elemental analysis of soils

Elemental Analysis of Soils - Dedicated instrument solutions in soil science -

October, 21st 2015

Dr. Marc Ruppenthal

Product Manager Elemental Analysis

Dr. Ralf Dunsbach

Product Manager TOC Analysis

Webinar

22/10/2015 Elemental analysis of soils - webinar - 2

Agenda About ElementarGroup 1

Why is elemental analysis of soils relevant? 2

Our technology - Your solutions in soil science 3

Summary 4

The elementargroup – about us


• The technology leader in

• Elemental Analysis (EA)

• Isotope Ratio Mass Spectrometry (IRMS)

• Offers an unmatched combination of

• innovative technologies,

• tailor-made solutions and

• comprehensive support.

The elementargroup – the subsidiaries


Elementar Americas

Elementar Headquarters

Elementar France

Isoprime Ltd.

Elementar Italia

Elementar Trading (Shanghai)

Elementar Australia

The elementargroup – the distribution network


Represented in all relevant world markets by our own sales

organisation and a network of well-chosen distributors

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

The elementargroup – key markets


Agriculture Chemicals Environmental Energy Materials Forensics

Tailor-made to customer needs

• Elemental analyzer optimized for different analytical tasks

• vario Series - Industry-leading versatility in elemental analysis

• rapid Series - Dedicated instruments serving today’s customer needs

• trace Series - Trace-level detection of elements

• TOC Series - Fast and easy determination of total organic carbon

• inductar Series – Dedicated instruments for the analysis of metals and inorganics


Some of our customers






Summary 4

Why is elemental analysis of soil relevant?


“Studies predict the world population to increase beyond 8.2 billion within

the next 10 years, demanding ways to optimise the use of agrarian land

to provide a larger food supply.”

• Agricultural science and analytics are the key to

manage the growing fundamental demands for

food, feed and water.



• Carbon and nitrogen are important drivers in the

element cycling of soils.

• Elemental analysis provides essential information

about microbiological activity and organic matter,

enabling a selective fertilisation of arable land.

• Understanding the carbon-nitrogen ratio of soil is

therefore of utmost importance.



• Sulphur is gaining importance: After a period of

overfertilization with S due to power plant

emissions, S is now starting to become a limiting

nutrient in certain locations (introduction of flue

gas desulfurization in the 80s).

Who is interested in soil analysis?


• Agricultural laboratories

• Government and public authorities

• Contract laboratories

• Research institutes





vario MAX cube 3.1

vario EL cube 3.2

vario TOC cube 3.3

Have you thought about stable isotopes? 3.4

Summary 4

Advanced Purge and Trap (APT) Technology


• High data quality

• Purge and Trap columns always provide complete

baseline separation

• Very long life time

• Compared to GC columns

• Outstanding sample flexibility

• Largest dynamic range thanks to 250-fold higher load

compared to GC columns

• C/N ratios of up to 7000:1

• In conjunction with the detection of the complete

combustion gas without gas splitting or dilution

H2O

N2

CO2

SO2

Blank free sample transfer

Elemental analysis of soils - webinar -

• Patented ball valve

• Well-proven reliability

• Simple maintenance

1. Sample insertion

2. Flush with carrier gas 3. Sample transfer

22/10/2015 19

Robustness and safety


• Robustness and longevity

Manufactured and quality-controlled exclusively in our

headquarter in Hanau.

• Safety

We manufacture according to strict EU norms and standards

such as the EMV low voltage directive 73/23/EEC and the EU

machinery directive 2006/42/EG. All our instruments are

operated at low voltage (48 volts).

Slide-out furnace and clamp connections


• Analysis of all combustion gases

All of the sample gas produced from combustion or pyrolysis

is directed to a single thermal conductivity detector (TCD)

without "gas splitting". This ensures quantitative and matrix-

independent determination of element concentrations even

in slowly digesting or difficult to digest substances.

• Easy maintenance

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.

The elementargroup – technological leadership


• 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 MAX cube 3.1

vario EL cube 3.2

vario TOC cube 3.3


Summary 4

Is sample homogeneity important?


Capacity of the purge & trap column

Sample homogeneity

• Low sample homogeneity requires that larger sample

amounts are analyzed

• Larger sample amounts in turn produce more combustion

gases and thus require larger gas adsorption capacities

How to guarantee sufficient homogeneity?


• 1) Through sample preparation…

• There are many effective ways to grind

samples including the use of a planetary ball

mill, Wiley mill, freezer mill, roller grinder, or

the standard mortar and pestle.



• …followed by analysis in a Micro or Semi-

Macro elemental analyzer, e.g., vario EL cube

• ! Microbalance necessary !

•OR

Simplified sample preparation – with vario MAX cube


• No grinding or milling

• Large capacity crucibles for large sample amount

• Broad sample weight range

• Up to 5 g / 5 ml sample

• Up to 500 mg total carbon and 330 mg total nitrogen

• Highest sample flexibility

• Inhomogeneous samples

• Samples with high ash content

Weigh in the crude samples into reusable crucibles

Place them on the autosampler

Start the sequence

Get the results!

vario MAX cube – simplified sample preparation


• Tedious sample preparation?

• Not necessary!

vario MAX cube – Automatic Ash Removal Technology


• Reusable stainless steel crucibles

• Robotic arm inserts the sample automatically and

removes the crucible including the ash after the

analysis

• Addresses any high throughput laboratory

• Designed for 24/7 operation

• Available in CN and CNS mode

vario MAX cube – a new dimension in throughput


vario MAX cube – analysis of soil

22/10/2015 Elemental analysis of soils - webinar -

• Soil from banana plantation in Ecuador

• Sample weight: 1000 mg

• CN mode

• exp. results ± abs. SD

Sample C [%]

N [%]

C/N ratio

Fluvisol Ah horizon 1.488 ± 0.003 0.051 ± 0.001 29.2

Fluvisol B horizon 0.670 ± 0.001 0.065 ±0.001 10.3

Fluvisol B/C horizon 1.921 ± 0.004 0.024 ± 0.001 80.0

31

vario MAX cube – analysis of soil


• Soil from a pasture Southwest USA

• Sample weight: 550 - 750 mg

• six-fold determination

• 1 : 1 addition of WO3

Sample C [%]

N [%]

S [%]

Cambisol Ah horizon 1.112 ± 0.001 0.104 ± 0.001 0.0229 ± 0.0005

Cambisol B horizon 1.782 ± 0.010 0.168 ±0.001 0.0231 ± 0.0004

Cambisol Cw horizon 0.335 ± 0.013 0.053 ± 0.027 0.0094 ± 0.003

Calcisol B horizon 4.187 ± 0.015 0.051 ± 0.001 0.0873 ± 0.0028

32





vario MAX cube 3.1

vario EL cube 3.2

vario TOC cube 3.3


Summary 4

The vario series


• Ideal sample weight therefore depends on a

combination of the type of samples you are

analyzing and the type of elemental analyzer you

are using

• Note: Aggresive samples (high halogen or salt

content) should be analyzed with the lowest

possible weight to increase lifetime of both

consumables and instrument

vario EL cube


Meet the gold standard



• Grinding followed by analysis in a Micro or

Semi-Macro elemental analyzer, e.g., vario

EL cube

• ! Microbalance necessary !

vario EL cube – analysis of soil and sediment


• From a coastal forest, Northwestern France

• Sample: 10 - 100 mg

• CHNS mode

• exp. results ± abs. SD

Industry-leading performance and versatility


• Optional conversion kits allow instrument

upgrade at any time for special applications

(e.g., S detection down to 2 ppm with IR, Cl

detection,…)

vario EL cube – sample weight and type


• Wide sample weight range

• From micro- (below 1 mg) to semi-macro

• Up to 40 mg total carbon content

• Highest sample flexibility

• From pure organic material (e.g. charcoal) to

sediments with only trace amounts of organic

material

• Challenging sample matrices

• Fluorinated compounds

• Compounds that are difficult to oxidise





vario MAX cube 3.1

vario EL cube 3.2

vario TOC cube 3.3


Summary 4

41

The Result of 40 years experience with TOC

Scope of parameters


TOC=Total Organic Carbon

TIC=Total Inorganic Carbon

TC=Total Carbon

NPOC=Non Purgeable Organic Carbon

POC=Purgeable Organic Carbon

TNb=Total bound Nitrogen

The Concept


Matrix separation


Soil extracts


0.5M K2SO4 fumigated

0.25M K2SO4

0.5M K2SO4 Non fum.

1st injection [mg/l] 71.0 5.64 28.8

2nd injection [mg/l] 70.7 5.76 29.4

3rd injection [mg/l] 71.3 5.76 29.4

Mean [mg/l] 71.1 5.72 29.2

SDr [%] 0.35 1.27 1.13

Conditions: 700°C comb. Temperature, 0.5ml injection volume





vario MAX cube 3.1

vario EL cube 3.2

vario TOC cube 3.3


Summary 4

GeovisION


• Designed specifically for the investigation of CNS and OH isotopic variations

in agricultural, geological and environmental samples

o o

Isoprime Market leading visION stable isotope analyzer

Elementar Market leading elemental analyzer

GeovisION – analysis of soil


• Soil and sediment samples from

different locations in Central Europe

• Sample weight: 5 - 100 mg

• six-fold determination

Sample δ13C [‰ VPDB]

δ15N [‰ AIR N2]

δ34S [‰ VCDT]

Anthrosol A horizon −29.96±0.02 14.01±0.10 7.08±0.13

Mollisol A horizon −26.85±0.05 6.79±0.11 9.46±0.16

Cambisol A horizon −28.56±0.03 8.43±0.08 5.02±0.11

Pleistocenic fluvial sediment −24.03±0.07 10.86±0.12 -

48

iso TOC cube


• The only truly integrated TOC-IRMS system

• 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 mostdilute aqueous samples

to aggressive soil extracts

• Liquid injection volume of up to 3 ml





Summary 4

Our technology – Your solution in soil science


Capacity of the purge & trap column

Sample homogeneity

• Advanced purge and trap

technology is key to highly

accurate soil analysis

H2O

N2

CO2

SO2

vario MAX cube

- a new dimension in throughput -


• Ease of use

• Samples up 5 g / 5 ml

• Automatic ash removal

• Simplified sample preparation

• Helium or argon as carrier gas

• Available as CN or CNS analyzer

• 24/7 unattended operation

• 10 years warranty on furnace and detector

vario EL cube

- meet the gold standard -


• The most versatile elemental analyzer in the

market (CHNS, CHN, CNS, CN, N, S, O, Cl, TIC,

TOC)

• Options for infrared detection of S down to

2 ppm, liquid sample injection,…

• Helium or argon as carrier gas

• Sample weight of <0.2 mg or up to 1 g

• High robustness – low maintenance

• 10 years warranty on furnace and TCD cell

GeovisION


• Straightforward analysis and intelligent control

for incredible ease of use

• Significantly reduced consumption of laboratory

resources

• Good-For-Go control drastically reduces

instrument contact time


Elementar thanks for your attention !