Elemental Analyzer inlets for IRMS applications

Elemental Analyzer inlets for IRMS applications

- EA-IRMS solutions from Elementar -

April, 26th 2016

Dr. Marc Ruppenthal

Product Manager Elemental Analysis

and EA-IRMS interfaces

Elementar Webinar Series

27/04/2016 Webinar EA-IRMS solutions 2

Agenda elementargroup - the company - 1

Functional principles of elemental analysis for IRMS interfaces 2

General features for better EA-IRMS analysis 3

High performance EA-IRMS systems from Elementar 4

Summary 5

110 years tradition… Heraeus


The elementargroup – tradition means trust

• Approx. 1860: W. C. Heraeus utilizes high temperature technologies in order to

process platinum

• Approx. 1900: Heraeus produces high purity quartz glass which is soon used in

elemental analysis


Wilhelm Carl Heraeus Pharmacy “White Unicorn”

The elementargroup – tradition means trust


• Approx. 1905: First generation of elemental analyzers

with electrical furnaces produced by

Heraeus

• 1923: Fritz Pregl receives the Nobel Prize in

Chemistry for his invention of the method

of micro-analysis of organic substances,

using dedicated analytical equipment

manufactured by Heraeus

The elementargroup history


was founded

1851

Dennstedt patent "über die vereinfachte Elementaranalytik" was the basis for the

1st instrument generation

1904

The first elemental analyzer for simultaneous detection of carbon, hydrogen

and nitrogen was invented.

1932

The first Dumas Nitrogen/Protein analyzer was introduced

1964

The EA business of Heraeus was sold in a management buyout and restructured

under the brand name Elementar.

1995

The High temperature TOC analyzer was introduced

1973

The first fully automatic elemental analyzer with TCD detection was introduced

1980



Introduction of the "cube" platform vario MICRO cube, vario EL cube, vario MACRO cube, rapid N cube

2006

vario TOC cube

2008

rapid CS cube, vario ISOTOPE cube, vario PYRO cube

2009

rapid N exceed, rapid OXY cube

2014

trace SN cube

2010

vario MAX cube, iso TOC cube

2012

Isoprime Ltd was acquired



Introduction of the inductar series inductar CS cube, inductar ONH cube,

inductar EL cube

2015

rapid MAX N exceed, rapid MiCRO N cube

2016

The elementargroup – Tradition means trust


• Inventor of the elemental analyser

The first automated elemental analyser was

developed by our direct predecessor

Heraeus

• We are a strong family

Family owned enterprise without the

uncertainties of a sudden change in ownership,

organisational structures, management and

staff

Heraeus historic elemental analyzer, type "CH Analysator", construction year 1932. The worldwide first elemental analyzer with electrical furnaces.



• Reliability

Since ELEMENTAR emerged from the Heraeus organisation

in 1990, the group management has not changed. The

fluctuation of staff is on an absolute minimum.

• Long-term orientation

ELEMENTAR is long term oriented. Spare parts are provided

for a minmum of 10 years – also after production stop of an

instrument – but also older instruments continue to get

technical support. Some of them are in operation for 30

years and more.



• Quality made in Germany

All instruments are manufactured in our headquarter in

Hanau - quality made in Germany by ELEMENTAR ensures

highest quality and reliability for the users.

• 100 % dedicated to elemental analysis

Due to our 100 % dedication to combustion type

elemental analyzers we are able to provide a large variety

of instruments in this segment. You will have the choice to

select according to your specific needs in performance and

price.






Summary 5

Theory of isotope fractionation


• Slight differences in atomic mass

• cause slight differences in bond energy

• cause slight differences in physical and

chemical properties 2H

1H 1H

1H

• Example: Hydrogen isotope

ratios in global precipitation

How can we investigate isotope ratio variation?


• An IRMS detects beams of ionized gases (gas

source mass spectrometry)

• The substance under investigation needs to

be converted quantitatively into the gas phase

• …of course in a reliable, reproducible,

uncomplicated, unbiased, fast and cost-saving

way

Burn, burn, burn,…


• 110 years of experience in combustion

analysis – your benefit

• High-temperature furnace for continuous

operation up to 1200°C

• Low voltage (48 V) concept for reliability and

safety

• Easy access for tube exchange

• 10 year warranty

Burn, burn, burn,…


• The oxygen is directed exactly to the spot of

combustion

• Oxygen is only added when needed

• Complete combustion is achieved with always the

right amount of oxygen per analysis

• With an EA-IRMS system from elementargroup

there can and will never be isotope fractionation

artefacts from incomplete combustion

o

Combustion elemental analysis

Webinar EA-IRMS solutions 17 27/04/2016

Sample combusts changing into a gas

Components converted to

uniform compounds

Separation and Detection

CHNS Mode at 1150°C


reduction on copper and binding of excess oxygen

oxidation on WO3 in presence of oxygen

O2, N2, NOx, CO2, SO2, SO3, H2O,

HCl,...

Organic and inorganic

compounds containing

C,H,N,S, Cl... Ag removes halogens

N2, CO2, H2O, SO2





uniform compounds


Isothermal gas chromatography – working principle


Combustion

Carrier Gas

Oxygen

Reduction

Carrier gas

TCD

Detector out

Detector in

Combustion Gas Formation Gas Handling Detection

Inlet Feeder

Sample Input

GC Column

Used in various Non-Elementar systems

Tin foil capsules Vertical furnace Closed sample inlet valve

Gas separation using GC column technology


• Unfocused SO2 sample peak

• Low peak amplitude

• Low sensitivity

• Danger of memory effects

• Danger of isotope fractionation

artefacts

• Very limited capacity/sample

amount

o

SO

2 R

efe

rence

Peak

SO

2 S

am

ple

Peak

Advanced Purge and Trap – working principle


Combustion

Carrier Gas

Oxygen

Reduction

Carrier gas

TCD

Detector out

Detector in

Combustion Gas Formation Gas Handling Detection

Inlet Feeder

Sample Input

SO2 Trap

Elementar vario ISOTOPE select, vario ISOTOPE cube, vario PYRO cube

U U U CO2 Trap

H2O Trap

Tin foil capsules Vertical furnace Closed sample inlet with patented ball-valve for blank-free sample transfer

Gas traps for collection and pre-concentration

Advanced Purge and Trap – sharpest peaks

27/04/2016 Webinar EA-IRMS solutions

Full baseline separation between

element peaks, even at C:N

elemental ratios of up to 7000:1

o

23

H2O

N2

CO2

SO2

Gas separation using Advanced Purge and Trap technology


• With APT technology, the

accuracy of your

elemental analysis will be

a benchmark for your

isotope ratio analysis

• APT technology will give

you the security that your

sample conversion into

gas is quatitative – a

prerequisite for accurate

stable isotope ratio

analysis

Gas separation using Advanced Purge and Trap technology


• Always focused SO2 sample peaks

• High peak amplitude

• High sensitivity

• No danger of isotope fractionation artefacts

• High capacity

Boost your δ34S sensitivity with APT technology


8x increase in δ34S sensitivity + 2x better precision

o





uniform compounds







Summary 5

Blank free sample transfer

Webinar EA-IRMS solutions

• Patented ball valve

• Well-proven reliability

• Simple maintenance

1. Sample insertion

2. Flush with carrier gas 3. Sample transfer

27/04/2016 29

The elementargroup – technological leadership


• Functional design

Our instruments have the most modern and most functional

design. Because functionality was the number one target for

the instrument design, elemental analysers from

ELEMENTAR offer highest operating comfort and easiest

maintenance.

• User-friendliness

The ELEMENTAR operating software is renowned for its

user-friendliness. The software is optimized for unattended

overnight operation and actively assists the user with self-

diagnosis, automated sleep/wake-up function, visual

guidance for maintenance tasks and full remote-control.


• Easy maintenance through clamp connections and

slide-out furnace

Easy-to-use clamp connections provide reliable sealing and

at the same time make maintenance easy and

straightforward. The slide-out furnaces make exchange of

reagents a quick and easy task.

• Longterm stability and reliability of the calibration

Stability of the calibration is in the range of several months

up to years. The straightforward and robust basic concept

make the ELEMENTAR analyzers real working horses in the

laboratory routine.




• Intelligent leak check

The fully automated leak check self-diagnoses leaks in the

system and actively assists the user in remedy of the cause.

It takes less than 10 minutes.

• Indestructible combustion furnace and TCD

The thermal conductivity detector (TCD) used in our

instruments is oxygen proof and is not affected by any kind

of malfunction – the warranty for both combustion furnace

and detector cell of the TCD is 10 years.






vario ISOTOPE select 4.1

vario ISOTOPE cube 4.2

vario PYRO cube 4.3

iso TOC cube 4.4

Summary 5

High performance EA-IRMS systems from Elementar


o

vario ISOTOPE select

o

vario ISOTOPE cube

o

vario PYRO cube

o

iso TOC cube








vario PYRO cube 4.3

iso TOC cube 4.4

Summary 5

vario ISOTOPE select - enter the world of EA-IRMS


Simultaneous CNS analysis with highest accuracy

120 positions large capacity + easy reload autosampler

Functional design for smallest footprint in the industry

o o

o o

Clearly arranged, easily accessible system components

36

The workhorse in isotope ratio analysis

vario ISOTOPE select - enter the world of EA-IRMS


• Simultaneous CNS analysis, optimized for micro samples

• Unique method for combustion gas separation by patented,

fractionation-free Temperature Programmed Desorption –

TPD, for highest precision and accuracy

• Outstanding robustness – low maintenance

• 10 year warranty on furnace and thermoconductivity detector cell

• Reliable results even for submilligram samples

• Fully automatic analysis with 120 position sampler and

blank-free ball valve injector, liquid autosampler option

37


• Detection range carbon of 0 to 7 mg – sample

weight <0.2 mg up to 500 mg

• Typical elemental performance of <0.1 % for C,

N, and S

• Elemental LOD <100 ppm

• Typical isotope ratio performance of <0.2 ‰ for

δ34S, <0.1 ‰ for δ13C and δ15N

Specifications

38


Performance

39








vario PYRO cube 4.3

iso TOC cube 4.4

Summary 5

EA-IRMS has come a long way…

o

Back in the days…

o

Today, after decades of continuous innovation made in Germany…


vario ISOTOPE cube – experience the gold standard


• Truly multielemental isotope ratio analysis, optimized for

both micro and macro samples

• Market-leading accuracy and precision across a broad range

of possible applications through Advanced Purge and Trap

technology, great flexibility

• Superior ease of use through sophisticated self-diagnosis and

tool-free routine maintenance

• 10 year warranty on furnace and thermoconductivity detector cell

• Fully automatic analysis with 80 position sampler and blank-free

ball valve injector

42

vario ISOTOPE cube – experience the gold standard


• Optional H2 conversion kit for patented simultaneous CHNS

determination

• Liquid autosampler option

• Optional δ18O determination

• Optional δ2H determination in water (patented Chrome HD)

• All optionally available conversion kits allow upgrading the vario

ISOTOPE cube at any time for special applications.

43



weight <0.2 mg up to 1 g


N, S and O



δ2H (Chrome HD), <0.3 ‰ for δ18O, <0.2 ‰ for

δ34S, and <0.1 ‰ for δ13C and δ15N

Specifications

44


Performance

45








vario PYRO cube 4.3

iso TOC cube 4.4

Summary 5


vario PYRO cube

CHNSOH isotope ratio analysis – all in one instrument

Direct Oxygen Analysis: Reductive Pyrolysis

• Sample is combusted in helium atmosphere in

presence of carbon black

• Sample oxygen (O) is converted to carbon

monoxide (CO)

• CO is detected

• Boudouard equilibrium:

CO2 + C 2 CO

2 CO CO2 + C

• Only quantitative conversion to CO results in

matrix-independence. The higher the

temperature, the better



Outer protective ceramic tube

Blank free, long-life glassy carbon tube

Blank free pyrolysis reactor operated at 1450 °C

Helium (or argon) purged cavity between outer and inner tube, complete separation of carrier gas from protective gas

o

o

o

Analysis of caffeine without backflush


Analysis of caffeine with backflush


vario PYRO cube – CNSOH isotope ratios all in one instrument


• OH and CNS isotope ratio analysis all in one universal

instrument

• The only instrument for blank-free δ18O analysis

• Patented backflush technology for matrix-independent, reliable

results

• Two compartment pyrolysis reactor for highest accuracy and

extended long lifetime

• Superior ease of use through sophisticated self-diagnosis

• Fully automatic analysis with 120 position sampler and

blank-free ball valve injector, liquid autosampler option

52



weight <0.2 mg up to 500 mg


N, S and O


• Typical isotope ratio performance of <2 ‰ for

δ2H, <0.2 ‰ for δ18O, <0.2 ‰ for δ34S, and

<0.1 ‰ for δ13C and δ15N

Specifications

53


Performance

54








vario PYRO cube 4.3

iso TOC cube 4.4

Summary 5


iso TOC cube

The world's first system for simultaneous isotope ratio analysis of dissolved C and N (TOC / TNb )

too many samples? not enough time?


• Isotope ratio analysis of DOM in

the liquid phase was not possible

• Samples are lyophilized to extract

solid OM from the liquid DOM

sample

• Isolation of DOM for isotope ratio

analysis is tedious, time-

consuming and expensive

iso TOC cube – the world premiere of TOC / TNb isotope ratio analysis


• Direct analysis of dissolved C and N isotope

ratios in the liquid phase is now possible

• For all types of liquids from drinking water,

industrial waste water, soil leachates, supensions,

to brines or marine samples

iso TOC cube – the world premiere of TOC / TNb isotope ratio analysis


• The only truly integrated TOC-IRMS system available

• Dissolved carbon and nitrogen isotope analysis at the highest level

• Unique applications for IRMS analysis of TOC and TNb

• 100% C and N recovery independent from sample type and matrix

• Matrices ranging from the most dilute aqueous samples to

aggressive soil extracts

• Large liquid injection volume of up to 3 ml

• Superior ease of use through sophisticated self-diagnosis

• Integrated 32 position autosampler for liquids as standard


• Detection range carbon 5 ppb – 60000 ppm


δ15N and <0.1 ‰ for δ13C

Specifications

60


Performance

61

Comparison between δ13C values determined by TOC-IRMS and by conventional EA-IRMS of lyophilized DOM extracts.






Summary 5

High performance EA-IRMS systems from Elementar


o

vario ISOTOPE select the workhorse

o

vario ISOTOPE cube the gold standard

o

vario PYRO cube the most universal

o

iso TOC cube the revolution

Thank you!


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Elemental Analyzer inlets for IRMS applications

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