Iraqi Journal of Chemical and Petroleum Engineering

Vol.17 No.4 (December 2016) 11- 23

ISSN: 1997-4884

Synthesis Of Nano Ni-Mo/γ-Al2O3 Catalyst

Abdul-Halim A. K. Mohamed* and Hawraa H. Atta

Chemical Engineering Department – College of Engineering – University of Baghdad (Iraq)

* Email: prof.abdulhaleem@gmail.com

Abstract

Nano γ-Al2O3 support was prepared by co-precipitation method by using

different calcination temperatures (550, 600, and 750)
o
C. Then nano NiMo/γ-Al2O3

catalyst was prepared by impregnation method were nickel carbonate (source of Ni)

and ammonium paramolybdate (source of Mo) on the best prepared nano γ-Al2O3

support at calcination temperature 550
o
C. Make the characterizations for prepared

nano γ-Al2O3 support at different temperatures and for nano NiMo/γ-Al2O3 catalyst

like X-ray diffraction, X-ray fluorescent, AFM, SEM, BET surface area, and pore

volume.

The Ni and Mo percentages in the prepared nano NiMo/γ-Al2O3 catalyst

determined by X-ray fluorescence were 2.924 wt % and 12.9 wt %, respectively. SEM

of prepared nano γ-Al2O3 support at calcination temperature 550
o
C. The average

particles diameter of prepared γ-Al2O3 support determined by AFM at calcination

temperatures 550, 600, and 750
o
C and for prepared nano NiMo/γ-Al2O3 catalyst at

calcination temperature 550
o
C.

Key words: Nanoparticles, γ-Al2O3, NiMo/ γ-Al2O3, Co-precipitation method.

Introduction

Gamma Al2O3 is one of the

important ceramic materials which are

mostly used as adsorbent, catalyst, and

catalyst support because its thermal,

chemical, and mechanical stability. For

use as catalyst or adsorbent alumina

with desirable characteristics such as

high surface area, and small particle

size is required [1]. Morphology of

synthetic gamma alumina can be

changed by varying some of the

reaction conditions such as:

temperature, pressure, reaction time,

thermal decomposition routes and

methods of preparation, precursors,

and reactants. The catalytic properties

of gamma alumina depend on its

physical properties such as surface

acidity, porosity, and pore size of

particles [2].

Alumina is a chemical compound

with melting point of 2072 °C and

specific gravity of 3.4. Alumina is

insoluble in water and organic liquids

and very slightly soluble in strong

acids and alkalies [3]. Alumina occurs

in two crystalline forms. Alpha

alumina is composed of colorless

spherical crystals shape. While gamma

alumina is composed of minute

colorless non spherical or irregular

hexagonal crystals shape depending on

the arrangement of oxygen anions [4].

University of Baghdad
College of Engineering

Iraqi Journal of Chemical and
Petroleum Engineering

mailto:prof.abdulhaleem@gmail.com

Synthesis Of Nano Ni-Mo/γ-Al2O3 Catalyst

12 IJCPE Vol.17 No.4 (December 2016) -Available online at: www.iasj.net

The gamma phase is transform to the

alpha form at high temperatures [3].

Also when high pressure the

transformation is used, phase

transformation occurs at low

temperature. For example the phase of

gamma alumina can be transformed to

alpha alumina by changing

temperature from750 to 1000
o
C at 1

atm. But when increase the pressure

from 1 atm to 8 GPa, gamma alumina

transforms phase to alpha alumina at

460
o
C because the high pressure

decrease the thermodynamic energy

barrier, and kinetic energy barrier

required for nucleation also causes the

phase transformation. High pressure

caused enough number of nucleation

sites to prevent the formation of the

vermicular structure and take the

equiaxed structure. The transition

phase and temperature depend on the

particles size chemical homogeneity,

heating rate, and water vapor pressure

[4].

The mechanical properties of

gamma alumina depend on their

nanostructure which are related with

the shape, and size of the alumina

particles. Alumina has many

advantages: hard, highly resistance

towards bases and acid, very high

temperature application, and excellent

wear resistance [5]. The phase of alpha

alumina with microsize is more stable

than gamma alumina phase, while the

phase of gamma alumina in nano

structure is more stable than alpha

alumina. This is because of the change

in the thermodynamic stability with the

size of nano particle [6].

Potdar, et al., (2007) prepared

nano sized γ-Al2O3 by precipitation /

digestion method at calcination

temperature 550
o
C. The surface area

of obtained nano alumina was 220

m
2
/g and the average pore diameter

was 4.5 nm [7]. Y. I. Tian-hong, el at.,

(2009) used precipitation method to

prepare nano alumina at calcination

temperature 450
o
C and pH range 8 to

9. The surface area of obtained nano

alumina was 269.9 m
2
/g, the pore

volume was 0.57 ml/g, with range of

size from 40 to 50 nm [8]. Parida, et

al., (2009) prepared nano spherical

shape γ-Al2O3 by control precipitation

method at calcination temperature 550
o
C. The surface area of prepared

catalyst was 190 m
2
/g and the

crystallite size was 5.7 nm [9].

Mandan, et al., (2010) prepared nano

sized γ-Al2O3 by sol gel method at

calcination temperature 600
o
C. The

surface area of obtained catalyst, the

pore volume, and the average pore

diameter were 242.9 m
2
/g , 1.42 cm

3
/g,

and 16.5 nm respectively [10]. Sarah,

et al., (2012) prepared nano sized γ-

Al2O3 by sol-gel method at calcination

temperature 500
o
C. The surface area

of obtained gamma alumina was 197

m
2
/g, the pore volume was 0.38 cm

3
/g

and the average pore diameter was 8.6

nm [11]. Asencios, et al., (2012)

prepared nano sized γ-Al2O3 by

precipitation method at calcination

temperature 500
o
C. The surface area

of prepared gamma alumina was 371

m
2
/g, while the pH was 6, the pore

volume was 0.275 cm
3
/g, and the

average pore diameter was 4.5 nm

[12]. S.Y. Hosseini, et al., (2012)

prepared nano γ-Al2O3 catalyst powder

by precipitation/digestion method at

calcination temperature 580
o
C for 5 h

1
in air. The obtained gamma alumina

surface area, average pore diameter

and total pore volume are 251 m
2
/g,

8.95 nm and 0.82 cm
3
/g, respectively

[13].

A. Rajaeiyan, et al., (2013)

prepared nanostructured gamma

alumina powder by sol gel and co-

precipitation methods at 750
o
C. The

surface area of prepared sample by sol

gel method was 30.72 m
2
/g and pore

diameter was 49.09 nm, while the

surface area of the prepared sample by

precipitation method, and the pore

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Abdul-Halim A. K. Mohamed and Hawraa H. Atta

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diameter were 206.2 m
2
/g, and 7.31

nm, respectively [14]. M. Edrissi, et

al., (2013) prepared nano sized

alumina by combustion synthesis. The

surface area of prepared nano alumina

and average pore diameter were

154m
2
/g, and 10 nm respectively

(15)
.

Ferechteh rashidi, et al., (2013)

prepared nano γ-Al2O3 support by sol-

gel method. The obtained nano γ-

Al2O3 with surface area 404.05 m
2
/g ,

pore volume 1.06 cm
3
/g and average

size 10.469 nm. HDS catalyst was

prepared by wet co-impregnation

method with percentage of 3% Co, 13

% Ni, and 3 % P on prepared γ-Al2O3.

The surface area of obtained catalyst

was 295.63 m
2
/g, the pore volume was

0.62 cm
3
/g, and the average pore

diameter was 8.355 nm. This catalyst

used for HDS diesel fuel which

decreased the sulfur content from 150

ppm to 38 ppm [16]. A. Eliassi, et al.,

(2014) prepared nanosized γ-Al2O3

with surface area 413 m
2
/g, average

pore diameter 38 nm and pore volume

1.624 cm
3
/g by using

precipitation/digestion method. This

catalyst used for methanol dehydration

to dimethyl ether using fixed bed

microreactor. The operation conditions

were LHSV from 20 to 50 h
-1

and

temperature from 250 to 300
o
C [17].

The aim of this work is to

prepare nano gamma alumina then use

it in the preparation of nano Ni-Mo/γ-

Al2O3 catalyst which can be used for

hydrodesulphurization of Iraqi gas oil.

Experimental

Synthesis of Alumina by Co-

Precipitation Method

1 M of AlCl3 was dissolved in

300 ml ethanol and 90 ml distilled

water was added to get a transparent

solution, then 120 ml NH3 was added

to the stirred AlCl3.6H2O solution drop

by drop with the rate of 2.5 ml/min

until the precipitate became white as

Al
3+

gel hydroxides was formed. After

gel filtering in vacuum system, it was

dried at 80 °C over night in the oven,

and calcinated at 550 °C, 600 °C for 2

h, and 750 °C for 1 h. A white fine

alumina nano-powder was obtained.

Synthesis of Nano Ni-Mo/γ-Al2O3
Catalyst

The Ni-Mo/γ-Al2O3 catalyst was

prepared by impregnation method. The

device used for impregnation consisted

of a conical flask with a separating

funnel, vacuum pump, electric shaker

and trap to absorb the moisture and

gases (Figure 1). An impregnated

aqueous solution was prepared by

dissolving 2.7 g nickel carbonate, 4.2 g

of ammonium para molybdate and 25

ml of distilled water with mixing at

room temperature. This solution was

poured in the conical flask of the

impregnation apparatus which contains

15 g of dried nano gamma alumina.

The impregnation took place drop by

drop for 1.5 hours. The impregnated

nano alumina was air dried at 80 °C for

16 hours and then calcined at 550 °C

for 16 hours.

Fig. 1: The device used for impregnation

Results and Discussion

XRD Analysis and XRF Analysis

X-Ray Diffraction analysis for

the samples was carried out using

Rigaku X-Ray Diffractometer with

CuKα radiation under identical

conditions. These conditions are:

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wavelength (λ) = 1.5406 A
0
, tube

voltage = 40 kV, tube current = 30

mA, and scan range: 10 – 70 (deg).

The XRD spectrum gives the

diffraction intensity verses 2θ plot. The

XRD spectra of prepared nano alumina

at different temperatures are shown in

the Figures 2 - 4, while the XRD

spectrum standard of gamma alumina

is shown in Figure 5. The comparison

of XRD spectra with standard

spectrum shows that all peaks of

prepared support approached the

standard gamma alumina. This means

that the prepared support at different

temperatures is gamma alumina. The

difference in the height of obtained

peaks may be due to the change in the

calcination temperature used during

support preparation. This mean the

prepared support is nano gamma

alumina because of that the peaks is

more wide than the standard peas.

Fig. 2: The XRD spectrum for prepared nano gamma alumina at calcination temperature 550

o
C

Fig. 3: The XRD spectrum for prepared nano gamma alumina at calcination temperature 600

o
C

Fig. 4: The XRD spectrum for prepared nano gamma alumina at calcination temperature 750

o
C

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Abdul-Halim A. K. Mohamed and Hawraa H. Atta

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Fig. 5: The XRD spectrum of synthetic of standard gamma alumina

The purity of solid crystal was

measured by comparing the X-ray

diffractogram pattern of prepared nano

alumina at different calcination

temperatures with X-ray diffractogram

pattern of standard gamma alumina

shown in Table 1. This comparison

proved that the prepared gamma

alumina at calcination temperature 550
o
C is more nearly to the standard.

The XRF analysis was used to

find the percentage of Ni and Mo in

the prepared catalyst. The percentages

of Ni and Mo were 2.924 wt % and

12.920 wt %, respectively. The

concentration of the metals on the

support usually varies from 8 to 25 %

for the active metal (Mo) and from 1 to

4 % for the promoter (Ni or Co) [20].

The percentage of Ni and Mo in

prepared nano catalysts are not far

from those obtained by Sandeep

Badoga,el at., (2014), who prepared

mesoporous NiMo/γ-Al2O3 by using

the sequential impregnation (3% Ni,

13% Mo).

Table 1: Comparison between prepared nano gamma alumina at different calcination temperatures and

standard synthetic gamma alumina

Gamma alumina

550
o
C

Gamma alumina

600
o
C

Gamma alumina

750
o
C

Standard gamma

alumina

Angle

(2ɵ) deg

d,spacing

(Å)

Angle

(2ɵ) deg

d,spacing

(Å)

Angle

(2ɵ) deg

d,spacing

(Å)

Angle

(2ɵ) deg

d,spacing

(Å)

20.462 4.33 20.000 4.43 21.246 4.18 20.494 4.33

31.641 2.82 31.691 2.82 31.728 2.81 31.936 2.80

37.486 2.39 37.385 2.40 37.323 2.40 37.603 2.39

39.521 2.28 39.434 2.28 39.492 2.27 39.401 2.28

45.930 1.97 45.930 1.97 45.905 1.98 45.764 1.98

60.349 1.53 60.224 1.53 59.974 1.54 60.457 1.53

66.422 1.40 66.827 1.39 66.688 1.40 66.761 1.40

Atomic Force Microscopy (AFM)

The morphology of prepared

alumina was studied using Atomic

Force Microscope. Figures 6 – 8 show

the images of AFM on two-

dimensional surface profile at different

calcination temperatures, while Figures

9 - 11 show AFM images for three-

dimensional surface profile at different

calcination temperature. The two

dimensional surface images in Figures

6 - 8 show the irregular hexagonal

structure of the gamma alumina

crystal. Three dimensional surface

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Synthesis Of Nano Ni-Mo/γ-Al2O3 Catalyst

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images shown in Figures 9 - 11

indicate that the agglomerates of

gamma alumina nano crystal are in

form of irregular hexagonal layers with

height terraces up to 9.8 nm [5].

Fig. 6: AFM on two-dimensional surface of

prepared nano alumina at calcination temp.

550
o
C

Fig. 7: AFM on two-dimensional surface of

prepared nano alumina at calcination temp.

600
o
C

Fig. 8: AFM on two-dimensional surface of

prepared nano alumina at calcination temp.

750
o
C

Fig. 9: AFM for three-dimensional surface of

prepared nano alumina at calcination temp.

550
o
C

Fig. 10: AFM for three-dimensional surface of

prepared nano alumina at calcination temp.

600
o
C

Fig. 11: AFM for three-dimensional surface of

prepared nano alumina at calcination temp.

750
o
C

Figures 12 – 14 show the particle

size distribution for prepared gamma

alumina at different calcination

temperatures. At calcination

temperature 550
o

C the results confirm

the largest volume percentage 19.27 %

at 50 nm and the lowest volume

percentage 0.36 % at 90 - 95 nm. The

prepared gamma alumina at 550
o
C

consisted of particles with diameters

ranged between 45 - 95 nm and

average diameter of 56.91 nm this

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Abdul-Halim A. K. Mohamed and Hawraa H. Atta

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result is near from that of A.

Rajaeiyan, et al., (2013), who prepared

nano structured gamma alumina

powder 49.09 nm [5]. While at 600
o
C

the results confirm the largest volume

percentage 7.11 % at 55 nm and the

lowest volume percentage 0.22 % at 99

- 100 nm. The prepared gamma

alumina at 600
o
C consisted of

particles with diameters ranged

between 15 - 180 nm and average

diameter of 68.72 nm. At 750
o
C the

results confirm the most volume

percentage 11.18 % at 105 nm and the

lowest volume percentage 0.62 % at 45

nm. The prepared gamma alumina at

750
o

C consisted of particles with

diameters ranged between 45 - 105 nm

and average diameter of 77.27 nm.

Fig. 12: Bar chart of particle size distribution for prepared alumina at calcination temperature 550

o
C

Fig. 13: Bar chart of particle size distribution for prepared alumina at calcination temperature 600

o
C

Fig. 14: Bar chart of particle size distribution for prepared alumina at calcination temperature 750

o
C

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Synthesis Of Nano Ni-Mo/γ-Al2O3 Catalyst

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Usually the range of nano

particles is 1 – 100 nano meter [21].

Figures 12 – 14 show that all prepared

alumina support at different calcination

temperature are nano type. It was

observed that the average particle

diameter of nano gamma alumina

increase with the increase in

calcination temperature. This is due to

the crystal sentering [22].

The AFM images of prepared

NiMo/γ-Al2O3 catalyst using nano

alumina support obtained at calcination

temperature 550
o
C are shown in

Figures 15 - 16. The two dimensional

surface images in Figure 15 show the

irregular hexagonal structure of the

gamma alumina crystal. Three

dimensional surface images shown in

Figure 16 indicating that the

agglomerate of gamma alumina nano

crystal are in form of irregular

hexagonal layers with height terraces

up to 3.96 nm [5].

Figure 17 show the particle size

distribution for prepared gamma

alumina and these results confirm the

largest volume percentage 23.85 % of

particle size distribution 70 nm and the

lowest volume percentage 5.38%, 85

nm. It also show the prepared gamma

alumina consisted of particles with

diameters ranged between 55 - 85 nm

and average diameter was 64.74 nm.

This means that the particle of

prepared nano NiMo/γ-Al2O3 catalyst

was nano type. The increasee in

average particle diameter of prepared

catalyst occurs due to loading Ni and

Co during impregnation on prepared

support and crystal centering during

impregnation method [22].

Fig. 15: For prepared NiMo/γ-Al2O3 AFM

image on two-dimensional surface profile at

550
o
C

Fig. 16: For prepared NiMo/γ-Al2O3 AFM for

three-dimensional surface profile at 550
o
C

Fig. 17: Bar chart of particle size distribution for prepared nano NiMo/γ-Al2O3 catalyst at calcination

temperature 550
o
C

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Abdul-Halim A. K. Mohamed and Hawraa H. Atta

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Scanning Electron Microscopy

(SEM)

SEM images of prepared gamma

alumina at calcination temperature 550
o
C are shown in Figure 18, at

magnification of 50.00, 20.00, 47.90,

10.00, 4.00, and 3.00 k x. It is very

convenient to compare the prepared

gamma alumina crystal with that

prepared by A. Rajaeiyan, et al.,

(2013), as shown in Figure 19.

a.SEM at a magnification of 4.00 kx b.SEM at a magnification of 20.00 kx

c.SEM at a magnification of 50.00 kx d.SEM at a magnification of 10.00 kx

e.SEM at a magnification of 606 x f.SEM at a magnification of 3.00 kx

Fig. 18: SEM images of prepared nano gamma alumina

The comparison of SEM images for

prepared gamma alumina with SEM

for prepared nano gamma alumina by

A. Rajaeiyan, et al., (2013) shows that

both gamma alumina are irregular

hexagonal shape particles with uniform

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distribution and has not strong

agglomeration [5].

a.SEM at a magnification of 47.90 kx of

prepared gamma alumina

b.SEM at a magnification of 15.00 kx of

prepared gamma alumina by A. Rajaeiyan,

Fig. 19: SEM images of prepared gamma

alumina and nano gamma alumina prepared by

A. Rajaeiyan, et al., [5]

General Properties of Catalyst

Physical and chemical properties

of prepared catalyst at different

calcinations temperature such as

surface area, and pore volume were

determined by BET device and

presented in Table 2.

This table shows that the surface

area decreased with increasing

calcination temperature and maximum

surface area 256.0 m
2
/g is obtained at

calcination temperature 550
o
C while

the surface area of prepared nano

gamma alumina by A. Rajaeiyan,

etal.,(2013) was 206.2 m
2
/g. The

higher surface area usually has a high

percentage of small pores [5]. Also the

using of high calcination temperature

causes quick water evaporation from

small pore to the large pore then to the

bulk and this gives pressure drop. This

pressure drop collapses part of pores

especially in hydrogel step resulting in

partial loss of surface area [9].

The pore volume of γ-Al2O3

decreases with the increase in

calcination temperature increasing and

the minimum pore volume 0.3742

cm
3
/g obtained at calcination

temperature 550
o
C which was not far

from 0.467 cm
3
/g obtained by Parida et

al. (2009) [1]. This occurs because

high calcination temperature increases

the reaction temperature, which rapidly

leads the crystallites to contact each

other. The contact occurs by two

smaller crystallites agitated at higher

temperatures resulting in coalescing to

a larger one causing an increase of the

pore volume and decrease the surface

area by sintering or agglomeration of

crystallites [9].

Table 5: Physical properties of prepared nano support γ-Al2O3

Calcined Temp
o
C

Surface Area

m
2
/g

Pore Volume

cm
3
/g

Pore volume distribution

550 256.0 0.3742 5

600 217.5 0.3715 -

750 213.5 0.4123 -

The prepared nano Ni-Mo/ɣ-

Al2O3 catalyst obtained at calcination

temperature 550
o
C has surface area

215.82 m
2
/g, and pore volume 0.2855

cm
3
/g which was near that by Sandeep

Badoga,el at., (2014) who prepared

nano Ni-Mo/ɣ-Al2O3 catalyst with

surface area of 225 m
2
/g . The decrease

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Abdul-Halim A. K. Mohamed and Hawraa H. Atta

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in surface area, and pore volume may

be due to blockage of some pores by

impregnation of Ni and Mo on the

prepared support [21].

Conclusion

Nano γ-Al2O3 support was

prepared by co-precipitation method

from aluminum chloride as a source of

alumina and ammonia hydroxide by

using different calcination

temperatures 550, 600, and 750
o
C.

From X-ray diffraction pattern and

when compared it with the standard of

gamma alumina found that prepared

supports at different temperatures are

mainly gamma alumina.

BET test found the surface area

of prepared nano gamma alumina at

550, 600, and 750
o

C are 256, 217, 213

m
2
/g. The decreasing in surface area

occur by increasing temperature.

From Atomic Force Microscopy

test found that the average diameter of

particles of prepared gamma alumina is

56.91 nm at 550
o
C, 68.72 nm at 600

o
C and 77.27 nm at 750

o
C. While the

average diameter of particles of

prepared NiMo/γ-Al2O3 catalyst is

64.74 nm, and this means that the

prepared γ-Al2O3 support and the

prepared NiMo/γ-Al2O3 catalyst are in

the range of nano type 1-100 nm.

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Abdul-Halim A. K. Mohamed and Hawraa H. Atta

-Available online at: www.iasj.net IJCPE Vol.17 No.4 (December 2016) 23

Appendix (A)

SPECTRO X-LabPro Job Number: 0

Description Hawraa Method TurboQuant-Powders

Sample Name 3 Date of Receipt 05/27/2015 11:56:06

Z Symbol Element Norm. Int Concentration Abs. Error

12 Mgo Magnesium 38.0224 0.927 % 0.027 %

13 Al2O3 Aluminum 12382.5502 79.85 % 0.066 %

14 SiO2 Silicon 66.3879 0.2311 % 0.0051 %

15 P2O5 Phosphorus 254.9972 0.3699 % 0.0039 %

16 SO3 Sulfur 0.0000 < 0.00050 % (0.0) %

17 Cl Chlorine 428.9963 0.06085 % 0.00036 %

19 K2O Potassium 6.5734 0.0374 % 0.0026 %

20 CaO Calcium 31.9450 0.1230 % 0.0023 %

22 TiO2 Titanium 0.0000 < 0.00034 % (0.0) %

23 V2O5 Vanadium 0.0000 < 0.00037 % (0.0037) %

24 Cr2O3 Chromium 0.0000 < 0.00015 % (0.0) %

25 MnO Manganese 7.2168 0.00373 % 0.00034 %

26 Fe2O3 Iron 205.1929 0.06025 % 0.00040 %

27 CoO Cobalt 96.6807 0.1328 % 0.0087 %

28 NiO Nickel 19686.3359 2.924 % 0.002 %

29 CuO Copper 40.2948 0.00447 % 0.00022 %

30 ZnO Zinc 2537.4834 0.2390 % 0.0004 %

31 Ga Gallium 0.0000 < 0.00005 % (0.0) %

32 Ge Germanium 0.0000 < 0.00005 % (0.0) %

33 As2O3 Arsenic 0.0000 < 0.00007 % (0.0) %

34 Se Selenium 0.0000 < 0.00005 % (0.0) %

35 Br Bromine 10.9351 0.00032 % 0.00002 %

37 Rb2O Rubidium 56.4448 0.00108 % 0.00002 %

38 SrO Strontium 439.2818 0.00821 % 0.00004 %

39 Y Yttrium 9.5877 0.00015 % 0.00003 %

40 ZrO2 Zirconium 44.4298 0.01603 % 0.00033 %

41 Nb2O3 Niobium 45.5775 0.01384 % 0.00053 %

42 Mo Molybdenum 40962.1338 12.92 % 0.01 %

47 Ag Silver 1.3400 0.00183 % 0.00055 %

48 Cd Cadmium 8.6726 0.00797 % 0.0004 %

50 SnO2 Tin 12.2892 0.01152 % 0.00041 %

51 Sb2O5 Antimony 9.2371 0.01027 % 0.00048 %

52 Te Tellurium 11.0299 0.00700 % 0.00030 %

53 I Iodine 7.0907 0.00644 % 0.00067 %

55 Cs Cesium 0.0000 < 0.00040 % (0.0) %

56 Ba Barium 0.0000 < 0.00020 % (0.0) %

57 La Lanthanum 3.8772 0.00188 % 0.00046 %

58 Ce Cerium 0.0000 < 0.00020 % (0.0) %

72 Hf Hafnium 34.4012 0.00660 % 0.00019 %

73 Ta2O5 Tantalum 141.1496 0.0344 % 0.0011 %

74 WO3 Tungsten 21.4133 0.00436 % 0.00094 %

80 Hg Mercury 0.0000 < 0.00010 % (0.0) %

81 Tl Thallium 15.2258 0.00058 % 0.00003 %

82 PbO Lead 735.5520 0.05019 % 0.00016 %

83 Bi Bismuth 0.0000 < 0.00010 % 0.00047 %

90 Th Thorium 21.5463 0.00100 % 0.00005 %

92 U Uranium 18.5451 0.00047 % 0.00002 %

Sum of concentration 54.88 %

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