Dumas Analytical System Laboratory Instruments Dumatherm.

Dumas Analytical System

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DUMATHERM

COMPETITION

LECO Corp. St. Joseph, Michigan, USA

Dr. Werner Küppers

C. Gerhardt GmbH, Königswinter

SALES TRAINING

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TOPICS

LECO competition

Company profile and history Product range of LECO Truespec N as direct competition

Principle Features and benefits Comparison with DUMATHERM Summary in table form

DUMATHERM – Keyfeatures

We are the fastest We have less

maintenance We have the easiest up-

to-date technology Helium technology

allows lowest nitrogen contents

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5Combustion technology

easy and straightforward

Combustion of samples with pure oxygen

Reduction of all nitrogen oxides

Easy separation of CO2 and H2O

Analysis of resulting gases with a thermal conductivity detector

Connector tubing

CO2 Adsorbers

Nafion tubing

Detector

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COMBUSTION PRINCIPLE

CnHmNx + a O2

950 °C

Must be separated !

Oxidation:

n CO2 + ½ m H2O + x N-Oxides

Combustion of samples with pure oxygen (i.e. system must be purged to get rid of air)

Remaining ash must be separated Reduction of all nitrogen oxides Separation of CO2 and H2O Analysing of resulting gases with a thermal conductivity

detector

COMPETITIONDUMATHERM

LECO Corp. Laboratory Equipment Corporation

St. Joseph, Michigan, USA

LECO Truespec N Long history of combustion

instruments since 1936 with an estimated market share of approximately 50% or more

TruespecN is the end of a long history of models in the combustion field

LECO is a specialist in carbon analysis with a focus on steel industry

Food and feed instruments were added in the early 90s to complete the product range

available since 2004

LECO Principle Combustion with high

excess of oxygen Separation of dust

with two filters Separation of water Collection of gases in

ballast volume Aliquot of 2 ml is

taken out and transported to the detector after passing some more scrubbers

Brochure FP-2000

LECO Autosampler

LECO Autosampler (silver) compared with our (black) plate

Who can put more sample weight into his autosampler ?

How to put in1gram into a LECO ?

LECO autosampler with a tin foil ball with 500 mg of milk powder

Impossible to analyse !!!

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Combustion Principle LECO

CnHmNx + 4500 ml O2

950 °C

Oxidation with tremendous excess of oxygen: x N-Oxides

Combustion is ALWAYS done with 4500 ml oxygen, not looking at the sample type (no difference between 5 mg EDTA or 1000 mg of animal feed)

We use e.g. 100 ml oxygen for 100 mg EDTA which saves 4400 liter gas

Handling oxygen lance: breaks often and has to be connected to the flange on top

Ash insert is a porous ceramic crucible

LECO Combustion Tube / Old Type

Tube is firmly fixed in the furnace and difficult to be taken out

Furnace has to be almost cool for exchanging tubes

While taking it out it is easily destroyed

Material inside is just for filtering off the dust particles from the combustion

LECO combustion

U-shaped tube cracks often and is difficult to mount and dismount

More O-rings=more leaks

Oxygen lance must be fixed very complicated at the lance holder and cracks very often during this operation (costs 350 Euro)

Crucible: 210 Euro Trapping material is to

absorb the dust during combustion

LECO Combustion Tube / New

DUMATHERM: Combustion Tubes

Easy to handle Exchange in hot

status possible Only two o-rings for

fixation and for sealing

Oxygen dosing is done according to the sample weight (200 mg EDTA = 200 ml oxygen)

1:1 dosing results in less dust

Separation of Dust with LECO

Combustion at lower temperature and with high excess of oxygen causes problems with dust

Dust filters are needed Extra filter is mounted in the

furnace The dust from the

combustion is separated to a large amount

Dust filter trap must be emptied and refilled by the customer (hazardous powders)

Ballast Volume and Aliquot Valve

Ballast tank collects all combustion gases

Aliquot valve takes out a loop of 2 ml from 4500 ml (0.04 %) and ONLY 2 ml are analysed with the detector

This operation is needed, because these 4400 ml non-consumed oxygen would oxidise the copper for reduction completely during one analysis

Ballast tank must be calibrated according to the surrounding air pressure. This calibration must be adjusted day by day

Ballast control needs 9 additional valves

Aliquot Valve with 2 ml loop

Ballast Volume LECO Gases should be filtered befor entering the ballast volume Effectivity of dust traps is very poor, because dust

particles are always passing the traps into the ballast volume which makes frequently cleaning and volume calibration necessary

More sample weight = more dust = MUCH more maintenance!

Used and brand new ballast volume

Water Absorber LECOSORB No specialty, just sodium

hydroxide on a little bit of silica support

Hazardous consumable Customer has to refill the

trap every week

Electronics and Structure

• Old fashioned and not up to date electronics with touch panel and keyboard at the instrument e.g. in the FP-2000• In general, electronic boards are not protected in a separated area • Cables everywhere in this chaotic construction !!

DUMATHERM Electronics

Clear structure One mainboard Easy to understand Electronics separated

from the rest of the instrument

…

Detector with LECO

• Old fashioned and not up to date detection technology based on the wheatstone resistance bridge principle• Measuring gas flow and reference gas flow MUST be kept 100% constant• Once again: chaotic construction

Detector CalibrationLECOData series for the calibration [in mg Aspartic acid or EDTA] : 1, 2, 3, 5, 7.5, 10, 15, 20, 25, 30, 50, 75, 100, 125, 150, 175, 200, 250, 300, 350

Daily Routine LECO:Two calibration standards are measured after the system has stabilized and the result is taken to shift the calibration upwards or downwards. System must be perfectly stable within this period.

DUMATHERM:

5-8 points

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SPEED: We are the fastest !

Based on the ballast volume principle, LECO has to fill the 4.5 litre ballast volume with every sample or blank value.

This takes always the same time while we adjust the combustion time on the sample weight (i.e. less sample weight means less analysis time, e.g. 100 mg EDTA = 15 s

No nitrogen analyser can do a nitrogen determination based on a reference method faster than DUMATHERM in about 3 minutes

„Duma“ is the Kisuaheli expression for „cheetah“, the worlwide fastest animal on land

Never ending list of O-rings of different sizes and materials

Single parts expensive (service kits available)

Often LECO service is needed for the change of those parts

Service expensive

35 valves (we have only 10!)

COSTS

O-Ringsreference card with 26 different types

DUMATHERM: just 4 different o-rings> 6 times less

Maintenance to be done by customer

Taken from the service manual for Truespec N

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Spare Parts and ServiceDUMATHERM vs. Truespec

No other instrument worldwide has less parts in the spare part catalogue than we have E.g. LECO has 26 different o-rings in the Truespec,

DUMATHERM needs only 4! No other instrument worldwide has such a service

friendly construction and such a clear structure Service with LECO can only be done by LECO

specialists while DUMATHERM can be maintained by the customer

No other instrument worldwide has less articles in the spare part catalogue LECO has a never ending list of spare parts

No other instrument worldwide can be installed in the morning and gives good analytical results in the afternoon LECO needs a set-up-time of 2-3 days at least bevor

starting the first EDTA…

Routine work on a LECO: If the combustion tube needs replacement you have to cool down the system and you need a full tool kit, which means that you are off for hours.

Customer experience:Very few people have a “comfortable” experience with LECO these days. They used to be very close to their customers and form strong relationships, but the current ethos leaves people feeling somewhat cheated and facing high costs.

Many users source their consumables and service from third parties because of high LECO prices

… Disadvantages of LECO

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Striking Arguments against LECO

Compacter DUMATHERM design (65 kg against 130 kg) Clearer construction easy to understand allows well-founded

customer training within one day. Analysis of all combustion gases and not only an aliquot is

analysed after passing the ballast volume Maintenance free parts for water and carbon dioxide

separation whereas LECO uses traps which must be emptied frequently

Low service and maintenance costs due to well-thought construction

Truespec must be kept ON to prevent long set-up-times after restarting the unit

20 times more oxygen consumption in every analysis, even with blanks

Gas dilution causes massive problems with low nitrogen ranges (e.g. < 0.1% N)

LECO only sells instruments because of their historic position

DUMATHERM is the better instrument, it is

reliable, precise, easy to use and to maintain

Flowchart DUMATHERM

Easy principle and only 10 valves!

DUMATHERM Combustion

Easy access without further dismounting of parts

No need to cool down the system completely

Well-priced ash inserts with high capacity

Catalyst to support the combustion reaction and avoid dust problems

DUMATHERM Bottom Connection

Easy access without further dismounting Well-priced plastic tubing as the only part to be exchanged If dust is passing the reactor, it is trapped in the quartz wool

Reduction

650 °C

copper reducedN- oxides N2

We have the best copper chips with the largest surface

More surface = more capacity for reaction

Easy to take out the tube

Easy to refill Costs acc. to price lists

: LECO 250g=132

EUR Gerhardt 250g=65 EUR

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Water Separation with NafionTM

• Maintenance free system !

• Inside: gas stream with helium, nitrogen, water and carbon dioxide

• Membrane: polar and chemical inert material

• Specific reaction with water

• In-built functional groups, each of them can trap 13 water molecules

• Outside: counterflow of pure nitrogen separates 100% of the absorbed water

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News: Water Trap to analyse as well liquid samples

• Target: pre-condensation of 95 % of all water with automated drainage controlled by software

• Remaining water is separated with Nafion

• Easy discharging of separated water

• With LECO the water is trapped with Peltier technique befor going into the ballast volume

• If the separation was not 100 %, water condensation is found in the ballast volume = cooling down and cleaning is a must

• With liquid samples we have now good chances to win against LECO !!

Direct Comparison of Specifications

Model LECO TRUSPEC N DUMATHERM

Positions Autosampler 30 (60, 90, 120) 40 (80, 120)Possible sample weights according to brochure up to 1 g up to 1 gTypical sample weights in reality 200-400 mg 50-300 mgDetection limit (in mg Nitrogen absolute) 0.01 mg N 0.ic01 mg N

All combustion gases analysed ? no (aliquot) yes

Detector classic TCD innovative TCD

Daily adjustment of calibration yes no

Analysis time 4 to 6 minutes 3 to 4 minutes

Number of valves 35 10

Number of o-rings 24 8

Combustion tubeu-shaped quartz with

dust filtersstraight quartz with

catalyst