XL3 Analyzer Users Guide Ver 7.0.1 Rev C Nov 2010

© 2010 Thermo Fisher Scientific Inc. All rights reserved.

Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase 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 supersede all previous information received by the purchaser. Thermo Fisher Scientific Inc. makes no representations that this document is complete, accurate or errorfree 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.

Release history:

For Research Use Only. Not for use in diagnostic procedures.

Contents

Thermo Scientific

Chapter 0

Contact Us...1

Chapter 1

Manual Overview...1 Warnings, Cautions, and Notes... 1 Figures... 1 Physical Buttons... 2 Other Hardware... 2

Chapter 2

Using Your Analyzer...3 Safely and Effectively Using Your Analyzer... 3 Monitoring your radiation exposure... 6 Safe Handling of Samples... 11 Niton XL3t Radiation Profile... 13 Niton XL3t GOLDD Plus Radiation Profile... 16 Niton XL3p Radiation Profile... 20 Primary Radiation... 22 Secondary Radiation... 22 Deep and Shallow Dose... 23 Proper and Improper Operation... 23 Emergency Response Information... 30 Startup Procedure... 32 Battery Installation and Charging... 33 The Control Panel... 38 Startup Procedure... 40 Performing a System Check... 42 The Data Ports... 49 Power Port... 49 Using the Navigation (NAV) Menu... 50 Using the Tools Menu... 50 Setting the Date and Time... 55 Data Entry... 60 The Results Screen... 62

Chapter 3

How to Analyze...65

Chapter 4

Metal Sample Prep...67

Chapter 5

Metals Analysis...81 General Metals Analysis... 84 PMI Analysis... 89 FAC Analysis... 96 Coatings Analysis... 105 Preparatory Tasks... 105 Coatings Entries and Standardization... 108 General Metals Analysis... 115

manual-name

1

Contents

PMI Analysis... 121 FAC Analysis... 129

2

manual-name

Chapter 6

Coatings Analysis...139

Chapter 7

Mining Analysis...149 Niton XL3 X-Ray Fluorescence (XRF) Analyzer – Version 7.0 and Higher... 149 Grade Control Samples... 155 Blast Hole Samples... 156 Process Control Samples... 157 Powders and Fine Aggregates... 157 Concentrates... 158 Slurry... 159

Chapter 8

Soil Analysis...161 Niton XL3 X-Ray Fluorescence (XRF) Analyzer – Version 7.0 and Higher... 161

Chapter 9

Consumer Goods Analysisniton...169 Niton XL3 X-Ray Fluorescence (XRF) Analyzer – Version 7.0 and Higher... 169 APPENDIX A... 190 Appendix B... 196

Chapter 10

Spectral Fingerprint...207

Chapter 11

Helium Purged Analysis...211

Chapter 12

Data Management...219 Viewing Data... 219 Viewing Fingerprints... 226 Erasing Data... 227 Managing Libraries... 232

Chapter 13

Connectivity...239 Using Your Analyzer With Your PC... 239 Starting Niton Data Transfer Software... 241 Connecting the XRF Analyzer to Your PC... 242 Connecting From Your Analyzer to Your PC... 247 Using a USB Cable to Connect Your Analyzer... 251 Downloading Data... 258 Creating and Using Reports... 266 Viewing the Spectra Graph... 283 Viewing Different Areas of the Spectra Graph... 293 Viewing the X-ray Line List... 298 Thermo Scientific

Contents

Using the Menus Instead of the Toolbar... 311 Renaming a Report... 317 Saving Selected Readings from a Report... 318 Copying a Report Into Excel... 319 Printing Certificates of Analysis... 325 Closing a Report... 330 Deleting a Report... 331 Printing from NDT... 332 Creating a Report File from Multiple Source Files... 344 Controlling Your Analyzer From Your PC... 351 Setting up Bluetooth... 355 Connecting the Bluetooth device to your XRF Analyzer... 361 Troubleshooting Your Connection... 374

Thermo Scientific

Chapter 14

Interfacing Thermo Scientific Niton Analyzers and the Trimble/ArcPad GIS System383 Setting Up Your Trimble Handheld... 383 Setting Up Your Analyzer... 388 Installing ArcPad GIS Software To Your PC... 389 Deploying ArcPad to the Trimble and Setting Up GPS... 398 Setup the ArcPad Port for Receiving Data from the Analyzer... 403 Installing the Analyzer Applet... 406 Using the Analyzer Applet... 409 Trimble-Niton Error Messages... 414

Chapter 15

Parts...417 Parts and Accessories... 417

Chapter 16

Extend-a-Pole...431 Setting Up the Extend-a-Pole... 431

Chapter 17

Test Stands...441 The Portable Test Stand... 441 The Mobile Test Stand... 449 Configuring the Analyzer for the Test Stand... 451 The Field Mate Test Stand... 457 Configuring the Analyzer for the Test Stand... 465 Reference Samples... 467 Electronics Metals Reference (Standard) Sample Care... 470 Lead Paint Reference (Standard) Sample Care... 471 Small Spot Reference (Standard) Sample Care... 472

manual-name

3

Contents

Chapter 18

4

manual-name

Learning More, Service, and Support...475 Tips and Troubleshooting... 476 Registration and Licensing FAQ... 482 Storing and Transporting Your Niton XL3 Analyzer... 486 Advanced Settings... 489 Tools Menu Options... 512 NDF Files: User Data Structuring... 534 Pseudo-Elements... 546 TestAll Geo... 555 Safety Settings... 557 Measuring the Standard Samples... 574 Calculating Calibration Factors Using Excel... 575 Uploading Calibration Factors from your PC... 581 Camera and Small Spot Video... 596 Reference Documents... 607 Service... 647 Warranty... 647

Thermo Scientific

Contact Us

Americas

Europe

Asia

[email protected] [email protected]

[email protected]

[email protected] [email protected]

1

0 Contact Us

2

Niton XL3 Analyzer User’s Guide

Thermo Scientific

1 Manual Overview Warnings, Cautions, and Notes

Manual Overview Warnings, Cautions, and Notes Warnings Warnings are extremely important recommendations, violating which may result in either injury to yourself or others, or damage to your analyzer and/or data. Warnings will always be identified as Warnings in the text, and will always be visually presented as follows: WARNING This is a Warning.

Example Warning: WARNING Tampering with the 5,500 ppm (Lead high) lead-in-soil standard may cause exposure to lead dust. Keep all standards out of reach of children.

Cautions Cautions are important recommendations. Cautions will always be identified as Cautions in the text, and will always be visually presented as follows: CAUTION This is a Caution.

Example Caution: CAUTION Never tamper with Test Standards. They should not be used unless they are completely intact

Notes Notes are informational asides which may help you with your analyses. Notes will always be identified as Notes in the text, and will always be visually presented as follows: Note This is a Note.

Example Note: Note For defensible Quality Control, keep a record of the time and precision of every calibration

Figures Figures are illustrations used to show what something looks like. Figures will always be labelled and identified as Figures directly below the Figure itself, and will always be visually presented as follows:

Thermo Scientific

Niton XL3 Analyzer User’s Guide

1

1 Manual Overview Physical Buttons

Figure 1.

This is a Figure

Physical Buttons Physical Buttons are actual buttons on the analyzer which must be pushed to activate their function. Physical Buttons will always be identified as Buttons in the text, and will always be visually presented as follows: This is a Physical Button.

Example Physical Buttons: On/Off/Escape Button, Clear/Enter Button, Interlock Button, and Trigger Button.

Other Hardware Other Hardware refers to any physical part of the analyzer which performs a necessary function. Other Hardware will always be visually presented as follows: This is an example of Other Hardware.

Example Other Hardware: Battery, Touch Screen Display, Measurement Window, and USB Cable

2

Niton XL3 Analyzer User’s Guide

Thermo Scientific

2 Using Your Analyzer Safely and Effectively Using Your Analyzer

Using Your Analyzer This section discusses the basics of using your analyzer, no matter the specific type of analysis you wish to perform. First we go over analyzer safety, particularly radiation safety. Using an X-ray based analyzer safely is very important, and not difficult, provided you read, understand, and follow these guidelines. Secondly, we outline the startup procedure we recommend for daily use to ensure that your analyzer is performing properly and at its most efficient level.

Safely and Effectively Using Your Analyzer

CAUTION Niton analyzers are not intrinsically safe analyzers. All pertinent Hot Work procedures should be followed in areas of concern.

Radiation and General Safety WARNING Always treat radiation with respect. Do not hold your analyzer near the measurement window during testing. Never point your analyzer at yourself or anyone else when the shutter is open.

Radiation and General Safety This section covers topics related to radiation safety and general safety when using a Thermo Scientific Niton XL3 analyzer. At a minimum all operators of the analyzer should be familiar with the instructions provided in this chapter in order to handle the analyzer in a safe manner. In addition to reading the information presented on the following pages, Thermo Fisher Scientific recommends that instrument users participate in a radiation safety and operational training class.

Radiation Protection Basics The Niton Model XL3t analyzer contains an x-ray tube which emits radiation only when the user turns the x-ray tube on. When the x-ray tube is on and the shutter is open, as during a measurement, the analyzer emits a directed radiation beam - see Figures 1 and 2. Reasonable effort should be made to maintain exposures to radiation as far below dose limits as is practical. This is known as the ALARA (As Low as Reasonably Achievable) principle. For any given source of radiation, three factors will help minimize your radiation exposure: Time, Distance, and Shielding. The Niton Model XL3p analyzer contains a radioactive sealed source. Radiation from this source is fully contained within the device when not in use and allowed to escape through the measurement window only while the user is analyzing a sample. Radiation emission is controlled by a shutter. The analyzer emits a directed radiation beam (See Figure 1 and Figure

Thermo Scientific

Niton XL3 Analyzer User’s Guide

3

2 Using Your Analyzer Safely and Effectively Using Your Analyzer

2) when the shutter is open during a measurement. Reasonable effort should be made to maintain exposures to radiation as far below dose limits as is practical. This is known as the ALARA (As Low as Reasonably Achievable) principle. For any given source of radiation, three factors will help minimize your radiation exposure: Time, Distance, and Shielding.

Time The longer you are exposed to a source of radiation the longer the radiation is able to interact in your body and the greater the dose you receive. Dose increases in direct proportion to length of exposure.

Distance The closer you are to a source of radiation, the more radiation strikes you. Based on geometry alone, dose increases and decreases with an inverse-squared relation to your distance from the source of radiation (additional dose rate reduction comes from air attenuation). For example, the radiation dose one foot from a source is nine times greater than the dose three feet from the source. Remember to keep your hands and all body parts away from the front end of the analyzer when the shutter is open to minimize your exposure.

Shielding Shielding is any material that is placed between you and the radiation source. The more material between you and the source, or the denser the material, the less you will be exposed to that radiation. Supplied or optional test stands are an additional source of shielding for analysis. A backscatter shield accessory is also available and may be appropriate in some applications.

Exposure to Radiation Human dose to radiation is typically measured in rem, or in one-thousandths of a rem, called millirem (mrem), 1 rem = 1000 mrem. Another unit of dose is the Sievert (Sv), 1 Sv = 100 rem. The allowable limit for occupational exposure in the U.S (and many other countries) is 5,000 mrem/year (50 mSv/year) for deep (penetrating) dose and 50,000 mrem/year (500 mSv/year) for shallow (i.e., skin) dose or dose to extremities. Deep, shallow, and extremity exposure from a properly used Niton XL3t analyzer should be less than 200 mrem per year, (2.0 mSv per year) even if the analyzer is used as much as 2,000 hours per year, with the shutter open continuously. The only anticipated exceptions to the 200 mrem maximum annual dose are: 1) routine and frequent analysis of plastic samples without use of a test stand, backscatter shield, or similar additional protective measures, or 2) improper use where a part of the body is in the primary beam path. Note NEVER OPERATE THE DEVICE WITH A PART OF YOUR BODY IN THE PRIMARY BEAM PATH OR WITH THE PRIMARY BEAM PATH DIRECTED AT ANYONE ELSE.

4

Niton XL3 Analyzer User’s Guide

Thermo Scientific

2 Using Your Analyzer Safely and Effectively Using Your Analyzer

Also, consider the use of protective accessories such as a shielded test stand or backscatter shield (or equivalent) when performing routine and/or frequent analysis of any of the following: • plastic (or similarly low density) samples, • thin samples (such as foils, circuit boards, and wires) • samples that are smaller than the analysis window. Shown in Table 1are the typical background radiation doses received by the average member of the public. The radiation dose limits for radiation workers in the US are also shown in Table 2. Table 1. Typical Radiation Doses Received (Source: NCRP 1987)

Thermo Scientific

Category

Dose in mrem

Dose in mSv

Average total dose in US (annual)

360

3.6

Average worker exposure (annual)

210

2.1

Average exposure for an underground miner

400

4.0

Exposure for airline crew (1,000 hours at 35,000 ft)

500

5.0

Additional from living in Denver at 5300’ (annual)

25

.25

Additional from 4 pCi/l radon in home

1,000

10.0

Typical Chest X-Ray

6

0.06

Typical Head or Neck X-Ray

20

0.2

Typical pelvis/hip x-ray

65

0.65

Typical lumbar spine x-ray

30

0.3

Typical Upper G.I. x-ray

245

2.45

Typical Barium enema x-ray

405

4.05

Typical CAT scan

110

1.10

Niton XL3 Analyzer User’s Guide

5

2 Using Your Analyzer Monitoring your radiation exposure

Table 2. Annual Occupational Dose Limits for Radiation Workers

(Source: Code of Federal Regulations Title 10, Part 20) Category

Dose in mrem

Dose in mSv

Whole Body

5000

50

Pregnant Worker (during gestation period)

500

5

Eye Dose Equivalent

15,000

150

Shallow dose equivalent to the skin or any extremity or organ

50,000

500

Maximum allowable dose for the general public (annual)

100

1.0

For a Minor

500

5.0

Monitoring your radiation exposure Individuals can be monitored for the radiation dose they receive by use of radiation dosimetry devices (dosimeters). Monitoring dose using a dosimeter can be a way of identifying improper use and at the same time demonstrating proper use. In some locations, dosimetry is required by regulations and in others it is optional. It is normally required when the user could reasonably be expected to receive in excess of 10% of the annual dose limit. Thermo Fisher Scientific recommends that you determine and obey the local regulatory requirements concerning radiation monitoring of occupational workers. Two common types of dosimeters are whole-body badges and ring badges. Whole body badges are often attached to the user’s torso (e.g., clipped to the collar, shirt pocket, or waist as appropriate). A ring badge is worn on the finger as a measure of maximum extremity dose. When worn, the specific location of the dosimeter should be that part of the body that is expected to receive the highest dose. This location will depend on how the analyzer is used and so it may not be the same for all users. Dosimetry services are offered by many companies. Two companies offering dosimetry services in the USA and much of the world are:

6

Niton XL3 Analyzer User’s Guide

Thermo Scientific

2 Using Your Analyzer Monitoring your radiation exposure

Table 3. Dosimeters

Company

Global Dosimetry Solutions

Landauer, Inc.

Address

2652 McGaw Avenue

2 Science Road

City and State

Irvine, CA 92614

Glenwood, IL 60425-9979

Website

www.dosimetry.com

www.landauerinc.com

Phone Number

(800) 251-3331

(800) 323-8830

Note Wearing a dosimeter badge does not protect you against radiation exposure. A dosimeter badge only measures your exposure (at the dosimeter location).

Pregnancy and Radiation Exposure International guidance documents (e.g., ICRP Publication 60 and NCRP Publication 116*) recommend that the radiation dose to the embryo/fetus of a pregnant woman should not exceed a total of 500 mrem (10% of normal radiation worker limit) during the gestation period. While this dose limit exceeds the dose limit to a trained operator, pregnant workers may want to take special precautions to reduce their exposure to radiation. For more information see the U.S. NRC Regulatory Guide 8.13 "Instruction Concerning Prenatal Radiation Exposure" which can be found on the resource CD. * The International Commission on Radiological Protection, ICRP, is an independent Registered Charity, established to advance for the public benefit the science of radiological protection, in particular by providing recommendations and guidance on all aspects of protection against ionizing radiation. * The National Council on Radiation Protection and Measurements (NCRP) was chartered by the U.S. Congress in 1964 as the National Council on Radiation Protection and Measurements.

How to Use the Niton XL3t Analyzer Safely The Niton XL3t analyzer is designed to be safe to operate provided that it is used in accordance with manufacturer's instructions. Under conditions of normal use, monitored operators seldom receive a measurable dose and have not been known to receive in excess of 10% of the annual occupational dose limits (a criteria that would require monitoring under regulation in the U.S.). In addition to proper use of the XL3t, it is recommended that you follow these precautions to ensure your safety and the safety of those around you.

Know where the beam is The primary beam is a directed beam out of the front of the analyzer that can have high dose rates. The secondary beam, or scattered beam, has much lower dose rates.

Thermo Scientific

Niton XL3 Analyzer User’s Guide

7

2 Using Your Analyzer Monitoring your radiation exposure

Figure 2.

8

Niton XL3 Analyzer User’s Guide

Primary Beam

Thermo Scientific

2 Using Your Analyzer Monitoring your radiation exposure

Figure 3.

Thermo Scientific

Secondary (Scattered) Beam

Niton XL3 Analyzer User’s Guide

9

2 Using Your Analyzer Monitoring your radiation exposure

The Shutter-Open Indicator Lights When the lights are flashing, the primary beam is on, and radiation is being emitted from the front of the analyzer.

Figure 4.

The X-ray Beam Indicator Lights

Handle and Use with Respect Avoid holding the front of the analyzer when the x-ray tube is energized and the shutter is open. Never point the instrument at yourself or anyone else when the shutter is open and the x-ray tube is energized. Never look into the path of the primary beam.

Follow a Radiation Protection Program Your organization should establish, document, and follow a Radiation Protection Program. An example of such a program can be found on the resource CD (provided with the instrument).

Take Proper Care of your Niton XL3 Keeping your analyzer maintained in good condition will help minimize the risk of accidental exposure. Mechanical malfunction of the shutter can be avoided by maintaining the measurement window, as described in the User Guide. This prevents foreign objects from entering your analyzer

10

Niton XL3 Analyzer User’s Guide

Thermo Scientific

2 Using Your Analyzer Safe Handling of Samples

Avoid Over-Exposures Direct contact with the window could result in overexposures in the times indicated inTable 4 below.

Table 4. Potential Exposure Limit Times

Location of Dose Limit

Time to Reach Limit

Deep Dose / Whole Body

5 rem (50 mSv)

2.1 minutes

Shallow Dose / Extremities

50 rem (500 mSv)

0.95 minutes

Member of Public (i.e. untrained operator)

0.1 rem (1 mSv)

2.5 seconds*

Extremity is defined by the NRC as the hand, elbow, arm below the elbow, foot, knee, or leg below the knee. Whole Body is defined by the NRC as the head, trunk (including male gonads), arms above the elbow, or legs above the knee. *Based on maximum deep dose rate and US exposure limit.

Safe Handling of Samples As mentioned many times in this chapter, never place any part of your body in the path of the x-ray beam. There is always a safe way to handle samples whether they are small, irregularly shaped, or of low density. Never look into the path of the primary beam.

Small Samples A small sample would be any sample that is smaller than the measurement window. Small samples present a unique risk because they don’t block the entire beam path. The difficulty with placing small samples down on a work surface to analyze them is that you may get readings from the work surface that interfere with analytical results. A test stand is an effective way of analyzing small samples accurately and safely. Never hold samples during analysis or look into the path of the primary beam.

Thermo Scientific

Niton XL3 Analyzer User’s Guide

11