Training XL3t 955 Ultra series

2018 - 06 - 27
FIELD & SAFETY INSTRUMENTS
THERMO FISHER SCIENTIFIC XRF NITON

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Content

• Theory
• Knowing your instrument – XL3t 955 series
• Interface and software
• NDTr and Download data NDT
• Interferences and Sample prep
• Cal Factory and modes available
• Considerations and effects of XRF
• Empirical Calibration
• Type Standardization
• Cal Factors
• Download data

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Theory - Analytical techniques

Analytical Systems and

why XRF

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OES Optical Emision Espectroscopy

Advantages of OES

•Fast, robust, precise, stable and

reliable technology
•Simplicity: Easy sample preparation
•Savings: Low capital investment and
operating costs
•Range: From trace (sub-ppm) to alloy
concentration levels
•Extremely fast and simple quantitative
determination of all the elements
needed (note: this is normally used for
X-Ray) in pure metals and alloys in < 1
minute
•Unmatched technique for fast analysis
of C, N, O, P and S in steel
•Ultra-fast analysis of non-metallic
inclusions

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ICP Mass Espectroscopy

ICP-MS is becoming a
workhorse for metal analysis in
water not only because it offers
lower detection limit. The
following features also
contribute its wide range of
geological applications:

•Wide dynamic range

•Efficiently remove polyatomic
spectral interferences using
collision cell technology
•Rapid semi-quantitative
analysis
•Isotopic analysis

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X-Ray Fluorescence

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How does it works

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X- Ray Fluorescence

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 Silicon Drift
Detectors (SDDs)
Residual elements can be
measured with a confidence once only
possible in the lab. SDD’s are also required
to analyze light elements such as
Magnesium (Mg), Aluminium (Al), Silicon
(Si), Phosphorus (P) and Sulfur (S).

PIN Detectors
measure the fluorescence radiation emitted
from the sample after it has been irradiated,
usually by an x-ray tube (occasionally by a
radioactive source). Instruments with Silicon
PIN detectors are sensitive to X-rays that
are higher on the periodic table than Sulfur
(S) and tend to be less expensive than
instruments with Silicon Drift Detectors.

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Knowing your instrument – XL3t 955 series

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 Opening your case

Quick Start guide Soil Sample

reference

USB Cable
NITON XL3t 955
Analyzer
Software
Installation
Belt Holster
Analyzer
Case Lock
Battery Charger

Battery
Battery Charger
Power Supply
Battery Holster

Padlock case

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Accessories and consumables

Soil Cups

Portable Test Stand

Prolene film

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XL3t 955 Ultra Analyzer

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Replacing the Measurement Window

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Battery Charger

1. Read indicates that there is not battery on charger

2. The yellow light indicates that the battery pack is currently being charged
3. The green light indicates that the battery pack has finished charging and
the battery is ready to be used
4. If there is a fully seated battery pack in the charger and only the red light is
on, there is a fault with the battery pack charger

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Interface and software Start up procedure

To turn on the analyzer, depress the On/off/escape button on the control panel until
the Touch Screen comes on.

On startup, the screen will show by a Start Screen which will automatically count
down from 4 to 0 in increments of one second.

When the start up is complete, the Start Screen will be replaced by the Logon
Screen. Tap anywhere on this screen to continue.

Select your 4 digit security

code, followed by the Enter
button. The default
password is 1-2-3-4

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Start up procedure

After you have completed the log on

procedure, the word "USER" will appear on
the bottom of the screen, then the Main
Menu will appear. Note that security codes
are editable. This will be covered in
‘advanced settings’. There we can change
passwords and set User Privileges.

Please Note - Your analyser will need to set the temperature of

the detector to -25ºC before it can be used. If you attempt to use
the analyser before this procedure the instrument will display the
warning ‘Please wait, cooling detector’. This procedure will take
no longer than 60 seconds once logged in and will remain stable
until the analyser is powered down.

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System check

Every XL2 analyser will have the ‘system check’ function.

This function is an internal check to maintain the instruments
fundamental parameters calibration, check tube output and
detector resolution.

This is an important operation to perform as over time the

instruments detector can suffer from electronic drift slightly
shifting the calibration curve.

Running the ‘system check’ can keep the instruments

calibration curve in line which will continue to provide the
best possible results from the analyser.

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System check

Select the System Check Once the system check starts

Icon on the Main Menu to you will hear the shutter close
perform a system check. We on the instrument. This has
recommend that you perform sealed the X-rays from leaving
a system check once every the front of the instrument.
working day, as part of your
normal start up procedure. You will notice that the
warning lights have
illuminated indicating the X-
Ray tube is generating X-
Rays.

Click yes to continue the

system check. Once the test is finished you
Please make sure at this time will see this screen. Click
there is nothing on the front close.
of the instrument that could
affect the reading. If however there is an error
message we advice you to call
to your local distributor
Thermo Fisher Scientific.

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Analyze mode

From the main

menu select
analyze to go in to
the testing mode for
the instrument.
From this mode you
will be able to
perform various
tasks including
taking an analysis
and viewing the
result.

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Tools menu

The Tools Menu enables you to perform common data-related

tasks such as printing and averaging readings. Select a task
from the menu to initiate that task. The options available can
vary depending on the selected mode.

Once you select

tools at the bottom
of the screen you
will be displayed
this screen on the
right. The various
options are
explained next.

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Live Spectrum

The Tools Menu contains a toggle

option to display live spectra as
sample analysis occurs.

To activate and Deactivate the

Live Spectrum from the Tools
Menu, select the Spectra:On
button to turn the Spectrum feed
on. Once the spectrum is
displayed, selecting Spectra:Off
from the Tools Menu will stop the
live spectrum display.

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Element Range

The XL2’s have two filters which can be found in the element range. Here
you can decide whether to enable/disable the Light/Low range. You can also
set the time for each filter/range to test for. Light Range will need to be at
least 30 seconds to measure the light elements accurately. Auto Switch on
time only will decide whether or not to change the fitler. If unticked, the
library will decide. If ticked, the analyser will change filters after each time
frame has expired.

Important!
Each filter
range looks
for different
elements to
excite

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Set Pass/Fail

You can set up your analyser to sort on a pass/fail basis. Pass/Fail uses the
chemistry of a user-generated list of alloys in the library as a basis for comparison. If
the sample analysis is entirely within the specifications for one of these alloys, a
PASS result is given, otherwise a FAIL result is returned.

To initiate Metals Pass/Fail, select the Metals Pass/Fail icon from the Metals
Screen. Your analyser will go into the Ready to Test Screen. To set up Metals
Pass/Fail, select the Tools Menu and select Set Pass/Fail from the menu. The
Pass/Fail Setup Screen will come up.

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Set Pass/Fail (cont)

Select alloys from the Available list and then

the Add Button to move the alloy to the
Selected List. Select alloys from the
Selected list and then the Remove Button to
remove the alloys from the Selected List.
Select the Save Button to save these criteria.

Once a test is To view the

performed the analysis of the
analyser will test simply press
give you two the magnifying
options. Either glass icon.
pass or fail.

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Data Management

Viewing Data

Use the Data Screen to view

previously taken test result
readings. When the View Data
icon is selected, the Results
screen of your most recent test
is shown on the Touch Screen.

Using the buttons on the control panel, you may view different readings or
additional data for individual readings. Your analyser will display the standard
screen analysis. Pressing the Down Button on the 4-way touch pad will
display a complete scrolling elemental chemistry listing. Each press of the
Down Button scrolls the screen down to the next element. You can also use
the scroll bar along the right side to scroll or page through the elements.
Pressing the Left Button on the 4-way touch pad of your analyser will display the
previous reading. Your analyser can store up to 10,000 readings.

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Erasing Data and Readings

Select the’ Data’ and then ‘Erase’ on the analyser. You now have three options;

1 Erase All Data; this will erase all readings and all fingerprints.
2 Erase All Readings; this will erase only the readings taken on the instrument.
3 Erase Fingerprints; this will erase all fingerprints stored on the analyser.
Caution: Never turn off the analyser while data is being erased!

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Managing Libraries

Select the ‘Manage Libraries’ icon to access the Library Management Menu.
The Library Management Menu allows you to view and modify data in the
Primary Library as well as the currently loaded alternate libraries. Just select
the library you wish to view or edit from the list on screen.

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Safety Settings

Access to the Safety Settings Screen is blocked unless the user logging in has
explicitly been granted Safety access. The default login of 1234 does not have
Safety access. See ‘Creating Passwords’.

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Pseudoelements

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Safety Settings

The Safety Settings Screen enables you to change the Method of Operation for your
analyser. Each checkbox on the screen enables or disables the safety device named
for purposes of the preconditions for operation. For example, checking the Proximity
Button Required checkbox sets the engagement of the Proximity Sensor as a
precondition for operation. Checking the Proximity Button Required checkbox and
the Interlock Button Required checkbox sets the engagement of both the Proximity
Button and the Interlock Button as preconditions for operation.

Safety settings always override start-stop settings. If your safety setting requires the
use of the Proximity Button, you cannot set start-stop settings which ignore the
Proximity Button. For example, the Easy Trigger start-stop setting must have the
Backscatter safety setting enabled. While using Easy Trigger, you cannot disable
Backscatter.

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Safety Settings

Warning! The backscatter sensor is enabled by default and acts as a

recommended safety feature for most applications. Some sample types, however,
cannot be analysed when this feature is enabled. Samples that present very little
mass to the analysis window, such as certain thin films, thin layers of plastic, and
very thin wires, may not be of sufficient mass to allow the analysis to continue
while backscatter is enabled. One should disable the backscatter feature only
when necessary to analyze such low mass samples, and re-enable the feature
when finished with these sample types. These samples also provide very little
absorption of the primary x-ray beam so it is typically most appropriate to analyze
these samples in a test stand when possible.

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Start/Stop Setup

The Start/Stop Setting Screen enables you to change the preconditions for operation
at a lower level than the Safety level. See Safety Settings for more information.
Start/Stop settings cannot contradict Safety settings. If your safety setting requires
the use of the Proximity Button, you cannot set start-stop settings which ignore the
Proximity Button. For example, the Easy Trigger start-stop setting must have the
Backscatter safety setting enabled. While using Easy Trigger, you cannot disable
Backscatter.

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Start/Stop Setup

The Start/Stop parameter options are Proximity Start, Remote Trigger, and Easy
Trigger. There is also a field to set the maximum time for sample analysis before the
analysis stops.

Proximity Start

Select the Proximity Start checkbox to use the Proximity Start parameters. Using
Proximity Start, once the reading has been started, release of the Proximity Button
will immediately stop the analysis. You cannot use Proximity Start with Easy Trigger.

Remote Trigger

Select the Remote Trigger checkbox to use the Remote Trigger parameters.
Remote Trigger is used with the Extend-a-Pole accessory to control the analysis.
With the Extend-a-Pole's input cable connected to the analyser's Remote Trigger
port, you can initiate and stop analysis remotely from the Extend-a-Pole's handle
trigger. You can use Remote Trigger with either Proximity Start or with Easy Trigger.

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Start/Stop Setup

Easy Trigger

Select the Easy Trigger checkbox to use the Easy Trigger parameters. Easy Trigger
uses a single press and release of the trigger to initiate analysis, and a second
press to stop analysis. Selecting Easy Trigger will immediately disable Proximity
Start.
Select the Max Time field to change the maximum analysis
Max Time Field
time parameter. Selecting the Max Time Field brings up a
Virtual Numeric Keypad. To input the maximum number of
seconds before automatic shutoff, select the C button to clear
the current time, then from the Virtual Numeric Keypad, select
each digit you want to input, then select the E button to enter.
Of the non-numeric screen buttons, C = Clear All, E = Enter,
and “<" will backspace over the current value. Selecting the E
button will enter the current value as the Max Time, and return
to the Start/Stop Settings Screen.

Selecting the Save Button will save your current settings.

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Changing Precision

Sigma is the symbol used for Standard Deviation, a measure of how much a set
of numbers deviates from the mean. For example, each of the three data sets
{0, 0, 14, and 14}, {0, 6, 8, and 14} and {6, 6, 8, 8} has a mean of 7. Their
standard deviations are 7, 5, and 1, respectively. The third set has a much
smaller standard deviation than the other two because its values are all close to
7. In a loose sense, the standard deviation tells us how far from the mean the
data points tend to be.

The number of standard deviations between the process mean and the nearest
specification limit is given in sigmas. As process standard deviation goes up, or
the mean of the process moves away from the center of the tolerance, the sigma
number goes down, because fewer standard deviations will then fit between the
mean and the nearest specification limit.

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Changing Precision

Confidence Intervals
Confidence intervals assume that the data are from an approximately normally
distributed population - generally, sums of many independent, identically distributed
random variables tend towards the normal distribution as a limit. Using this
assumption, about 68 % of the values must be within 1 standard deviation of the
mean, about 95 % of the values must be within two standard deviations, about 99.7
% must lie within 3 standard deviations, and about 99.99% of the values must lie
within 4 standard deviations.
The greater the sigma value of the test, the more confident you can be that the
sample is as it appears, but the more difficult and time consuming the testing must
be to verify this. That's why it's important to use the most appropriate sigma value
for the test. By adjusting the sigma value for each type of test, you can optimize the
process for your needs.

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Changing Precision

Adjusting the Sigma Values

The sigma values When you have

are listed in the changed the
column headed s. sigma values to
The default value is the appropriate
2 sigma. You can number, select
change this value the Save button
by selecting the to save these
down arrow next to settings for use.
the value, which Select the Close
opens up a drop- button to return
down menu from to the previous
which you can screen without
select the desired saving any
sigma value by changes.
clicking on it.

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Sorting the Element Display

Select the Sort

Element Display .
icon to configure
sorting criteria
used for
analysis display.
Selecting the
Sort Element
Display icon
opens up the
Sort Criteria
Screen.

Select the mode you wish to change, and the Sorting Options Screen will
appear (next slide).

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Sorting the Element Display

On the left of the

display are elements,
each with its currently .
selected display option
beside it to the right.
The element list is
ranked by importance,
with the most important
element on top, and
each one lower down of
less importance than
the one above it.

By selecting an element and using the arrow buttons to the right of the list, you can
change its ranking. Use the Top Arrow Button to move an element one rank closer to
the top with each click. Use the Bottom Arrow Button to move an element one rank
closer to the bottom with each click.

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Sorting the Element Display

Display Options
The Display Options Drop Down Menu, allows you to change the display status
.
of any element to one of three states:

• Normal - The standard state. Element displays only when the elemental value
is greater than the limit of detection.

• Always - Always display the results for this element. Use this state for
elements critical to all of your analyses.

• Never - Never display the results for this element. Use this state for
elements which are unimportant to your work. This makes your instrument
display less complex.

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Sorting the Element Display

Select the element you

Select the Save Button
want to change, then
to save your current
select the menu option
status as the new
corresponding to your
default. After saving,
choice of display status.
you will go back to the
The currently selected
Element Display
element is displayed in
Menu.
white on black.

Select the Close Button to exit without saving. When you select the Close Button
after changing the display state of any element, a screen will open asking you if you
want to save the changes you made. Selecting the Yes Button will save these
changes as the new default. Selecting the No Button will return you to the Element
Display Menu without saving the changes.

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NDTr and Download data NDT - Installing NDT

1. Close all the programs that you have open on your PC.
2. Insert the CD into the CD-ROM drive.
If the installation program starts automatically, follow the instructions on the
screen. If the installation program does not start, go to the next step.
3. Double-click My Computer.
4. Double-click the Compact Disc icon:
5. Double-click the Setup Application icon.
6. Follow the instructions on the screen.

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Starting NDT Software

1. Click the Start button.

2. Select Programs.

3. Select Thermo Niton.

4. Click NDT.

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Connecting the XRF Analyser to Your PC

There are three ways to connect the XRF Analyser to your computer:

The serial cable;

1. Insert the DB9 connector on the serial cable into the COM port on your computer.
2. Tighten the screws of the DB9 connector with your fingers. You do not need to
use a screwdriver.
3. Open the Port Cover on the XRF Analyser
4. Insert the micro stereo connector on the serial cable into the Serial port in the
handle of the XRF Analyser.

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Connecting the XRF Analyser to Your PC

The USB cable

1. Insert the NDT CD and close out any dialogue box that
pops up. The driver is located on this disk.

2. Click on
“Control Panel”
and locate the
“Device
Manager”. If it is 3. Open “Device Manager”
not available
direct under
“Control Panel”, 4. Plug in instrument using the USB cable
look under provided
“System and
Security” then
5. Message will appear “Device Driver
“System”.
Software Not Successfully Installed”

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Connecting the XRF Analyser to Your PC (cont)

6. In “Device Manager”,
“Unknown Device” will appear
under “Other Devices”

7. Right click on “Unknown

Devices”; select “Update Driver
Software”

8. Click on “Browse My
Computer for Driver Software”

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Connecting the XRF Analyser to Your PC

9. Click “Browse” button; select CD drive or

the location of the driver if you are not
installing from the NDT CD (recommended).
10. Click “OK”
11. Click “Next”
12. A Security Dialog Box will appear. Select
“Install This Driver Software Anyway?”
13. Driver will install; close out.
14. Insert the Standard USB connector on the
USB cable into a USB port on your computer.

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Connecting the XRF Analyser to Your PC

15. Open
the Port
Cover on the
XRF
Analyser.

16. Turn on
the analyser
and insert the
mini USB
connector on
the USB cable
into the USB
port in the
handle of the
XRF Analyser.

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Interferences and Sample prep

Bauxite samples were first ground to particle size below 200 µm and dried, and then
annealed at 1075 ° C. The loss on ignition was calculated at that temperature.

Pressed poder method Cell / Soil cups

Pressed pellets are prepared by pressing loose powders Cell used where loose powder sample is supprted
filled in a ring or cup using a set of dies and press between a sample film attached to the sample cell and
machine. To prepared pressed beads, 47.5 g of the semi permeable microporous filter. The simple cells are
annealed sample should be separated and mixed with 2.5 reusable when thoroughly cleaned.
g of wax and ground in a mill. The sample (10 g) prepared
in this way was then transferred to the mould in the press
and subjected to a pressure of 150 KN for 10 seconds

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Sample prep

bauxite samples are sieved until the required

sample size is obtained. The sample size required
for Element Al readings is 75 um / 200 mesh

Samples that have obtained size are

as per Al (75um)

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Sample prep

Cup samples are prepared in such a way, with

coated mylar plastic on one side

Bauxite sample is inserted into the sample Cup

little by little until it covers the surface of mylar
plastic

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Sample prep

Cover the top side with paper, so that the sample

does not scatter

Paper covered sample

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Sample prep

Get in with Poly Stuffing,

The sample is closed with a sample cup lid,

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Sample prep

Samples ready to be shot. Repeat the steps above

for the next sample

In an experiment to increase the level of precision and accuracy in this tool, the experiment carried
out several stages of firing on these samples including

1. Trial shooting

2. to make a Calfactor series

3. Shooting to test the results of Calfactor

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 Prepare the equipment used in this test, including the Test
stand, Niton Xl3t 955 Ultra, USB cabel, and computer. All
equipment is connected and in a state ready to use

Open the top of the test stand then the sample is placed in
it right in the hole on the muzzle of the XRF ray

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 Close again

One of the functions of a standard test is to protect the

analysis from X-ray radiation released by the instrument

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 The picture on the side is a display of the monitor screen
on the computer, this shows between the device and the
computer has been connected and the device is ready to
be operated by computer.

The value of the results of the sample shooting is directly

visible on the computer monitor screen.

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 Take the sample back in the stand test, then replace it with
the next sample. For the experimental phase of the
Shooting trial, Shooting to make a Calfactor series and
Shooting to test the results of the Calfactor carried out the
same plot of experiment shooting.

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Cal Factory

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Modes available

Fundamental Parameters (FP)

Parts per million (ppm) to high percent levels

Compton Normalization (CN)

Soil samples that contain less than 5% of all
elements Z > 23 (summing them together)

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Factory Calibration

Fundamental Parameters (FP) Fundamental Parameters (FP)

Parts per million Parts per million
(ppm) to high percent levels (ppm) to high percent levels

Compton Normalization (CN)

Soil samples that contain
less than 5% of all elements Z
> 23 (summing
them together)

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Considerations and effects of XRF

Spectral Effects

Some elements have lines that overlap other elements. Fortunately the software will strip out
and correct most of these overlaps (as long as the interfering element is in the mode being
used), but limits of detection may be worse when 2 overlapping elements are present.

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Effects of XRF

Matrix Effects
The matrix is any other element present in or on the sample other than the 1 element being
considered.
Enhancement and absorption effects are typically taken care of in the software if you are
using a fundamental parameters based calibration with all the necessary elements present.

• Enhancement Effects
Some fluorescent x-rays have more energy than the binding energy of other elements present in the sample, and so their
energy will excite those other elements. These elements will give a greater signal return to the detector, i.e. “enhancing” the
reading.

• Absorption Effects
The fluorescent x-ray does not reach the detector as it is scattered or absorbed by other elements
present in the sample, so the signal is weaker.

• Sample Effects
The surface of the material being analyzed is not representative of the entire sample (particle size,
inhomogeneity, surface contamination, etc.). XRF is a surface analysis technique, so inhomogeneity
or contamination will skew the results.

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Effects of XRF

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Effects of XRF

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Effects of XRF
There is a high correlation between data from portable XRF and lab
methods in direct shoot analysis

Sample preparation significantly improves quality of data. For example,

correlation between Zn data from portableXRF and lab jumps from 72% in
the unprepared samples to 96% in the prepared samples.

Although portable XRF provides reliable and consistent data, calibration

adjustment may beneeded to increase accuracy further.

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Empirical Cal

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Empirical Cal

Silicon Si Correlation
6.000 6.000
y = 1.6x + 0.029
5.000 5.000 R² = 0.9223
4.000
4.000
3.000
3.000
2.000

1.000 2.000

0.000 1.000
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
0.000
Si PRIMUS % Si NITON % 0.000 0.500 1.000 1.500 2.000 2.500 3.000 3.500 4.000

Aluminum Al Correlation
4.000 4.000
3.500 3.500 y = 2.4602x + 0.3771
R² = 0.9921
3.000
3.000
2.500
2.500
2.000
1.500 2.000
1.000 1.500
0.500 1.000
0.000
0.500
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
0.000
Al PRIMUS % Al NITON % 0.000 0.200 0.400 0.600 0.800 1.000 1.200 1.400

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Empirical Cal
Iron Fe Correlation
0.900 0.700
0.800 y = 0.8857x - 0.0829
0.600
0.700 R² = 0.9697
0.600 0.500
0.500
0.400 0.400
0.300 0.300
0.200
0.100 0.200
0.000 0.100
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
0.000
Fe PRIMUS % Fe NITON % 0.000 0.200 0.400 0.600 0.800 1.000

Calcium Ca Correlation
40.000 40.000
35.000 35.000 y = 1.1938x - 4.2906
30.000 R² = 0.9854
30.000
25.000
25.000
20.000
15.000 20.000
10.000 15.000
5.000 10.000
0.000
5.000
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
0.000
Ca PRIMUS % Ca NITON % 0.000 5.000 10.000 15.000 20.000 25.000 30.000 35.000 40.000

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Choosing the empyrical calibration method

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Type Standardization

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Type Standardization

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Choosing the empyrical calibration method

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Type Standardization

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CalFactors

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CalFactors
Make the graph to know the trend of the results and obtain the
correlation to identify the correspondence of the information
obtained with the analyzer XRF Niton Thermo Scientific

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CalFactors

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CalFactors

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Downloading Data

1. Make sure that the XRF Analyser is connected to your computer.

2. Turn on the XRF Analyser.

Note - Wait at least 30 seconds after turning on the XRF Analyser
to begin downloading files. The System Start screens do not allow
downloading.
3. Start the Niton Data Transfer program (NDT) from your PC.

4. Click the Download button.

The Download dialog box will open.

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Downloading Data

5. In the Download dialog box, Select the Test button to test the serial
connection to the Analyser.
6. You should get a
pop-up window
informing you that the
connection tested
successfully.

If the test fails, there

is a problem with
your serial port
setup. Press
‘settings’ to set the
correct com port and
try again

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Downloading Data

7. In the Download dialog box, click the Connect button.

8. Click the
Query Readings
button. This will
return a list of all
current readings
on your analyser.
The list appears
in the large white
box in the
Download dialog
box.

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Downloading Data

9. Select the readings that you want to download. There are two ways to do this.

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Downloading Data

a. Click the boxes next to each of the

reading numbers to select or de-select
individual readings. You can select a range
of readings by pressing the shift key, then
selecting the first and last reading in the
range. All readings from the first reading
selected to the last will then be selected.

b. When the readings are downloaded,

the available modes are also downloaded.
Click the boxes on the left to select or de-
select all the readings of a specific
available type. You can also use the Shift-
Click method of selecting a range of
readings as described above.

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Downloading Data

10. The download generates a data file containing the selected readings. To
save the file for later use:

a. Enter the path for the file in the

Destination Folder field. You can use the ...
button to browse.

b. Enter a name for the file in the File

Name field.

Caution: - Some characters are not allowed in the file name. Characters
such as the "#" sign will cause an error. Niton recommends using only
alphanumeric characters "-", "_" and the space character when naming a
file.

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Downloading Data

When the progress bar shows that all the

c. Click the Download button. readings are downloaded, click the Done
button.

You should now see the readings you selected for download displayed, one reading
per horizontal line. The data has been saved to the folder and filename you
indicated prior to downloading.

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 Mining stages

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Layout Mining Process

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Exploration

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Prospecting

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Advance Exploration

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Interpretation Data

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Estimation of Reserves

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Development of a project

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Strengths and Limitations

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Components

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Thermo Scientific Niton XRF Instruments

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Guidelines

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 Knowed your devise

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 Using your
Niton XRF
Analyser

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 Opening your case

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 Inspecting your analyser

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 Inspecting your analyser

The control panel is located on the

analyser's top housing, directly below the
Touch Screen. The control panel consists
of a 4 Way Touch Pad, an Interlock Button,
and two Control Buttons, one on each side.
Using either the control panel or the touch
screen you may navigate through all of the
analyser's screens and menus. You can
control the movement of the screen cursor
by pressing the 4 Way Touch Pad in one of
four directions to highlight each of the
menu options. The Clear/Enter button to
the right of the 4 Way Touch Pad is used to
select highlighted menu options. The
On/Off/Escape Button both controls the
power to the analyser and serves as an
"escape" button. When the On/Off/Escape
Button is pushed and immediately
released, it functions as an "escape", and
brings you back to the Main Menu from the
current screen in the menu system.

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 Replacing the Measurement Window

Measurement Windows for Niton XL2 analysers can be

purchased from Thermo Fisher Scientific. Ask local
distributor for part number.

Remove the
backing from the
Measurement CAUTION! Do not use fingers to press
Window. Place the window into place! Use a smooth, hard
window on the surface such as back of tweezers.
Bracket gently.
Replace
Make sure the
Window
opaque portions of
Bracket on
the window do not
the front of
intrude over the
your analyser,
large
then insert
measurement hole
screws.
in the Bracket.

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 Testing prepared samples
with pXRF

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 Considerations for
applications on field

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 Strengths

X-Ray Fluorescence is:

• Non Destructive – No digestion
acids required
• Fast – Little sample preparation
required
• Portable - Get results at sample
location
• Quantitative from Mg to U with
New Large Area SDD Systems
• Multielemental Analysis

• Analytical accuracy In-Situ

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 Requirements

• Humans – the XRF user

• Training and experience

• Applying a methodology to an XRF
program
• Lack of global Standard Operating
Procedures (CAMIRO, AIG)
• XRF Supplier Training
• XRF Supplier Experience

• Analytical Experience

• Junior Geologist / Senior Geo

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 Keep in mind using Niton XRF Portable

• Limits of Detection (not sub

ppm)
• Results affected by variations in
matrix (geological chemistry).
Does the analyzer need
calibration in-Situ?
• Sample heterogeneity/sample
preparation required.
• Limited area XRF measurement
window is 1cm2
• XRF Spectrum e.g. overlaps
like Fe on Co, Zn on Au, etc.

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 Follow a procedure

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 • Work with people with successful experiences using XRF
• Training - understand XRF strengths and weaknesses
• Set some Aims and Objectives for the portable XRF
• Be clear about its role within the organisation
• Adopt robust and “fit for purpose” sampling and testing methodologies – they aren’t
that complicated
• Replicate some of the protocols you follow for samples you send to the laboratory
• Manage the data responsibly, as automated as you can make it

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 Powefull tool to take decisions on fiel

Field Sampling
• Rapid instantaneous results
• Cover large areas very quickly
• Ability to sample multiple
horizons
• Infill sample spacing “on the fly”
• Pre-Screen results to Lab
• Speed up decision making
timeframes
• GPS-GIS integration packages
enable real-time thematic
mapping via

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 Lets go and use the XRF
on field

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 What do we need to keep in mind testing on field
•Effectiveness of using pXRF:
•What Elements will Work?
•What Concentrations?
•What Detection Limits (LOD)?
•What is Anomalous?
•Is it homogeneous?
•Is it representative?
•Ensure you are comparing “Appropriate” assay techniques ie. Full vs. Partial Digests…!

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 Common field sample conditions

•Typically heterogeneous
robust samples

•Irregular surfaces

•Different particle sizes

•Humidity

•Density of the sample

•Matrix changes

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 Interpretation of pXRF on field

Factory calibrations are often done with (PF) or (CN) calculations

but even two models from the same manufacturer may not offer the
same results in samples with the same matrix. In theory, FP
calculations must be superior to influencing coefficients but in
practice they are destitute.

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 What we can expect?

• Effects of Matrix
• False positives
• Homogeneity
• Packing
• Response time

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 Tipically preparation samples on a Laboratory
The samples in a laboratory are subjected to processes under which it is possible to
obtain the highest quality of the results of the chemical elements present in the sample.

They are generally subjected to processes of; Crushing, Spraying, Preparation of

glasses or beads, Preparation of Pills, Acid Digestion

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 Interpretation of results
There is a high correlation between data from portable XRF and lab
methods in drill core samples

Sample preparation significantly improves quality of data. Forexample,

correlation between Zn data from portableXRF and lab jumps from 72% in
the unprepared samples to 96% in the prepared samples.

Although portable XRF provides reliable and consistent data, calibration

adjustment may beneeded to increase accuracy further.

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 How we can increase accuracy

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 Is it neccesary to make an empirical calibration for uses on field
Samples with certified laboratory results should be evaluated with the XRF
Niton Thermo Scientific analyzer.

It is necessary to be careful the mode to be used as well as its

configuration, filters in operation and test times.

In this way it is possible to compare the results by integrating them into a

spreadsheet

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 Always compare your Niton XRF with lab samples
6.000

y = 1.6x + 0.029
5.000 R² = 0.9223

4.000
% Si PRIMUS

3.000

2.000

1.000

0.000
0.000 0.500 1.000 1.500 2.000 2.500 3.000 3.500 4.000
% Si NITON
4.000
3.500 y = 2.4602x + 0.3771
3.000 R² = 0.9921

% Al PRIMUS 2.500
2.000
1.500
1.000
0.500
0.000
0.000 0.200 0.400 0.600 0.800 1.000 1.200 1.400
% Al NITON

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 Always compare your Niton XRF with lab samples
0.700

0.600
y = 0.8857x - 0.0829
0.500 R² = 0.9697
% Fe PRIMUS

0.400

0.300

0.200

0.100

0.000
0.000 0.200 0.400 0.600 0.800 1.000
% Fe NITON

16.000
14.000
y = 1.002x + 1.2087
12.000 R² = 0.9444

% Mg PRIMUS
10.000
8.000
6.000
4.000
2.000
0.000
0.000 2.000 4.000 6.000 8.000 10.000 12.000 14.000
% Mg NITON

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 Always compare your Niton XRF with lab samples
40.000
35.000
y = 1.1938x - 4.2906
30.000 R² = 0.9854
% Ca PRIMUS

25.000
20.000
15.000
10.000
5.000
0.000
0.000 5.000 10.000 15.000 20.000 25.000 30.000 35.000 40.000
% Ca NITON
0.900
0.800
0.700 y = 1.3416x - 0.0014
R² = 0.9953
0.600

% K PRIMUS 0.500
0.400
0.300
0.200
0.100
0.000
0.000 0.100 0.200 0.300 0.400 0.500 0.600 0.700
-0.100
% K NITON

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 Conclusions

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 Questions

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 50,000 Thermo Fisher employees in 50+ countries
supporting the global business of science

Portable Analytical Instruments

Americas Europe, Middle East, Asia Pacific

Africa and South Asia New Territories, Hong Kong
Boston, MA, USA
Munich, Germany +852 2885 4613
+1 978-670-7460
+49 89 3681 380 [email protected]
[email protected]
[email protected]

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