Manual - XL3t - Mining

Us er Manual , Mining A ppl icat io ns
Thermo Scientific
Niton XL3t and Ultra
X-Ray Fluorescence
(XRF) Analyzers
Version 1
January 2014
Table of Contents
Introduction...............................................................................................................2
Standard Operating Procedure......................................................................................2
Warnings and Disclaimers.............................................................................................2
Chapter 1 Analyzer Preparation.................................................................................................3
Chapter 2 General Testing Protocol...........................................................................................7
Sample Preparation......................................................................................................7
Sample Prep.........................................................................................................7
Matrix effect, calibration adjustment (Cal-factor).....................................................8
Pseudo Elements........................................................................................................11
Mode Selection...........................................................................................................13
Mining Mode.......................................................................................................13
Soil Mode...........................................................................................................13
TestAll Geo Mode................................................................................................15
Entering Sample ID..............................................................................................16
Average Forward Mode........................................................................................17
Audio Cues.........................................................................................................18
Testing Duration.........................................................................................................19
General Rules......................................................................................................19
Chapter 3 Sample Types and Settings....................................................................................20
In situ Measurements.................................................................................................20
Direct Rock Sample....................................................................................................20
Drill Core Sample........................................................................................................20
Powders and Fine Aggregates.....................................................................................21
Blast Hole Samples.....................................................................................................21
Process Control Samples............................................................................................21
Concentrates..............................................................................................................22
Slurry.........................................................................................................................22
Oil and gas related samples/light elements..................................................................22
Soil Samples..............................................................................................................23
In Situ Analysis ................................................................................................ 23
Ex Situ Analysis................................................................................................. 23
Environmental Assessment................................................................................. 24
Chapter 4 Results Interpretation.............................................................................................25
Introduction
This manual is a guide to using the Thermo Scientific™ Niton™ XL3t Ultra and the Thermo
Scientific™ Niton™ XL3t GOLDD+ in mining applications.
Standard Operating Procedure

Operators should read the Thermo Scientific Niton XL3 Series Resource Guide that comes with
your instrument carefully before using the system. Users are strongly urged to attend the Thermo
Scientific Niton XRF Analyzer Radiation Safety and Operations Training courses offered regularly
(U.S. only), or contact their local representative for product and safety training. For more
information, visit www.niton.com.
Warnings and Disclaimers

Thermo Fisher Scientific Inc. makes this document available to its customers to use in the
product operation. This document is copyright protected and any reproduction of the whole or any
part of this document is strictly prohibited, except with the written authorization of Thermo Fisher
Scientific Inc.
The contents of this document are subject to change without notice. All technical information in
this document is for reference purposes only. System configurations and specifications in this
document are not meant to supersede all previous information received by the purchaser.
Thermo Fisher Scientific Inc. makes no representations that this document is complete, accurate
or error free and assumes no responsibility and will not be liable for any errors, omissions, damage
or loss that might result from any use of this document, even if the information in the document is
followed properly.
This document is not part of any sales contract between Thermo Fisher Scientific Inc. and a
purchaser. This document shall in no way govern or modify any Terms and Conditions of Sale, which
Terms and Conditions of Sale shall govern all conflicting information between the two documents.
Thermo Scientific Niton XL3t and Ultra X-Ray Fluorescence (XRF) Analyzers | 2
Analyzer Preparation
1. Insert a charged battery into the analyzer and turn it on.
1
2. Follow the screen instructions to log on using either the default password or one designated
by the user in an NDU file.
3. Wait a few minutes before using the analyzer (particularly for light elements). This will allow
the instrument electronics to stabilize.
4. Verify that the date is set properly for data tracking purposes.
a. From the Main Menu, select the System icon and then select the Specs icon. The date will
be displayed for verification.
b. If the date is incorrect, correct it by closing out of the Specs screen and selecting the Date
& Time icon from the System Menu. Change the date, and select the Return button to go
back to the Main Menu.
5. (Optional) Connect the analyzer to a computer with the serial cable included, USB cable, or
BluetoothTM wireless module. The instrument can be mounted on a test stand and operated
from the computer using the NDT program. This is recommended if a large number of
samples are going to be analyzed.
6. During analysis and System Check, it is important not to expose the analyzer to strong
electromagnetic fields, including those produced by computer monitors, hard drives, cellular
telephones, walkie talkies, etc. Keep a minimum two feet (0.7 meters) distance
between the analyzer and electronic devices. It is better to perform System Check
under the same conditions (e.g. temperature) that the samples will be analyzed.
7. From the Main Menu, select the System Check icon, and select the Yes button (Figure 1).
a. System Check calibrates the detector and verifies that it is operating to specifications.
Once the process is started, no further user interaction is required. When the instrument
is finished performing the check, the unit will show either System OK or a failure error.
b. If the unit shows a failure error, then perform a second System Check by selecting the
Recheck button. If the unit still does not show a System OK, please contact Thermo
Scientific Niton Analyzers or your local representative for assistance.
Chapter 1 | Analyzer Preparation
Figure 1. System Check Menu Path
8. Verify and/or change filter position time. Niton XL3 (including Niton Ultra) analyzers are
equipped with excitation filters that optimize the analyzers’ sensitivity for various elements.
The High Range filter is used to optimize barium (Ba) through silver (Ag). The Main Range filter
provides optimum sensitivity for the elements manganese (Mn) through bismuth (Bi). The
Low Range filter is used to optimize the sensitivity for the elements from titanium (Ti) through
chromium (Cr). Note that the main range filter can be used to analyze Ti, V and Cr, but
sensitivity is improved when using the low filter. The amount of time that the analyzer spends
in each filter position is user defined. Please note that the analyzer will continue alternating
excitation filters until the user-selected maximum analysis time is reached or the operator
terminates the measurement. To verify or change the length of time that each filter will be
active, do the following:
a. From the Main Menu select the Advanced icon, then the Element Range icon (Figure 2).
In the drop-down menu, select the mode that is intended for use (i.e., Mining Mode).
Figure 2. Element Range Menu
b. Select the boxes next to Main Range, High Range, Low Range and Light Range so that a
check mark appears in each box.
c. Enter the desired length of time for each filter. For example, set values of 30 seconds for
each range as shown in Figure 3.
d. Select the Save button and return to the Main Menu by selecting the Return icon.
Figure 3. List of Elements in Each

Mode / Filter Main Low High Light
Filter in Mining Mode. This list may vary
Mining Mode Ag Mn Se Ca Ag A1
depending on the calibration.
As Mo Sn Cr Ba Cl
Au Nb Sr K Cd Mg
Bi Ni Ta Ti Pd P
Cd Pb Ti V Sb Si
Co Pd V Sn S
Cr Rb W
Cu Re Zn
Fe Sb Zr
Hf
9. Verify instrument measurement accuracy. Depending on the configuration of your instrument,

you will have been supplied with a set of multi-element reference samples. These samples
are used to verify that the instrument is performing properly. Use CCRMP TILL-4 (180-601)
to verify the instrument performance in Mining Mode and Soil Mode. The nominal element
concentrations and acceptable ranges of results for each reference sample are shown in
Table 1-1.
a. Mining: From the Main Menu, select the Sample Type icon, then the Soils & Minerals icon,
then the Mining Cu/Zn icon or Mining Ta/Hf icon as appropriate (Figure 4). You can also
use this procedure with TestAll Geo Mode.
Figure 4. Mining Cu/Zn Analysis

Menu Path
b. Place the reference sample CCRMP TILL-4 (180-601) in the test stand for analysis, or set
the reference sample on a clean surface. The unlabeled side should face the
spectrometer. Grasp the analyzer by the handle, ensuring the wrist strap is placed on the
wrist. Place the front end of the instrument against the sample with the window centered
on the sample. The camera can help to position the window. Position the analyzer so that
the nose of the analyzer is making contact with the sample.
c. Take a measurement on the reference sample (30 sec. on each filter). Prior to measuring,
be sure the analyzer’s maximum test time is set to 120 seconds or greater. To do so,
select the Advanced icon from the Main Menu, then the Start/Stop Setup icon. Edit the
Max.Time dialog box to display the proper setting. If you were using Cal-factor, change the
calibration factors to factory values.
d. Compare the result with the acceptable ranges listed in Table 1.1; Fe and K for Mining
Mode and Cu, Ti for Soil Mode. The result should fall within these specified values.
e. If the analyzer reports values within the acceptable ranges of the reference values, it is
ready to measure unknown samples. Proceed to GENERAL TESTING PROTOCOL section.
f. If the analyzer reports values outside the acceptable tolerance ranges specified in Table 1-1,
repeat the System Check described in step 7, then repeat the reference sample analysis
in step 9a.
g. If the analyzer again fails to meet the acceptable tolerance ranges specified in Table 1-1,
please contact Thermo Scientific Niton Analyzers or your local representative for assistance.
Table 1.1 Nominal Concentrations and Acceptable Ranges
Minimum Maximum
Element – Mode Certified Value Acceptable* Acceptable*
% Fe – Mining 3.97 % 3.50 % or 35000 ppm 5.0 % or 50000 ppm
% K – Mining 2.68 % 2.3 % or 23000 ppm 3.5 % or 35000 ppm
ppm Cu – Soil 237 ppm 0.02% or 200 ppm 0.028% or 280 ppm
ppm Ti – Soil 4840 ppm 0.41% or 4100 ppm 0.52% or 5200 ppm
* Depending on whether % or ppm is selected for reporting concentration.
General Testing Protocol
2
This section outlines general testing protocols for a variety of geological samples, from
heterogeneous to homogeneous, in situ or in a portable lab. Consider the data quality
requirements when determining the number of samples and the amount of preparation to
undertake.
To ensure data accuracy, two criteria must be met when samples are analyzed.
1. The sample must cover the analysis window. The window is located on the nose of the
analyzer, and it is the point at which the x-ray beam is emitted from the analyzer and
fluoresced x-rays are collected by the detector. It must be as close to the sample as possible
and contact with the sample must be maintained for the entire measurement time. The
size of this window is about 0.5 cm2 (about 8 mm diameter). Generally, lower than actual
concentration will be detected on rough surfaces because air in the space between sample
and x-ray detector will absorb some of the x-rays. This air effect is more prominent for light
elements (Mg, Al, Si, P, S) so sample preparation is required for these elements.
2. The sample needs to be “infinitely thick.” Infinite thickness refers to having enough sample
depth so that even if the depth of the sample were increased, no additional fluoresced x-rays
would be produced and reach the detector. This thickness is about 1-1.5 cm in the prepared
(powder) samples and much less (maximum a few millimeters) in the rough samples.
Sample Preparation
Sample preparation is the grinding or milling of a rock sample to produce powder which in turn
is mixed and formed into pellets or cups. The uniform surface and homogeneous nature of a
prepared sample can improve the detection limits and the accuracy of field portable XRF analyzers.
Using He-purged GOLDD or Ultra analyzers will expand your element range (down to Mg) and give
low LODs. Any sample, even in situ, must be as clean as possible, given the nature of the sample
and the circumstances of the reading. If the analyzer is used directly on powder or soil samples,
make sure that the x-ray window is clean for the next sample.
32 mm sample cups first must be assembled if they are going to be used as part of the sample
preparation process. To assemble a sample cup:
Chapter 2 | General Testing Protocol
1. Place a Mylar film (2.5" diameter, 6 micron thick) or Polypropylene film (2.5" diameter,
4 micron thick) on top of the sample cup collar.
2. Press the sample cup cylinder into the collar so that the film is pulled tightly between the
collar and cylinder, creating an enclosure.
3. Turn the sample cup over with the film down so that sample material can be placed and
tamped into the cup.
4. Place a filter paper 2.4 cm in diameter on top of the material, when the material reaches the
line close to the top of the cup.
5. Place polystuffing on top of the filter so that when the sample is inverted, the material is held
firmly against the film.
6. Place the sample cap on top of the batting and affix a label to the cap.
7. A portable test stand is available for fixed bench or portable location (such as the tailgate of
a truck).
Sample Prep
Analysis may be performed on either in situ or ex situ samples. The XRF results from unprepared
samples may differ with those from prepared specimens. This is generally caused by non-
homogeneous samples, particle size effects and moisture content. The more sample prepared, the
higher accuracy of data. In situ analysis may only provide “screening” type data. The decision to
prepare a sample may be determined by your data quality objectives.
Soil mode is a Compton normalized calibration which works over a fairly limited element concen-
tration range. It is highly recommended that samples containing high concentrations of elements
(such as ore samples) be analyzed using the Mining mode (see Mode Selection section below).
Matrix effect, calibration adjustment (Cal-factor)

Natural geological samples have a variety of matrices (e.g., carbonate, silicate, oxide, sulfate, etc.).
Although the FP software automatically corrects for most inter-element matrix effects, Niton XL3
analyzers cannot currently detect elements lighter than magnesium. As a result, the oxidation state
of elements can bias measurements of other elements. In many cases, this bias is small, and
uncorrected results provide sufficient accuracy, especially when data is for screening purposes
only. A slope/intercept calibration software (called Cal-factor) is installed in the analyzer to improve
the quality of the data. The calibration software is element specific, and calibration can be
adjusted for individual elements, independent of the other elements. A user may choose to correct
a single element or a suite of elements.
The degree of severity of the bias should be evaluated before proceeding with routine
measurement. A few test samples should be carefully measured by another technique, or by an
outside lab. These samples should then be analyzed using the analyzer. If the agreement is good
enough to provide the accuracy required for the application, the instrument can be operated as
shipped. If it is determined that a bias correction is necessary, the procedure for establishing
calibration factors should be followed (see steps below). As geological site characteristics change,
it is good practice to run a few check standards to ensure that the instrument results are still
within an acceptable error range.
1. From Main Manu, select Advanced and then Adjust Calibration (Figure 5).
Figure 5. The Adjust Calibration Menu Path
2. Select Type Stand, then in the Type Standardization window choose Mining Cu/Zn or Mining
Ta/Hf, enter number of standards (known samples) and name the data set. Click on Next and
in the new window, select elements that need to be re-calibrated, and then click Ready To
Test (Figure 6).
Figure 6. The Adjust Calibration Menu Path
3. In Enter Type Standardization screen, enter known values for the chosen elements. Enter
Standard name (name of known samples that are going to be analyzed), and then click Next.
The new Type Standardization screen prompts you to Place Standard (that was named before)
in front of the X-ray window. Click Ok and measure that standard (Figure 7).
Figure 7. Entering known values and

measuring standards (known samples).
4. After measuring the first standard, click on Accept or Retake depending on if the results are
acceptable or not. The next screen shows the results for the first standard (Figure 8).
Figure 8. Screens after analyzing the

first standard sample.
5. Follow above steps for all standard samples. After accepting the last analysis, click on
Create and then click on Close in the Type Standardization Final screen. The created type
standardization data set name will appear in the TS List (Figure 9).
Figure 9. Created Type Standardization

in the TS list.
6. In order to use this TS (Cu Test in this example) in the analysis, go to the main screen and
click on Sample Type. Select TS, and then select the type standardization that was created
(Cu Test in this example). In the Ready to Test screen, name of this TS will appear (Figure 10).
Figure 10. Using created Type

Standardization.
Pseudo Elements
Pseudo Elements are constructs you can create which will be treated like elements in the analysis,
showing up in the analysis as if they were actual elements. For example, elements can be shown
as oxides (which are already available in the Pseudo Elements Library) or as any combinations
(combinations, rations, etc).
To use Pseudo Elements, follow these steps:

1. From the main screen, select Advanced, then scroll down and select Presudo Elements
(Figure 11).
2. In the Pseudo Elements screen, select the Mode (Soils or Mining).
3. Select the desired mode by touching the screen (e.g., Mining Mode). You may use the Library
which includes most common oxides (converted elements to oxides). Select Library and then
Add required oxides. You may also create a New formula (Figure 12).
4. After analyzing the sample, these Pseudo Elements will show in the results screen along with
the elemental concentrations.
Figure 11. Using Pseudo Elements.
Figure 12. Selecting Pseudo Elements

from the Library or creating new formula.
The bottom right figure shows results
after analyzing a sample.
Mode Selection
For the best analytical results, use the proper mining calibration mode. To decide which mode to
use, consider the following:
1. Mining Mode (divided into Mining Cu/Zn and Mining Ta/Hf) is used for measuring
concentrations of elements that are 0.5% (5000 ppm) or greater.
2. In analyzing a concentrate sample, use Mining Mode even if the required element is less than
0.5% (5000 ppm). For example if you are analyzing a lead-zinc ore which may have some
silver, use Mining Mode.
3. Mining Mode is a fundamental parameter (FP) calibration and will do the best job for any
sample that contains either >1% of any single element in the K-U range, or any combination
of elements (K-U) that add up to >10%.
4. You may choose to show the elements concentration as % or ppm in Mining Mode.
5. Soil Mode is best for low concentration elements at 0.5% (5000 ppm) or less. For samples
containing high concentrations of elements (other than those of primary interest), it is best to
use Mining Mode for analysis.
6. Soil samples shouldn’t necessarily be analyzed using Soil Mode. Some elements may be
concentrated even in the soil samples.
7. There are direct overlaps between the spectral peaks for copper (Cu) and tantalum (Ta) and
zinc (Zn) and hafnium (Hf). Handheld XRF technology cannot distinguish between these sets
of elements. Cu and Zn are associated with each other as are Ta and Hf. Therefore, if the
samples contain Cu or Zn, choose Mining Cu/Zn; if the samples contain Ta or Hf, choose
Mining Ta/Hf Mode.
8. TestAll Geo Mode can analyze any type of sample with any concentration (from ppm to %).
This mode uses FP calibration for high concentration elements and Compton normalized
calibration for low concentration elements. If you know the range of concentration for an
element of interest, use Soil or Mining Modes.
9. For trending purposes, it is better to use one mode for a project that has similar sample types
(rather than using different modes and switching back and forth between modes).
Mining Mode
To use Mining Mode, please see “filter position time” in the Analyzer Preparation section and also
the Mode Selection section discussed above.
Soil Mode
The standard operating procedure for soil analysis is the same as those for mining analysis.
However, the filters and range of elements are different.
In Soil Mode, up to three filters may be selected, depending on the elements required. The amount
of time that the analyzer spends in each filter is user-defined. Please note that the analyzer will
continue alternating excitation filters until the user selected maximum analysis time is reached or
the operator terminates the measurement. To verify or change the filter time, do the following:
1. From the Main Menu select the Advanced icon, then the Element Range icon (Figure 13). In
the drop-down menu, select Soil Mode.
2. Select the box next to High Range, Main Range, and Low Range so that a check mark
appears in each box.
3. Enter the desired length of time for each filter. For example, set values of 60 seconds for the
Main Range, 60 seconds for the Low Range, and 60 seconds for the High Range as shown in
Figure 14.
Figure 13. Element Range Main Path
4. You may click on question mark (?) to view list of elements in each range. The list of
elements will be similar to Figure 14.
5. Select the Save button and return to the Main Menu by selecting the Return icon.
Figure 14. List of Elements in Main, Low Mode / Filter Main Low High
and High Filters in Soil Mode. This list
may vary depending on the calibration. Soil Mode As Pb Ca Ag
Au Rb Cr Ba
Co Se K Cd
Cu Sr S Cs
Fe Th Sc Pd
Hg U Ti Sb
Mn W V Sn
Mo Zn Te
Ni Zr
6. Perform a quality control check by selecting the Sample Type icon from the Main Menu, then
the Soils & Minerals icon, then the Soils icon (Figure 15).
7. Place TILL4 Reference Sample (P/N 180-601) (or any other reference sample supplied with
your instrument) in the test stand for analysis, or set the reference sample on a clean surface.
The unlabeled side should face the spectrometer. Place the front end of the instrument against
the sample with the Analysis Window centered on the sample.
8. Take one 180-second measurement on this reference sample (60 seconds on each Range).
Be sure the analyzer has the maximum test time set to 180 seconds or greater. From the
Main Menu, select the Advanced icon, then the Start/Stop Setup icon. (Edit the Max. Time
dialog box to display the proper setting.)
Figure 15. Soil Analysis Menu Path
9. Compare the results with the acceptable ranges listed in the original accompanying
Certificate of Calibration sheet. The results should fall within these specified values.
Depending on the element calibrations provided with your Niton XRF analyzer, some of
the reference sample elements may not be displayed. If your instrument is not displaying
all elements, check the Element Display option to determine which elements are being
displayed. To force elements to display:
a) Select the Advanced icon from the Main Menu.
b) Select the Element Sorting icon, then select Soil Mode from the menu.
c) Select the element you wish to modify, select Always Display from the drop down list, then
select the Save Button.
d) Repeat this process for each element you want to change.
e) Select the Close Button, select the Close Button again, then select the Return icon.
10. If the analyzer reports values within the acceptable ranges of the reference values, it is ready
for measurement of unknown samples.
11. If the analyzer reports values outside the acceptance ranges specified in the accompanying
Certificate of Calibration sheet, repeat the System Check described above, then repeat the
reference sample analysis.
If the analyzer again fails to meet the acceptable ranges specified in the accompanying Certificate
of Calibration sheet, please contact Thermo Fisher Scientific or your local Thermo Fisher
representative for assistance.
TestAll Geo Mode

TestAll Geo Mode allows you to test powder, rock, and ore samples without first determining
whether the samples would best be analyzed with Mining or Soil Mode. TestAll Geo Mode uses
both the Compton Normalization calibration (Soil) and the Fundamental Parameters calibration
(Mining) to determine whether the soil calibration is acceptable or whether the total metal content
is too high for Compton mode. To select this mode, follow the steps in Figure 16.
Figure 16. The TestAll Geo Menu Path
If the sample can be analyzed via soil mode, then the analyzer will display results from both Soil
and Mining Modes in one unified list. If both calibrations contain the same element, then the
mode that has the lower detection limit will be displayed. Elements will be displayed in both ppm
(mg/kg) and wt.% with 0.10% being the cutoff point (Figure 17).
Figure 17. The TestAll Geo Analysis Screen.

Notice the ppm heading, but % is listed
with results where appropriate.
Entering Sample ID
From the Main Menu, select the Sample Type icon, then the Soils & Minerals icon, then the Soils
or Mining (Cu/Zn or Ta/Hf) icon depending on the sample type (see Mode Selection section for
details) which brings you into the Ready to Test screen (e.g., Soil Mode in Figure 18).
1. From the Ready to Test screen, select the Data Entry button, then select the Keyboard icon
next to the word Sample Type (Figure 19). This takes you to the virtual keyboard with which
you can enter the sample identification. When complete, select the Return button to take you
back to the Ready to Test screen.
2. Additional sample identification information may be entered into other fields if required.
Average Forward Mode

Sample homogeneity is extremely important when considering whether or not to average readings.
Non-homogenous samples contain different concentrations of elements at different points
across the sample. Averaging measurements using the Average Forward mode is often the best
way to determine whole rock or area concentrations because the average represents a more
complete information set over a specific area than would a single measurement. The other option
with inhomogeneous samples is to fully prepare them. Thermo Scientific offers various types
of performance packages, including portable sample preparation tools, based on your projects
needs. For measuring light elements (Mg, Al, Si, P, S) it is strongly recommended to pulverize and
prepare samples.
Average Forward enables you to average several readings together from a designated starting
point (Figure 20).
1. Select the Avg Forward button on the Tools in the Ready to Test screen (just before initiating
the analysis) to initiate sample averaging. Avg Forward will set up an automatic personal
averaging protocol to be followed until your analyzer is shut down, or this feature is disabled.
2. Select the number of readings you want to average from the virtual numeric keypad and
select the “E” button to enter the number. The “C” button will clear all, and the “<“ button will
clear the last digit entered. For example, if you select three on the virtual keypad, the analyzer
will automatically calculate, average, and store a reading for every three tests you take. The
average will display automatically.
Figure 20. Example Averaging Screens
Audio Cues
1. Selecting the Audio icon opens the Beep Times Setup Screen, enabling changes to the beep
settings for various modes (Figure 21).
2. You can change the beep settings for different modes independently. Select the Down Arrow
Screen button to access the list of modes.
Figure 21. The Beep Setup Menu Path
Testing Duration
The duration a sample is interrogated with XRF affects detection limit and precision. For best
results, each required filter time should be set for a minimum of 30 seconds. For mining sample
analysis, measurements usually require 60 seconds or more per filter (particularly for light
elements; Mg, Al, Si, P, S). If element concentrations are high enough, and the range of acceptable
values broad enough, shorter measurement times may be sufficient to achieve the desired results.
For example, if it is necessary to determine whether a sample contains more or less than 1000
ppm of lead (Pb), 30 seconds on the Main Filter may be sufficient analysis time. In contrast, if the
question is whether or not a sample contains 100 ppm of copper, a minimum of 60 seconds on
the Main Filter is suggested. If the error is too great, increasing the testing time by a factor of four
will decrease the error by 50%.
General Rules:
1. Set at least 30 seconds of testing time on the filter that contains the element of interest.
Depending on the project type, this time may be decreased to less than 30 seconds (if low
accuracy is acceptable) or increased to more than 30 seconds (if high accuracy is needed).
2. The same applies to Low and High filters. However, for elements in the Light Filter, a longer
time period (up to 300 seconds or more) is needed for the highest accuracy.
3. Set the Main filter for at least 10 seconds even if the element of interest is not in this filter.
4. I t is better to use all filters for each assay (i.e., do not un-tick a filter). Less important filters
can be given less assaying time than the desired filter.
5. The Main range filter can be used to analyze Ti, V and Cr, but sensitivity is improved when
using the Low filter for these elements.
Sample Types and Settings
In situ Measurements
3
Measurements taken directly on the rock outcrop, wall or floor of the mine are in situ. This is the
most basic type of measurement because there is no sample preparation performed.
1. Determine whether to average readings over a selected area. (See Average Forward)
2. Set the appropriate filters and reading times.
3. Set beeps to activate at the end of the predetermined measurement time. (See Audio Cues).
4. Start the reading and continue until the measurement is complete.
5. Repeat to complete averaging over an area or move to different spot and repeat for a new
measurement.
Direct Rock Sample

If analysis of grab samples is required without sample preparation, they can be analyzed and
interpreted much like in situ samples. The Standard Operating Procedure is the same as that for
in situ samples.
Drill Core Sample

Drill core samples can be analyzed in three ways:
1. Prepare pulverized samples taken from one to two meter intervals (shorter or longer intervals
may be used depending on mineralization and scope of analysis). XRF data from these
samples will have the highest correlation with lab assays. Samples can be pulverized using
sample preparation tools offered by Thermo Scientific.
2. Shoot pre-determined intervals of drill core at every 20-25 cm (e.g. 4-5 analysis per one
meter of core) using the Average Forward function. Assay results from this method may not
have high correlation with lab assays because of random nature of mineralogy at various
shooting points.
Chapter 3 | Sample Types and Settings
3. Scan pre-determined intervals of drill core by moving the analyzer along the length of the
core. The speed of movement should be adjusted with the filter time (e.g. 30 cm per 15
seconds). This method should be used only for elements that are in one filter. This filter
should be used while other filters are closed (to prevent changing filters while moving the
analyzer).
Powders and Fine Aggregates

Samples that come out of a mill or similar device are fine-grained and contain more consistent
particle sizes than any other type of sample. A powdered sample is more representative of the
sampling media and will produce consistent and repeatable assay data. It is appropriate to use a
sample cup for such analysis.
1. Determine whether to average multiple readings or to take one measurement per bag or cup.
2. If using 32 mm sample cups, follow the sample cup preparation protocol outlined in the
Sample Preparation section above.
3. Set the appropriate ranges and reading times.
4. Set beeps to activate at end of predetermined measurement time.
6. Repeat to complete averaging, or choose a new sample and repeat.
Note: For analyzing a large number of cupped samples, it is easier to use a test stand or a field
mate and operate the instrument from a computer using NDT software.
Blast Hole Samples

Blast hole samples contain material sizes from fine-grained to chips and chunks. Fine-grained
material could be more representative of the blasted area. These materials can be placed in a
sample cup and analyzed following the same SOP as Powders and Fine Aggregates.
Large chunks can be treated as grab specimen and analyzed following the same SOP as Hand
Specimen. Smaller chips can be analyzed in a bag if light elements are not the desired elements.
Note: In direct assay of chunks and chips make sure that sharp points do not pierce the x-ray
window.
Process Control Samples

Measurements taken after the initial crushing of mine material can be treated much like blast hole
samples because of their inconsistently-sized particles. The same SOP can be followed for this
type of samples.
Note: If such samples contain high concentrations of elements of interest, you may need to use
Cal-factor or User Method.
Concentrates
Concentrate samples contain relatively high concentrations of the elements of interest and are
typically measured using Mining Mode.
Note 1: Two types of samples can be categorized in this group.
1. Samples from production stage in a mine operation. These samples are generally fine-grained
and therefore a cup is appropriate for analysis. Follow SOP for Powders and Fine Aggregates
2. Highly concentrated grab samples such as a piece of lead-zinc ore or bauxite sample. They
can be analyzed following SOP for In Situ Measurement.
Note 2: Concentrate samples (in any form) might be different than the samples that are used in
factory calibration. Cal-factor or User Method might be needed to get accurate results.
Slurry
The level of moisture in slurry samples is relatively high. Depending on the data quality needs,
it may be necessary to dry the sample prior to analysis. Like some of the previously discussed
sample types, 32 mm sample cups or bags may be used as long as infinite thickness is
maintained.
1. If samples need to be dried, remove them from the bath and place in the oven for 1 to 24
hours, then place in a sample bag or cup. Break up the sample if necessary.
2. If using 32 mm sample cups, follow the sample cup preparation protocol outlined in the
Sample Preparation section above.
3. Determine whether to average multiple readings or to take one measurement per bag or cup
and set the appropriate filters and reading times.
5. Repeat to complete averaging, or choose a new sample and repeat.
Oil and Gas Related Samples/Light Elements

Light elements (Mg, Si, Al), Fe, Ca, and K are the major components of many oil and gas reservoir
rocks that can be analyzed by portable XRF. The SOP for these samples is the same as that for
Powders and Fine Aggregates discussed above. The following hints may improve the accuracy of
XRF data:
1. All filters should be ON when analyzing these samples.

2. At least 30 seconds (preferably 1-3 minutes) is needed for the light filter.
3. Light elements are very sensitive to the thickness of the film used in the cup. Polypropylene
film is preferred.
4. Although these rocks are fine-grained and homogenous, they may have weathered surface.
If in-situ analysis is preferred, the surface should be cleaned (and preferably ground).
Soil Samples
In Situ Analysis
This is the most basic type of measurement as there is little to no sample preparation performed.
It is typically used for providing screening data to help rapidly define an area of contamination
for example.
1. After performing a QC check (see above), place the In Situ Test Guard over the front nose
of the instrument. This test guard has two main purposes; first, it helps to keep the front of
the instrument clean by preventing soil particles from collecting on the window. Second, it
provides a solid base for the Proximity Button to engage properly, which can be difficult on
very loose or powdery samples.
2. Set the appropriate range and analysis times. The analysis times should be previously
determined, as discussed above.
3. If desired, set beeps to activate at the end of the predetermined measurement time. (See
Audio Cues).
4. Remove any large or non-representative debris from the soil surface before analysis. This
debris includes rocks, pebbles, twigs, leaves, concrete, etc. If the surface is unlevel, it may be
smoothed with a stainless steel trowel or other similar implement. If the soil is saturated with
water, allow it to dry before starting the analysis.
5. Enter the sample name, or any other pertinent information regarding the sample to maintain
appropriate chain-of-custody.
7. Confirm that the readings are appropriate and then proceed to next sampling area.
8. Per USEPA Method 6200, a minimum of one sample for every 20 analyses (i.e. 5%) should
be taken and submitted for laboratory analysis. Make sure that the sample taken is the
sample that you analyzed because soil samples can vary immensely over very short distances
(a few cm).
9. After a few hours of analysis, rerun the QC standard to confirm instrument stability.
10. Download all results (unknown sample readings, QC samples, and system check) and save
as an appropriately named file. The NDT file created during the download is encrypted and
provides data integrity.
Ex Situ Analysis
This is a more labor-intensive type of analysis as the sample undergoes full preparation. It is
typically used to quickly provide on-site personnel with laboratory grade data without waiting for
laboratory analysis, allowing for more immediate and accurate decision making.
1. It is highly recommended that you read and follow the USEPA Method 6200 for soil analysis.
2. Samples are procured in the field and taken to a fixed location such as an office or a vehicle
for preparation and analysis. Sample collection is very important as samples collected
incorrectly may bias the results. Non-representative debris should be removed before sample
collection begins. The sample is collected from a 4" by 4" square that is 1" deep (10cm by
10cm and 2.5cm deep). This provides enough material to fill an 8 oz or 250 cm3 specimen
jar. Label the jar immediately to maintain chain-of-custody requirements.
3. Collect all samples in a similar fashion, and return samples to sample preparation area.
4. To perform sample preparation, dry, homogenize, ground, and sieve the samples.
5. Samples may be dried rapidly in a convection or a toaster oven, or spread out on a tray
and air dried if power is not available. It is generally not recommended to dry samples in a
microwave oven.
6. The dried sample should then be well mixed and then split using a technique such as
coning and quartering that will ensure an even particle size distribution (so you do not bias
the results). This procedure should be repeated until you have approximately 1oz (25 g) of
representative sample. The samples can be ground using a mill (such as Portable Mill offered
by Thermo Fisher) until it passes a 60-mesh (250 micron) sieve.
Note: The remaining unprepared sample should be returned to the container to allow
duplicate XRF or laboratory analysis if required. It is possible to fully prepare the entire
sample, but this can be a lengthy process and in-field work does not always allow the analyst
the time to do this.
7. The ground sample should then be cupped. Follow the 32mm sample cups protocol outlined
above.
8. Perform instrument QC check.
9. The sample cups may then be analyzed. It is best to analyze these in test stands so that the
cup is held firmly against the instrument window.
10. Enter the sample name or any other pertinent information regarding the sample to maintain
appropriate chain-of-custody. See Entering Soil Sample ID for details.
11. Confirm that the readings are appropriate and then proceed to the next cup.
12. Per USEPA Method 6200, a minimum of 1 sample for every 20 analyses (i.e. 5%) should be
taken and submitted for laboratory analysis. Some of the remaining split can be used for
this purpose.
13. After a few hours of analysis, rerun the QC standard to confirm stability of the instrument.
14. Download and save all results. The NDT file created during the download is encrypted and
provides data integrity.
Environmental Assessment
Environmental assessment samples are generally analyzed to assess level of some toxic elements
in the soil or specific sample types. Commonly these levels are in a range that can be analyzed
using Soil Mode. Such samples can be in powder/soil form which can be analyzed using a cup or
direct assay on the soil. See SOP for in situ and ex situ analyses above.
Note 1: Direct analysis of soil samples could cause contamination of the x-ray window. This
window should be cleaned after each analysis.
Note 2: Make sure that random sharp objects do not pierce the x-ray window when analyzing in
situ soil samples.
Results Interpretation
4
Data from field-portable XRF will be comparable with laboratory results on the same samples.
Samples that are less than fully prepared may show some discrepancies with lab data depending
upon the homogeneity of the material in its in situ condition. However, XRF instruments are
capable of acquiring large volumes of data from multiple samples that together yield a statistically
better result when compared to a lab analysis of a single sample. If the user determines that one
sample is not representative of an area, then two or more samples from that area may be quickly
analyzed and averaged to aid in data interpretation. As mentioned above, for some sample types
(such as concentrates) using Ca-factor or User Method might be necessary.
If results differ greatly from the user’s expectations, they can always be verified by inspecting the
spectrum generated by the sample. Two peaks from each element that is present in the sample will
always be present in the spectrum. X-ray energies for each element can be found either on the Thermo
Scientific Niton X-ray Energy Reference chart or on the right hand side of the NDT software program.
In Figure 22 the Ka and Kb peaks of iron (Fe) are displayed between the 5.40 and 7.20 energies.
Looking at the peaks, make sure that element of interest does not overlap with any potential
interference elements.
Figure 22. Sample

Spectrum with Fe
Ka and Kb Peaks
at 6.40 and 7.06
Respectively
Thermo Fisher Scientific,
San Jose, CA USA is ISO Certified.
© 2014 Thermo Fisher Scientific Inc. All rights reserved. LEXAN is a trademark of SABIC. Leica is a trademark of Leica Geosystems. Bluetooth is a registered
trademark of SIG, Inc. All other trademarks are the property of Thermo Fisher Scientific Inc. and its subsidiaries. Specifications, terms and pricing are subject to
change. Not all products are available in all countries. Please consult your local sales representative for details.
XRF Analyzers Americas Europe, Middle East, Asia Pacific www.thermoscientific.com/niton

Boston, MA, USA Africa and South Asia New Territories, Hong Kong
+1 978-670-7460 Munich, Germany +852 2885 4613
niton@thermofisher.com +49 89 3681 380 niton.asia@thermofisher.com
niton.eur@thermofisher.com
5-1101 01/2014

Manual - XL3t - Mining

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Us er Manual , Mining A ppl icat io ns

Standard Operating Procedure

Warnings and Disclaimers

Figure 1. System Check Menu Path

Figure 2. Element Range Menu

Figure 3. List of Elements in Each

9. Verify instrument measurement accuracy. Depending on the configuration of your instrument,

Figure 4. Mining Cu/Zn Analysis

Table 1.1 Nominal Concentrations and Acceptable Ranges

Matrix effect, calibration adjustment (Cal-factor)

Figure 5. The Adjust Calibration Menu Path

Figure 6. The Adjust Calibration Menu Path

Figure 7. Entering known values and

Figure 8. Screens after analyzing the

Figure 9. Created Type Standardization

Figure 10. Using created Type

To use Pseudo Elements, follow these steps:

Figure 11. Using Pseudo Elements.

Figure 12. Selecting Pseudo Elements

Figure 13. Element Range Main Path

Figure 15. Soil Analysis Menu Path

TestAll Geo Mode

Figure 16. The TestAll Geo Menu Path

Figure 17. The TestAll Geo Analysis Screen.

Figure 18. Soil Analysis Menu Path

Figure 19. Soil Analysis Menu Path

Average Forward Mode

Figure 20. Example Averaging Screens

Figure 21. The Beep Setup Menu Path

Direct Rock Sample

Drill Core Sample

Powders and Fine Aggregates

Blast Hole Samples

Process Control Samples

Note 1: Two types of samples can be categorized in this group.

Oil and Gas Related Samples/Light Elements

1. All filters should be ON when analyzing these samples.

Figure 22. Sample

XRF Analyzers Americas Europe, Middle East, Asia Pacific www.thermoscientific.com/niton

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