1、Environmental Chemistry Facility Instrumentation htp:/ww.brown.edu/Research/Evchem David Muray, Director MacMilan 114, dmuraybrown.edu, 401-863-3531 CE Instruments NC2100 Elemental Analyzer (MacMilan 221): analysis of carbon, nitrogen, and sulfur concentration of solid samples Sample type: dried, ho
2、mogenized, ground Sample amount: 5-15 mg- depending on concentration Detection: 5-10 g of C or N, 50-100 g S Time: dry, grind, and homogenize samples, weigh out standards and samples, calibrate analyzer (9 analyses), analysis: 3.5 minutes per sample, 63 position autosampler. Cost: $2.50 / sample INO
3、V-X Systems Alpha 4000 Handheld XRF (in GeoChem 134, with use coordinated by David Muray): Non-destructive elemental analysis on a variety sample types for concentrations of some metals ranging from about 20 ppm to 10%. Sample type: most items with a surface 1 cm diameter, highest precision and acur
4、acy on dried, ground, and homogenized samples Sample amount: 1 cm diameter and 1 m thick Detection: 10 ppm-10% for a suite of about 20 element- some more acurate than other Time: 2 minutes per sample, 30 minutes to set up, calibrate, and to put away instrument Cost: N/A Milestone DMA80 Mercury Analy
5、zer (in Barus&Holly 031, with use coordinated by David uray): analysis of mercury in solid or liquid samples Sample type: solids should be ground and homogenized Sample amount: 50-400 mg- depending on concentration Detection: 0.1 ng Hg Time: prepare and weigh samples, calibrate analyzer (2-3 standar
6、ds), analysis: 5 minutes per sample, 40 position autosampler. Cost: $2/sample Lachat QuikChem 8500 Flow Injection Analyzer (FIA (in Osvaldo Salas lab with use coordinated by David Muray)- This wil be replaced by a Westco Smartchem 200 Discrete Analyzer in MacMilan 103, with use coordinated by David
7、Muray: Analysis of Nitrate/Nitrite, Phosphate, and Amonia in waters and chemical extracts, and silicate in water samples Sample type: liquid Sample amount: 5-10 ml Detection: 0.1 ppm Time: prepare sample and standards, calibrate analyzer, 1-3 minutes per analysis Cost: expendable supplies, mostly ch
8、emical reagents asociated with analyses Jobin Yvon JY2000 Inductively Coupled Plasma Atomic Emision Spectrometer (ICP-AES) MacMilan 221: analysis of most elements with atomic weights above 10. Sample type: filtered liquid, either natural waters or digested soil and plant material in an acid matrix (
9、2-10%). Sample amount: 10 ml, 40-500 mg depending on sample preparation and concentrations of elements of interest Detection: 10-20 ppb, note that digested soils and plants are diluted by at least 140x before analysis. Time: dry, grind, and homogenize samples, digest samples (6 hrs/10 samples), cali
10、brate analyzer (30 minutes), analysis: 2-5 minutes per sample depending on number of elements up to 12 elements, 176 position autosampler Cost: $3-$5/sample with minimum charge of $25. Perkin Elmer 4100ZL Graphite Furnace-Atomic Absorption Spectrometer (AS-GF) (MacMilan 221): analysis of metals in l
11、iquids Sample type: filtered liquid, either natural waters or digested soil and plant material in an acid matrix (2-10%) Sample amount: 2 ml, 40-500 mg depending on sample preparation and concentrations of elements of interest Detection: 1-4 ppb, concentrations need to be below 100 ppb Time: dry, gr
12、ind, and homogenize samples, digest samples (6 hrs/10 samples), calibrate analyzer (1 hr), analysis: 5 minutes/sample, 80 position autosampler Cost: $3.00/sample Dionex Modular DX500 Ion Chromatography/HPLC system (MacMilan 221): Column separation of chemical species in liquids Detectors are conduct
13、ivity, UV/is, and fluorescence. Sample type: liquid, fre of high concentrations of interfering components (e.g. salts, acids) Sample amount: 2-3 ml Detection: 0.2-0.5 ppm Time: filter samples, calibrate analyzer (5-10 standards), analysis: 15 minutes per sample, 72 position autosampler for IC, manua
14、l injection for HPLC. Cost: $4-$5/sample with additional with additional costs for interfering component removal. Philips PW1480 X-ray Fluorescence Spectrometer (XRF) (MacMilan 312): Analysis of most elements with atomic weights above 10 (acurate for Si, Al, Fe, Mn, Mg, Ca, Na, K, Ti, Co, Cr, Cu, Ni
15、, Pb, Sr, V, Zn). Sample type: dried, homogenized, fine powder Sample amount: 4-5 g Detection: 5 ppm- requires some procesing of data to get low detection Time: dry, grind, homogenize samples, mix with binder (2 samples/10 minutes), make pelet (5 minutes/pelet), analysis: 25 minutes per sample, 30 p
16、osition autosampler Cost: $7-$10/sample Agilent Technologies 6890+ Series Gas Chromatograph (GC) with flame ionization, electron capture, or mass spectrometer detectors and Purge and Trap sample concentrator (Available in Yongsong Huangs lab with use coordinated by David Muray): Analysis of volatile
17、 organic compounds extracted from solid or liquid samples including SVOCs (PAHs), VOCs (MTBE), and chlorinated organic compounds (PCBs, DT, and Dioxin) Sample type: dried, homogenized, fine powder or organic solvent extraction from soils or water. Sample amount: 1 g dry weight Detection: varies depe
18、nding on detector (ng to g/g) Time: Can be long lead time to schedule machine. 1-2 days of sample preparation, analysis on GC (1 day setup for nonstandard detection 1 hour per sample analysis, 6 position autosampler on GC/MS and 100 position autosampler on GC/FID, 50 position autosampler for Purge a
19、nd Trap. Cost: reimburse lab for expendable supplies, primarily gas and organic solvents Note- the Purge and Trap sample concentrator used for VOC analysis was moved to Eric Suuburgs Lab (PL127) during the Summer 07 and atached to a Shimadzu 2010 GC-ECD, FID Yongsong Huang also has an Agilent Tech.,
20、 1200 LC/MS system that is used to measured organic biomarkers and contaminants. Use is aranged by Yongsong Huang and his technician, Sample preparation Drying Ovens (MacMilan 010): mechanical and gravity convection, dry overnight Drying racks (acilan 010): for air-drying samples Large chest frezers
21、 (MacMilan 010): two for storing samples Cold room (MacMilan 010): 4C room for storing samples Freze Dryer (acilan 010): used to dry samples, freze overnight, then minimum 48 hrs to dry Wiley Mil (MacMilan 011B): used to grind plant material into a fine powder Mixer il (acilan 011A): used to grind s
22、oils and rock material into a fine powder ortar and Pestle: used to grind plants and soils into a coarse powder Milestone Ethos 1600 Microwave digestion (MacMilan 316): used to digest solid material in concentrated acid, 6-7 hr continuous proces w/2 hr break in middle, 12-sample rotor, 10 samples pe
23、r 6 hrs, Cost: $5/sample Dionex Advance Solvent Extraction (ASE) (Available in Yongsong Huangs lab GeoChem 123, with use coordinated by David Muray): used to extract organic compounds from solid samples, 3 hours load time for up to 24 samples, 40 minutes/sample for extraction, 4 hours to unload samples and clean up cels, Cost: expendable supplies and some hardware.