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XRD and XRF are highly complementary

materials analysis methods which, when used

together, greatly improve the accuracy of

phase identification and quantitative analysis.

The combination of both methods provides an

increase in the numbers of measured parameters,

which means that fewer assumptions are needed

for analysis. This in turn provides not only greater

accuracy of results, but also increases the range

of samples that can be measured to include

samples about which little or nothing is known in

advance.

XRD is the most direct and accurate analytical

method for determining the presence and

absolute amounts of mineral species in a sample.

Ambiguous results may be obtained however, if

the sample chemistry and/or origin are unknown.

In these cases phase identification can be difficult;

in particular, isostructural phases with similar

chemical composition will give similar powder

diffraction patterns.

In contrast to XRD, XRF provides highly accurate

information about the elemental composition

of a sample, but it cannot deliver direct phase

information. Mass-balance calculations may give

sufficient phase information in some cases, but

can also lead to meaningless results e.g. in the

presence of polymorphs.

It is the complimentary nature of the XRD and

XRFmethods which makes them a valuable

tool for quantitative phase analysis in numerous

applications ranging from scientific research

to industrial high-throughput quality control.

Particularily in mineralogical and geological

application areas, the combined use of XRD and

XRF is booming, offering completely new insights

into materials and processes. Typical examples

are the cement, minerals & mining, and industrial

minerals industries, where the quality of products

and / or efficiency of processes is governed by

both phase and elemental composition. The

combined use of XRD and XRF methods allows

the reliable analysis of materials, for which the

individual methods fail to deliver accurate and

reliable results.

Page 2

Quantitative phase and element analysis of

host/waste rocks and tailings is an important

application in the minerals and mining industry

with respect to both process optimization (e.g.

acid leaching) and environmental protection:

Mining and milling operations are responsible

for the production of billions of tonnes of waste

rock and finely crushed tailings worldwide. An

important application is the knowledge of the

relative amounts of the minerals with acid-

producing or neutralization potential for successful

acid-base accounting with respect to both the

leaching process as well as acid mine drainage,

with its detrimental effects on environment.

As an example, we report combined XRD-XRF

analysis of an intrusive rock with unknown

composition. Of particular interest was its

classification by mineral content as well as

the detection and accurate quantification of

potentially present minerals with significant acid-

producing or neutralization potential.

Powder diffraction data were recorded using a

D4 ENDEAVOR powder diffractometer equipped

with a LynxEye

TM

detector (Fig. 1); the total

measurement time required was about 5 minutes.

For phase identification and quantification,

the DIFFRAC

plus

software packages EVA,

SEARCH and TOPAS were used. Standardless

XRFmeasurements on the same sample were

performed with the S4 PIONEER and the

SPECTRA

plus

software (Fig. 1).

Fig. 1: D4 ENDEAVOR diffractometer (right)

and S4 PIONEER spectrometer (left) connected

with conveyer belt. The D4 is equipped with

Super Speed LynxEye

TM

detector.

Fig. 2: EVA phase identification results.

1) Phase identification

Fig. 2 and Tab. 1 show the XRD powder data and

the phase identification results. The major rock

forming minerals plagioclase, quartz, diopside

and muscovite are easily and correctly identified

in a single default run. Note, that the highly

sensitive SEARCH algorithm clearly prefers albite

(Na-plagioclase) versus anorthite (Ca-plagioclase)

as a result of the slightly different lattice

parameters of both plagioclase solid solution

end members. Best SEARCH figure-of-merits

obtained for the individual phases were 0.65 and

1.48, respectively. Neither ore minerals nor any

K-feldspars or feldspathoids could be detected.

Tab. 1: EVA phase identification results.

SS-VVV-PPPP

Compound Name

00-009-0466 (*)

Albite

00-041-1480 (I)

Albite, calcian

03-065-0466 (C)

Quartz low, syn

01-087-0700 (C)

Diopside, syn

01-089-5402 (C)

Muscovite 2M1

Page 3

Fig. 3: EVA combined XRD-XRF results -

comparison of calculated (column "SQD") versus

observed (column "XRF") element concentrations.

The difference is given in column "Delta".

2) Combined XRD-XRF analysis

To confirm the phase identification results,

and to obtain semi-quantitative phase amount

estimates consistent with the actual elemental

composition of the sample, combined XRD-XRF

analysis has been performed with EVA. EVA

enables semi-quantitative analysis based on the

reference-intensity-ratio (RIR) method using both

XRD as well as XRFdata simultaneously: On

scaling the maximum intensities of the ICDD PDF

patterns to the observed peaks in the powder

pattern, EVA calculates both phase and element

concentrations, and compares the latter with the

actually measured element concentrations.

Element concentrations as obtained by XRF and

used by EVA are provided in Tab. 2. Already at

first glance, the XRF data fully confirm the absence

of any significant acid-producing ore minerals

due to the minor concentrations found for heavy

elements and the absence of sulphur.

Tab. 2: Element concentrations [%] as obtained by XRF.

Oxygen

47.7

Silicon

30.0

Aluminum 9.75

Sodium

6.1

Calcium

3.66

Magnesium 0.456

Iron

1.35

Potassium

0.271

Phosphorus 0.114

Chlorine

0.0445

Titanium

0.252

Manganese 0.0173

Cobalt

0.0182

Nickel

0.0142

Strontium

0.0595

Zirconium

0.0143

Barium

0.0258

Wolfram

0.101

The results for combined XRD-XRF analysis with

EVA are shown in Fig. 3 and Tab. 3. The high Na

vs. Ca concentrations confirm the presence of Na-

plagioclase as found by XRD (diopside accounts

for about 60% of the total Ca, as calculated

by EVA). The present Na-plagioclase is most

successfully modelled using two albite phases

with different Ca amounts. Note the excellent

agreement found between the calculated and

observed element concentrations, which is better

than 1% for all elements, and therefore confirms

the correctness of the XRD phase identification

results for all phases.

The accuracy of the RIR method is limited by

several factors such as preferred orientation

effects and the quality of the ICDD PDF data used

(e.g. quality of relative intensities, I/Icor values,

idealized chemical formula).

Tab. 3: EVA semi-quantitative phase analysis

results based on combined XRD-XRF using

reference intensities as given in the ICDD PDF

patterns.

SS-VVV-PPPP

Compound Name

Phase

amounts

00-009-0466 (*)

Albite

58.2%

00-041-1480 (I)

Albite, calcian

15.4%

03-065-0466 (C) Quartz low, syn

14.0%

01-087-0700 (C) Diopside, syn

9.9%

01-089-5402 (C) Muscovite 2M1

2.6%

The most accurate quantitative results will be

obtained from a TOPAS Rietveld refinement. The

combined XRD-XRF results obtained are of high

value for defining the refinement model.

Page 4

BRUKER AXS, INC.

5465 EAST ChERYL pARKwAY

MADISON, wI 53711-5373

USA

TEL. (+1) (800) 234-XRAY

TEL. (+1) (608) 276-3000

FAX (+1) (608) 276-3006

email info@bruker-axs.com

www.bruker-axs.com

All configurations and specifications are subject to change without notice. Order No. L88-E00058. © 2006 BRUKER AXS GmbH. Printed in Germany.

BRUKER AXS GMBh

OESTLIChE RhEINBRUECKENSTR. 49

D-76187 KARLSRUhE

GERMANY

TEL. (+49) (0)(721)595-2888

FAX (+49) (0)(721)595-4587

EMAIL info@bruker-axs.de

www.bruker-axs.de

BRUKER AXS K.K

3-9-A, MORIYA, KANAGAwA

YOKOhAMA, KANAGAwA 221-0022

Japan

TEL. (+81) 45 453 1963

FAX (+81) 45 440 0757

www.bruker-axs.com

3) Quantitative TOPAS refinement

Quantitative Rietveld analysis has been

performed using TOPAS, the results are shown

in Fig. 4 and Tab. 4. For the final refinement

two Na-plagioclases with different compositions

have been used to model the data to take the

elemental analysis results into account: Albite (0%

Ca) and Oligoclase (25% Ca).

From the results in Tab. 4 the following

conclusions can be drawn:

1. The sample can be unambiguously classified as

a quartzdiorite according to Streckeisen, see Fig. 5.

2. Combined XRD-XRF analysis and TOPAS

Rietveld refinement can allow a distinction of even

neighboring plagioclase solid solution members

(here albite and oligoclase) if present in sufficient

amounts.

The present sample can be characterised as

a rock with insignificant acid producing or

neutralisation potential. Remarkable is the easy

and reliable determination of the plagioclase type

for estimation of the neutralisation potential. This

ability is of particular interest, as anorthite has

an about 14x higher neutralisation potential than

albite (e.g. Jambor et al., 2002).

Fig. 4: Quantitative TOPAS refinement results.

Tab. 4: Quantitative TOPAS refinement results.

Compound Name

Phase amounts

Albite

49.6%

Oligoclase

30.5%

Quartz

9.9%

Diopside

8.8%

Muscovite

1.2%

Fig. 5: Streckeisen diagram for intrusive rocks.

Q: quartz, A: alkali-feldspar, P: plagioclase.

Reference

J.L. Jambor, J.E. Dutrizac, L.A. Groat, M. Raudsepp.

Environmental Geology (2002) 43, 1-17.

Q

A

P

granite

grano-

diorite

quartz-rich

granodiorite

quartz-

syenite

quartz-

monzonite

quartz-

monzo-

diorite

quartz-

diorite

tonalite

XRD and XRF are highly complementary

materials analysis methods which, when used

together, greatly improve the accuracy of

phase identification and quantitative analysis.

The combination of both methods provides an

increase in the numbers of measured parameters,

which means that fewer assumptions are needed

for analysis. This in turn provides not only greater

accuracy of results, but also increases the range

of samples that can be measured to include

samples about which little or nothing is known in

advance.

XRD is the most direct and accurate analytical

method for determining the presence and

absolute amounts of mineral species in a sample.

Ambiguous results may be obtained however, if

the sample chemistry and/or origin are unknown.

In these cases phase identification can be difficult;

in particular, isostructural phases with similar

chemical composition will give similar powder

diffraction patterns.

In contrast to XRD, XRF provides highly accurate

information about the elemental composition

of a sample, but it cannot deliver direct phase

information. Mass-balance calculations may give

sufficient phase information in some cases, but

can also lead to meaningless results e.g. in the

presence of polymorphs.

It is the complimentary nature of the XRD and

XRFmethods which makes them a valuable

tool for quantitative phase analysis in numerous

applications ranging from scientific research

to industrial high-throughput quality control.

Particularily in mineralogical and geological

application areas, the combined use of XRD and

XRF is booming, offering completely new insights

into materials and processes. Typical examples

are the cement, minerals & mining, and industrial

minerals industries, where the quality of products

and / or efficiency of processes is governed by

both phase and elemental composition. The

combined use of XRD and XRF methods allows

the reliable analysis of materials, for which the

individual methods fail to deliver accurate and

reliable results.

Page 2

Quantitative phase and element analysis of

host/waste rocks and tailings is an important

application in the minerals and mining industry

with respect to both process optimization (e.g.

acid leaching) and environmental protection:

Mining and milling operations are responsible

for the production of billions of tonnes of waste

rock and finely crushed tailings worldwide. An

important application is the knowledge of the

relative amounts of the minerals with acid-

producing or neutralization potential for successful

acid-base accounting with respect to both the

leaching process as well as acid mine drainage,

with its detrimental effects on environment.

As an example, we report combined XRD-XRF

analysis of an intrusive rock with unknown

composition. Of particular interest was its

classification by mineral content as well as

the detection and accurate quantification of

potentially present minerals with significant acid-

producing or neutralization potential.

Powder diffraction data were recorded using a

D4 ENDEAVOR powder diffractometer equipped

with a LynxEye

TM

detector (Fig. 1); the total

measurement time required was about 5 minutes.

For phase identification and quantification,

the DIFFRAC

plus

software packages EVA,

SEARCH and TOPAS were used. Standardless

XRFmeasurements on the same sample were

performed with the S4 PIONEER and the

SPECTRA

plus

software (Fig. 1).

Fig. 1: D4 ENDEAVOR diffractometer (right)

and S4 PIONEER spectrometer (left) connected

with conveyer belt. The D4 is equipped with

Super Speed LynxEye

TM

detector.

Fig. 2: EVA phase identification results.

1) Phase identification

Fig. 2 and Tab. 1 show the XRD powder data and

the phase identification results. The major rock

forming minerals plagioclase, quartz, diopside

and muscovite are easily and correctly identified

in a single default run. Note, that the highly

sensitive SEARCH algorithm clearly prefers albite

(Na-plagioclase) versus anorthite (Ca-plagioclase)

as a result of the slightly different lattice

parameters of both plagioclase solid solution

end members. Best SEARCH figure-of-merits

obtained for the individual phases were 0.65 and

1.48, respectively. Neither ore minerals nor any

K-feldspars or feldspathoids could be detected.

Tab. 1: EVA phase identification results.

SS-VVV-PPPP

Compound Name

00-009-0466 (*)

Albite

00-041-1480 (I)

Albite, calcian

03-065-0466 (C)

Quartz low, syn

01-087-0700 (C)

Diopside, syn

01-089-5402 (C)

Muscovite 2M1

Page 3

Fig. 3: EVA combined XRD-XRF results -

comparison of calculated (column "SQD") versus

observed (column "XRF") element concentrations.

The difference is given in column "Delta".

2) Combined XRD-XRF analysis

To confirm the phase identification results,

and to obtain semi-quantitative phase amount

estimates consistent with the actual elemental

composition of the sample, combined XRD-XRF

analysis has been performed with EVA. EVA

enables semi-quantitative analysis based on the

reference-intensity-ratio (RIR) method using both

XRD as well as XRFdata simultaneously: On

scaling the maximum intensities of the ICDD PDF

patterns to the observed peaks in the powder

pattern, EVA calculates both phase and element

concentrations, and compares the latter with the

actually measured element concentrations.

Element concentrations as obtained by XRF and

used by EVA are provided in Tab. 2. Already at

first glance, the XRF data fully confirm the absence

of any significant acid-producing ore minerals

due to the minor concentrations found for heavy

elements and the absence of sulphur.

Tab. 2: Element concentrations [%] as obtained by XRF.

Oxygen

47.7

Silicon

30.0

Aluminum 9.75

Sodium

6.1

Calcium

3.66

Magnesium 0.456

Iron

1.35

Potassium

0.271

Phosphorus 0.114

Chlorine

0.0445

Titanium

0.252

Manganese 0.0173

Cobalt

0.0182

Nickel

0.0142

Strontium

0.0595

Zirconium

0.0143

Barium

0.0258

Wolfram

0.101

The results for combined XRD-XRF analysis with

EVA are shown in Fig. 3 and Tab. 3. The high Na

vs. Ca concentrations confirm the presence of Na-

plagioclase as found by XRD (diopside accounts

for about 60% of the total Ca, as calculated

by EVA). The present Na-plagioclase is most

successfully modelled using two albite phases

with different Ca amounts. Note the excellent

agreement found between the calculated and

observed element concentrations, which is better

than 1% for all elements, and therefore confirms

the correctness of the XRD phase identification

results for all phases.

The accuracy of the RIR method is limited by

several factors such as preferred orientation

effects and the quality of the ICDD PDF data used

(e.g. quality of relative intensities, I/Icor values,

idealized chemical formula).

Tab. 3: EVA semi-quantitative phase analysis

results based on combined XRD-XRF using

reference intensities as given in the ICDD PDF

patterns.

SS-VVV-PPPP

Compound Name

Phase

amounts

00-009-0466 (*)

Albite

58.2%

00-041-1480 (I)

Albite, calcian

15.4%

03-065-0466 (C) Quartz low, syn

14.0%

01-087-0700 (C) Diopside, syn

9.9%

01-089-5402 (C) Muscovite 2M1

2.6%

The most accurate quantitative results will be

obtained from a TOPAS Rietveld refinement. The

combined XRD-XRF results obtained are of high

value for defining the refinement model.

Page 4

BRUKER AXS, INC.

5465 EAST ChERYL pARKwAY

MADISON, wI 53711-5373

USA

TEL. (+1) (800) 234-XRAY

TEL. (+1) (608) 276-3000

FAX (+1) (608) 276-3006

EMAIL info@bruker-axs.com

www.bruker-axs.com

All configurations and specifications are subject to change without notice. Order No. L88-E00058. © 2006 BRUKER AXS GmbH. Printed in Germany.

BRUKER AXS GMBh

OESTLIChE RhEINBRUECKENSTR. 49

D-76187 KARLSRUhE

GERMANY

TEL. (+49) (0)(721)595-2888

FAX (+49) (0)(721)595-4587

EMAIL info@bruker-axs.de

www.bruker-axs.de

BRUKER AXS K.K

3-9-A, MORIYA, KANAGAwA

YOKOhAMA, KANAGAwA 221-0022

JApAN

TEL. (+81) 45 453 1963

FAX (+81) 45 440 0757

www.bruker-axs.com

3) Quantitative TOPAS refinement

Quantitative Rietveld analysis has been

performed using TOPAS, the results are shown

in Fig. 4 and Tab. 4. For the final refinement

two Na-plagioclases with different compositions

have been used to model the data to take the

elemental analysis results into account: Albite (0%

Ca) and Oligoclase (25% Ca).

From the results in Tab. 4 the following

conclusions can be drawn:

1. The sample can be unambiguously classified as

a quartzdiorite according to Streckeisen, see Fig. 5.

2. Combined XRD-XRF analysis and TOPAS

Rietveld refinement can allow a distinction of even

neighboring plagioclase solid solution members

(here albite and oligoclase) if present in sufficient

amounts.

The present sample can be characterised as

a rock with insignificant acid producing or

neutralisation potential. Remarkable is the easy

and reliable determination of the plagioclase type

for estimation of the neutralisation potential. This

ability is of particular interest, as anorthite has

an about 14x higher neutralisation potential than

albite (e.g. Jambor et al., 2002).

Fig. 4: Quantitative TOPAS refinement results.

Tab. 4: Quantitative TOPAS refinement results.

Compound Name

Phase amounts

Albite

49.6%

Oligoclase

30.5%

Quartz

9.9%

Diopside

8.8%

Muscovite

1.2%

Fig. 5: Streckeisen diagram for intrusive rocks.

Q: quartz, A: alkali-feldspar, P: plagioclase.

Reference

J.L. Jambor, J.E. Dutrizac, L.A. Groat, M. Raudsepp.

Environmental Geology (2002) 43, 1-17.

Q

A

P

granite

grano-

diorite

quartz-rich

granodiorite

quartz-

syenite

quartz-

monzonite

quartz-

monzo-

diorite

quartz-

diorite

tonalite

XRD and XRF are highly complementary

materials analysis methods which, when used

together, greatly improve the accuracy of

phase identification and quantitative analysis.

The combination of both methods provides an

increase in the numbers of measured parameters,

which means that fewer assumptions are needed

for analysis. This in turn provides not only greater

accuracy of results, but also increases the range

of samples that can be measured to include

samples about which little or nothing is known in

advance.

XRD is the most direct and accurate analytical

method for determining the presence and

absolute amounts of mineral species in a sample.

Ambiguous results may be obtained however, if

the sample chemistry and/or origin are unknown.

In these cases phase identification can be difficult;

in particular, isostructural phases with similar

chemical composition will give similar powder

diffraction patterns.

In contrast to XRD, XRF provides highly accurate

information about the elemental composition

of a sample, but it cannot deliver direct phase

information. Mass-balance calculations may give

sufficient phase information in some cases, but

can also lead to meaningless results e.g. in the

presence of polymorphs.

It is the complimentary nature of the XRD and

XRFmethods which makes them a valuable

tool for quantitative phase analysis in numerous

applications ranging from scientific research

to industrial high-throughput quality control.

Particularily in mineralogical and geological

application areas, the combined use of XRD and

XRF is booming, offering completely new insights

into materials and processes. Typical examples

are the cement, minerals & mining, and industrial

minerals industries, where the quality of products

and / or efficiency of processes is governed by

both phase and elemental composition. The

combined use of XRD and XRF methods allows

the reliable analysis of materials, for which the

individual methods fail to deliver accurate and

reliable results.

Page 2

Quantitative phase and element analysis of

host/waste rocks and tailings is an important

application in the minerals and mining industry

with respect to both process optimization (e.g.

acid leaching) and environmental protection:

Mining and milling operations are responsible

for the production of billions of tonnes of waste

rock and finely crushed tailings worldwide. An

important application is the knowledge of the

relative amounts of the minerals with acid-

producing or neutralization potential for successful

acid-base accounting with respect to both the

leaching process as well as acid mine drainage,

with its detrimental effects on environment.

As an example, we report combined XRD-XRF

analysis of an intrusive rock with unknown

composition. Of particular interest was its

classification by mineral content as well as

the detection and accurate quantification of

potentially present minerals with significant acid-

producing or neutralization potential.

Powder diffraction data were recorded using a

D4 ENDEAVOR powder diffractometer equipped

with a LynxEye

TM

detector (Fig. 1); the total

measurement time required was about 5 minutes.

For phase identification and quantification,

the DIFFRAC

plus

software packages EVA,

SEARCH and TOPAS were used. Standardless

XRFmeasurements on the same sample were

performed with the S4 PIONEER and the

SPECTRA

plus

software (Fig. 1).

Fig. 1: D4 ENDEAVOR diffractometer (right)

and S4 PIONEER spectrometer (left) connected

with conveyer belt. The D4 is equipped with

Super Speed LynxEye

TM

detector.

Fig. 2: EVA phase identification results.

1) Phase identification

Fig. 2 and Tab. 1 show the XRD powder data and

the phase identification results. The major rock

forming minerals plagioclase, quartz, diopside

and muscovite are easily and correctly identified

in a single default run. Note, that the highly

sensitive SEARCH algorithm clearly prefers albite

(Na-plagioclase) versus anorthite (Ca-plagioclase)

as a result of the slightly different lattice

parameters of both plagioclase solid solution

end members. Best SEARCH figure-of-merits

obtained for the individual phases were 0.65 and

1.48, respectively. Neither ore minerals nor any

K-feldspars or feldspathoids could be detected.

Tab. 1: EVA phase identification results.

SS-VVV-PPPP

Compound Name

00-009-0466 (*)

Albite

00-041-1480 (I)

Albite, calcian

03-065-0466 (C)

Quartz low, syn

01-087-0700 (C)

Diopside, syn

01-089-5402 (C)

Muscovite 2M1

Page 3

Fig. 3: EVA combined XRD-XRF results -

comparison of calculated (column "SQD") versus

observed (column "XRF") element concentrations.

The difference is given in column "Delta".

2) Combined XRD-XRF analysis

To confirm the phase identification results,

and to obtain semi-quantitative phase amount

estimates consistent with the actual elemental

composition of the sample, combined XRD-XRF

analysis has been performed with EVA. EVA

enables semi-quantitative analysis based on the

reference-intensity-ratio (RIR) method using both

XRD as well as XRFdata simultaneously: On

scaling the maximum intensities of the ICDD PDF

patterns to the observed peaks in the powder

pattern, EVA calculates both phase and element

concentrations, and compares the latter with the

actually measured element concentrations.

Element concentrations as obtained by XRF and

used by EVA are provided in Tab. 2. Already at

first glance, the XRF data fully confirm the absence

of any significant acid-producing ore minerals

due to the minor concentrations found for heavy

elements and the absence of sulphur.

Tab. 2: Element concentrations [%] as obtained by XRF.

Oxygen

47.7

Silicon

30.0

Aluminum 9.75

Sodium

6.1

Calcium

3.66

Magnesium 0.456

Iron

1.35

Potassium

0.271

Phosphorus 0.114

Chlorine

0.0445

Titanium

0.252

Manganese 0.0173

Cobalt

0.0182

Nickel

0.0142

Strontium

0.0595

Zirconium

0.0143

Barium

0.0258

Wolfram

0.101

The results for combined XRD-XRF analysis with

EVA are shown in Fig. 3 and Tab. 3. The high Na

vs. Ca concentrations confirm the presence of Na-

plagioclase as found by XRD (diopside accounts

for about 60% of the total Ca, as calculated

by EVA). The present Na-plagioclase is most

successfully modelled using two albite phases

with different Ca amounts. Note the excellent

agreement found between the calculated and

observed element concentrations, which is better

than 1% for all elements, and therefore confirms

the correctness of the XRD phase identification

results for all phases.

The accuracy of the RIR method is limited by

several factors such as preferred orientation

effects and the quality of the ICDD PDF data used

(e.g. quality of relative intensities, I/Icor values,

idealized chemical formula).

Tab. 3: EVA semi-quantitative phase analysis

results based on combined XRD-XRF using

reference intensities as given in the ICDD PDF

patterns.

SS-VVV-PPPP

Compound Name

Phase

amounts

00-009-0466 (*)

Albite

58.2%

00-041-1480 (I)

Albite, calcian

15.4%

03-065-0466 (C) Quartz low, syn

14.0%

01-087-0700 (C) Diopside, syn

9.9%

01-089-5402 (C) Muscovite 2M1

2.6%

The most accurate quantitative results will be

obtained from a TOPAS Rietveld refinement. The

combined XRD-XRF results obtained are of high

value for defining the refinement model.

Page 4

BRUKER AXS, INC.

5465 EAST ChERYL pARKwAY

MADISON, wI 53711-5373

USA

TEL. (+1) (800) 234-XRAY

TEL. (+1) (608) 276-3000

FAX (+1) (608) 276-3006

EMAIL info@bruker-axs.com

www.bruker-axs.com

All configurations and specifications are subject to change without notice. Order No. L88-E00058. © 2006 BRUKER AXS GmbH. Printed in Germany.

BRUKER AXS GMBh

OESTLIChE RhEINBRUECKENSTR. 49

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3) Quantitative TOPAS refinement

Quantitative Rietveld analysis has been

performed using TOPAS, the results are shown

in Fig. 4 and Tab. 4. For the final refinement

two Na-plagioclases with different compositions

have been used to model the data to take the

elemental analysis results into account: Albite (0%

Ca) and Oligoclase (25% Ca).

From the results in Tab. 4 the following

conclusions can be drawn:

1. The sample can be unambiguously classified as

a quartzdiorite according to Streckeisen, see Fig. 5.

2. Combined XRD-XRF analysis and TOPAS

Rietveld refinement can allow a distinction of even

neighboring plagioclase solid solution members

(here albite and oligoclase) if present in sufficient

amounts.

The present sample can be characterised as

a rock with insignificant acid producing or

neutralisation potential. Remarkable is the easy

and reliable determination of the plagioclase type

for estimation of the neutralisation potential. This

ability is of particular interest, as anorthite has

an about 14x higher neutralisation potential than

albite (e.g. Jambor et al., 2002).

Fig. 4: Quantitative TOPAS refinement results.

Tab. 4: Quantitative TOPAS refinement results.

Compound Name

Phase amounts

Albite

49.6%

Oligoclase

30.5%

Quartz

9.9%

Diopside

8.8%

Muscovite

1.2%

Fig. 5: Streckeisen diagram for intrusive rocks.

Q: quartz, A: alkali-feldspar, P: plagioclase.

Reference

J.L. Jambor, J.E. Dutrizac, L.A. Groat, M. Raudsepp.

Environmental Geology (2002) 43, 1-17.

Q

A

P

granite

grano-

diorite

quartz-rich

granodiorite

quartz-

syenite

quartz-

monzonite

quartz-

monzo-

diorite

quartz-

diorite

tonalite

XRD- provides most direct analytical methol for determining presence and absolute amounts of minerals species in sample. XRD can also identify phases

XRF- provides direct information about chemical composition but cannot deliver direct phase information. Mass-balance calculations can be deducted but may lead to useless results in the presence of a polymorph.

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Why use copper in xrd analysis?

Copper is often used in XRD analysis as a standard reference material or calibration standard due to its well-defined and sharp diffraction peaks. It also has a simple crystal structure which makes it easy to interpret the XRD data. Additionally, copper has good thermal and chemical stability, making it suitable for use in XRD instruments.


What are the XRD peaks for glass?

Glass does not exhibit distinct X-ray diffraction (XRD) peaks because it is amorphous in nature, lacking a regular crystalline structure. This is in contrast to crystalline materials, which display sharp, well-defined peaks in XRD patterns due to their ordered atomic arrangement.


Why FWHM increase with increase in grain size in XRD?

The Full Width at Half Maximum (FWHM) in XRD increases with an increase in grain size because larger grains have more crystalline imperfections (e.g., grain boundaries, dislocations) that contribute to broadening of the diffraction peaks. As the grain size increases, these imperfections become more pronounced, leading to broader diffraction peaks and a larger FWHM.


Where does ionization energy come from with XRD?

Ionization energy in X-ray diffraction (XRD) comes from the interaction of X-rays with atoms in a crystal sample. When the X-rays strike the sample, they can displace electrons from the inner shells of atoms, leading to the ionization of the atoms. This process can result in the emission of characteristic X-ray radiation, which is used to determine the atomic structure of the sample.


What is Differentiate between polymorphism and isomerism?

Polymorphism and Allotropy are same thing. Polymorphism is used for compounds and the allotropy is reserved for elements. You can go for XRD to check the crystal structure and their composition to distinguish.

Related Questions

Why use copper in xrd analysis?

Copper is often used in XRD analysis as a standard reference material or calibration standard due to its well-defined and sharp diffraction peaks. It also has a simple crystal structure which makes it easy to interpret the XRD data. Additionally, copper has good thermal and chemical stability, making it suitable for use in XRD instruments.


What are the XRD peaks for glass?

Glass does not exhibit distinct X-ray diffraction (XRD) peaks because it is amorphous in nature, lacking a regular crystalline structure. This is in contrast to crystalline materials, which display sharp, well-defined peaks in XRD patterns due to their ordered atomic arrangement.


What does the acronym XRD stand for?

XRD stands for Extensible Resource Descriptor Sequence. It is a version of the XML format that allows users to discover various metadata aspects from documents being used.


How do you determine the identity of a green crusty mineral on a stalagmite?

by the use of XRD.


What is external standard method for XRD technique and how to calculate it?

In the external standard method for X-ray diffraction (XRD) technique, a known standard sample is used to calibrate the XRD instrument before analyzing unknown samples. The intensity of characteristic peaks from the standard sample is measured and used to calculate the correction factor or calibration curve, which is then applied to quantify the phases in the unknown samples based on their XRD patterns.


Why sharp peak and diffuse peak are observed in powder XRD?

Sharp peaks in powder XRD indicate well-ordered crystal structures with long-range periodicity. Diffuse peaks, on the other hand, suggest the presence of defects, disorders, or amorphous regions within the material. In powder XRD, the diffraction pattern results from a combination of many crystallites with different orientations, leading to a mixture of sharp and diffuse peaks.


What are the applications of cobalt XRD in materials science and how does it contribute to the analysis of crystal structures?

Cobalt X-ray diffraction (XRD) is used in materials science to analyze the crystal structures of materials. It is commonly used to determine the atomic arrangement and composition of materials, as well as their physical and chemical properties. Cobalt XRD can help researchers identify phases, defects, and grain sizes in materials, providing valuable insights into their structure and behavior. Overall, cobalt XRD plays a crucial role in advancing our understanding of materials and their properties in various fields such as metallurgy, nanotechnology, and solid-state physics.


What are the differences between SAXS and XRD techniques in material analysis?

SAXS (Small-Angle X-ray Scattering) and XRD (X-ray Diffraction) are both techniques used in material analysis, but they have different purposes and applications. SAXS is used to study the structure of materials on a nanometer scale, providing information about the size, shape, and arrangement of particles in a material. It is particularly useful for analyzing disordered or amorphous materials. XRD, on the other hand, is used to determine the crystal structure of materials, providing information about the arrangement of atoms in a material's crystal lattice. It is commonly used to identify crystalline phases and study the composition of materials. In summary, SAXS is used for analyzing nanoscale structures and disordered materials, while XRD is used for studying crystal structures and crystalline materials.


What does XRD tell us?

XRD (X-ray diffraction) is a technique used to analyze the crystallographic structure of materials. It provides information on the crystal structure, phase composition, and crystallite size of a sample, helping to identify the different phases present in the material and their arrangement in the crystal lattice.


What is the use of XRD?

XRD, or X-ray diffraction, is used to analyze the crystalline structure of materials by measuring the scattering of X-rays. It can provide information on the crystal structure, atomic arrangement, and orientation of crystalline materials, making it valuable for material identification and characterization in various fields such as chemistry, physics, geology, and material science.


What is XRD pole figure?

An XRD pole figure is a graphical representation of the orientation distribution of crystallites in a sample based on X-ray diffraction data. It provides information on the preferred orientation or texture of the crystalline material, showing how the crystals are aligned in different directions within the sample. Pole figures are useful for understanding the crystallographic orientation relationships and anisotropic properties of materials.


What is the disadvantage and advantage of using XRD instead of XRF?

Actually the type of compound and its molecular structure designates which technique will be more effective. XRD is used to measure crystalline compounds and provides a quantitative and qualitative analysis of compounds that cannot be measured by other means.XRF is a technique that is used to measure the percentage of metals within inorganic matrices such as cement and metal alloys. XRF is an especially useful research and development tool in construction industries. This technique is extremely useful for determining the make-up of these materials, allowing for higher-quality cements and alloys to be developed. Disadvantage : XRD has some size limitations. It is much more accurate for measuring large crystalline structures rather than small ones. Small structures that are present only in trace amounts will often go undetected by XRD readings, which can result in skewed results.