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Carbon/Sulfur, Oxygen/Nitrogen & Hydrogen Analyzer

TECHNICAL NOTE

Oxygen, Nitrogen and Hydrogen Analyzer EMGA-930/EMGA-830:In pursuit of High performance, Speed and Operability

Alain Salaville and Jocelyne Marciano, Application Laboratory, HORIBA Jobin Yvon S.A.S.,Longjumeau, FRANCESeiji Sakakura and Satoshi Yoshida, HORIBA Application Laboratory, Kyoto, JAPANWritten by Kinumi Hayashi, HORIBA R&D Department, Kyoto JAPAN

Keywords: EMGA 830, EMGA 930, Oxygen, Nitrogen, Hydrogen, Elemental Analyzer


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Figure 1: Model EMGA-930 for analysis of O/N/H concentration in solids

1 Introduction

Whether you are working for quality control inthe steel industry or in a R&D laboratory for newmaterials our Oxygen, Nitrogen and Hydrogenelemental analyzers will give you very accurateand repeatable results. Thanks to the improvedNDIR and TCD detectors, a standard deviation of 0.02 ppm is obtained for Oxygen and Nitrogen(Worlds best precision) and 0.04 ppm forHydrogen together with wide measurementranges enables the analysis of high concentra-tion samples as well as traces.

In addition, with the EMGA-930 model, thefully supported accessories policy leads up toan easy and simple instrument to operate. Theautomation systems (Cleaning and Crucible

loading) and user-friendly software includingmaintenance navigation will facilitate the train-ing of new operators and reduce the variation inresults between operators.

As this new generations models have beenoptimized to fit users requests they will answermost of the analytical problems you couldencounter.

2 Instrumentation

2.1 Principle (see figure 2)

The sample is loaded into a graphite crucible

which has been placed on the lower electrodeand then elevated to make contact with theupper electrode of the impulse furnace. A highcurrent passes through the crucible to create ahigh temperature (up to 3 000C).The gases extracted during the fusion are direct-ly analyzed after the dust filter.The Oxygen concentration is measured by twonon dispersive Infra-red analyzers (NDIR), CO,CO 2, depending on the concentration in order toachieve very good accuracy along the full meas-urement range.

The Nitrogen in the sample is extracted as nitro-gen gas (N 2) and its concentration is deter-mined by a thermal conductivity detector (TCD).

The Hydrogen is measured with NDIR as H 2Oafter H 2 is oxidized throuh the CuO converter.

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2.2 Super High Performance

Wide measurement rangeThanks to dual NDIR detectors measuring CO andCO 2 for Oxygen determination, one NDIR detectormeasuring H 2O for Hydrogen and optimized TCDdesign for Nitrogen determination, the EMGAseries provide the widest measuring range: for a1g sample Oxygen can be measured up to 5%,Nitrogen up to 3% and Hydrogen up to 0.25 %.

Precision

Likewise these optimizations lead to the Worldsbest Oxygen/Nitrogen precision with a SD 0.02 ppmor a RSD 0.5%, whichever is larger, and a Hydrogenprecision with SD 0.04 ppm or a RSD 2 %, meas-ured with reference gas.

Standard methodFinally the EMGA-830/930 fulfills requirements of the standard methods for analysis of steel, titani-um, tantalum, ceramics, etc. The main ones arelisted here:- ISO 10720:1997, ISO17053:2003- JIS G1228:1997- ASTM E1019,E1569, E1409

2.3 Unique features of EMGA-series

Dual Sample/Flux Introduction mechanism (figure 3)This system allows the decontamination of thecrucible and the flux. The following diagrams illus-trate the 3 steps and the graphs illustrate the asso-ciated parameters evolution1. The crucible is outgassed by a high current (hightemperature).2. The flux is introduced into the crucible and it isalso outgassed.3. The sample drops into the crucible for the analy-

sis.

2


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Figure 2: Gas flow diagram of the EMGA-830/EMGA-930

Figure 3: Dual sample/flux introduction mechanism

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3

Programmable temperature curves

Different functions allow the users to easily opti-mize the fusion temperature according to the sam-ple. Some customized temperature curves can becarried out in order to observe various phenome-na such as surface contamination, different phas-es or forms of Oxygen, Nitrogen and Hydrogen.Hold mode automatically optimizes the differenttemperature phases according to the samples.

User friendly software with maintenance counter navigator

In the maintenance window, you can reach pic-tures and videos illustrating maintenance opera-tions by a simple click. Operators can freely have alook at the concerned area by playing with the 3Ddisplay. As the navigator describes the easy to-understand procedure for replacing parts, opera-tors can perform routine maintenance without anyexperience or technical knowledge. In the samespirit of a multi-user facility, a maintenance count-er informs operators about replacing consumablesto assure consistent and accurate results.

EMGA-930 model: Fully integrated accessorieswith simplified operations(These accessories are optional with the EMGA-830 series)

With integrated automations, operations are muchsimpler and faster. Just enter sample name,weight and put the sample in the EMGA. Analysisstarts immediately and all operations are donefully automatically till next sample. It is totalhands clean use, so the operator doesnt need totouch crucibles anymore and doesnt have contactwith carbon dust. Furthermore, as automaticpreparations are done while the next sample isbeing prepared, the gain in terms of time is about40 s. compared with conventional systems.


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210 sec0 sec

Temperature curve

N

O

0

N 0.00010 %O 0.00400 %

0 C

3000 C

Enter sample name

Sample weighing

Measurement

Sample loading (start)

Crucible removal

Electrodes cleaning

New crucibles loading

Ready for nextmeasurement

Figure 6: Sequence of measurement.(Steps in green are automatic)

Figure 4: Oxide differentiation in iron powder

Figure 5: Software with maintenance counter

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