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Intepretasi hasil pengukuran XRD

Grafik Intensitas-2theta

Karakter dasar yang


terlihat:
Posisi (2Theta)

Tinggi kurva (intensitas)


Lebar dan bentuk
puncak

Perbandingan
polimer

difraktogram

bahan

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


dengan metode Hanawalt
d()

I/Io

diidentifikasi

d()

I/Io

3.25

10

1.00

20

2.82

100

0.95

2.18

0.94

20

1.99

60

0.89

20

1.71

0.86

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

Hanawalt card
QM

STRONGEST REFLECTION

PSC

Chemical
formula

Common
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

2.82X

1.99X

1.998

CP2

BePd

Hallite,syn

PDF#

05-628
18-428

d()

Result

I/Io

d()

I/Io

3.25

10

1.00

20

2.82

100

0.95

2.18

0.94

20

1.99

60

0.89

20

1.71

0.86

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

QM

STRONGEST REFLECTION

PSC

Chemical
formula

Common
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

2.82X

1.99X

1.998

CP2

BePd

Hallite,syn

PDF#

05-628
18-428

Analisis Kualitatif

Sampel
2

intensitas

PDF No :

PDF No :

intensitas

PDF No :
intensitas

intensitas

Contoh analisis kualitatif

Contoh analisis kualitatif#1

Sampel
2

PDF No :
intensitas

PDF No :
intensitas

PDF No :
intensitas

intensitas

Contoh analisis kualitatif#2

Contoh analisis kualitatif#2

Sampel
2

PDF No :
intensitas

PDF No :
intensitas

PDF No :
intensitas

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

Posisi puncak (2Theta) Fasa kristal/identifikasi


Struktur kristal
Parameter kisi
Regangan seragam

Tinggi puncak
(intensitas)

Identifikasi
Komposisi
Hamburan tak-koheren
Extinction
Preferred-orientation

Lebar dan bentuk


puncak

Ukuran kristal (bukan


partikel atau grain)
Distribusi ukuran kristal
Regangan tak-seragam
Dislokasi, cacat kristal

Informasi dari instrumen

Kesalahan 20
Ketidaktepatan penempatan
sampel

Hasil analisis lanjut


Menghitung

komposisi Wrel,i

s i ZMV i
N

s ZMV
k 1

Menghitung

Menghitung

ukuran kristal

estimasi regangan

rms

H L H L, S

U U S
32 ln 2

Contoh data pengujian difraksi


Al-TiO2.xls