X射線-物相XRD-PDF4學習資料-19：SIeveplus Tutorial

SIeve+

Introduction1

SIeve+

is

a

Plug-In

module

integrated

in

the

PDF-4

products.

SIeve+

iseparately

at

an

additional

cost

except

for

the

PDF-4/Organics

dataSIeve+

will

activate

for

a

free

30-day

trial

period

or

until

the

prodregistered.

A

license

for

SIeve+

may

be

purchased

along

with

a

PDF-4or

following

the

free

30-day

trial

period.

SIeve+

accepts

user

data

and

searches

the

ICDD

reference

databases

(Organics,

and

Minerals)

for

comparison.

There

are

several

hundred

tentries

for

both

PDF-4+

and

Organic

databases.

Therefore,

various

mespecially

the

newly

implemented

features

andimprovements

listedare

used

to

ensure

efficient

searches

to

obtained

the

accurate

matcNew

Similarity

Index

with

normalized

R

indexNew

data

processing

menu

for

background

subtraction,

Ka2stripping,

smoothing,

and

peak

findingNew

Matches

Filter

with

Common

Filters

of

Primary

Patterns

or

MineralRelated

or

Common

PhasesInstant

display

of

overlappinginput

and

reference

patterns

The

matched

results

depend

on

the

criteria

and

methods

specified.

Thtutorial

demonstrates

the

available

methods

andthe

operational

prof

SIeve+.SIeve+

Purpose2SIeve+

will

identify

patterns

of

various

X-ray

powderdiffraction

(XRPD)

data

files:Single

phase

XRPD

patternsMulti-phase

XRPD

patternsData

file

containing

only

XRPD

peaks

(*.xml)Raw

instrumental

and/or

converted

data

file

formats:ICDDCIFX-YGSASBrukerMDIPANalyticalScintagSietronics(*.csv,

*.prn,

*.

*.pd3)(*.cif)(*.xrd)(*.gsas,

*.gss,

*.gsa,

*.raw,

*.dat)(*.uxd)(*.mdi)(*.xrdml,

*.udf)(*.ard)(*.cpi)SIeve+

Methods3There

are

different

search

methods

and

match

criteria

used

toget

accurate

results.

They

include:

Hanawalt

with

the

option

of

3

rotations

–

This

uses

thestrongest

line

for

the

search.

The

rotation

involves

up

to

thestrongest

lines

Fink

with

the

option

of

8

rotations

–

This

uses

the

longest

of

t8

strongest

lines

for

the

search.

The

rotation

involves

up

to

t8

strongest

lines.

Eight

largest

d-spacings

with

the

option

of

8

rotations

–

Thismethod

uses

the

largest

of

the

8

longest

lines

for

the

search.

Search

window

and

Match

window

are

options

for

user

tospecify

the

error

margin.

Weighted

GOM,

Pattern

GOM,

and

Similarity

Index

arequantities

used

to

rank

the

matched

reference

patterns.

Data

fileimport

processing

options

–

Manually

add/deletepoints

or

use

Cubic

Spline

function

for

background

subtractioAdd

diffraction

peaks;

Strip

Ka2

peaks

prior

to

file

import.SIeve+

Search/Match

ProcedureInput

User

DataCombine

withDDView+Search

CriteriaAccept

PhaseSpecifySearch/Matchoptions(Preferences)SpecifySearch/Matchoptions(Preferences)EndSinglePhase?ReasonableNew

Match?LastPhase?yesyesyesnonono443.

Import

Session:Raw

experimentaldigitized

data

files12345678910111213141.

New

Session:Manuallyinput

peaks(or

Copy/Paste)2.

Open

Session:Peak

files

-56

sample

multiphasepeak

files

in

theexamples

directorySIeve+

User

Data

InputFrequently

Used

Icons5SIeve+

Miscellaneous

OptionsFrequently

Used

Icons7.

SIeve+

Preference:Methods

and

Criteria

window?Search/Match

errormargin?Wavelength

specification?GOM

limit

specification?Hanawalt/Fink/Long8

selection?Show/Hide

All

Rotation?Show/Hide

Pattern

GOM?Show/Hide

Similarity

Index?D-Spacings/2Theta

selection11.

Accept

PhaseComparison

between

theuser

data

andreference

data

continues

after

“accepting”

the

matched1234567891011121314SIeve+

Phases

Table

–

Multiphase

Hit

LiThree

matched

referenced

patterns

from

the

PDF

database:?The

mixed

phases

contain

Zinc

Oxide,

Aluminum

Oxide,

and

Calcium

Fluoride?Sum

(intensities)

of

matched

peaks

for

reference

pattern

04-007-9627/Sum

(intensities)

of

matched

peaks

forunknown

mixed

phase

=

1.1?(1.1

/(1.1+0.27+0.89))

*

100

=

49?I/Ic:

reported

reference

intensity

ratio

inPDF

databasefor

50/50

weight

percent

for

[Reference

Pattern]/CorundumMatches

Filter:Combine

the

chemical,

physical,and

crystallographic

propertyfrom

the

previous

search

withthe

d-spacings/intensity

searchresults

.78SIeve+

Lines

Table

-

Phase

Comparisond-spacings/Intensities

ofMulti-phases

and

those

ofreference

patternscomparison

table:1st

&

2nd

columns:Experimental

data.3rd

&

4th

columns:First

matched

referencepattern

data.5th

&

6th

columns:Second

matched

referencepattern

data.7th

&

8th

columns:Third

matched

referencepattern

data.9SIeve+

Case-1Objective:

Search

for

reference

patterns

in

the

PDFdatabase

to

match

mixed

phase

peaks

in

a

user

file1.File

=>

Open

Session

=>From

Examples

Directory2.

Select

a

peak

file:Session_7_4_5.xml3.Select

Matches

Filter“ICDD

Pharmaceutical”

fromthe

previous

search

results3.Accept

“Ibuprofen”,continue

Searching5.2nd

matched

phaseβ

–Lactose

withhighest

GOM5.Diffraction

Patterns:unknown

andmatched

referencepatterns’

d-spacingsand

intensities10SIeve+

Case-1Interpretation

of

matched

resultsΔ

=

window

*

d

/

tan(arcsin(λ

/

(2

*

d)

))A

Match:reference

d-spacing<=

experimental

d-spacing+/-

ΔRed:

matched

lines;

Black:non-matched

lines;

Purple:

overlapped

linesGoodness

of

Match

(GOM):GOM

(each

line)

=

(

1

-

(line

error

/

Δ)

)

*

(

1

-

(line

error

/

Δ)

)

*

1000GOM

(Final

Weighted)

=

(D1

GOM

*

3)

+

(D2

GOM

*

2)

+(D3

GOM)

+

(D4

GOM

*

0.4)

+

(D5

GOM

*

0.4)

+

(D6

GOM

*

0.4)

+

(D7

GOM

*

0.4)

+

(D8

GOM

*

0.4)If

a

suspected

reference

pattern

is

not

in

the

“Matches”table,

users

can

use

the

new

option

“Add

PDF

#

“

underthe“Matches”

tab

to

manually

add

the

pattern

to

the

“Matches”table.SIeve+

Case-2Objective:

Find

matched

patterns

in

the

PDF

database

with

theexperimental

raw

data

containing

three

phases

of

compounds.Import

raw

experimental

data

file

–

amixture

of

three

phases

for

search/matchZero

po