Elemental Analyzer Consumables
Our products are
intimately involved with your samples
Scott Hughes, EA Consumables, Inc.
Jon Davies, Elemental Microanalysis, Ltd.
Intimately Involved
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A lot of focus is on the laboratory instruments
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Things that cost a lot get a lot of attention
Impressive and shiny for lab tours
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The Big
The Tenacious
The Colorful
Intimately Involved
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Simple truth
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If you do not get complete conversion of your analyte to N2,
CO2, SO2, CO or H2, then the big expensive shiny “detectors”
will not help you.
The instrumentation IS important. Has to provide:
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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
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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
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Sample Encapsulation
Combustion Aides-Reaction Blocking
Oxidation Reagents
Interference removal
Reduction
Absorption materials
Sample Encapsulation
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Many Choices – Over 400 from Elemental Microanalysis
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Material – Tin, Silver, Nickel, Copper, Aluminum, Cellulose
Form
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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
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Tin
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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
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In situ carbon blank
Tin oxide is corrosive to quartz at operating temperatures
Encapsulation
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Silver
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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 375oC.
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
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Aluminum
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Can be pre-combusted at 550oC to remove contaminants
There is an art to get it to combust. Can inhibit full sample reaction.
Forms
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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
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Purchase of special purity foil of the
appropriate thickness and width
Life Cycle of a Pressed Capsule
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Purchase of special purity foil of the
appropriate thickness and width
Feeds into custom made cutting/pressing
machine.
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Cuts round disk
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Pin forms capsule in die
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Ejects capsule to collection bin
Life Cycle of a Pressed Capsule
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Purchase of special purity foil of the
appropriate thickness and width
Feeds into custom made cutting/pressing
machine.
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Cuts round disk
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Pin forms capsule in die
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Ejects capsule to collection bin
Waste is melted down and cast into ingots.
Life Cycle of a Pressed Capsule
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Purchase of special purity foil of the
appropriate thickness and width
Feeds into custom made cutting/pressing
machine.
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Cuts round disk
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Pin forms capsule in die
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Ejects capsule to collection bin
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Waste is melted down and cast into ingots.
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Ingots are rolled into sheets suitable for the
extruded smooth wall capsules
Life Cycle of a Pressed Capsule
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Purchase of special purity foil of the
appropriate thickness and width
Feeds into custom made cutting/pressing
machine.
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Cuts round disk
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Pin forms capsule in die
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Ejects capsule to collection bin
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Waste is melted down and cast into ingots.
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Ingots are rolled into sheets suitable for the
extruded smooth wall capsules
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Ultra-Pure capsules get an additional solvent
wash.
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Weighed into final package.
Your sample and our products
have an intimate relationship
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Sample Encapsulation
Combustion Aides-Reaction Blocking
Oxidation Reagents
Interference removal
Reduction
Absorption materials
The path to N2, CO2, SO2
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The combustion soup
Organicish Sample + O2 + heat (~1,000oC) =
Volatile combustion products
CO, CO2, CH4,CO3,H2O,N2,NxOx,SO2,SO3,X-,HF
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Block the formation of…
Chemical Oxidation to CO2
Reduce
Absorb
Combustion aides
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Added to sample
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Additional oxygen source at point of combustion
Block undesired side reaction
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Stable sulfides and carbonates
Will fuse with alkali and alkaline earth oxides
Vanadium Pentoxide
Toxic
Tungstic Oxide
Powdered
Combustion aides
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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
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Sample Encapsulation
Combustion Aides-Reaction Blocking
Oxidation Reagents
Interference removal
Reduction
Absorption materials
Reduction
Combustion
Active Reagents, NC analysis
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 Vanadate
Silver wool
Silver Gauze
Copper
Copper
Copper
Copper
Silver wool
Quartz chips
Copper Oxide
Silver wool
Reduction
Combustion
Active Reagents, S or NCS analysis
CE/Costech/
Eurovector
Elementar
Sercon/
Eurpoa
Perkin Elmer
Tungstic Oxide
Tungstic Oxide
Tungstic Oxide on
Zirconium Oxide
Tungstic Oxide on
Zirconium Oxide
Copper
Copper
None
None
Copper
None
Copper
Silver wool (cooler
zone)
Not all the same
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Chromium Oxide
Key impurities in the Chromium Oxide can cause
devitrification of quartz
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Devitrification is accelerated in the
presence of Na & P ions.
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Most Cr2O3 is formed from sodium
dichromate, so Na is always present
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Elemental Microanalysis uses a
different process to form Cr2O3 to
results in lower sodium impurities.
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After granulation, it is further heat
treated to drive off other impurities
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The results is much longer tube life
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The tube on the left showed no
signs of devitrification after 1,000
determinations.
Not all the same
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Tungsten (VI) Oxide, Tungsten Trioxide, Tungstic Oxide
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B1025 Tungstic Oxide, granular for
Costech/Thermo/Europa
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These actually are all the same.
Produced by reacting Scheelite (CaWO4) with HCl to form tungstic acid,
followed by decomposition to WO3
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
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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
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Sample Encapsulation
Combustion Aides-Reaction Blocking
Oxidation Reagents
Interference removal
Reduction
Absorption materials
Interference Removal Reagents
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Things to remove
Sulfur
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
Cl, Br, I
F
H2O
Oxidative
help
Your sample and our products
have an intimate relationship
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Sample Encapsulation
Combustion Aides-Reaction Blocking
Oxidation Reagents
Interference removal
Reduction
Absorption materials
Reduction - Copper
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Available in many forms
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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 + O2 + NxOx + SO3  CuO + Cu2O + N2 + SO2
Cu + SO2 (lower temperature)  CuS + CuO + Cu2O
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Surface reaction
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More available surface area, more capacity
In general wrt capacity
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Granular > Wires
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Fine > Standard > Coarse
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An old penny > Electrolytic copper
“Normal Copper” has very low capacity
Copper is first oxidized and then subsequently reduced
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IRMS grade – longer reaction time
Your sample and our products
have an intimate relationship
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Sample Encapsulation
Combustion Aides-Reaction Blocking
Oxidation Reagents
Interference removal
Reduction
Absorption materials
Absorption Materials
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Water
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Magnesium Perchlorate
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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)
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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)
Absorption Materials
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Carbon Dioxide
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All above are HazMats
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Carbosorb (NaOH on support)
EMAsorb (our version of Carbosorb – black to grey)
Soda Lime (mostly calcium hydroxide, some NaOH, and KOH)
25g bottles can be shipped under excepted quantity rules
Chromosorbs
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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
Intimately Involved
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Conclusions
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For successful EA-IRMS determinations:
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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!