Elemental Analyzer Consumables Our products are intimately involved with your samples

Size: px

Start display at page:

Download "Elemental Analyzer Consumables Our products are intimately involved with your samples"

Loreen McGee
6 years ago
Views:

1 Elemental Analyzer Consumables Our products are intimately involved with your samples Scott Hughes, EA Consumables, Inc. Jon Davies, Elemental Microanalysis, Ltd.

2 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

3 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

4 Intimately Involved Analyzers and Consumables Like the Chicken & Pig in making Breakfast The Analyzer participates The Consumables are intimately involved

5 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

smooth, round bottom smooth Boats, Pans, Disks/Squares, Cones Size 1.

6 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

Very pliable and easy to fold/work Issues

7 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

Also used for removal of inorganic carbon from sample by acid fumigation or addition. No exothermic reaction.

8 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!

9 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

10 Life Cycle of a Pressed Capsule Purchase of special purity foil of the appropriate thickness and width

11 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

12 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.

Cuts round disk Pin forms capsule in die Ejects capsule to collection bin Waste is

13 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.

14 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.

15 Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials

16 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

17 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 Tungstic Oxide Toxic Powdered

18 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

19 Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials

20 Active Reagents, NC analysis Combustion CE/Costech/ Eurovector Elementar Sercon/ Europa Perkin Elmer Chromium Oxide Copper Oxide Chromium Oxide Chromium Oxide Cobaltous/ic Oxide, silvered Lead Chromate Copper Oxide Silver Tungstate on Magnesium Oxide (Silver Wool) (Silvered Copper Oxide) Silver wool Silver Vanadate Silver Gauze Reduction Copper Copper Copper Copper Silver wool Quartz chips Copper Oxide Silver wool

21 Active Reagents, S or NCS analysis Combustion CE/Costech/ Eurovector Elementar Sercon/ Eurpoa Tungstic Oxide Tungstic Oxide Tungstic Oxide on Zirconium Oxide Copper Copper Copper Perkin Elmer Tungstic Oxide on Zirconium Oxide 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.

22 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.

23 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.

24 Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials

25 Interference Removal Reagents Things to remove 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 Sulfur Cl, Br, I F H 2 O Oxidative help

26 Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials

27 Reduction - Copper Available in many forms Copper Wires fine 0.5 x 4mm Copper Wires course 0.65 x 6mm Copper Granules fine mm Copper Granules standard mm Copper Granules course mm Copper wires highest purity for IRMS Electrolytic Copper Copper turning extra fine long strands Copper turnings fine long strands

28 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

29 Your sample and our products have an intimate relationship Sample Encapsulation Combustion Aides-Reaction Blocking Oxidation Reagents Interference removal Reduction Absorption materials

30 Absorption Materials Water Magnesium Perchlorate Regular and Indicating 25g can ship as a HazMat excepted quantity Gets hard when wet, can cause blockages Sicapent (phosphorous pentoxide on inert support indicating) Very low water vapor pressure Most effective desiccant Good flow properties when wet easy to remove Nobody likes to handle (forms phosphorous acid when wet)

31 Absorption Materials Carbon Dioxide Carbosorb (NaOH on support) EMAsorb (our version of Carbosorb black to grey) Soda Lime (mostly calcium hydroxide, some NaOH, and KOH) All above are HazMats 25g bottles can be shipped under excepted quantity rules Chromosorbs Polymers based on diatomaceous earth (mostly SiO2) P types have twice the density and capacity of W types Low blank for CNS so OK for liquid absorbant

specific types of samples Preparation of the reagents has a significant effect on

32 Intimately Involved Conclusions For successful EA-IRMS determinations: Complete conversion of sample into analyte gases Removal of interfering substances Reagents can be tailored for specific types of samples Preparation of the reagents has a significant effect on effectiveness and life of the reagents. Chickens and Pigs can get along together Let just skip breakfast!

How To Break Quartz Combustion Tubes Scott Hughes, EA Consumables Ian Smith, Paul Stevens, Jon Davies, Elemental Microanalysis

How To Break Quartz Combustion Tubes Scott Hughes, EA Consumables Ian Smith, Paul Stevens, Jon Davies, Elemental Microanalysis Quick Answer: Use them in an Elemental Analyzer What is quartz? Second to