Elemental Analyzer Consumables Our products are intimately involved with your samples Scott Hughes, EA Consumables, Inc. Jon Davies, Elemental Microanalysis, Ltd.
Intimately Involved A lot of focus is on the laboratory instruments Things that cost a lot get a lot of attention Impressive and shiny for lab tours The Big The Tenacious The Colorful
Intimately Involved Simple truth If you do not get complete conversion of your analyte to N 2 , CO 2 , SO 2 , CO or H 2 , then the big expensive shiny “detectors” will not help you. The instrumentation IS important. Has to provide: Ability to transfer sample Hot environment with a steady carrier flow Ability to add oxygen at correct time and place and …the “detector” does matter
Intimately Involved Analyzers and Consumables Like the Chicken & Pig in making Breakfast The Analyzer participates The Consumables are intimately involved
Your sample and our products have an intimate relationship Focus on the nature and applications of consumables for NC and NCS determinations Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials
Sample Encapsulation Many Choices – Over 400 from Elemental Microanalysis Material – Tin, Silver, Nickel, Copper, Aluminum, Cellulose Form Capsules: Pressed, Flat bottom smooth, round bottom smooth Boats, Pans, Disks/Squares, Cones Size – 1.06mm to 32mm diameter Weight – Standard, light weight, ultra light weight Preparation – Standard, Pre-cleaned
Encapsulation Tin The “go to” encapsulation material Exothermically reacts with oxygen to help in the thermal decomposition of the sample. Very pliable and easy to fold/work Issues In situ carbon blank Tin oxide is corrosive to quartz at operating temperatures
Encapsulation Silver Typically used for oxygen determination, as there is no formation of an oxide (at combustion temperatures) as is the case with tin Can tarnish in storage. Will be removed at 375 o C. Also used for removal of inorganic carbon from sample by acid fumigation or addition. No exothermic reaction. No ash, forms a silver melt in the reaction tube It is stiffer and not as easy to fold/work compared to tin Higher cost Big savings in the lightweight silver capsule options HINT: Collect the waste. Can fund a wild lab party!
Encapsulation Aluminum Can be pre-combusted at 550 o C to remove contaminants There is an art to get it to combust. Can inhibit full sample reaction. Forms Pressed – Solids Pre-cleaned in sample well Smooth wall (flat or round bottoms) – liquids Disks/Squares/Cones – sticky, fibrous, big samples Evaporating cups – liquid reduction
Life Cycle of a Pressed Capsule Purchase of special purity foil of the appropriate thickness and width
Life Cycle of a Pressed Capsule Purchase of special purity foil of the appropriate thickness and width Feeds into custom made cutting/pressing machine. Cuts round disk Pin forms capsule in die Ejects capsule to collection bin
Life Cycle of a Pressed Capsule Purchase of special purity foil of the appropriate thickness and width Feeds into custom made cutting/pressing machine. Cuts round disk Pin forms capsule in die Ejects capsule to collection bin Waste is melted down and cast into ingots.
Life Cycle of a Pressed Capsule Purchase of special purity foil of the appropriate thickness and width Feeds into custom made cutting/pressing machine. Cuts round disk Pin forms capsule in die Ejects capsule to collection bin Waste is melted down and cast into ingots. Ingots are rolled into sheets suitable for the extruded smooth wall capsules
Life Cycle of a Pressed Capsule Purchase of special purity foil of the appropriate thickness and width Feeds into custom made cutting/pressing machine. Cuts round disk Pin forms capsule in die Ejects capsule to collection bin Waste is melted down and cast into ingots. Ingots are rolled into sheets suitable for the extruded smooth wall capsules Ultra-Pure capsules get an additional solvent wash. Weighed into final package.
Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials
The path to N 2 , CO 2 , SO 2 The combustion soup Organicish Sample + O 2 + heat (~1,000 o C) = Volatile combustion products CO, CO 2 , CH 4 ,CO 3 ,H 2 O,N 2 ,N x O x ,SO 2 ,SO 3 ,X - ,HF Block the formation of… Chemical Oxidation to CO2 Reduce Absorb
Combustion aides Added to sample Additional oxygen source at point of combustion Block undesired side reaction Stable sulfides and carbonates Will fuse with alkali and alkaline earth oxides Vanadium Pentoxide Toxic Tungstic Oxide Powdered
Combustion aides Fine Powders Niobium Pentoxide Added oxygen Silver Oxide Added oxygen Cobalt Oxide Added oxygen Magnesium Oxide Added oxygen – bind F - Sucrose For inorganic fertilizers Carbon powder (high purity) as above Tin powder Added heat
Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials
Active Reagents, NC analysis CE/Costech/ Elementar Sercon/ Perkin Elmer Eurovector Europa Chromium Oxide Copper Oxide Chromium Oxide Chromium Oxide Combustion Cobaltous/ic Oxide, Lead Chromate Copper Oxide Silver Tungstate on silvered Magnesium Oxide (Silver Wool) (Silvered Copper Silver Vanadate Oxide) Silver wool Silver Gauze Reduction Copper Copper Copper Copper Silver wool Quartz chips Copper Oxide Silver wool
Active Reagents, S or NCS analysis CE/Costech/ Elementar Sercon/ Perkin Elmer Eurovector Eurpoa Tungstic Oxide Tungstic Oxide Tungstic Oxide on Tungstic Oxide on Combustion Zirconium Oxide Zirconium Oxide Copper Copper Copper Reduction None Copper None None Silver wool (cooler zone)
Not all the same Chromium Oxide Key impurities in the Chromium Oxide can cause devitrification of quartz Devitrification is accelerated in the presence of Na & P ions. Most Cr 2 O 3 is formed from sodium dichromate, so Na is always present Elemental Microanalysis uses a different process to form Cr 2 O 3 to results in lower sodium impurities. After granulation, it is further heat treated to drive off other impurities The results is much longer tube life The tube on the left showed no signs of devitrification after 1,000 determinations.
Not all the same Tungsten (VI) Oxide, Tungsten Trioxide, Tungstic Oxide These actually are all the same. B1025 Tungstic Oxide, granular for Costech/Thermo/Europa Produced by reacting Scheelite (CaWO 4 ) with HCl to form tungstic acid, followed by decomposition to WO 3 The material is tableted under very high pressure, and then ground to the appropriate size. Results is very dense material. B1217 Tungstic Oxide, granular for Elementar Requires a less dense granular material Produced by reacting tungsten metal with oxygen at elevated temperature. Results in a much less dense granule.
Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials
Interference Removal Reagents Things to remove Sulfur Cl, Br, I F H 2 O Oxidative help Silver Wool/Gauze Coboltous/ic Oxide Silvered Copper granules silvered Copper Oxide silvered Silver Vanadate Silver Tungstate/Magnesium Oxide Magnesium Oxide Lead Chromate Iron Wool
Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials
Reduction - Copper Available in many forms Copper Wires fine 0.5 x 4mm Copper Wires course 0.65 x 6mm Copper Granules fine 0.05 – 0.2mm Copper Granules standard 0.1 – 0.5mm Copper Granules course 0.3 – 0.85mm Copper wires highest purity for IRMS Electrolytic Copper Copper turning extra fine long strands Copper turnings fine long strands
Reduction – Copper Cu + O 2 + N x O x + SO 3 CuO + Cu 2 O + N 2 + SO 2 Cu + SO 2 (lower temperature) CuS + CuO + Cu 2 O Surface reaction More available surface area, more capacity In general wrt capacity Granular > Wires Fine > Standard > Coarse An old penny > Electrolytic copper “Normal Copper” has very low capacity Copper is first oxidized and then subsequently reduced IRMS grade – longer reaction time
Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials
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