Manual EDX 700 Shimadzu

8/19/2019 Manual EDX 700 Shimadzu

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Instruction Manual P/N 305-32056A

EDX Series

Measuring Hazardous Elements

SHIMADZU CORPORATION

ANALYTICAL MEASURING

INSTRUMENTS DIVISION


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About this manual

About this manual

This manual describes how to make analytical condition for measuring hazardous elements (Cd, Pb, Hg,Cr and Br) in EDX series.

The descriptions are based on the functionality offered by EDX software version 1.00, release 017.

Furthermore, the parameters described in this manual are based primarily on examples of settings for

elements in plastic.


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Contents

Contents

About this manual

1. Sensitivity and Precision in X-Ray Fluorescence Spectrometry........ ...... ...... ...... ...... ..... 1

1.1 Precision of X-Ray Spectrometry ...................................................... 1

1.1.1 Standard Deviation ...................................................... 1

1.1.2 Lower Detection Limit ...................................................... 2

1.2 Differences in Sensitivity Due to Sample Material and Shape ...... ...... ...... ...... ...... . 3

1.2.1 Differences in Sensitivity Due to Sample Material .......... ...... ...... ...... ...... ...... .. 3

1.2.2 Differences in Sensitivity Due to Sample Size or Thickness ...... ...... ...... ...... ... 4

1.2.3 Scattered X-ray and Fluorescent X-ray ...... ...... ...... ...... ...... ...... ...... ...... ...... 4

1.2.4 Correcting for Sample Shape and Material ...................................................... 5

2. Analytical Conditions ...................................................... 6

2.1 Example of Setting Parameters ...................................................... 62.1.1 Example of Setting Parameters ...................................................... 6

2.2 Key Points for Setting Parameters ...................................................... 6

2.2.1 Overview ...................................................... 6

2.2.2 Element Registration ...................................................... 8

2.2.3 Element Information ...................................................... 9

2.2.4 Measurement Conditions ...................................................... 10

2.2.5 Process for Spectra ...................................................... 12

2.2.6 Internal Standard Correction ...................................................... 13

2.2.7 Result Format ...................................................... 14

2.2.8 Standard Sample Registration ...................................................... 15

2.2.9 Standard Sample Measurements ...................................................... 17

2.2.10 Calibration Curve Preparation ...................................................... 183. Controlling Precision ...................................................... 22

3.1 Drift Check Analysis ...................................................... 22

3.1.1 Analyzing Control Sample ...................................................... 22

3.1.2 Results Outside the Control Range ...................................................... 22

3.2 Drift Standardization ...................................................... 23

3.2.1 What is Drift Standardization? ...................................................... 23

3.2.2 Registration of Reference Intensities for Standardization Samples ...... ...... ...... 23

3.2.3 Drift Coefficient Renewal ...................................................... 27

3.2.4 Drift Coefficient Criteria ...................................................... 28

3.3 Measurement Time Reduction ...................................................... 29

3.3.1 Measurement Time Reduction ...................................................... 29

4. Interpreting Data and Making Determination ...................................................... 30

4.1 The possibility of Determination Errors ...................................................... 30

4.1.1 Determination Errors Due to Overlapping Spectra ......... ...... ...... ...... ...... ...... ... 30

4.1.2 Determination Errors Due to Diffracted Lines ....... ...... ...... ...... ...... ...... ...... ..... 31

4.2 ExReport Function ...................................................... 32

4.2.1 ExReport Function ...................................................... 32

5. Hints for Configuring Conditions ...................................................... 33


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1. Sensitivity and Precision of X-Ray Fluorescence Spectrometry

1. Sensitiv ity and Precision of X-Ray Fluorescence

Spectrometry

1.1 Precision of X-Ray Fluorescence Spectrometry

1.1.1 Standard Deviation

The precision level of x-ray fluorescence analysis is related to the standard deviation of the x-ray intensity

from target elements. In general, the standard deviation of the x-ray count for an x-ray measurement is

expressed as the square root of the x-ray counts, where

Standard Deviation of X-Ray Intensity (Count)

= X-Ray Counts

In the case of x-rays per unit time (cps), the standard deviation is as follows.

Standard Deviation of X-Ray Intensity (cps)

= X-Ray Counts / Measurement Time (sec)

The x-ray count is proportional to the measurement time, having the following relationship.

When Time is Doubled --> Std. dev. of x-ray intensity (count) is multiplied by

Std. dev. of x-ray intensity (cps) is multiplied by 1/2 (or 2/2)

When Time is Quadrupled --> Std. dev. of x-ray intensity (count) is multiplied by 2 (or 4)

Std. dev. of x-ray intensity (cps) is multiplied by 1/2 (or 4/4)

Therefore, when the measurement time is increased, the standard deviation of intensity (cps) decreases. In

other words, the longer the measurement time, the higher the reliability of measurement values.


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1.1.2 Lower Detection Limit

The minimum level of target elements that can be detected is determined by the following parameters.

a) Standard deviation B of intensity for a sample containing no target elements.

b) Calibration curve coefficient b

In general, the lower detection limit is defined as 3 x B x b.


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1.2 Differences in Sensit ivity Due to Sample Material and Shape

1.2.1 Differences in Sensitivity Due to Sample Material

The minimum detectable quantity will vary depending on the sample material. The reasons for this

variation are as follows.

a) X-ray fluorescence emission from target elements is absorbed by surrounding materials.

b) Primary x-rays from the x-ray tube are absorbed by the surrounding material and do not excite the

target elements.

Generally high atomic number materials absorb more x-ray than low atomic number material. In addition,

absorption also increases if the material has a higher density. Therefore, in general, sensitivity is higher in

plastics and lower in metals, as shown in the example below.

Differences in Lower Detection Limits Due to Sample Material

(as a proportion of the detection limit for target elements in polyethylene)

Polyethylene PVC Aluminum Copper Tin Lead

Cd 1 1.2 1.5 6 50 200

Pb 1 2.3 2.5 20 30 ---------

Note that even though they are both plastics, the lower detection limit for polyethylene and polyvinyl

chloride (PVC) is quite different. This is due to x-ray fluorescence from target elements being absorbed

by the chlorine contained in polyvinyl chloride.


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1.2.2 Differences in Sensi tiv ity Due to Sample Size or Thickness

Theoretically, the larger the sample is, the greater the x-ray intensity is. This also applies to thickness.

X-ray intensity is greater for thicker samples.

The x-ray irradiation diameter can be changed using an optional collimator. Using a smaller diameter for

analysis generally decreases x-ray intensity levels. However, for samples comprised of differing sections,

this can reduce the undesirable x-rays emitted from non-target areas, improving the relative sensitivity for

the target area.

In general, thicker samples result in higher x-ray intensities, but x-ray intensity does not increase when it

reaches a certain constant thickness. That saturation thickness varies depending on the sample material.

For the EDX series, the following table shows the saturation thickness of X-ray intensity for different

sample materials.

Polyethylene PVC Aluminum Copper Tin LeadCd 5mm 5mm 3mm 100m 150m 20m

Pb 5mm 0.7mm 0.5mm 20m 30m ---------

1.2.3 Scattered X-ray and Fluorescent X-ray

When primary x-ray from x-ray tube irradiates to a sample, fluorescent x-ray and scattered x-ray are both

detected. Fluorescent x-ray is x-ray generated when primary x-ray excites target elements in a sample.

Scattered x-ray is detected as background intensity. This scattered x-ray includes valuable information

also, such as the sample size, thickness and composition.


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1.2.4 Correcting for Sample Shape and Material

Even for samples having the same concentration level, intensities vary depending on sample size and

thickness. This affects the calculated quantitative values. To avoid this bias, differences in quantitative

values due to sample size and thickness can be corrected by preparing calibration curves using the ratio

between fluorescent x-ray and scattered x-ray intensities.

In the case of plastics, there is a significant difference in sensitivity between polyethylene and PVC.

Therefore, if calibration curves are prepared without factoring in intensity ratios, the calibration curve

coefficient values for lead, for example, will differ by 3 to 5 times. Using BG internal standard correction

compensates to some degree for the difference in calibration curve coefficients, but even so, the

difference can be 1.2 to 2 times, depending on the element.

For that reason, these spectrometers allow switching between calibration curves prepared using standard

samples containing chlorine and not containing chlorine.


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2.Analytical Conditions

2. Analytical Conditions

2.1 Example of Setting Parameters

2.1.1 Example of Setting Parameters

As an example of how to set up parameters for analyzing hazardous elements, the EDX software includes

the following file.

Folder: c:\edx\user\grpqn\rohs_exGroup Name: [Quantitative] Plastic5Elem

2.2 Key Points for Setting Parameters

2.2.1 Overview

Refer to Section 4.2 in the main EDX unit instruction manual regarding calibration curve measurements

using standard samples. For plastic samples, commercially marketed 5-element standard samples for

EDX systems can be used as standard samples.

This section indicates some important points for preparing calibration curves using standard plastic

samples.


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[Example]

Element

Registration

Register Cd,Pb,Hg,Cr,Br in Periodic Table.

Also register Cl,Sb.

Element

Information

“Quant.” – Calibration Curve For Cd,Pb,Hg,Cr,Br

“Correct” For Cl,Sb

Change Line to La. For Pb

Change Unit to ppm. For Cd,Pb,Hg,Cr,Br

Voltage Meas. Time (sec) Filter (*1) DT%(*2)

Cd 50kV 100 MoNi 40

Sb 50kV 100 MoNi 40

Pb 50kV 100 Ag 40

Hg 50kV 100 Ag 40

Br 50kV 100 Ag 40

Cl 50kV 100 Ag 40

Measurement

Condition

( For EDX-720 )

Cr 30kV 100 Al 40

Smoothing BG Calculation

No. of Points Repeat

Times

Repeat Times Calculation

Points

Cd 11 1 100 20

Sb 11 1 100 20

Pb 11 1 100 5

Hg 11 1 100 5

Br 11 1 100 5

Cl 5 1 100 5

Process for

Spectra

Cr 11 1 100 5

Internal Standard

Correction

With internal standard correction For Cd,Pb,Hg,Cr,Br,Cl

Without internal standard correction For Sb

Calibration

Curve

Multiple calibration curve -- Set “Co-Exist” mode with Cl.

For Pb,Hg,Br,Cr

Result Format Digit -- Set “Place of Decimal” to 1. For Cd,Pb,Hg,Br,Cr

(*1) For EDX-700HS/800HS, use Mo filter instead of MoNi filter. Use Ni filter instead of

Ag filter. For EDX-900HS, use Zr filter instead of a MoNi filter. Use Ni filter instead of

Ag filter.

(*2) For EDX-700HS/800HS spectrometers, set DT% to 25. For EDX-900HS, set DT% to

10.


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2.2.2 Element Registration

Register Cd, Pb, Hg, Cr and Br via the periodic table. In addition, register Cl and Sb as elements for

correction.


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2.2.3 Element In formation

For Cd, enter the following element information.

0û Proc. – Calc. Quant.

0û Type of Quantification Calibration Curve

0û Unit ppm

Enter settings for Pb, Hg, Cr and Br in the same way. However, in the case of Pb, also change the line to

“La”.

For Cl and Sb, enter the following element information.

0û Proc. – Calc. Correct


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2.2.4 Measurement Condi tions

For Cd, enter the following measurement conditions.

Voltage : 50 kV

Current : Auto

Filter(*1) : MoNi

Integration Time : Live Time and 100 sec

DT%(*2) : 40

Intensity Calculation : Fitting

Analysis Range (keV) : 22.72 – 23.52


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Similarly, use the following table to enter settings for the other elements. Regarding other parameters, set

Current to “Auto” for all of the elements, and Intensity Calculation Method to “Fitting”. The initial

voltage setting for Cl is 15 kV. In this case, change it to 50 kV to allow simultaneous measurement with

Pb, Hg and Br.

Voltage Meas.Time (sec) Analysis Range(keV) Filter(*1) DT%(*2)

Cd 50kV LiveTime 100 22.72-23.52 MoNi 40

Sb 50kV LiveTime 100 25.88-26.68 MoNi 40

Pb 50kV LiveTime 100 10.32-10.82 Ag 40

Hg 50kV LiveTime 100 9.74-10.24 Ag 40

Br 50kV LiveTime 100 11.66-12.16 Ag 40

Cl 50kV LiveTime 100 2.42-2.82 Ag 40

Cr 30kV LiveTime 100 5.12-5.62 Al 40

(*1) For EDX-700HS/800HS, use Mo filter instead of MoNi filter. Use Ni filter instead of

Ag filter. For EDX-900HS, use Zr filter instead of a MoNi filter. Use Ni filter instead of

Ag filter.

(*2) For EDX-700HS/800HS spectrometers, set DT% to 25. For EDX-900HS, set DT% to

10.


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2.2.5 Process For Spectra

For Cd, enter the following peak integration settings.

Smoothing Number of Points : 11

Repeat Times : 1

Method: Savitzky-Golay

BG Calculation Repeat Times : 100

Calculation Points : 20

Similarly, use the following table to enter settings for the other elements.

Smoothing BG Calculation

No. of Points Repeat Times Repeat Times Calculation Points

Cd 11 1 100 20

Sb 11 1 100 20

Pb 11 1 100 5

Hg 11 1 100 5

Br 11 1 100 5

Cl 5 1 100 5

Cr 11 1 100 5


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2.2.6 Internal Standard Correction

For Cd, enter the following internal standard correction settings.

Correction : On

Internal Std. Line : CdKa_BG

Similarly, enter the internal standard settings for Pb, Hg, Br, Cr and Cl. However, do not enter internal

standard settings for Sb.


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2.2.7 Result Format

For Cd, enter the following format settings for the number of digits to display.

Place of Decimal 1

Similarly, enter the result format settings for Pb, Hg, Br and Cr.


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2.2.8 Standard Sample Regist ration

Register standard sample names via “Standard Sample Name” window.

Example: Using both standard PVC samples and standard PE samples.

Standard PVC Samples Standard PE Samples

PVC-1 PE-1

PVC-2 PE-2

PVC-3 PE-3

PVC-4 PE-4

PVC-5 PE-5

PVC-6 PE-6


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Next, enter standard values via “Standard Value Input” window.

After entering the values, close the window by clicking [OK]. Then click [Apply] in the Standard Sample

window to confirm the settings.

Once all the necessary settings have been entered, save the current parameters via the “File” menu in the

Group Condition window, then close the Group Condition window.


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2.2.9 Standard Sample Measurements

Next, measure x-ray intensities of the standard samples.

From the Sample Schedule in the Analysis window, open the Sample Registration window and select the

group file just created. Select “Standard” from “Purpose of Measurement” field. Then the standard

samples registered appear automatically in the Sample Name fields.

Click [Apply] to register the standard samples in the Sample Schedule. Place the first standard sample in

the instrument. Then click [Start] button in the Analysis window to start measurement.

After the first sample has been measured, the sample chamber will open automatically. After exchanging

samples, click the [Start] button to resume measurement.


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2.2.10 Calibration Curve Preparation

Open the group condition after the standard sample measurements finished.

Open Calibration Curve window to calculate calibration curve coefficient. Click [Calculate] to calculate

coefficient and click [Apply] to save the result.


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If standard samples of both PVC and PE are measured, it is possible to switch automatically between

calibration curves calculated with and without chlorine. An example for Pb is shown below.

Set parameters as follows.

a) Click [Multiple Calibration Curve] to open “Multiple Calibration Curve” window.

b) Choose [Co-Exist] as “Use for ”.c) Select Cl from the list of choice displayed.

d) Set “ Number of Curves” to 2.

e) Enter 2.0 in the “Boundary” field.

Once the settings have been entered, click [OK].

Now that settings are configured for multiple calibration curves, back in the Calibration Curve window, a

choice of 1 or 2 is available in the “Curve No.” field.


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Select calibration curve number 1 and click [Calculate]. This will calculate a calibration curve using

standard sample Cl intensities ratio that are below 2.0. In other words, this calculates the calibration

curve for the standard PE sample.

Next, select calibration curve number 2 and click [Calculate]. This will calculate a calibration curve using

standard sample Cl intensities (ratio) that are 2.0 or higher. In other words, this calculates thecalibration curve for the standard PVC sample.

Once both calibration curves are calculated, click [Apply] to save the results.


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Settings for Pb, Hg, Br and Cr are also configured for automatic switching between calibration curves.

For Cd, the difference between coefficients for PVC and PE is not large, so the process of configuring

automatic switching between calibration curves may be skipped.


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3. Controlling Precision


3.1 Drift Check Analysis

3.1.1 Analyzing Control Sample

It is possible to determine whether an instrument is working normally or not by analyzing control samples

and confirming whether the quantitative values are within their respective control ranges.

Normally, of the standard samples used to prepare calibration curves, the sample with the highest

concentration is analyzed and the quantitative values are checked to determine whether they are within

the control range.

The control range is determined as approximately three times the standard deviation for repeated

measurements of a control sample or approximately three times the standard deviation indicated in the

quantitative results for a single measurement.

Make sure the energy calibration has been done before analyzing control samples.

3.1.2 Results Outside the Control Range

There is a possibility that x-ray intensity changes due to changes in the instrument over time or due to

other reasons.

If energy calibration is normal and values of control sample analysis are outside the control range, x-ray

intensity values can be corrected using drift standardization.


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3.2 Drift Standardization

3.2.1 What is Drift Standardization?

The intensity of standardization samples are measured and registered in advance. Then, if the control

sample analysis results in values outside the control range, re-measure the intensity of the standardization

sample. Any change in intensity can be corrected by multiplying the ratio of reference intensity to the

current intensity of the standardization sample. This is referred to as drift standardization.

3.2.2 Registration of Reference Intensities for Standardization Samples

Register standardization samples to the group condition used to create calibration curve.

Open “Standardization Sample” tab of “Standardization” window to register standardization samples.


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Next, open “Drift Coefficient” tab and turn drift standardization on by checking the checkbox to the left

of each element name. Also, set “alpha-Control Range” to 0.8 to 1.2. If low concentration standardization

samples will also be analyzed, set “ beta-Control Range” to -1.0 to 1.0.

Once the settings have been entered, click [OK] to close “Standardization” window. Then save the group

condition via the File menu.


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The intensity of standardization samples is registered via the Analysis window, in the same manner as for

standard sample measurements.

From “Sample Schedule” in the Analysis window, open “Sample Registration” window and select the

group condition that was just saved. Then select “Drift Standardization” and “Intensity Registration” from

“Purpose of Measurement” section. This will cause the standardization samples, registered when

parameters were entered, to appear automatically in the sample name fields.

Click [Apply] to register the standardization samples in the Sample Schedule. Place the first

standardization sample in the instrument. Then click [Start] button in the Analysis window to start

measurement.


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The measured intensities are automatically registered in the original group condition. The intensities can

be confirmed via “Standardization Sample” tab in “Standardization” window.


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The drift coefficient is calculated automatically after the measurement is finished and displayed on

“Result Display” window. These results are automatically saved into the original group condition only if

the drift coefficient is within the control range.

3.2.4 Drif t Coeffici ent Criteria

If the alpha drift coefficient is not between 0.8 and 1.2, new calibration curves need to be prepared. Refer

to Sections 2.2.8 “Standard Sample Registration” through 2.2.10 “Calibration Curve Preparation”

regarding preparing calibration curves.


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3.3 Measurement Time Reduction

3.3.1 Measurement Time Reduct ion

Generally you need longer measurement times for measuring trace elements, but if target elements are

present in larger quantities they can be detected with shorter measurement times.

If you set the allowable relative error of intensity in “Measurement Condition”, program can reduce

measurement time adequately. These settings are only applicable for quantitative analysis.

Given relative error (CV) = std. dev. of x-ray intensity / x-ray intensity x 100, there is an approximately

99% probability that the true value for the x-ray intensity is within the range ±(x-ray intensity x relative

error x 3.0).


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4. Interpreting Data and Making Determination


4.1 The Possibility of Determination Errors

4.1.1 Determination Errors Due to Overlapping Spectra

Depending on the sample composition, peaks for other elements can appear near the target peaks, making

it difficult to interpret results.

Overlapping peaks that might appear for the five elements Cd, Pb, Hg, Cr and Br, are listed below. In the

case of overlapping peaks, the accuracy of quantitative values could suffer if measuring trace quantities.

Cd When Pb is present in large quantities (PbSUM)

PbLa When As is present (AsKa)

When Bi is present (BiLa)

Hg When Ge is present (GeKa)

When Zn is present in large quantities (ZnKb)

When Br is present in large quantities (BrKaESC)

When W is present (W Lb2)

BrKa When Hg is present (HgLb1)

Cr When Cl is present in large quantities (ClSUM)

When Fe is present in large quantities (FeKbESC)

When Ba is present (BaLb2,BaLg1)

When V is present (V Kb)

When Ni is present in large quantities (NiKaESC)

When Co is present in large quantities (CoKaESC)

PbLb1 When Bi is present (BiLb1)

When Br is present (BrKb)

When Se is present (SeKb)

When Fe is present in large quantities (FeKaSUM)

BrKb When Pb is present in large quantities (PbLb5)

When Au is present in large quantities (AuLg1)


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4.1.2 Determination Errors Due to Diff racted Lines

In general, when a sample is irradiated with x-rays, in addition to fluorescent x-rays, scattered incident

x-rays are also observed. With some samples, the scattered x-ray intensity increases significantly at

specific energies by X-ray diffraction.

For EDX series spectrometers, these diffraction lines are observed at the following energies.

Note, this diffraction phenomenon only occurs when the angle between the crystal face and x-ray tube

and the angle between the crystal face and detector are the same. However, crystal faces are oriented in

multiple directions and samples are generally not single crystals, so it is not possible to accurately predict

which crystal faces will generate intense diffraction line emissions.

Diffraction lines observed with EDX series have the following properties.

a) They mainly appear between 3 keV and 15 keV.

b) The line widths are often about the same or wider than x-ray fluorescence peaks.

c) The diffraction pattern may change if the sample orientation or tilt angle is changed.

d) They are rarely observed in plastic samples. Tiny diffraction lines appear in metal samples.

e) They become lower when you use x-ray filter.

Currently program cannot determine automatically whether detected peaks are fluorescent x-ray lines or

diffraction lines. Therefore, be aware that the program treats diffraction lines as though they were peaks

from fluorescent x-rays, so peaks could be misidentified as other elements.

In some cases, using a primary x-ray filter for measurements can reduce the diffraction lines more than

peaks from fluorescent x-rays. If in doubt regarding whether a peak is a diffraction line or not, measure

the sample using a filter and compare the results to not using the filter.

Currently, the following cases have been reported.

Fe-based samples – Tiny peaks near 10 keV may appear to be Hg peaks.

Ag-based samples – Tiny peaks near 5.4 keV may appear to be Cr peaks.

Sn-based samples –

Tiny peaks near 5.4 keV may appear to be Cr peaks.

E: Energy of Diffracted X-ray (keV)

n: Order(1,2,3, … )

d: Crystal Face Distance in Sample (A)


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4.2 ExReport Function

4.2.1 ExReport Funct ion

The quantitative value determination results can be summarized in a one-page report. For more

information regarding report creation features (ExReport), refer to the separate instruction manual of

ExReport.


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5. Hints for Configuring Conditions

5. Hints for Configur ing Conditions

Temporarily swi tching o ff measurement of specific elements

[Method 1] Uncheck “Do Analysis” in “Element Information” window of “Condition” program.

[Method 2] Uncheck the checkbox to the left of “Analyte” in “Change Measuring Time” window of

“Analysis” program..


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Changing the name of standard samples

1. Select standard sample name to be changed in “Standard Sample” window of “Condition”

program.

2. Manually input a different name in “Standard Sample” field. And click any other location in the

window.


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Measurement for only specific standard samples

[Method 1] Delete the samples not to be measured in “Sample Registration” window.

[Method 2] Measure the sample as an “Unknown” sample and load the standard sample intensities by

clicking [Read Intensity from Data] in “Standard Sample” window. Then reenter standard

values as necessary.


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Deciding when to use BG internal s tandard correction and when not to use correction

Regular calibration curve methods are recommended for samples with low scattered x-ray intensities

(metal samples). Regular calibration curves are also recommended if samples are measured using a

smaller collimator.

Measuring metals using plastic standard samples

The calibration curve coefficients for metals and plastics differ significantly, so calculated

quantitative values would be unreliable.

Negative quantitative values

When measuring samples with concentrations near or below the lower detection limit, the variance of

x-ray intensity can result in negative quantitative values being displayed. This does not indicate a

problem with the instrument or software.

Whether to use La or Lb1 analytical lines for Pb analysis

In the case of plastic samples, the La line is preferred in order to prevent overlapping by Br.

(However, it is possible Pb could be incorrectly detected if the sample contains As.)

If using model EDX-720 to measure the Pb content in brass samples, the absorption by copper is less

for Lb1, so sensitivity will be higher with Lb1.

Documents

Manual EDX 700 Shimadzu