Beaker Glass Erlenmeyer Cawan Porselen

(1)

(2)

Lampiran 1. Peralatan

Mortar dan Pestle

Beaker Glass

(3)

Buret

Magnetik Stirrer

Oven

Neraca Analitik

(4)

Lampiran 2. Sampel

nga cangkang kerang bulu

Ca serbuk cangkang

kerang bulu

(5)

Lampiran 3. Grafik hasil uji FT-IR untuk HA murni.

Lampiran 4. Tabel Bilangan Gelombang FT-IR (Coates, 2000)

Gugus Fungsi

Rentang Bilangan Gelombang

_(cm-1)

OH

-3570-3200

3400-3200

3550-3450

3570-3540

3645-3600

3645-3630

3635-3620

3620-3540

3640-3530

PO

4

3-1350-1250

1050-990

1240-1190

995-850

(6)

Lampiran 5. Grafik Hasil Uji FT-IR HA dengan Suhu Sintering 700

o

_C

(7)

Lampiran 7. Grafik Hasil Uji FT-IR HA dengan Suhu Sintering 900

o

_C

(8)

(9)

Lampiran 10. Menghitung jumlah energi yang diserap pada uji FT-IR

Untuk menghitung energi serapan:

𝐸

𝑠

=

ℎ𝑐

_𝜆

Untuk menghitung % Energi Terserap:

%𝐸𝑡 =

𝐸

𝑖𝑟

_𝐸

− 𝐸

𝑠

a.

Untuk Sampel HA dengan Suhu Sintering 700

o

_C

Gugus

b.

Untuk Sampel HA dengan Suhu Sintering 800

o

_C

Gugus

OH

-

_3570.96

_2.80037E-06

_7.10264E-20

_7.96E-20

_10.77

PO

43-

1042.62

9.59122E-06

2.07377E-20

7.96E-20

73.95 PO

43-

945.33 1.05783E-05

1.88026E-20

7.96E-20

76.38

(10)

c.

Untuk Sampel HA dengan Suhu Sintering 900

o

_C

OH

-

_3570.91

_{2.80041E-06 7.10254E-20 7.96E-20}

_10.77

OH

-

_3497.13

_{2.85949E-06 6.95579E-20 7.96E-20}

_12.62

PO

43-

1042.24

9.59472E-06 2.07302E-20 7.96E-20

73.96 PO

43-

945.47 1.05768E-05 1.88054E-20 7.96E-20

76.38 d.

Untuk Sampel HA dengan Suhu Sintering 1000

o

_C

Gugus

e.

Untuk Sampel HA dengan Suhu Sintering 1100

o

_C

(11)

Lampiran 11. Hasil uji SEM-EDX HA dengan suhu sintering 900

o

_C

Lampiran 9. Perhitungan Rasio perbandingan Ca/P

Perhitungan rasio perbandingan Ca/P

Mol Ca

= % Ca : Ar Ca

= 0.14 : 40.08

= 0.00349

Mol P

= %P : Ar P

= 0.03 : 30.97

= 0.00097

Ca/P

= Mol Ca : Mol P

(12)

Lampiran 12. Perhitungan Rasio perbandingan Ca/P

Perhitungan rasio perbandingan Ca/P

Mol Ca

= % Ca : Ar Ca

= 0.14 : 40.08

= 0.00349

Mol P

= %P : Ar P

= 0.03 : 30.97

= 0.00097

Ca/P

= Mol Ca : Mol P

= 0.00349 : 0.00097

= 3.59

(13)

(14)

(15)

(16)

Lampiran 17. Perhitungan ukuran Kristal sampel HA.



Ukuran kristal sampel HA dengan suhu sintering 700

o

_C

𝑛 =

_{𝐹𝑊𝐻𝑀(cos 𝜃)}

0.9(𝜆 𝐶𝑢 𝐾𝛼)

=

0.9(1.5046𝑥10

−10

)

(3.4889𝑥10

−3

_)(cos

31.20

2

)

=

_{(3.4889𝑥10}

1.3865𝑥10

₋₃

_)(0.9999)

−10

=

1.3865𝑥10

_3.4854𝑥10

−10₋₃

_{= 40 𝑛𝑚}



Ukuran kristal sampel HA dengan suhu sintering 800

o

_C

𝑛 =

_{𝐹𝑊𝐻𝑀(cos 𝜃)}

0.9(𝜆 𝐶𝑢 𝐾𝛼)

=

0.9(1.5046𝑥10

−10

)

(3.4889𝑥10

−3

_)(cos

31.06

2

)

=

_{(3.4889𝑥10}

1.3865𝑥10

₋₃

_)(0.9999)

−10

=

1.3865𝑥10

_3.4854𝑥10

−10₋₃

_{= 40 𝑛𝑚}



Ukuran kristal sampel HA dengan suhu sintering 900

o

_C

𝑛 =

_{𝐹𝑊𝐻𝑀(cos 𝜃)}

0.9(𝜆 𝐶𝑢 𝐾𝛼)

=

0.9(1.5046𝑥10

−10

)

(2.791𝑥10

−3

_)(cos

31.06

2

)

(17)

Lampiran 18. Menentukan hkl sampel HA

a.

Untuk sampel HA dengan suhu sintering 700

o

_C

No

2θ (

o

₎

_{sin θ}

_{d (Å)}

_d

_hkl

_(Å)

_hkl

_Senyawa

b.

Untuk sampel HA dengan suhu sintering 800

o

_C

No

2θ (

o

₎

_{sin θ}

_{d (Å)}

_d

_hkl

_(Å)

_hkl

_Senyawa

c.

Untuk sampel HA dengan suhu sintering 900

o

_C

(18)

Lampiran 19. Menghitung Parameter Kisi HA

Hidroksiapatit mempunyai struktur Heksagonal, sehingga:

1 

Parameter kisi untuk HA dengan suhu sintering 700

o

_C

d

1

= 2,8124

Å

Gabungkan persamaan (1) dan (2):

Sehingga diperoleh nilai a dan c:

a = 9,4181 Å

c = 5,9028 Å

(19)

0.1297 =

_3𝑎

12

₂

+

_𝑐

4

₂

… … . . (2)

Gabungkan persamaan (1) dan (2):

Sehingga diperoleh nilai a dan c:

a = 9,4168 Å

c = 5,9054 Å



Parameter kisi untuk HA dengan suhu sintering 900

o

_C

d

1

= 2,8124

Å

hkl

1

= 211

d

2

= 2,7192

Å

hkl

2

= 112

∎

_(2,8124)

1

₂

=

4 _{3 .}

(2

2

+ (2.1) + 1

_𝑎

₂ 2

)

+

1 _𝑐

2₂

0,1264 =

_3𝑎

28

₂

+

_𝑐

1

₂

… … . . (1)

∎

_(2,7192)

1

₂

=

4 _{3 .}

(1

2

+ (1.1) + 1

_𝑎

₂ 2

)

+

2 _𝑐

2₂

0.1352 =

_3𝑎

12

₂

+

_𝑐

4

₂

… … . . (2)

Gabungkan persamaan (1) dan (2):

Sehingga diperoleh nilai a dan c:

a = 9,4864 Å

c = 5,7693 Å

(20)

Sample Data

File name SampelS8A.ORG

File path E:/data FT-IR/xrd/SampelS8A Data collected Jul 3, 2014 11:00:43 Data range 5.070º - 70.070º Number of points 3251

Step size 0.020

Rietveld refinement converged No Alpha2 subtracted No Background subtr. No

Data smoothed No

2theta correction 0.07º

Radiation X-rays

Wavelength 1.540600 Å

Matched Phases

Index Amount (%) Name Formula sum

A 100.0 Hydroxylapatite Ca5 H O13 P3

41.0 Unidentified peak area

A: Hydroxylapatite (100.0 %)

Formula sum Ca5 H O13 P3 Entry number 96-900-1234 Figure-of-Merit (FoM) 0.872869 Total number of peaks 134 Peaks in range 58

Peaks matched 46

Intensity scale factor 0.67

Space group P 63/m

Crystal system hexagonal

Unit cell a= 9.4166 Å c= 6.8745 Å

I/Icor 1.60

Calc. density 3.160 g/cm³

Reference Hughes J M, Cameron M, Crowley K D, "Structural variations in natural F, OH, and Cl apatites Locality: Holly Springs, Georgia, USA", American Mineralogist 74, 870-876 (1989)

Candidates

Name Formula Entry No. FoM

Whitlockite Ca9.06 Fe0.079 H0.87 Mg0.921 O28 P7 96-901-0492 0.8917

Whitlockite Al0.02 Ca9 Fe0.35 H Mg0.62 Mn0.02 O28 P7 96-901-5249 0.8880

Bobdownsite Al0.04 Ca9 F0.84 H0.16 Mg0.96 O27.16 P6.97 96-901-4799 0.8684 Whitlockite Ca9.181 Fe0.429 H0.693 Mg0.571 O28 P7 96-901-0490 0.8683 Whitlockite Ca9.036 Fe0.084 H0.831 Mg0.916 O27.28 P7 96-901-0493 0.8622

Whitlockite Ca9 H Mn O28 P7 96-901-1162 0.8574

Whitlockite Ca9 H Mg O28 P7 96-901-2416 0.8545

Clinozoisite Al3 Ca1.843 H O13 Si3 Sr0.157 96-901-0278 0.8003

Bussyite-(Ce) Be5.176 Ca0.764 Ce0.824 Eu0.008 F4 Gd0.078 H7.72 La0.236 Mg0.012 Mn0.485

Na3.652 Nd0.374 O33.15 Pr0.114 Si8.824 Sm0.08 Th0.174 Y0.242 96-901-3788 0.7994

Ca4 H34 O41 V8 96-450-1915 0.7981

Epidote Al2.6 Ca2 Fe0.4 H O13 Si3 96-900-0301 0.7957

Ca2 Fe0.5 H4 In0.5 O13 P3 96-432-2548 0.7951

Lakebogaite Al0.09 Ca0.87 Fe1.91 H15.72 Na1.13 O29 P4 U1.888 96-901-0436 0.7948 Ferroaxinite Al1.893 B Ca2 Fe0.657 H K0.022 Mg0.185 Mn0.13 Na0.065 O16 Si4 Ti0.005 96-900-0816 0.7905

Clinozoisite Al2.79 Ca2 Fe0.21 H O13 Si3 96-900-1800 0.7901

Manganaxinite Al1.8 B Ca1.65 Fe0.2 H0.5 Mg0.1 Mn1.2 O16 Si4 96-900-9950 0.7893 Manganaxinite Al1.8 B Ca1.65 Fe0.2 H Mg0.1 Mn1.2 O16 Si4 96-901-2630 0.7893 Axinite-(Mn) Al1.8 B Ca1.65 Fe0.2 H Mg0.1 Mn1.2 O16 Si4 96-901-2631 0.7893 Ferro-axinite Al1.984 B Ca2 Fe0.958 H Mg0.059 O16 Si4 96-901-0591 0.7870 Axinite-(Fe) Al1.984 B Ca2 Fe0.958 H Mg0.059 O16 Si4 96-901-0592 0.7870

Tassieite Ca2 Fe3.254 H4 Mg2.746 Na0.478 O26 P6 96-901-0618 0.7854

Clinozoisite Al3 Ca2 H O13 Si3 96-900-0181 0.7853

Tassieite Ca2 Fe3.314 H4 Mg2.686 Na0.463 O26 P6 96-901-0617 0.7850

(21)

Kentbrooksite Ca2.1 Ce0.579 Cl0.3 F0.5 Fe0.15 H3.816 Hf0.051 K0.099 La0.342 Mn3.6 Na16.002 Nb0.4

Nd0.228 O77.11 Si25.6 Sr0.45 Ti0.099 Zr3.3 96-901-2639 0.7682 Jinshajiangite Ba1.44 Ca0.76 F2 Fe6 H8 K0.8 Mg0.5 Mn1.5 Na Nb0.2 O38 Si8 Ti3.6 Zr0.2 96-901-2683 0.7667

Poldervaartite Ca1.67 H2 Mn0.33 O5 Si 96-900-1565 0.7650

Wendwilsonite As2 Ca2 Co0.1 H4 Mg0.9 O10 96-901-0745 0.7646

Zoisite Al3 Ca2 H O13 Si3 96-901-5960 0.7644

Ammonium Calcium Tetraborate Octohydrate B8 Ca H32 N2 O26 96-200-6402 0.7641 Surkhobite Ba3.3 Ca2.4 F8 Fe8 H4 K0.7 Mn7.4 Na2.2 Nb0.8 O68 Si16 Ti6.4 Zr0.8 96-901-2658 0.7637

and 150 others...

Search-Match

Settings

Reference database used COD-Inorg REV107951 2014.03.25 Automatic zeropoint adaptation Yes

Minimum figure-of-merit (FoM) 0.60 Parameter/influence 2theta 0.50 Parameter/influence intensities 0.50 Parameter multiple/single phase(s) 0.50

Selection Criteria

Elements:

Elements that must be present: H, O, Ca

Elements that may be present: All elements not mentioned above

Peak List

No. 2theta [º] d [Å] I/I0 FWHM Matched

(22)

60 57.74 1.5954 46.98 0.2000 61 57.92 1.5910 48.15 0.2000 A 62 59.85 1.5440 132.17 0.2000 A 63 61.64 1.5035 39.96 0.2000 A 64 61.82 1.4996 41.05 0.2000 A 65 63.02 1.4738 56.62 0.2000 A 66 63.74 1.4590 45.70 0.2000 A 67 63.92 1.4552 68.90 0.2000 68 64.08 1.4520 65.43 0.2000 A 69 64.24 1.4487 59.73 0.2000 A 70 65.05 1.4326 63.98 0.2000 A 71 65.24 1.4290 39.13 0.2000 A 72 66.36 1.4075 35.83 0.2000 A 73 66.63 1.4024 50.21 0.2000

Rietveld Refinement using FullProf

Calculation was not run or did not converge.

Integrated Profile Areas

Based on calculated profile

Profile area Counts Amount

Overall diffraction profile 237344 100.00%

Background radiation 93214 39.27%

Diffraction peaks 144130 60.73%

Peak area belonging to selected phases 46742 19.69% Unidentified peak area 97388 41.03%

Peak Residuals

Peak data Counts Amount

Overall peak intensity 2467 100.00% Peak intensity belonging to selected phases 886 35.91% Unidentified peak intensity 1581 64.09%

(23)

Sample Data

File name SampelS8B.ORG

File path E:/data FT-IR/xrd/SampelS8B

Data collected Jul 3, 2014 11:00:17

Data range 5.090º - 70.090º

Number of points 3251

Step size 0.020

Rietveld refinement converged No

Alpha2 subtracted No

Background subtr. No

Data smoothed No

2theta correction 0.09º

Radiation X-rays

Wavelength 1.540600 Å

Matched Phases

Formula sum Ca5 H O13 P3

Entry number 96-900-1234

Figure-of-Merit (FoM) 0.878918 Total number of peaks 134

Peaks in range 59

Peaks matched 47

Intensity scale factor 0.66

Space group P 63/m

Crystal system hexagonal

Unit cell a= 9.4166 Å c= 6.8745 Å

I/Icor 1.60

Reference Hughes J M, Cameron M, Crowley K D, "Structural variations in natural F, OH, and Cl apatites Locality: Holly Springs, Georgia, USA", American Mineralogist 74, 870-876 (1989)

Candidates

potassium decacalcium iron heptaphosphate Ca9.8 Fe0.2 K0.8 O28 P7 96-222-6014 0.9018 Silver(I) decacalcium heptakis(orthophosphate) Ag Ca10 O28 P7 96-223-8072 0.9009

Calcium Thorium Phosphate Ca10.381 O28 P7 Th0.119 96-901-3987 0.8968

Whitlockite Ca10.115 Mg0.385 O28 P7 96-901-2137 0.8855

decacalcium potassium heptakis(orthophosphate) Ca10 K O28 P7 96-221-1652 0.8771

C6 Cl3 N3 O6 96-200-1647 0.8275

barium yttrium silicate Ba O10 Si3 Y2 96-201-5697 0.8271

Silver chromium phosphorus sulfide (.5/.5/1/3) Ag0.5 Cr0.5 P S3 96-100-0192 0.8269

C Cl N2 S2 96-701-1348 0.8265

Silver chromium phosphorus sulfide (.5/.5/1/3) Ag0.5 Cr0.5 P S3 96-100-0193 0.8242

Merrillite Ca9.45 Fe0.22 Mg0.78 O28 P7 96-901-6664 0.8239

Ba2 (B4 Se13) B4 Ba2 Se13 96-151-1728 0.8227

B La Ni3 96-433-1517 0.8215

Octadecabromidobis(dicarbido)decadysprosium C4 Br18 Dy10 96-221-7355 0.8209

Dipotassium dimanganese tristrontium tris(diphosphate) K2 Mn2 O21 P6 Sr3 96-201-3005 0.8200

As Cs5 P4 Se12 96-431-6680 0.8200

Pentaterbium-Nonabromide-Monoethanide C2 Br9 Tb5 96-810-0801 0.8198

barium copper indium nitride Ba14 Cu2 In4 N7 96-201-2638 0.8193

Cl Cs6 Dy21 Se34 96-432-8911 0.8192

Lead molybdenum oxide: Pb~5~MoO~8~ Mo O8 Pb5 96-200-7542 0.8189

Tribarium tetranitridotungstate(VI) Ba3 N4 W 96-810-1308 0.8183

Niocalite Ca7 F Nb O17 Si4 96-900-9613 0.8179

Ca4 H34 O41 V8 96-450-1915 0.8172

Marthozite Cu H16 O22 Se2 U3 96-900-4630 0.8166

O9 Pb4 V2 96-900-4785 0.8166

Te3 Tl2 Zr 96-400-0784 0.8165

Ag7 As8 Fe3 O28 96-705-1675 0.8155

Whitlockite Al0.02 Ca9 Fe0.35 H Mg0.62 Mn0.02 O28 P796-901-5249 0.8141

H8 Na O14 P2 V2 96-700-9226 0.8138

Rubidium gadolinium bis(tungstate) Gd O8 Rb W2 96-201-4858 0.8132

Ca4 F2 O7 Si2 96-110-0154 0.8128

Magnesium borohydride ammonia B2 H14 Mg N2 96-430-4782 0.8126

Cl Cs6 Ho21 Se34 96-432-8912 0.8124

Cuspidine Ca3.69 F2 Na0.17 O7 Si2 Zr0.14 96-900-5693 0.8117

Bi8 Cu13.08 I11 S14 96-210-0185 0.8114

(24)

Cobalt Co 96-901-1617 0.8093

Calcium Silicon Nitride Ca8 N16 Si8 96-431-1198 0.8090

Bismuth molybdenum vanadium oxide (26/6.14/3.86/68) Bi26 Mo6.14 O68 V3.86 96-100-4119 0.8089

Pb2 S25 Ti7 Tl18 96-433-3827 0.8087

cesium tin bismuth telluride (0.88/1.88/3.12/7) Bi3.12 Cs0.88 Sn1.88 Te7 96-411-4686 0.8084 and 152 others...

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Settings

Peak List

No. 2theta [º] d [Å] I/I0 FWHM Matched

1 6.01 14.6953 35.18 0.2000

2 6.19 14.2724 39.51 0.2000

3 6.35 13.9113 38.66 0.2000

4 6.52 13.5530 48.46 0.2000

5 6.89 12.8137 35.88 0.2000

6 10.87 8.1341 136.67 0.2000 A

7 13.63 6.4916 148.31 0.2000

8 14.21 6.2281 35.24 0.2000

9 16.99 5.2140 202.76 0.2000 A

10 20.22 4.3880 52.09 0.2000

11 21.85 4.0648 156.26 0.2000 A

12 25.83 3.4470 441.14 0.2000 A

13 26.52 3.3579 79.91 0.2000

14 27.47 3.2445 74.64 0.2000

15 27.81 3.2052 580.05 0.2000

16 28.15 3.1670 58.20 0.2000 A

17 28.77 3.1002 57.01 0.2000

18 28.92 3.0844 80.44 0.2000 A

19 29.64 3.0113 125.34 0.2000

20 31.06 2.8770 1000.00 0.2000

21 31.79 2.8125 554.77 0.2000 A

22 32.21 2.7765 364.32 0.2000 A

23 32.45 2.7570 317.18 0.2000

24 32.94 2.7173 376.91 0.2000 A

25 33.51 2.6718 81.75 0.2000

26 34.15 2.6235 180.50 0.2000 A

27 34.36 2.6075 678.31 0.2000

28 35.12 2.5532 93.19 0.2000

29 35.60 2.5199 131.95 0.2000 A

30 35.90 2.4992 41.11 0.2000

31 37.36 2.4050 95.37 0.2000

32 37.86 2.3747 55.59 0.2000 A

33 39.25 2.2937 43.09 0.2000 A

34 39.42 2.2840 36.06 0.2000

35 39.87 2.2594 214.49 0.2000 A

36 41.08 2.1956 111.53 0.2000 A

37 41.72 2.1634 97.17 0.2000

38 41.95 2.1518 35.27 0.2000 A

39 43.61 2.0736 67.13 0.2000

40 43.89 2.0610 70.34 0.2000 A

41 44.51 2.0338 73.04 0.2000 A

42 44.64 2.0281 51.62 0.2000

43 45.33 1.9991 78.22 0.2000 A

44 46.73 1.9423 172.65 0.2000 A

45 46.97 1.9330 258.85 0.2000

46 48.00 1.8940 164.24 0.2000 A

47 48.38 1.8799 128.02 0.2000 A

48 49.53 1.8388 184.96 0.2000 A

49 49.78 1.8302 79.61 0.2000

(25)

68 63.33 1.4674 57.73 0.2000

69 63.49 1.4640 38.16 0.2000 A

70 64.15 1.4507 64.69 0.2000 A

71 64.68 1.4400 41.50 0.2000

72 64.86 1.4363 37.34 0.2000

73 65.03 1.4330 41.67 0.2000 A

74 66.24 1.4099 49.42 0.2000

75 66.43 1.4062 40.79 0.2000 A

76 67.43 1.3878 36.38 0.2000 A

Rietveld Refinement using FullProf

Integrated Profile Areas

Overall diffraction profile 229238 100.00%

Background radiation 91398 39.87%

Diffraction peaks 137840 60.13%

Peak area belonging to selected phases 42841 18.69%

Unidentified peak area 94999 41.44%

Peak Residuals

Overall peak intensity 2485 100.00%

Peak intensity belonging to selected phases 825 33.18%

Unidentified peak intensity 1661 66.82%

Diffraction Pattern Graphics

(26)

Sample Data

File name SampelS8C.ORG

File path E:/data FT-IR/xrd/SampelS8C Data collected Jul 3, 2014 11:00:19 Data range 5.080º - 70.080º Number of points 3251

Step size 0.020 Rietveld refinement converged No Alpha2 subtracted No Background subtr. No Data smoothed No 2theta correction 0.08º Radiation X-rays Wavelength 1.540600 Å

Matched Phases

Formula sum Ca5 H O13 P3 Entry number 96-901-1092 Figure-of-Merit (FoM) 0.904810 Total number of peaks 134 Peaks in range 58 Peaks matched 47 Intensity scale factor 0.67 Space group P 63/m Crystal system hexagonal

Unit cell a= 9.4240 Å c= 6.8790 Å

I/Icor 1.61

Reference Sudarsanan K., Young R. A., "Significant precision in crystal structural details: Holly Springs hydroxyapatite Locality: Holly Springs, Cherokee County, Georgia, USA Sample: X-23-4", Acta Crystallographica, Section B 25, 1534-1543 (1969)

Candidates

potassium decacalcium iron heptaphosphate Ca9.8 Fe0.2 K0.8 O28 P7 96-222-6014 0.9145 Silver(I) decacalcium heptakis(orthophosphate) Ag Ca10 O28 P7 96-223-8072 0.9126 Calcium Thorium Phosphate Ca10.381 O28 P7 Th0.119 96-901-3987 0.9055 decacalcium potassium

heptakis(orthophosphate) Ca10 K O28 P7 96-221-1652 0.8964

Whitlockite Ca10.115 Mg0.385 O28 P7 96-901-2137 0.8946

C6 Cl3 N3 O6 96-200-1647 0.8374

Octadecabromidobis(dicarbido)decadysprosiumC4 Br18 Dy10 96-221-7355 0.8274

C Cl N2 S2 96-701-1348 0.8262

Silver chromium phosphorus sulfide (.5/.5/1/3) Ag0.5 Cr0.5 P S3 96-100-0192 0.8210 Silver chromium phosphorus sulfide (.5/.5/1/3) Ag0.5 Cr0.5 P S3 96-100-0193 0.8207

Cl Cs6 Dy21 Se34 96-432-8911 0.8200

lanthanum germanium antimonide Ge2.8 La6 Sb13.2 96-431-9314 0.8197

Ba2 (B4 Se13) B4 Ba2 Se13 96-151-1728 0.8184

Ca4 H34 O41 V8 96-450-1915 0.8149

Pentaterbium-Nonabromide-Monoethanide C2 Br9 Tb5 96-810-0801 0.8147 cesium tin bismuth telluride (0.88/1.88/3.12/7) Bi3.12 Cs0.88 Sn1.88 Te7 96-411-4686 0.8134

Cl Cs6 Ho21 Se34 96-432-8912 0.8127

Titanite Ca O5 Si Ti 96-900-2444 0.8125

Seidozerite Ca0.26 F3 Fe0.32 Mg0.305 Mn0.425 Na3.91 Nb0.04 O15 Si4 Ti1.36 Zr1.38 96-900-4796 0.8123

Te3 Tl2 Zr 96-400-0784 0.8115

Manitobaite Al6.78 Ca1.84 Fe12.22 Mn12.91 Na13.5 O120 P30 96-901-6714 0.8108

Ba2 In Sm Te5 96-433-0903 0.8107

F15 Mo5 O15 Rb15 96-450-8553 0.8101

Gatehouseite As0.06 H4 Mn5 O12 P1.76 Si0.18 96-901-4915 0.8100

In9 Li2 Y5 96-430-9585 0.8098

Ag7 As8 Fe3 O28 96-705-1675 0.8094

(27)

Mo5 O8 Sr 96-200-9382 0.8007

Ag V (P S3)2 Ag P2 S6 V 96-150-9506 0.8005

Cobalt Co 96-901-1617 0.7999

Ca Mo5 O8 96-220-1243 0.7998

Ca Mo5 O8 96-900-7923 0.7998

Bismuth strontium copper oxide (4/8/5/20.5) Bi4 Cu5 O20.5 Sr8 96-100-6013 0.7997

Titanite Ca O5 Si Ti 96-900-2443 0.7995

Keyite As3 Cd Cu1.5 H4 O14 Zn2 96-900-4425 0.7986

and 153 others...

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Peak List

(28)

66 64.02 1.4532 44.78 0.1600 A 67 64.18 1.4499 50.05 0.1600 A 68 65.00 1.4337 34.19 0.1600 A 69 65.12 1.4313 33.99 0.1600 A 70 66.25 1.4096 34.13 0.1600 71 66.43 1.4063 30.67 0.1600 A 72 67.45 1.3874 36.63 0.1600 A

Rietveld Refinement using FullProf

Integrated Profile Areas

Overall diffraction profile 228870 100.00% Background radiation 80278 35.08% Diffraction peaks 148592 64.92% Peak area belonging to selected phases 41978 18.34% Unidentified peak area 106614 46.58%

Peak Residuals

Overall peak intensity 2334 100.00% Peak intensity belonging to selected phases 841 36.05% Unidentified peak intensity 1493 63.95%