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Transcript of DMA-80 Direct Mercury Analyzer - IQ USPallchemy.iq.usp.br/agregando/wpa/Palestra19.pdf · DMA-80...
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DMA-80 Direct Mercury Analyzer
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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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Aqueous samplesand extracts
ASV7472
Solid or semi-solid wasteCV-AAS7471A
Liquid wasteCV-AAS7470A
Sample typeTechniqueMethod
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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
Few minutesAASAnalysis
Mercury reduction1 hour
Interference removalWet chemistry
20 minutes- 1 hourClosed vessel microwave
2 hours- 2 daysHot plateSample acid digestion
TimeDescriptionStep
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CV-AAS and ASV
• Both methods require sample digestion and further wet chemistry
• Sample digestion can be problematic because of Hg volatility
• Sample preparation is the bottleneck for higher analytical productivity
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DMA-80 Direct Mercury Analyzer
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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-80Principle of operation
• Solid or liquid samples are weighed and introduced in the DMA-80
• The sample is initially dried and then thermally decomposed in a oxygen flow
• Combustion products are carried off and further decomposed in a hot catalyst bed
• Mercury vapors are trapped on a gold amalgamator and subsequently desorbed for quantitation
• The mercury content is determined using atomic absorption spectrophotometry at 254 nm
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DMA-80
• Major components– Sample dosing system– Thermal process furnaces– Atomic absorption spectrophotometer– System controller
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Sample Dosing System
• Built-in 40 position auto-sampler for high throughput unattended operation, for solid and liquid samples
• Maximum sample weight 500 mg• Maximum sample volume 500 µl• Possibility of multiple sample dosing for Hg pre-
concentration on amalgamator
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Sample Introduction
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Fully Loaded Autosampler
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Pipetting Liquid Samples
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Thermal process
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Thermal Process
12 s0-30 s900°C850-950°CAmalgam
600°C550-650°CCatalysis
180 s0-420 s
850°C800-1.000°CDecomposition
60 s0-300 s300°C20-300°CDrying
Typical timeTime rangeTypical temperature
Temperature rangeStep
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Oxygen
“Research” grade(O2 > 99,95%)
Purity
200 ml/minuteFlow rate
4 bar (60 psig)Inlet pressure
Carrier and decomposition gasFunction
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Atomic Absorption Spectrophotometer
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AAS Technical Data
Si-photodiode sensorDetector
254 nm, 9 nm bandwidthInterference filter
253,65 nmWavelength
Low pressure mercury lampLight source
Single beam spectrophotometer with sequential flow through of
measurement cellsInstrument optics
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Typical Absorbance Profile
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DMA-80Performance Specifications
(1)Sample weight 100 mg(2)Automatic switching when absorbance 0,8
0,20,02Detection limit
(1st) 0,2-350(2nd) 350-6.000
(1st) 0,02-35(2nd) 35-600
Working range(2)
Hg concentration(1)
(µg/kg)Total Hg (ng)Data
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DMA-80Performance Specifications
6 minutesTypical analysis time
< 1,5%Typical reproducibility
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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
• Standard bench-top computer with similar specifications
• Dedicated Terminal 1024
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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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1st Cell Linear Calibration
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1st Cell Square Calibration
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Measurement/Graphic
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Balance Setup
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History Trail CFR 21 Part 11
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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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DMA-80Analytical Performance
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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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Calibration 1st Cell
0,6%0,722330 ng
1,2%0,499620 ng
2,2%0,254910 ng
1,5%0,12725 ng
16,7%0,0012Blank
RSD (n=3)AbsorbanceSolution
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Calibration 2nd Cell
0,9%0,7285500 ng
1,9%0,3117200 ng
2,2%0,1546100 ng
RSD (n=3)AbsorbanceSolution
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Calibration Curves
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DMA-80 Accuracy
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Certified Reference Materials
6.250 ± 190NIST 2711 Soil
1.400 ± 80NIST 2709 Soil
141 ± 19NIST 1633b Fly Ash
93,8 ± 3,7NIST 1630a Coal
34 ± 4NIST 1573a Tomato Leaves
5,8 ± 0,5NIST 1568a Rice Flour
Hg content (µg/kg)Sample
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NIST 1568a Rice Flour
2,03,04,05,06,07,08,0
Hg (µ
g/kg
)
Certified DMA-80
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NIST 1573a Tomato Leaves
24,0
28,0
32,0
36,0
40,0
Hg
( µg/
kg)
Certified DMA-80
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NIST 1630a Coal
80,0
85,0
90,0
95,0
100,0
Hg
( µg/
kg)
Certified DMA-80
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NIST 1633b Fly Ash
100,0
120,0
140,0
160,0
180,0
Hg
( µg/
kg)
Certified DMA-80
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NIST 2709 Soil
1,0
1,2
1,4
1,6
1,8
Hg
(mg/
kg)
Certified DMA-80
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NIST 2711 Soil
5,8
6,0
6,2
6,4
6,6
Hg
(mg/
kg)
Certified DMA-80
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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
56,20,29925
58,00,34044
57,80,23303
54,10,22962
55,40,28491
Hg (µg/kg)Weight (g)Run
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Fresh Salmon
5N
1,6Sd (µg/kg)
56,3Average (µg/kg)
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DMA-80 Detection Limit
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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
0,0006100,00075
0,000890,00084
0,001080,00063
0,000870,00102
0,001060,00071
AbsorbanceRunAbsorbanceRun
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Detection Limit
0,02 ngDL
0,0004683*Sd
0,000156Sd
0,0008Average
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DMA-80 Memory Effect
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DMA-80 Memory Effect
0,40,0097 (1st)Blank 2
1,50,0374 (1st)Blank 1
500 (set)0,7285 (2nd)Standard 500 ng
Mercury content (ng)AbsorbanceSample
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DMA-80 Memory Effect
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Quartz Boats
• Analysis of liquids with DMA-80 autosampler
• Improved performance – Lower memory effect– Better reproducibility
• Longer life time
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Quartz vs. Metal Boats
0
0,1
0,2
0,3
0,4
1 2 3 4 5 6 7 8 9 10Run
Sig
nal
Metal Quartz
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Memory Effect
0,010,000,0000,1001
0,450,050,00110,1001
1.106,01110,600,14740,1001
Result (µg/kg)Hg (ng)HeightWeight (g)Sample ID
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Reproducibility at Low Concentrations
AVG 8,55SD 0,09 µg/kgRSD 1,01%Statistics
8,500,850,02170,100
8,490,850,02160,100
8,510,850,02170,100
8,530,850,02180,100
8,720,870,02220,100
Results (µg/kg)Hg (ng)HeightWeight (g)
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Reproducibility at High Concentrations
AVG 1.143,7RSD 0,69%SD 7,88 µg/kgStatistics
1.143,4114,340,15230,100
1.158,7115,870,15430,100
1.141,3114,130,15200,100
1.136,2113,620,15140,100
1.138,8113,880,15170,100
Results (µg/kg)Hg (ng)HeightWeight (g)
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Lifetime
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• US EPA method 7473– Mercury in solids and solutions by thermal
decomposition amalgamation and atomic absorption spectrophotometry
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ComparisonDMA-80 vs. CV-AAS
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ComparisonDMA-80 vs. CV-AAS
YesMinimalWaste generation
Yes, to eliminate interferencesNot requiredWet chemistry
ElevatedModerateRunning cost
Limited to low rangeUp to 600 ngWorking range
100 ml solutionUp to 500 mg sampleSample size
AqueousLiquid and solidsSample type
Acid digestionNot requiredSample preparation
CV-AASDMA-80Technique
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Time ComparisonDMA-80 vs. CV-AAS
0
60
120
180
240
DMA-80 CV-AAS
Tim
e (m
inut
es)
Sample preparation Analysis
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DMA-80 Major Applications
• Biological– Blood, urine, hair, tissue, plankton
• 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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DMA-80 Direct Mercury Analyzer