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Application notes

IMPORTANT NOTE: THE PROCEDURES DESCRIBED IN HERE, APPLY ONLY TO THE CATALYTIC ACTIVATED AND HALOGEN RESISTANT DECOMPOSITION VESSEL C 5012. THEY CAN NOT BE USED WITH THE C 5010 DECOMPOSITION VESSEL!

If you needs to analyze Halogens and/or sulfur after the decomposition, a variety of different methods to do so are shown below.

The examples described below are done with the IKA – Control standards AOD 1.11 and AOD 1.12. These control standards are mineral oils that contain a known amount of Chlorine, Sulfur and Fluorine, Bromine.

To get the best results on Halogens and Sulfur it is required to use the special decomposition vessel C5012 or the AOD 1 Decomposition System. The C 5012 decomposition vessel can be used with the C 2000 or C 5000 Calorimeter. We also offer them in Packages “C 2000 basic Version 2 (Package)” and “C 5000 Package 1/12”. This vessel can not be used with the C 200 Calorimeter!


Sample preparation PHOTOMETRY - Sulfur (S)
Preparing the decomposition vessel ION-CHROMATOGRAPHY - Iodine (I)  
ION-CHROMATOGRAPHY AAS - Mercury (Hg) & Arsenic (As)
TITRATION- Chlorine (Cl) Rinsing the decomposition vessel
ION SELECTIVE ELECTRODES Cleaning the decomposition vessel C 5012


Sample preparation

From the homogeneous standard oil AOD 1.11 0.2 - 0.5 g of the sample are filled directly into the quartz crucible and/or into the C 10 Acetobutyrate Capsule.

The originally weighted-in quantity of the sample material is noted or entered into the Calorimeter. It is required later again for the content calculation. If using the capsules the weight of the empty capsule has to be noted as well, or entered into the Calorimeter, since the energy additionally introduced thereby must be deducted from the gross calorific value as foreign (aka spike) energy that is not created by the sample itself. We do have special automated solutions for this procedure in combination with a balance connected to the Calorimeter. Please contact us for further details.


Preparing the decomposition vessel

5-10 ml of the absorption solution is filled into the decomposition vessel.

The absorption solution can vary in composition and concentration depending on the specifications of the sample and the method used to analyze the Halogens and/or Sulfur.

The most common used absorption solution is composed of:
10 ml of 0.25 Sodium hydroxide (NaOH) and
200?l of 30% Hydrogen peroxide (H2O2)

This standard absorption solution is suitable for almost all applications. If a different solution is used in any of the following application, it is mentioned separately

In some cases it is necessary to use the “C 5030 Venting station”. Especially when looking at Iodine (I) or traces respectively high quantities of Halogens. In this case the washing-bottle of the station is filled with the appropriate amount of absorption solution as well.

A cotton thread is connected to the ignition wire and the quartz crucible (with the weighed in sample) is inserted into the crucible holder of the decomposition vessel. The cotton thread is hung into the crucible that it will ignite the Acetobutyrate Capsule or oil when the ignition is done by the Calorimeter.

The decomposition vessel is closed and hung into the Calorimeter’s decomposition vessel acceptance.

The Calorimeter is started and fills oxygen into the vessel. In some cases it is necessary to fill and vent the decomposition vessel several times before starting the actual measurement. This procedure varies depending on the Calorimeter that is used. Please contact IKA for further details.


ION-CHROMATOGRAPHY - Sulfur (S) & Halogens (F, Cl, Br, I)

The determination was done with an Ion chromatograph manufactured by Dionex (DX- 1000/120) by means of a conductivity measurement.

This procedure allows the determination of all Halogens and Sulfur in one run! It is probably the most convenient, but also most expensive solution.

The absorption solution is specially created around the Eluent used with the IC, in order to get rid of the “water-peak”, and to optimize the performance of the IC.

1 Liter of the absorption solution consist of: 1 Liter stock solution consists of:

50 ml stock solution 21.2 g Na2CO and 6.30 g NaHCO3
25 ml 30% H202
7 - 8 NaOH – pellets

Follow the steps described in the section “Rinsing the decomposition vessel”.

A sample is taken and injected into the IC that will show all Halogens and Sulfur on one chromatogram only


TITRATION - Chlorine (Cl)

The determination of Chlorine was done with a Titration processor by titrating against with silver nitrate (AgNO3).

Follow the steps described in the section “Rinsing the decomposition vessel”.

An aliquot is removed for the measurement (50.0 ml or 100.0 ml) and transferred into a titration cup.

The aliquot factor is noted and needed later for the calculation of the result. The titration cup is then filled approximately halfway with distilled water and 2 ml of concentrated Nitric acid (HNO3) are added.

The titration cup is then placed into the analysis processor and the corresponding procedure is started. After several minutes the result is shown on the display in milligrams. The halogen concentration can be calculated from this taking the originally weighted-in quantity and the aliquot factor into consideration


ION SELECTIVE ELECTRODES (ISE) - Chlorine (Cl)

The determination of Chlorine (Cl) was done with a Potentiometer, equipped with a Solid-Ion-selective-Electrode Cl 500 in combination with the Reference-electrode R 502.

Follow the steps described in the section “Rinsing the decomposition vessel”.

Experience from these measurements as well with other samples showed that this method is not suitable for all applications. If the sample contains other Halogens than just Chlorine (Cl), Bromine (Br) can interfere with the Chlorine (Cl) electrode for example.


PHOTOMETRY - Sulfur (S)

Sulfur can be found in the absorption solution in the form of Sulfate (SO42-). The determination of Sulfate (SO42-) was done with a Photometer.

Follow the steps described in the section “Rinsing the decomposition vessel”.

The error of this test is probably a little too high for some customer requirements. But might still be good enough for „quick-test“ applications.


ION-CHROMATOGRAPHY - Iodine (I)

The sample analyzed in this application was a mineral fodder for cows. Similar tests have been done with birdseeds as well.

The determination of Iodine (I) was done with an Ion-chromatograph with a UV/VIS-Detection unit.

NOTE: For this application the C 5030 Venting station is absolutely required to get good results. 50 ml of the absorption solution described above are filled into the washing bottle.

Follow the steps described in the section “Rinsing the decomposition vessel”.

There are two important things to mention for this application.
The vessel needs to be shaken before venting it very slowly (for 90 minutes) through the absorption solution in washing bottle of the C 5030 venting station.


AAS - Mercury (Hg) & Arsenic (As)

IKA has a lot more applications and experience than what is shown here.

Please contact us directly for further detailed information and more details on the applications shown above.


Rinsing the decomposition vessel

After the experiment is done, the Calorimeter opens up. Remove the decomposition vessel, vent the gases under a fume hood, or connect it to the “C5030 Venting station”. The gases need to be vented slowly through the absorption solution inside the washing bottle of the venting station.

Rinse the vessel carefully with distilled water or if using an Ion-chromatograph, use the Eluent. Care should be taken to ensure that all parts of the vessel are rinsed.

Rule of thumb: better rinse 2-3 times with small quantities of distilled water or Eluent than only once with a lot of distilled water or Eluent!

The absorption solution in the decomposition vessel, as well as the absorption solution in the washing-bottle of the “C 5030 Venting station” are filled from the washing bottle into a volumetric flask with the appropriate volume, and is filled up to its calibration mark.


Cleaning the decomposition vessel C 5012

IMPORTANT NOTE: THE PROCEDURES DESCRIBED IN HERE, APPLY ONLY TO THE CATALYTIC ACTIVATED AND HALOGEN RESISTANT DECOMPOSITION VESSEL C 5012. THEY CAN NOT BE USED WITH THE C 5010 DECOMPOSITION VESSEL!

It must be guaranteed that no contamination is present in the decomposition vessel, and it needs to be cleaned in a way that the elements to be determined are not present in the cleaning agent. For example, do not use Hydrochloric acid (HCl) to clean the vessel if Chlorine has to be determined!

Suitable cleaning agents are acetone, isopropyl alcohol and distilled water. In cases of trace analysis the decomposition vessel can be cleaned with concentrated nitric acid (HNO3). Contact IKA for more details on this procedure before performing it!

The decomposition vessel is then dried using a lint-free cellulose cloth or the like, and can be prepared for the decomposition.