Intepretasi hasil pengukuran XRD

Grafik Intensitas-2theta

Karakter dasar yang

terlihat:
Posisi (2Theta)
Tinggi kurva (intensitas)
Lebar dan bentuk
puncak
Perbandingan difraktogram bahan
polimer
 Uses: fingerprinting
Single or multi-phase

Two different crystalline

phases are present in this
pattern one in a very
small amount

NOT like spectroscopy. Whole patterns match.

Intepretasi hasil XRD-identifikasi fasa

Menggunakan kartu Hanawalt

Menggunakan kartu PDF

Search-Match
 Databases
To match, we need a very large database of
powder patterns

ICDD (International Centre for Diffraction Data)

Powder Diffraction File contains (2007) 199,574
entries (172,360 inorganic & 30,728 organic)

In now days it was called JCPDS(Joint

Committee for Powder Diffraction Standards) and
before that ASTM
Hanawalt card
JCPS card model lama
JCPDS-ICDD card, database ITS
 PDF Data
Example

Why d and not 2 ??

 ICDD
Good
.
 ICDD
Bad.
e.g data hasil pengujian diidentifikasi
dengan metode Hanawalt
d() I/Io d() I/Io
3.25 10 1.00 20
2.82 100 0.95 5
2.18 5 0.94 20
1.99 60 0.89 20
1.71 5 0.86 5
1.63 30 0.85 20
1.42 20 0.82 10
1.25 30 0.79 10
1.15 30 0.78 20
1.09 5
 Hanawalt card
QM STRONGEST REFLECTION PSC Chemical Common PDF#
formula name

* 2.82X 1.993 3.992 CP5 Ca0.6Sr0.4NbO3 47-35

2.82X 1.999 3.266 CF8 PdO 46-1211

* 2.829 1.99X 2.306 CP5 KMgF3 18-1033

* 2.82X 1.996 1.632 CF8 NaCl Hallite,syn 05-628

c 2.82X 1.99X 1.998 CP2 BePd 18-428

 d() I/Io d() I/Io
Result 3.25 10 1.00 20
2.82 100 0.95 5
2.18 5 0.94 20
1.99 60 0.89 20
1.71 5 0.86 5
1.63 30 0.85 20
1.42 20 0.82 10
1.25 30 0.79 10
1.15 30 0.78 20
1.09 5

QM STRONGEST REFLECTION PSC Chemical Common PDF#

formula name
* 2.82X 1.993 3.992 CP5 Ca0.6Sr0.4NbO3 47-35

2.82X 1.999 3.266 CF8 PdO 46-1211

* 2.829 1.99X 2.306 CP5 KMgF3 18-1033

* 2.82X 1.996 1.632 CF8 NaCl Hallite,syn 05-628

c 2.82X 1.99X 1.998 CP2 BePd 18-428

 Analisis Kualitatif

Sampel PDF No : PDF No : PDF No :

2 intensitas 2 intensitas 2 intensitas 2 intensitas

Contoh analisis kualitatif
Contoh analisis kualitatif#1

Sampel PDF No : PDF No : PDF No :

2 intensitas 2 intensitas 2 intensitas 2 intensitas

Contoh analisis kualitatif#2
Contoh analisis kualitatif#2

Sampel PDF No : PDF No : PDF No :

2 intensitas 2 intensitas 2 intensitas 2 intensitas

Contoh analisis kualitatif#3
Search-match
 Search/Match
Search programs assist in identifying
phase mixtures:
Analisis data difraksi
Example: hasil
pengujian xrd
 Hasil pengujian
XRD

Talc is a major ingredient in certain cosmetic products. If it contains quartz or other abrasive
minerals, it is unsuitable for cosmetic applications. Chemical analysis cannot differentiate
between SiO2 present as quartz and SiO2 present as talc. X-ray diffraction analysis is an easy and
reliable way to ascertain the presence and quantity of quartz. The peaks in the x-ray pattern below
reveal that a minor amount of quartz (brown), along with some chlorite (green), is present in the
talc (blue). Through special procedures and with the use of quartz and talc standards, the amount
of quartz can be quantitatively determined to levels of less than 1%.
In other industrial mineral applications, health hazards such as respirable silica and asbestos in
dust samples or products of commerce can be determined by x-ray diffraction. Crystallization
chemistry is a complex science used in the production of compounds ranging from table salt and
potash to borax and Epsom salts. Minute changes in the crystallization system can cause
significant changes in the product that may not be detectable by chemical analysis or microscopy.
One project required that we determine quickly whether the particles forming in a sodium
carbonate process were hydrated, anhydrous, or a mixture of the two. The pattern below was
obtained by x-ray diffraction analysis and showed the presence of both forms. This permitted us
to change the process to generate the desired product.
Dust sample
XRD analysis pada produk korosi lingkungan
NaHSO3
XRD analisis produk korosi lingkungan NaCl
XRD analisis produk korosi lingkungan NaNO3
 Informasi hasil xrd
No Karakter Informasi dari material Informasi dari instrumen

1 Posisi puncak (2Theta) Fasa kristal/identifikasi Kesalahan 20

Struktur kristal Ketidaktepatan penempatan
Parameter kisi sampel
Regangan seragam

2 Tinggi puncak Identifikasi

(intensitas) Komposisi
Hamburan tak-koheren
Extinction
Preferred-orientation

3 Lebar dan bentuk Ukuran kristal (bukan

puncak partikel atau grain)
Distribusi ukuran kristal
Regangan tak-seragam
Dislokasi, cacat kristal
Hasil analisis lanjut
si ZMV i
Menghitung komposisi Wrel ,i N

s ZMV
k 1
k k

Menghitung ukuran kristal

D
H L H L, S

Menghitung estimasi regangan

U U S
rms
32 ln 2
 Contoh data pengujian difraksi
Al-TiO2.xls