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Carbon, sulphur, oxygen and nitrogen: elemental analysis for steel, cement and foundry laboratories

By Vvon Engineering Team | Published | Updated

Compare induction, resistance and inert-gas fusion methods for carbon, sulphur, oxygen and nitrogen analysis, including sample compatibility, reference materials and operating costs.

Steel, foundry and cement laboratories may need different elemental-analysis configurations because their sample matrices, target elements and reporting ranges differ. Furnace type and detector configuration must be considered together: a carbon/sulphur combustion analyser and an oxygen/nitrogen/hydrogen inert-gas-fusion analyser do different jobs. Start with representative samples and the method the laboratory must report against.

Ask the manufacturer to demonstrate the proposed configuration on representative material, with blanks and suitable certified reference materials. A high maximum temperature alone does not establish recovery, detection capability or freedom from interference.

The furnace decides which carbon and sulphur analyser you need

There are three furnace types in routine use and they split the work cleanly.

Induction, for inorganic material. The ELEMENTRAC CS-i: Carbon / Sulphur Analyser burns steel, cast iron, ores and ceramics above 2,000 degrees Celsius in oxygen, and measures the resulting carbon dioxide and sulphur dioxide by solid state infrared absorption. The detail that matters on site is the handling of dust: these materials throw a lot of it, and the CS-i carries a heated dust trap and a platinum based catalyst reactor for exactly that reason. A steel or foundry laboratory in Bangladesh, running many samples a shift on the same alloy family, wants this machine.

Horizontal resistance, for organic material. The ELEMENTRAC CS-r: Carbon / Sulphur Analyser uses ceramic boats, which allow a high sample weight, and runs at a furnace temperature adjustable to 1550 degrees Celsius in one degree steps. Its infrared path is made of solid gold, which resists the halogen and acid combustion products that corrode aluminium cells. If the laboratory is analysing coal, coke, biomass, soil or anything containing chlorine, the gold path is not a refinement; it is what stops the cells being consumed.

Both, in one cabinet. The ELEMENTRAC CS-d: Carbon / Sulphur Analyser carries an induction furnace and a resistance furnace together, so organic and inorganic samples run on the same instrument without a configuration change, with up to four independent infrared cells covering different concentration ranges. For a contract laboratory or a group with mixed sample types, that avoids owning two machines and calibrating both.

Two further configurations exist for organic work in a vertical furnace. The CS-580A: Carbon / Sulphur Analyser covers simultaneous carbon and sulphur and also total organic and total inorganic carbon, and it requires an autoloader with 36 or 130 crucible positions for unattended running. Where hydrogen has to be reported as well, the ELEMENTRAC CHS-r: Carbon / Hydrogen / Sulphur Analyser measures all three simultaneously to DIN, EN and ISO methods in a horizontal resistance furnace, and the CHS-580A: Carbon / Hydrogen / Sulphur Analyser is the vertical equivalent. The high sample weight the ceramic boats allow matters more than it sounds for coal, coke and biomass, where a small aliquot of a heterogeneous material is simply not representative of the consignment.

Cement and gypsum are a separate case, because the question is not really carbon at all. The CW-800: Carbon Dioxide / Water Analyser determines carbon dioxide and water simultaneously in a quartz tube resistance furnace held at a fixed temperature up to 1000 degrees Celsius under nitrogen, measuring through a gold path so no halogen trap is needed. Where organic and inorganic carbon have to be separated, the CW-800M: Carbon / Water Analyser steps the furnace through up to five programmed temperatures in one run and separates them by release temperature rather than by acid treatment, which removes a wet chemistry step and the errors that go with it. Its maximum sample size is 32 by 145 mm in a quartz boat. And where the carbon of interest is a surface residue rather than bulk carbon, the SurfaceC-800: Surface Carbon Analyser varies both furnace temperature and carrier gas to a user defined programme so the surface fraction is driven off and measured separately from the matrix.

Oxygen, nitrogen and hydrogen come from a different machine entirely

Carbon and sulphur are measured by burning the sample in oxygen. Oxygen, nitrogen and hydrogen cannot be, for the obvious reason. They are measured by hot extraction: the sample is fused in a graphite crucible under an inert carrier, and the gases released are carried to the detectors. That means a different furnace, a different gas system and a different consumable.

AnalyserElementsNote
ELEMENTRAC ONH-psOxygen, nitrogen and hydrogenElectrode impulse furnace; oxygen and hydrogen measured through infrared channels and nitrogen through thermal conductivity. Confirm the carrier-gas arrangement for the required elements and method.
ELEMENTRAC ONH-pOxygen, nitrogen and hydrogenImpulse furnace on the hot extraction principle for steel, non-ferrous metals and ceramics
ELEMENTRAC ON-pOxygen and nitrogenOxygen measured as carbon dioxide by infrared, nitrogen by thermal conductivity. For laboratories where hydrogen is not in the specification
ELEMENTRAC OH-pOxygen and hydrogenFor methods requiring oxygen and hydrogen; confirm measurement range, gas arrangement and analysis sequence with the manufacturer.
ELEMENTRAC H-rHydrogen onlyHot extraction below the melting point, so diffusible hydrogen is released without fusing the matrix

Carrier gas is part of the method and the recurring budget. ELTRA describes the ONH-ps detector arrangement and carrier-gas options, but its functional description specifically associates optional argon with oxygen and nitrogen. Ask ELTRA to confirm the approved gas and configuration for hydrogen-inclusive work before substituting helium.

For a cracking investigation, distinguish diffusible hydrogen from total hydrogen and define the specimen handling and extraction method. A below-melting-point extraction configuration can address a different hydrogen fraction from fusion analysis; the result also depends on extraction temperature, duration and the sample history.

Two instruments in the range sit outside the metals world. The ELEMENTRAC CN-r: Carbon / Nitrogen / Protein Analyser is a Dumas combustion analyser that calculates protein from the nitrogen result, and it is the alternative to Kjeldahl digestion for food, feed, soil and fertiliser laboratories, avoiding the concentrated acid and catalyst the wet method requires. For a Bangladeshi feed mill or soil testing laboratory, removing sulphuric acid from a routine method is a safety improvement as much as an analytical one. And the TGA THERMOSTEP: Thermogravimetric Analyser determines moisture, volatile matter, ash and loss on ignition in one programmed run by weighing continuously as the furnace steps through temperature stages, carrying up to 19 samples on a carousel. For coal, coke, biomass and mineral laboratories running proximate analysis, that single instrument replaces a morning of oven and muffle work.

Consumables, blanks and the cost nobody quotes

Combustion analysis consumes something on every single run. Crucibles, ceramic and quartz boats, reagents, catalysts and furnace parts are all listed as Consumables for Elemental Analysers, and the reason they belong in the analytical method rather than in general stores is that the grade of crucible and reagent sets the blank value. A cheaper crucible with a higher carbon background raises the blank, and at low carbon levels the blank is a large fraction of the result.

Three practical consequences follow.

  1. Price the consumables per analysis, not per pack. Two quotations for the same instrument can differ by a factor over five years entirely on the consumable line. Ask for a cost per determination at your expected sample count.
  2. Hold enough stock for a shipping delay. Crucibles are heavy, low value and slow to clear customs, and a works laboratory that runs out stops reporting. The general shipping and clearance problem is set out in what actually delays a laboratory equipment shipment into Bangladesh.
  3. Run and record the blank as a control chart, not as an occasional check. A rising blank is the earliest visible sign that a reagent tube is exhausted or a crucible batch has changed, and it appears well before the results start disagreeing with a reference material.

Sample preparation is upstream of the analyser. Agree the required particle size, homogenisation and splitting method for each matrix. Excessive grinding or an unsuitable grinding medium can introduce contamination or change volatile content; the finest obtainable powder is not automatically the right preparation.

Finally, the software layer. ELEMENTS: Elemental Analyser Software handles method setup, calibration, result filtering and report generation for the ELEMENTRAC generation, and it is the operating layer of the instrument rather than an optional extra. ELEMENTS Cloud: Remote Instrument Management allows an analyser to be monitored and managed remotely, which is aimed at organisations running several analysers across sites. For a group with plants in Dhaka, Chattogram and Gazipur, remote visibility of instrument status is a practical way to keep three laboratories reporting the same way, and it shortens the diagnostic conversation when one of them stops.

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