DMA-80 Direct Mercury Analyzer
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1 DMA-80 Direct Mercury Analyzer Milestone Srl Milestone Srl 1
2 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 Milestone Srl 2
3 Milestone Srl 3
4 Mercury Analysis Milestone Srl 4
5 Method Technique Sample type 7470A CV-AAS Liquid waste 7471A CV-AAS Solid or semi-solid waste 7472 ASV Aqueous samples and extracts Milestone Srl 5
6 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 Milestone Srl 6
7 CV-AAS Step Description Time Sample acid digestion Hot plate Closed vessel microwave 2 hours- 2 days 20 minutes- 1 hour Wet chemistry Interference removal Mercury reduction 1 hour Analysis AAS Few minutes Milestone Srl 7
8 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 Milestone Srl 8
9 DMA-80 Direct Mercury Analyzer Milestone Srl 9
10 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 Milestone Srl 10
11 DMA-80 Principle 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 Milestone Srl 11
12 Milestone Srl 12
13 DMA-80 Major components Sample dosing system Thermal process furnaces Atomic absorption spectrophotometer System controller Milestone Srl 13
14 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 preconcentration on amalgamator Milestone Srl 14
15 Sample Introduction Milestone Srl 15
16 Fully Loaded Autosampler Milestone Srl 16
17 Pipetting Liquid Samples Milestone Srl 17
18 Thermal process Milestone Srl 18
19 Thermal Process Step Temperature range Typical temperature Time range Typical time Drying C 300 C s 60 s Decomposition C 850 C s 180 s Catalysis C 600 C Amalgam C 900 C 0-30 s 12 s Milestone Srl 19
20 Oxygen Function Carrier and decomposition gas Inlet pressure 4 bar (60 psig) Flow rate 200 ml/minute Purity Research grade (O 2 > 99,95%) Milestone Srl 20
21 Atomic Absorption Spectrophotometer Milestone Srl 21
22 AAS Technical Data Instrument optics Single beam spectrophotometer with sequential flow through of measurement cells Light source Wavelength Interference filter Detector Low pressure mercury lamp 253,65 nm 254 nm, 9 nm bandwidth Si-photodiode sensor Milestone Srl 22
23 Typical Absorbance Profile Milestone Srl 23
24 DMA-80 Performance Specifications Data Total Hg (ng) Hg concentration (1) (µg/kg) Working range (2) (1 st ) 0,02-35 (2 nd ) (1 st ) 0,2-350 (2 nd ) Detection limit 0,02 0,2 (1) Sample weight 100 mg (2) Automatic switching when absorbance 0,8 Milestone Srl 24
25 DMA-80 Performance Specifications Typical reproducibility < 1,5% Typical analysis time 6 minutes Milestone Srl 25
26 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 Milestone Srl 26
27 Terminal 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 Milestone Srl 27
28 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 Milestone Srl 28
29 System Status Milestone Srl 29
30 1 st Cell Linear Calibration Milestone Srl 30
31 1 st Cell Square Calibration Milestone Srl 31
32 Measurement/Graphic Milestone Srl 32
33 Balance Setup Milestone Srl 33
34 History Trail CFR 21 Part 11 Milestone Srl 34
35 Mercury Trap Optional mercury trap to be located at DMA-80 outlet Activated charcoal Safe operation Easy and ready to install Milestone Srl 35
36 DMA-80 Analytical Performance Milestone Srl 36
37 Getting Started Oxygen cylinder with gas regulator stable at 4 bar (60 psig) Power V/50-60 Hz Analytical balance with serial interface Windows compatible printer Standard reference materials Aqueous standards Precision pipettes Milestone Srl 37
38 DMA-80 Calibration Milestone Srl 38
39 DMA-80 Calibration Liquid standards Different concentrations, same volume Same concentration, different volumes Use fresh standards, stabilized with HNO 3 or HCl/K 2 Cr 2 O 7 Solid standards Certified mercury content Vary by weight Milestone Srl 39
40 0 ng Milestone Srl 40
41 10 ng Milestone Srl 41
42 20 ng Milestone Srl 42
43 30 ng Milestone Srl 43
44 100 ng Milestone Srl 44
45 200 ng Milestone Srl 45
46 500 ng Milestone Srl 46
47 Calibration 1 st Cell Solution Blank 5 ng 10 ng 20 ng 30 ng Absorbance 0,0012 0,1272 0,2549 0,4996 0,7223 RSD (n=3) 16,7% 1,5% 2,2% 1,2% 0,6% Milestone Srl 47
48 Calibration 2 nd Cell Solution Absorbance RSD (n=3) 100 ng 0,1546 2,2% 200 ng 0,3117 1,9% 500 ng 0,7285 0,9% Milestone Srl 48
49 Calibration Curves Milestone Srl 49
50 DMA-80 Accuracy Milestone Srl 50
51 Certified Reference Materials Sample NIST 1568a Rice Flour NIST 1573a Tomato Leaves NIST 1630a Coal NIST 1633b Fly Ash NIST 2709 Soil NIST 2711 Soil Hg content (µg/kg) 5,8 ± 0,5 34 ± 4 93,8 ± 3,7 141 ± ± ± 190 Milestone Srl 51
52 NIST 1568a Rice Flour Hg (µg/kg) 8,0 7,0 6,0 5,0 4,0 3,0 2,0 Certified DMA-80 Milestone Srl 52
53 NIST 1573a Tomato Leaves 40,0 Hg (µg/kg) 36,0 32,0 28,0 24,0 Certified DMA-80 Milestone Srl 53
54 NIST 1630a Coal 100,0 Hg (µg/kg) 95,0 90,0 85,0 80,0 Certified DMA-80 Milestone Srl 54
55 NIST 1633b Fly Ash 180,0 Hg (µg/kg) 160,0 140,0 120,0 100,0 Certified DMA-80 Milestone Srl 55
56 NIST 2709 Soil 1,8 Hg (mg/kg) 1,6 1,4 1,2 1,0 Certified DMA-80 Milestone Srl 56
57 NIST 2711 Soil 6,6 Hg (mg/kg) 6,4 6,2 6,0 5,8 Certified DMA-80 Milestone Srl 57
58 DMA-80 Precision Milestone Srl 58
59 Fresh Salmon Milestone Srl 59
60 Collecting Sample Milestone Srl 60
61 Weighing Milestone Srl 61
62 Loading Autosampler Milestone Srl 62
63 Loading Furnace Milestone Srl 63
64 After Analysis Milestone Srl 64
65 Fresh Salmon Run Weight (g) 0,2849 0,2296 0,2330 0,3404 0,2992 Hg (µg/kg) 55,4 54,1 57,8 58,0 56,2 Milestone Srl 65
66 Fresh Salmon Average (µg/kg) 56,3 Sd (µg/kg) 1,6 N 5 Milestone Srl 66
67 DMA-80 Detection Limit Milestone Srl 67
68 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 Milestone Srl 68
69 Detection Limit Run Absorbance Run Absorbance 1 0, , , , , , , , , ,0006 Milestone Srl 69
70 Detection Limit Average 0,0008 Sd 0, *Sd 0, DL 0,02 ng Milestone Srl 70
71 DMA-80 Memory Effect Milestone Srl 71
72 DMA-80 Memory Effect Sample Absorbance Mercury content (ng) Standard 500 ng 0,7285 (2 nd ) 500 (set) Blank 1 0,0374 (1 st ) 1,5 Blank 2 0,0097 (1 st ) 0,4 Milestone Srl 72
73 DMA-80 Memory Effect Milestone Srl 73
74 Quartz Boats Analysis of liquids with DMA-80 autosampler Improved performance Lower memory effect Better reproducibility Longer life time Milestone Srl 74
75 Quartz vs. Metal Boats 0,4 0,3 Signal 0,2 0, Run Metal Quartz Milestone Srl 75
76 Memory Effect Sample ID Weight (g) Height Hg (ng) Result (µg/kg) 1 0,100 0, , ,01 1 0,100 0,0011 0,05 0,45 1 0,100 0,000 0,00 0,01 Milestone Srl 76
77 Reproducibility at Low Concentrations Weight (g) Height Hg (ng) Results (µg/kg) 0,100 0,0222 0,87 8,72 0,100 0,0218 0,85 8,53 0,100 0,0217 0,85 8,51 0,100 0,0216 0,85 8,49 0,100 0,0217 0,85 8,50 Statistics RSD 1,01% SD 0,09 µg/kg AVG 8,55 Milestone Srl 77
78 Reproducibility at High Concentrations Weight (g) Height Hg (ng) Results (µg/kg) 0,100 0, , ,8 0,100 0, , ,2 0,100 0, , ,3 0,100 0, , ,7 0,100 0, , ,4 Statistics SD 7,88 µg/kg RSD 0,69% AVG 1.143,7 Milestone Srl 78
79 Lifetime Milestone Srl 79
80 US EPA method 7473 Mercury in solids and solutions by thermal decomposition amalgamation and atomic absorption spectrophotometry Milestone Srl 80
81 Comparison DMA-80 vs. CV-AAS Milestone Srl 81
82 Comparison DMA-80 vs. CV-AAS Technique Sample preparation Wet chemistry Waste generation Sample type Sample size Working range Running cost DMA-80 Not required Not required Minimal Liquid and solids Up to 500 mg sample Up to 600 ng Moderate CV-AAS Acid digestion Yes, to eliminate interferences Yes Aqueous 100 ml solution Limited to low range Elevated Milestone Srl 82
83 Time Comparison DMA-80 vs. CV-AAS Time (minutes) DMA-80 Sample preparation CV-AAS Analysis Milestone Srl 83
84 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 Milestone Srl 84
85 DMA-80 Direct Mercury Analyzer Milestone Srl 85
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