Beaker Glass Erlenmeyer Cawan Porselen
LAMPIRAN Lampiran 1. Peralatan Mortar dan Pestle Beaker Glass Erlenmeyer Cawan Porselen Corong Indikator pH Universal
Buret Magnetik Stirrer Oven Neraca Analitik
Desikator Furnace Lampiran 2. Sampel nga cangkang kerang bulu Ca serbuk cangkang kerang bulu nga Serbuk CaO nga Endapan HA nga sampel HA yg telah dihaluskan
Lampiran 3. Grafik hasil uji FT-IR untuk HA murni.
Lampiran 4. Tabel Bilangan Gelombang FT-IR (Coates, 2000) Rentang Bilangan Gelombang Gugus Fungsi (cm-1)
3570-3200 3400-3200 3550-3450 3570-3540
- OH 3645-3600 3645-3630 3635-3620 3620-3540
3640-3530 1350-1250 1050-990
3-
4 PO
1240-1190 995-850 2-
CO
3 2300-2500 Lampiran 5. Grafik Hasil Uji FT-IR HA dengan Suhu Sintering 700 o
C Lampiran 6. Grafik Hasil Uji FT-IR HA dengan Suhu Sintering 800 o
C o Lampiran 7. Grafik Hasil Uji FT-IR HA dengan Suhu Sintering 900 C o
Lampiran 8. Grafik Hasil Uji FT-IR HA dengan Suhu Sintering 1000 C
Lampiran 9. Grafik Hasil Uji FT-IR HA dengan Suhu Sintering 1100 o
C Lampiran 10. Menghitung jumlah energi yang diserap pada uji FT-IR Untuk menghitung energi serapan: ℎ =
Untuk menghitung % Energi Terserap:
−
% = 100%
Dimana:E s : Energi Serapan (J)
-20
E ir : Energi Infra Red (7.96 x 10 J) t
%E : Energi Terserap (%) λ : Panjang Gelombang (m)
- 34
h : Konstanta Planck (6.63 x 10 Js)
8 c : Kecepatan Cahaya (3.00 x 10 m/s) o a.
C Untuk Sampel HA dengan Suhu Sintering 700 Bilangan Energi Energi Gugus Energi Gelombang λ (m) Infra Red Terserap Fungsi Serapan (J) -1 (cm ) (J) (%)
- OH 3572.39 2.79925E-06 7.10548E-20
7.96E-20
10.74 3-
PO 4 1092.85 9.15039E-06 2.17368E-20
7.96E-20
72.69 2-
CO 3 2359.09 4.23892E-06 4.69223E-20
7.96E-20
41.05 2-
CO 3 1651.74 6.05422E-06 3.28531E-20
7.96E-20
58.73 o b.
C Untuk Sampel HA dengan Suhu Sintering 800 Bilangan Energi Energi Gugus Energi Gelombang λ (m) Infra Red Terserap Fungsi Serapan (J) -1 (cm ) (J) (%)
- 2.80037E-06 7.10264E-20
7.96E-20
10.77 OH 3570.96 3-
PO 4 1042.62 9.59122E-06 2.07377E-20
7.96E-20
73.95 3- 4 1.05783E-05 1.88026E-20
7.96E-20
76.38 PO 945.33 2-
CO 3 2359.87 4.23752E-06 4.69378E-20
7.96E-20
41.03
3570.91 2.80041E-06 7.10254E-20 7.96E-20
3497.13 2.85949E-06 6.95579E-20 7.96E-20
3571 2.80034E-06 7.10272E-20 7.96E-20
3569.73 2.80133E-06 7.1002E-20 7.96E-20
3496.23 2.86022E-06 6.9540E-20 7.96E-20
3 2-
2360.06 4.23718E-06 4.6942E-20 7.96E-20
41.48 CO
3 2-
2342.11 4.26965E-06 4.6585E-20 7.96E-20
73.86 CO
4 3-
1046.06 9.55968E-06 2.0806E-20 7.96E-20
12.64 PO
10.8 OH
OH
C Gugus Fungsi Bilangan Gelombang (cm -1 ) λ (m) Energi Serapan (J) Energi Infra Red (J) Energi Terserap (%)
73.48 e. Untuk Sampel HA dengan Suhu Sintering 1100 o
4 3-
1061.52 9.42045E-06 2.11136E-20 7.96E-20
OH
10.77 PO
C Gugus Fungsi Bilangan Gelombang (cm -1 ) λ (m) Energi Serapan (J) Energi Infra Red (J) Energi Terserap (%)
76.38 d. Untuk Sampel HA dengan Suhu Sintering 1000 o
4 3-
945.47 1.05768E-05 1.88054E-20 7.96E-20
73.96 PO
4 3-
1042.24 9.59472E-06 2.07302E-20 7.96E-20
12.62 PO
10.77 OH
OH
C Gugus Fungsi Bilangan Gelombang (cm -1 ) λ (m) Energi Serapan (J) Energi Infra Red (J) Energi Terserap (%)
Untuk Sampel HA dengan Suhu Sintering 900 o
c.
41.03 o Lampiran 11. Hasil uji SEM-EDX HA dengan suhu sintering 900 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 = 0.00349 : 0.00097 = 3.59 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 Lampiran 13. Tabel Hannawalt untuk HA
Lampiran 14. Data Hasil Uji XRD sampel HA dengan Suhu Sintering 700 o
C Lampiran 15. Data Hasil Uji XRD sampel HA dengan Suhu Sintering 800 o
C Lampiran 16. Data Hasil Uji XRD sampel HA dengan Suhu Sintering 900 o
C Lampiran 17. Perhitungan ukuran Kristal sampel HA. o
Ukuran kristal sampel HA dengan suhu sintering 700 C 0.9( ) = (cos ) −10
0.9(1.5046 10 ) = 31.20 −3
) (3.4889 10 )(cos 2 −10
1.3865 10 = −3
(3.4889 10 )(0.9999) −10
1.3865 10 = −3
3.4854 10 = 40 o
C Ukuran kristal sampel HA dengan suhu sintering 800 0.9( ) = (cos )
−10 0.9(1.5046 10 ) =
31.06 −3 ) (3.4889 10 )(cos
2 −10 1.3865 10 =
−3 (3.4889 10 )(0.9999)
−10 1.3865 10 =
−3 3.4854 10 = 40 o
C Ukuran kristal sampel HA dengan suhu sintering 900 0.9( ) = (cos )
−10 ) 0.9(1.5046 10
=
31.06 −3 (2.791 10 )(cos )
2 −10 1.3865 10 =
−3 (2.791 10 )(0.9999)
−10 1.3865 10 =
−3 2.7910 10 = 50 Lampiran 18. Menentukan hkl sampel HA
= 2 sin
ℎ= ℎ
2 sin Dimana : λ : Panjang gelombang (1.5406 Å) d hkl : Jarak antar bidang (Å) o
θ : Sudut Bragg ( ) o a.
C Untuk sampel HA dengan suhu sintering 700 o hkl
No 2θ ( ) sin θ d (Å) d (Å) hkl Senyawa
1 31.79 0.2739 2.8124 2.8123 2 1 1 HA
2 27.96 0.2416 3.1885 3.1883 1 0 2 HA
3 25.89 0.2240 3.4383 3.4388 0 0 2 HA
4 32.91 0.2833 2.7192 2.7190 3 0 0 HA
5 32.22 0.2775 2.7758 2.7759 1 1 2 HA o b.
C Untuk sampel HA dengan suhu sintering 800 o
Senyawa hkl No ) d (Å) d (Å) hkl 2θ ( sin θ HA
1 31.79 0.2739 2.8125 2.8123 2 1 1 HA 2 32.94 0.2835 2.7173 2.7171 3 0 0 HA 3 32.21 0.2774 2.7765 2.7769 1 1 2 HA 4 39.87 0.3409 2.2594 2.2596 3 1 0
5 16.99 0.1477 5.2140 5.2153 1 0 1 HA o c.
C Untuk sampel HA dengan suhu sintering 900 o hkl Senyawa No ) d (Å) d (Å) hkl 2θ ( sin θ
HA
1 31.80 0.2739 2.8124 2.8123 2 1 1 HA 2 32.94 0.2835 3.1885 2.7171 3 0 0 HA 3 25.84 0.2236 3.4383 3.4449 0 0 2 HA 4 32.22 0.2775 2.7192 2.7758 1 1 2 HA 5 39.86 0.3409 1.7193 2.2596 3 1 0 Lampiran 19. Menghitung Parameter Kisi HA Hidroksiapatit mempunyai struktur Heksagonal, sehingga:
2
2
2 1 ) 4 (ℎ + ℎ +
- =
2
2
2
3 o
C Parameter kisi untuk HA dengan suhu sintering 700
1 d = 2,8124 Å
1 hkl = 211
2 d = 2,7758 Å hkl 2 = 112
2
2
2
1 4 (2 + (2.1) + 1 )
1 ∎ = +
2
2
2 (2,8124) 3 .
28
1 … … . . (1) + 0,1264 =
2
2
3
2
2
2
1 4 (1 + (1.1) + 1 )
2 ∎ = +
2
2
2 (2,7758) 3 .
12
4 0.1298 = … … . . (2) +
2
2
3 Gabungkan persamaan (1) dan (2): Sehingga diperoleh nilai a dan c: a = 9,4181 Å c = 5,9028 Å o
C Parameter kisi untuk HA dengan suhu sintering 800
1 d = 2,8125 Å hkl 1 = 211
2 d = 2,7765 Å hkl 2 = 112
2
2
2
1 4 (2 + (2.1) + 1 )
1 ∎ = +
2
2
2 (2,8125) 3 .
28
1
- 0,1264 = … … . . (1)
2
2
3
2
2
2
1 4 (1 + (1.1) + 1 )
2 ∎ + =
2
2
2 (2,7765) 3 .
12
4 … … . . (2) + 0.1297 =
2
2
3 Gabungkan persamaan (1) dan (2): Sehingga diperoleh nilai a dan c: a = 9,4168 Å c = 5,9054 Å o
C Parameter kisi untuk HA dengan suhu sintering 900 d
1 = 2,8124 Å hkl
1 = 211 d 2 = 2,7192 Å
2 hkl = 112
2
2
2
1 4 (2 + (2.1) + 1 )
1 ∎ = +
2
2
2 (2,8124) 3 .
28
1 0,1264 = + … … . . (1)
2
2
3
2
2
2
1 4 (1 + (1.1) + 1 )
2
- ∎ =
2
2
2 (2,7192) 3 .
12
4
- 0.1352 = … … . . (2)
2
2
3 Gabungkan persamaan (1) dan (2): Sehingga diperoleh nilai a dan c: a = 9,4864 Å c = 5,7693 Å
Lampiran 20. Data Hasil Uji XRD dengan menggunakan software Match2!®
Sample: Sampel_S8_A (S8A)
Sample DataFile 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 sumA 100.0 Hydroxylapatite Ca5 H O13 P3
41.0 Unidentified peak area
A: Hydroxylapatite (100.0 %)
46 Intensity scale factor
Clinozoisite Al3 Ca1.504 H O13 Si3 Sr0.496 96-901-0281 0.7979 Clinozoisite Al3 Ca1.7 H O13 Si3 Sr0.3
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
96-900-7612 0.7781
96-900-7429 0.7827 Manganaxinite Al1.86 B Ca1.95 Fe0.18 H0.9 Mg0.015 Mn0.995 O16 Si4 96-900-3567 0.7816 Afwillite Ca3 H6 O10 Si2
96-900-0181 0.7853 Tassieite Ca2 Fe3.314 H4 Mg2.686 Na0.463 O26 P6 96-901-0617 0.7850 Piemontite Al2.25 Ca2 H Mn0.75 O13 Si3 96-900-3498 0.7848 Viitaniemiite Al Ca0.592 F2 H Mn0.401 Na O5 P 96-900-0943 0.7837 Lamprophyllite Ba0.667 Ca F0.667 Fe H0.667 K0.667 Mn0.5 Na O17.333 Si4 Sr0.667 Ti2.5 96-901-1905 0.7828 Samfowlerite Be7.24 Ca14 H6 Mn3 O58 Si14 Zn2.76 96-900-4289 0.7827 Afwillite Ca3 H6 O10 Si2
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
96-432-2548 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
96-900-0301 0.7957 Ca2 Fe0.5 H4 In0.5 O13 P3
96-901-0279 0.7960 Clinozoisite Al3 Ca1.518 H O13 Si3 Sr0.482 96-901-0280 0.7959 Epidote Al2.6 Ca2 Fe0.4 H O13 Si3
Ca4 H34 O41 V8 96-450-1915 0.7981
0.67 Space group P 63/m Crystal system hexagonal Unit cell a= 9.4166 Å c= 6.8745 Å I/Icor
Na3.652 Nd0.374 O33.15 Pr0.114 Si8.824 Sm0.08 Th0.174 Y0.242 96-901-3788 0.7994
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
58 Peaks matched
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 Whitlockite Ca9.061 Fe0.014 H0.89 Mg0.986 O28 P7 96-901-0491 0.8756 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
Entry No. FoM
Candidates
Name FormulaUSA", American Mineralogist 74, 870-876 (1989)
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,
96-901-1162 0.8574 Whitlockite Ca9 H Mg O28 P7 Pumpellyite-(Al) Al2.8 Ca2 Fe0.2 H4 O14 Si3 96-900-0978 0.7694
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
31 39.82 2.2620 140.65 0.2000 A
19 32.66 2.7397 242.94 0.2000
20 32.91 2.7192 357.91 0.2000 A
21 33.69 2.6581 53.39 0.2000
22 34.06 2.6303 133.99 0.2000 A
23 34.56 2.5931 643.56 0.2000
24 35.29 2.5410 83.19 0.2000
25 35.53 2.5246 47.93 0.2000 A
26 35.76 2.5087 123.10 0.2000
27 37.57 2.3924 79.60 0.2000
28 38.04 2.3637 46.78 0.2000 A
29 39.24 2.2939 44.80 0.2000 A
30 39.55 2.2768 34.78 0.2000
32 39.96 2.2546 145.09 0.2000
17 31.79 2.8124 591.25 0.2000 A
33 41.31 2.1837 106.70 0.2000
34 41.92 2.1532 140.23 0.2000 A
35 43.75 2.0673 64.53 0.2000 A
36 44.14 2.0501 42.24 0.2000 A
37 44.77 2.0227 68.13 0.2000
38 45.03 2.0118 37.76 0.2000
39 45.55 1.9900 55.97 0.2000 A
40 46.72 1.9429 158.12 0.2000 A
41 47.23 1.9228 201.51 0.2000
42 48.25 1.8847 191.42 0.2000 A
43 48.66 1.8697 131.79 0.2000 A
44 49.52 1.8394 193.67 0.2000 A
45 50.02 1.8219 45.11 0.2000
18 32.22 2.7758 351.80 0.2000 A
16 31.20 2.8647 1000.00 0.2000
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
No. 2theta [º] d [Å] I/I0 FWHM Matched
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
SettingsReference 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
1 6.63 13.3255 35.03 0.2000
15 29.83 2.9930 112.48 0.2000
2 10.88 8.1252 98.69 0.2000 A
3 13.67 6.4732 149.82 0.2000
4 14.31 6.1832 37.71 0.2000
5 17.07 5.1890 253.84 0.2000 A
6 20.32 4.3664 67.84 0.2000
7 21.95 4.0456 122.45 0.2000 A
8 22.85 3.8887 35.85 0.2000 A
9 25.89 3.4383 516.60 0.2000 A
10 26.36 3.3783 52.40 0.2000
11 26.66 3.3404 89.79 0.2000
12 27.60 3.2295 54.55 0.2000
13 27.96 3.1885 518.47 0.2000 A
14 28.91 3.0854 89.12 0.2000 A
46 50.13 1.8182 40.15 0.2000
57 53.84 1.7015 74.62 0.2000
69 64.24 1.4487 59.73 0.2000 A
Overall peak intensity 2467 100.00% Peak intensity belonging to selected phases 886 35.91% Unidentified peak intensity 1581 64.09%
Peak Residuals Peak data 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%
Rietveld Refinement using FullProf Calculation was not run or did not converge. Integrated Profile Areas Based on calculated profile Profile area Counts Amount
73 66.63 1.4024 50.21 0.2000
72 66.36 1.4075 35.83 0.2000 A
71 65.24 1.4290 39.13 0.2000 A
70 65.05 1.4326 63.98 0.2000 A
68 64.08 1.4520 65.43 0.2000 A
58 54.69 1.6770 47.85 0.2000 A
67 63.92 1.4552 68.90 0.2000
66 63.74 1.4590 45.70 0.2000 A
65 63.02 1.4738 56.62 0.2000 A
64 61.82 1.4996 41.05 0.2000 A
63 61.64 1.5035 39.96 0.2000 A
62 59.85 1.5440 132.17 0.2000 A
61 57.92 1.5910 48.15 0.2000 A
60 57.74 1.5954 46.98 0.2000
59 56.99 1.6146 39.31 0.2000 A
Diffraction Pattern Graphics
Sample: Sampel_S8_B (S8B)
Sample DataFile 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
Index Amount (%) Name Formula sumA 100.0 Hydroxylapatite Ca5 H O13 P3
41.4 Unidentified peak area
A: Hydroxylapatite (100.0 %)
47 Intensity scale factor
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
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
Magnesium borohydride ammonia B2 H14 Mg N2 96-430-4782 0.8126 Cl Cs6 Ho21 Se34 96-432-8912 0.8124
Rubidium gadolinium bis(tungstate) Gd O8 Rb W2 96-201-4858 0.8132 Ca4 F2 O7 Si2 96-110-0154 0.8128
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
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
Ca4 H34 O41 V8 96-450-1915 0.8172 Marthozite Cu H16 O22 Se2 U3 96-900-4630 0.8166
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
0.66 Space group P 63/m Crystal system hexagonal Unit cell a= 9.4166 Å c= 6.8745 Å I/Icor
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
C Cl N2 S2 96-701-1348 0.8265 Whitlockite Ca9.06 Fe0.079 H0.87 Mg0.921 O28 P7 96-901-0492 0.8249 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
59 Peaks matched
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 Ca9 H Mn O28 P7 96-901-1162 0.8951 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
Candidates
Name Formula Entry No. FoMUSA", American Mineralogist 74, 870-876 (1989)
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,
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
Ca Mo5 O8 96-900-7923 0.8096 Lipscombite Fe1.473 H O5 P 96-900-1208 0.8095 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
40 43.89 2.0610 70.34 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
41 44.51 2.0338 73.04 0.2000 A
25 33.51 2.6718 81.75 0.2000
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
50 50.41 1.8087 91.92 0.2000 A
51 50.67 1.8001 67.49 0.2000
52 51.25 1.7810 87.79 0.2000 A
53 51.42 1.7757 116.36 0.2000
54 52.12 1.7535 59.96 0.2000 A
55 53.01 1.7260 255.89 0.2000
26 34.15 2.6235 180.50 0.2000 A
24 32.94 2.7173 376.91 0.2000 A
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
7 13.63 6.4916 148.31 0.2000
and 152 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
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
8 14.21 6.2281 35.24 0.2000
23 32.45 2.7570 317.18 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
56 53.14 1.7220 195.19 0.2000 A
67 63.04 1.4735 39.59 0.2000 A
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 Calculation was not run or did not converge. Integrated Profile Areas Based on calculated profile Profile area Counts Amount
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 Peak data Counts Amount
Overall peak intensity 2485 100.00% Peak intensity belonging to selected phases 825 33.18% Unidentified peak intensity 1661 66.82%
Diffraction Pattern Graphics Match! C opyright © 2003-2014 C RYSTAL IMPAC T, Bonn, Germany
Sample: Sampel_S8_C (S8C)
Sample DataFile 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
Index Amount (%) Name Formula sumA 100.0 Hydroxylapatite Ca5 H O13 P3
46.6 Unidentified peak area
A: Hydroxylapatite (100.0 %)
47 Intensity scale factor
Gatehouseite As0.06 H4 Mn5 O12 P1.76 Si0.18 96-901-4915 0.8100 In9 Li2 Y5
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
96-430-9585 0.8098 Ag7 As8 Fe3 O28
Ca4 H34 O41 V8 96-450-1915 0.8149
96-705-1675 0.8094 Ag7 As8 Fe3 O28
96-705-1674 0.8091 Seidozerite Ca1.28 F2 Fe0.42 Mn0.56 Na3.56 O16 Si4 Ti0.78 Zr1.4 96-901-1850 0.8086 Barium dicalcium pentalanthanum pentayttrium oxide
Ba Ca2 La5 O18 Y5 96-200-2477 0.8084
Ba5.4 Eu0.6 Ge25 96-810-0506 0.8069
Magnesium borohydride ammonia B2 H14 Mg N2 96-430-4782 0.8066
Bussyite-(Ce) Be5.176 Ca0.764 Ce0.824 Eu0.008 F4 Gd0.078 H7.72 La0.236 Mg0.012 Mn0.485 96-901-3788 0.8050
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
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
Ba2 (B4 Se13) B4 Ba2 Se13 96-151-1728 0.8184
0.67 Space group P 63/m Crystal system hexagonal Unit cell a= 9.4240 Å c= 6.8790 Å I/Icor
Calcium Thorium Phosphate Ca10.381 O28 P7 Th0.119 96-901-3987 0.9055 decacalcium potassium heptakis(orthophosphate)
1.61 Calc. density 3.153 g/cm³ 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
Name FormulaEntry No. FoM
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
Ca10 K O28 P7 96-221-1652 0.8964
96-432-8911 0.8200 lanthanum germanium antimonide Ge2.8 La6 Sb13.2 96-431-9314 0.8197
Whitlockite Ca10.115 Mg0.385 O28 P7 96-901-2137 0.8946 Whitlockite Ca9 H Mn O28 P7
96-901-1162 0.8944 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
58 Peaks matched
96-100-0193 0.8207 Cl Cs6 Dy21 Se34
96-100-0192 0.8210 Silver chromium phosphorus sulfide (.5/.5/1/3) Ag0.5 Cr0.5 P S3 Gatehouseite H4 Mn5 O12 P2 96-900-9893 0.8012
Mo5 O8 Sr 96-200-9382 0.8007
37 44.53 2.0331 80.29 0.1600 A
23 34.11 2.6267 158.63 0.1600 A
24 34.37 2.6073 679.54 0.1600
25 35.11 2.5539 92.02 0.1600
26 35.58 2.5209 124.76 0.1600 A
27 35.88 2.5005 48.59 0.1600
28 37.37 2.4045 94.15 0.1600
29 37.84 2.3755 58.12 0.1600
30 39.19 2.2969 36.28 0.1600 A
31 39.86 2.2600 225.57 0.1600 A
32 41.09 2.1951 117.57 0.1600 A
33 41.70 2.1640 94.70 0.1600
34 42.02 2.1485 32.53 0.1600 A
35 43.57 2.0754 62.80 0.1600
36 43.91 2.0603 76.56 0.1600 A
38 45.34 1.9988 80.40 0.1600 A
21 32.94 2.7166 417.36 0.1600 A
39 46.70 1.9433 175.20 0.1600 A
40 46.97 1.9331 222.38 0.1600
41 48.00 1.8938 154.38 0.1600 A
42 48.38 1.8800 119.11 0.1600 A
43 49.52 1.8392 168.22 0.1600 A
44 49.84 1.8283 54.65 0.1600
45 50.49 1.8060 99.73 0.1600 A
46 50.62 1.8018 81.71 0.1600
47 51.28 1.7802 109.64 0.1600 A
48 51.38 1.7768 110.72 0.1600
49 52.13 1.7531 67.15 0.1600 A
50 53.02 1.7258 249.19 0.1600 A
51 53.13 1.7224 190.33 0.1600 A
52 53.59 1.7089 83.46 0.1600
22 33.52 2.6715 67.18 0.1600
20 32.47 2.7550 245.60 0.1600
Ag V (P S3)2 Ag P2 S6 V 96-150-9506 0.8005
2 13.62 6.4944 152.06 0.1600
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
Whitlockite Ca9.06 Fe0.079 H0.87 Mg0.921 O28 P7 96-901-0492 0.7992 Keyite As3 Cd Cu1.5 H4 O14 Zn2
96-900-4425 0.7986 and 153 others...
Search-Match
SettingsReference 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
Peak List
No. 2theta [º] d [Å] I/I0 FWHM Matched1 10.86 8.1426 144.86 0.1600 A
3 14.22 6.2250 32.89 0.1600
19 32.22 2.7757 330.16 0.1600 A
12 27.48 3.2432 68.03 0.1600
18 31.80 2.8121 576.55 0.1600 A
17 31.06 2.8772 1000.00 0.1600
16 29.65 3.0109 124.09 0.1600
15 28.96 3.0808 91.24 0.1600 A
14 28.17 3.1647 60.38 0.1600 A
13 27.81 3.2058 555.84 0.1600
11 26.53 3.3571 82.91 0.1600
4 16.99 5.2147 204.69 0.1600 A
10 26.17 3.4024 55.44 0.1600
9 25.84 3.4453 408.84 0.1600 A
8 25.48 3.4927 31.77 0.1600 A
7 22.89 3.8815 38.12 0.1600 A
6 21.84 4.0658 158.10 0.1600 A
5 20.23 4.3869 53.63 0.1600
53 54.41 1.6850 58.71 0.1600
64 63.24 1.4693 32.07 0.1600
65 63.35 1.4669 38.98 0.1600 A
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 Calculation was not run or did not converge. Integrated Profile Areas Based on calculated profile Profile area Counts Amount
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 Peak data Counts Amount
Overall peak intensity 2334 100.00% Peak intensity belonging to selected phases 841 36.05% Unidentified peak intensity 1493 63.95%
Diffraction Pattern Graphics Match! C opyright © 2003-2014 C RYSTAL IMPAC T, Bonn, Germany