Cutting costs within cutting edge EAS REGAINER technology in N-protein determination

Cutting Costs within Cutting Edge EAS REAGINER Technology in N-Protein Determination

Christian Schmidt

Webinar Series

Agenda Introduction 1

Current Situation 2

The Revolutionary EAS REGAINER® Technology 3

Our Next Generation N/Protein Analyzers 4

Experimental Data 5

The elementargroup – About us

12/15/2015 3

• 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.

Webinar

The elementargroup – Key Markets

12/15/2015 Webinar 4

Agronomy Chemicals Environmental Energy Materials Forensics

Tailor-Made to Customer Needs

• Elemental analyzers 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

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Current Situation 2



Experimental Data 5

Protein Analysis – Either you have to or you want to!

• legally bound protein determination for labeling

purposes

• protein content corresponds to product

properties e.g.:

• foam formation and taste of beer

• gluten-free starch

• dough properties

• protein content = price

Different Methods for N-Protein Determination

• Primary methods

• Dumas

• Kjeldahl

• Secondary methods (omitted)

• e.g. NIR (require primary method for calibration purposes)

Kjeldahl vs. Dumas Chemistry

Kjeldahl Dumas

Sample digested in sulfuric acid and a catalyst for 1-2 hours

Sample is introduced into a furnace at high temperature in the presence of oxygen, in a inert gas stream. Digestion time: < 1 min

(CHNO) + H2SO4 CO2 + SO2 + H2O + NH4+ Formation of N2 and NOx as well as other

products of combustion

Neutralization of sulfuric acid with sodium hydroxide, formation of ammonia gas and distillation of ammonia

Reduction of NOx to N2, trapping or removal of other gases, detection of N2 on a TCD detector

NaOH + NH4+

NH3 + H2O + Na+

Ammonia is typically trapped in a boric acid solution to form ammonium borate and titrated with sulfuric acid.

Kjeldahl vs. Dumas

Kjeldahl Dumas

Entire time of analysis for one sample several hours.

Entire time of analysis for one sample approx. 3-4 minutes Big benefit for re-determination of urgent and/or suspect samples.

Large quantities of concentrated acids, and a lot of flasks to wash

No concentrated acids. No toxic substances. Sample prep in tin foils. No flasks.

Sample size: 100 mg - many grams Big benefit for virtually unlimited sample size

Sample size: mg - 5 g

Very low initial price. Semi-automatic analysis with automatic distillation and titration devices available but expensive.

Low price for fully automated unit. No add-ons, upgrades required.

Cost per Test using the Kjeldahl Method

Kjeldahl Method – Cost Per Test

Amount per Test 1 Test per Day 20 Tests per Day 50 Tests per Day

NaOH (Sodium Hydroxide ) 60ml $0.66 $11.91 $28.13

H2SO4 (Concentrated Sulfuric Acid) 20 ml $0.77 $13.89 $32.80

Catalyst (Copper Sulfate) 2 tablets $1.13 $20.31 $47.96

Weighing Paper 1 sheet $0.01 $0.11 $0.26

Standard Hydrochloric Acid Solution, 0.2 N 20 ml $1.37 $24.65 $58.19

Kel-Sorb (Boric Acid buffer solution with indicator) 60 ml $0.49 $8.88 $20.96

Waste Cost 200 ml $3.60 $64.80 $153.00

Total Cost Per Day $8.03 $144.55 $341.31

Cost per Test $8.03 $7.23 $6.83 Time to Analyze Samples 3.2 hours 5.5 hours 13.5 hours

Source: www.cem.com


Current Situation 2



Experimental Data 5

Combustion According to Dumas Method

Organic compounds consists of C, H, N, O, S, Cl …

Combustion in O2 on oxygen donor at ~ 900°C

O2, N2, NOx, CO2 CO, CH4, SO2, H2O, HCl...

Typical problem of macro analysis (50 – 5000 mg)

and greasy samples Combustion

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Blank-Free Ball Valve

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Unique Post-Combustion

Organic compounds consists of C, H, N, O, S, Cl …

Combustion in O2 on oxygen donor at ~ 900°C

O2, N2, NOx, CO2 CO, CH4, SO2, H2O, HCl...

post-combustion (and H2O and halogen removal)

O2, N2, NOX, CO2, SO2,... Combustion

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Patented EAS REGAINER® Technology

• EAS REGAINER

• Metal free oxygen binding agents

• Reacts with excess oxygen and releases reducing gases

as by-product.

• Inexpensive, metal free, non-toxic

Combustion

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Patented EAS REGAINER Technology

• EAS REDUCTOR®

• Reduction of NOx to N2

• Resulting metal oxide is reduced back to active metal by

reducing gases released from EAS REGAINER

• Binding of SO2

• Only N2 and CO2 exit the reduction tube

• N2 quantification and conversion to protein content

Combustion

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Main Cost Drivers with “Classical” Duma Analyzers

• Consumption of reduction metal to bind excess

of oxygen

• Reduction tube filling for ~300 samples

• Increase lifetime by reducing just a part of the

combustion gas at the cost of sensitivity

• Helium as carrier gas

Changes with EAS REGAINER Technology

• Inexpensive binding of excess oxygen using

EAS REGAINER

• EAS REDUCTOR tube for up to 2000 samples

• No expensive helium as carrier gas required

Proof of Principle EAS REGAINER Technology

• 2000 consecutive samples shown with a rapid N exceed (7 days, 24/7)

• All results well below required repeatability according to ISO 16634-1

0.30

0.25

0.20

0.15

0.10

0.05

0.00

Dif

f. N

[%

]

2000150010005000

sample number

required repeatability according to ISO 16634- 1

soy flour

dry yeast

wheat flour

starch

Matrix Protein [%]

Soy flour 34.97

Dry yeast 45.99

Wheat flour 20.59

Starch 2.31

Reagent Usage of the rapid N exceed for 2000 Analyses


Current Situation 2



Experimental Data 5

Our Next Generation N/Protein Analyzers

exceed stands for EAS REGAINER Technology

Targets Laboratories

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• For laboratories with limited budget

• For laboratories that needs lowest

possible cost-per-sample for Dumas

analyzer

• For laboratories that needs maximum

sample flexibility

• For high-throughput laboratories that

needs maximum laboratory efficiency

Sample Preparation

Sample Preparation

Combustion

3-Fold Drying Detection

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TCD

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Carrier Gas: Carbon Dioxide

Combustion

Gas Separation in Tandem Operation

Detection

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Blank-Free Crucible Feeding

TCD

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Carrier Gas: Argon (Helium Optional)

The tandem operation of two CO2 selective trap columns assures fast analysis times down to 5 minutes.

Cost-per-Sample

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• Carbon dioxide as carrier gas

• EAS REDUCTOR for up to 2000 samples

• More than 300 samples/day possible

• 0.25€-per-sample including gases

• 10 years warranty on furnace and TCD cell

• Argon as carrier gas

• EAS REDUCTOR for more than 1000 samples

• 300 samples/per day possible


• 10 years warranty on furnace and TCD cell

Starting at 8-10 samples/day the rapid N exceed gives a better ROI compared to Kjeldahl Analyzer


Current Situation 2



Experimental Data 5

0.20

0.15

0.10

0.05

0.00

rep

eata

bil

ity N

[%

]

wheat flour wheat flour rye flour wheat buckwheat glutenfree

required repeatability according to DIN EN ISO 16634- 2

grape seedflour flour flourtype 1050type 550 type 1150 bran

carbon dioxide

rapid N exceed – Analysis of Grain

• According to DIN EN ISO 16634-2

• Average repeatability of 0.020%

• Exceed 5 times the requirement

Grain Protein [%] Wheat flour Type 550 11.35 Wheat flour Type 1050 12.67 Rye flour Type 1150 8.10 Wheat bran 15.94 Buckwheat flour 9.78 Grape seed flour 12.38 Glutenfree flour 3.17

0.20

0.15

0.10

0.05

0.00

rep

eata

bil

ity N

[%

]

horse cow piglet ox


pigchicken lamb rabbit quail

carbon dioxide

rapid N exceed – Analysis of Animal Feed



• Exceed 3.6 times the requirement

Feed Protein [%]

Horse 18.51

Cow 18.59

Chicken 14.91

Piglet 18.79

Lamb 18.18

Rabbit 18.59

Quail 21.13

Ox 19.03

Pig 14.50

0.03

0.02

0.01

0.00

rep

eata

bil

ity N

[%

]

required repeatability according to DIN EN ISO 14891

cow milk ewe's milkcamel milk goat milk soy milk

argon

rapid MAX N exceed – Analysis of Milk

• According to DIN EN ISO 14891



Milk Protein [%]

Cow 3.41

Camel 2.69

Sheep 5.01

Goat 2.77

Oat 1.07

Soy 3.01

0.20

0.15

0.10

0.05

0.00

rep

eata

bil

ity N

[%

]


wheat flour rye flour buckwheat glutenfreewheat flour wheat grape seed

type 550 type 1050 type 1150 flour flour flourbran

argon

rapid N exceed – Analysis of Grain




Grain Protein [%] Wheat flour Type 550 11.35 Wheat flour Type 1050 12.67 Rye flour Type 1150 8.10 Wheat bran 15.94 Buckwheat flour 9.78 Grape seed flour 12.38 Glutenfree flour 3.17

Summary

• Carbon dioxide as carrier gas

• EAS REDUCTOR for up to 2000 samples


• Argon as carrier gas (Helium optional)

• EAS REDUCTOR for more than 1000 samples


Take Home Message

• Our N/Protein Analyzers with EAS REGAINER technology are:

• The industry leading Duma-type N/Protein analyzer on the market

• A serious option for any Kjeldahl user with more than 8-10 samples/day

Thank you! Questions? Please use chat window

Cutting costs within cutting edge EAS REGAINER technology in N-protein determination

Technology

Transcript of Cutting costs within cutting edge EAS REGAINER technology in N-protein determination