (g) 0,2849 0,2296 0,2330 0,3404 0,2992
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Fresh Salmon
Average (g/kg) 56,3
Sd (g/kg)
1,6
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Detection Limit
The detection limit is defined as the concentration which will give an absorbance signal of two (sometimes three) times the magnitude of the baseline noise. The baseline noise may be statistically quantified typically by making ten or more replicate measurements of the baseline absorbance signal observed for an analytical blank, and determining the standard deviation of the measurements. The detection limit is then defined as the concentration which will produce an absorbance signal twice (or three times) the standard deviation
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Detection Limit
Run 1 2 3 4 5 Absorbance 0,0007 0,0010 0,0006 0,0008 0,0007
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Detection Limit
Average 0,0008
Sd
0,000156
3*Sd
0,000468
DL
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0,02 ng
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Standard 500 ng
0,7285 (2nd)
500 (set)
Blank 1
0,0374 (1st)
1,5
Blank 2
0,0097 (1st)
0,4
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Quartz Boats
Analysis of liquids with DMA-80 autosampler Improved performance
Lower memory effect Better reproducibility
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0,3 Signal
0,2
0,1
0 1 2 3 4 5 Run Metal
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6 Quartz
10
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Memory Effect
Sample ID Weight (g) Height Hg (ng) Result (g/kg)
0,100
0,1474
110,60
1.106,01
0,100
0,0011
0,05
0,45
0,100
0,000
0,00
0,01
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Lifetime
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CV-AAS Acid digestion Yes, to eliminate interferences Yes Aqueous 100 ml solution Limited to low range Elevated
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Liquids
Waste water, crude oil, heavy oil, detergents, paints
Solids
Coal, fly ash, soil, sediment, sludge, minerals, food, feed, plastic, wood, vegetables, leaves, waxes
Medicinal
Pharmaceuticals, gelatin capsules, lipstick, lotions
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