IR2014-11-04 - PT Black Bear, Indonesia - 001 PDF

Date: 17 Dec.
14
Investigation Report
IR2014-11-04 - PT Black
Bear, Indonesia - 001.doc
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
1. Subject
Process type: Ammonia Oxidation
Sample type: HA gauzes
Campaign No. / Gauze pack name: received April 2014
Amount of samples: 2
Position of samples on gauze pack: center, edge
2. Investigation
Analysis methods used:
Scanning Electron Microscopy (SEM)
Energy Dispersive X-Ray Analysis (EDXA)
Optical Microscopy (OM)
Auger Electron Spectrometry (AES)
Secondary Ion Mass Spectrometry (SIMS)
X-Ray Fluorescence Spectrometry (XRF)
3. Summary of results and conclusions

-
Cauliflower structure only lightly developed or nearly undeveloped in all samples

possible reasons:
Contamination of the gauzes at the beginning of the campaign resulting in
poor development of the cauliflower structure
Cauliflowers fell off from the wire during the campaign because of mechanical
abrasion or weakening of the cauliflower structure due to platinum loss
Breakage of single wires observed possible reasons:

Vibrations caused by changes of pressure or of ammonia load
Backflow of the gas stream
Damage during the removal or the sampling
Contamination of the gauze samples with iron oxide, even found in the area analysis
of the center sample probable origin:
Plant components consisting of steel
Iron present as impurity in ammonia and transferred into feed gas
Metallic impurities probably as oxides (Cr, Mn, Ni) often found going along with iron
oxide probable origin: plant components consisting of steel (alloying elements)
1 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Frequent detection of ceramic compounds, on the center sample even found in the
area analysis probable origin:
gasket materials
filter materials
Contamination with carbon, sulphur and alkaline chlorides frequently found

probable origin:
oil leak of machinery equipment
presence of oil in ammonia
impurities from pipes/vessels
Na, K and Cl also found as salts in form of aerosols in the atmosphere/air
Small amounts of gold (Au) found on the gauzes origin unknown
4. Suggested Action Items

-
No massive contamination of the gauzes was observed no urgent action necessary

The gauzes show a low contamination with iron oxide: An iron contamination can be
responsible for a lower efficiency. As a precaution you should check:
State of the filter system (ammonia and mixed-gas filter)
Possible corrosion of feed gas tubes
In addition a low contamination of the gauzes with ceramics observed Ceramic
compounds covering the wires reduce the catalyst surface and can affect the efficiency. It
should be avoided to improve the performance!
5. Results
5.1. HA Sample Edge
Top side
-
Cauliflower structure nearly undeveloped Fig. 1

Overview photo shows many contaminants on the wire surface Fig. 1
Local analyses of the gauze sample show:

ceramic compounds (Ca, Si, Al, Ti, O) partially combined with carbon or Na
and K covering the wire surface Fig. 1, 2, 4, 5
particles of iron oxide and metallic impurities (Cr, Ni, Mn) probably as oxides
Fig. 1, 3, 6, 7
Bottom side
-
Cauliflower structure completely undeveloped Fig. 8

Overview photo shows several contamination spots on the wire surface Fig. 8
2 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
-
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Local contamination of the gauzes with:

carbon in form of black spots in combination with sulphur and alkaline
chlorides Fig. 9, 10
iron oxide covering some wires Fig. 11, 12
ceramic compounds (Ca, Al, Si, Mg, Ti, O) in form of films on the wires Fig.
13, 14
5.2. HA Sample Center

Top side
-
Cauliflower structure only very lightly developed Fig. 15

Overview photo shows many contamination spots on the wires Fig. 15
Area analysis results in a contamination of the gauze sample with iron oxide and
alumina Fig. 16
The contamination spots consist of:

ceramic compounds (Ca, Si, Al, Mg, Zr, O) Fig. 17-21
particles of iron oxide and metallic impurities (Cr, Ni) probably as oxides
Fig. 20, 21
Bottom side
-
Cauliflower structure nearly undeveloped Fig. 22

Breakage of single wires observed Fig. 22
In the overview photo many contamination spots visible Fig. 22
Local analyses show:

carbon in form of black spots (up to 50 m) in combination with sulphur,
alkaline chlorides and ceramic compounds (Al, Si, Ca, Ti, Zr, O) Fig. 23, 24
iron oxide accompanied by chromium probably as oxide in form of particles
(up to 100 m) Fig. 25, 26
small amounts of gold (Au) Fig. 23, 24
Verena Wald
Development Project Manager
FMD-TCE
Heraeus Materials Technology GmbH & Co. KG
verena.wald@heraeus.com
Phone: +49-6181-35-3072
Fax: +49-6181-35-5318
3 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 1
Figure 2
4 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 3
Figure 4
5 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 5
Figure 6
6 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 7
Figure 8
7 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 9
Figure 10
8 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 11
Figure 12
9 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 13
Figure 14
10 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 15
Figure 16
11 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 17
Figure 18
12 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 19
Figure 20
13 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 21
Figure 22
14 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 23
Figure 24
15 / 16
Date: 17 Dec. 14
IR2014-11-04 - PT Black
HMT-FMD-CAT
957 21 402
Used Catalyst Pack
Customer: PT Black
Bear, Indonesia
Figure 25
Figure 26
16 / 16

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Date: 17 Dec.

Used Catalyst Pack

3. Summary of results and conclusions

Cauliflower structure only lightly developed or nearly undeveloped in all samples

Breakage of single wires observed possible reasons:

Used Catalyst Pack

Contamination with carbon, sulphur and alkaline chlorides frequently found

Small amounts of gold (Au) found on the gauzes origin unknown

4. Suggested Action Items

No massive contamination of the gauzes was observed no urgent action necessary

Cauliflower structure nearly undeveloped Fig. 1

Local analyses of the gauze sample show:

Cauliflower structure completely undeveloped Fig. 8

Used Catalyst Pack

Local contamination of the gauzes with:

5.2. HA Sample Center

Cauliflower structure only very lightly developed Fig. 15

The contamination spots consist of:

Cauliflower structure nearly undeveloped Fig. 22

Local analyses show:

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

Used Catalyst Pack

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