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XRF Instrument Operating Instructions - English

The document outlines the operating procedures for XRF measuring instruments, aiming to standardize their operation and ensure safety and accuracy in testing. It includes sections on the purpose, scope, responsibilities, and detailed instructions for operating the XRF device, including sample preparation, measurement steps, and environmental requirements. The document also contains a change history and is effective as of November 22, 2023.
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0% found this document useful (0 votes)
14 views17 pages

XRF Instrument Operating Instructions - English

The document outlines the operating procedures for XRF measuring instruments, aiming to standardize their operation and ensure safety and accuracy in testing. It includes sections on the purpose, scope, responsibilities, and detailed instructions for operating the XRF device, including sample preparation, measurement steps, and environmental requirements. The document also contains a change history and is effective as of November 22, 2023.
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd

Document No.

41QAD-WI-111
XRF Device Work Instructions Document Number
Version
B2
Revision Number
XRF Instrument Operating page number
1of 17
Sheet Number
Instructions Effective
22 -Nov-202
Date
Effective Date 3

Revision
Written by Version Change History
Date
Originator Revision Change History
Amend Date
Version upgrade;
Ma Wanqiu A3 12-Oct-2016
Added 5.17.3
Robin Xu A4 Added 5.20.8 XRF storage period 1-Mar-2019

Robin Xu A5 Added [Link] Macallan project ink dry test 23-Dec-2019

Robin Xu B0 Update 5.20.8 Temperature Units 30-July-2021


Fengxiaojin
B1 Update 5.20.8 Increase the storage of liquids 16-Nov-2021
g
22 -Nov-202
Sylvia Liu B2 Updated 5.7 & 5.19.7 standard block self-calibration data
3

approve Name date


Approved Name Date
General Manager

CS Manager

Countersig HR Manager
n QA Manager - Flexo
Signature
QA Manager -RDC Yu Yang 202 3 -11- 22

MFG Manager
Document No.
41QAD-WI-111
XRF Device Work Instructions Document Number
Version
B2
Revision Number
XRF Instrument Operating page number
2of 17
Sheet Number
Instructions Effective
22 -Nov-202
Date
Effective Date 3

Table of contents
TABLE OF CONTENTS

Chapter title page


Number Contents number
Section Page
1.0 Purpose P3

2.0 Scope P3

3.0 Definitions P3

4.0 Responsibility P3

5.0 Contents P3

6.0 Reference Documents P15

7.0 Related Records P15

8.0 Reference Records P15

9.0 Process Flow Charts P15

10.0 Appendix P15


Document No.
41QAD-WI-111
XRF Device Work Instructions Document Number
Version
B2
Revision Number
XRF Instrument Operating page number
3of 17
Sheet Number
Instructions Effective
22 -Nov-202
Date
Effective Date 3

1.0Purpose:
The purpose of this document is to standardize the operating procedures of XRF measuring
instruments to enable them to operate normally and safely and ensure the correctness of the test
process.

2.0Scope:
The scope of this document is operating systems applicable to XRF measurement instruments.

3.0Definitions:
XRF full name: Energy Dispersive X-ray Fluorescence Spectrometer.

4.0Responsibility:
IQC staff: responsible for the operation and daily maintenance of the instrument, and will manage
the relevant XRF test records .

5.0Contents:
5.1 Qualification of XRF operators
5.1.1 XRF operators must obtain a "Radiation Personnel Work Permit" and an "Operation
Qualification Certificate" before they can take up their posts.
5.2 Requirements for the environment in which the XRF instrument is used
5.2.1 Temperature is controlled at 23±5 ℃ , humidity is controlled at 30%-70%RH
5.2.2 AC 220±5V.
5.3 XRF Instrument Software Introduction
5.3.1 Main interface
[Link] Login interface, double-click the desktop XRF to run the software and enter the
login interface. The software login interface (Figure 1) selects the user name and
password to enter the main interface of the software.
Document No.
41QAD-WI-111
XRF Device Work Instructions Document Number
Version
B2
Revision Number
XRF Instrument Operating page number
4of 17
Sheet Number
Instructions Effective
22 -Nov-202
Date
Effective Date 3

Figure 1
5.3.2 System main interface

[Link] The main interface of the system mainly consists of the following parts: menu bar,
toolbar, status bar, work area, spectrum display area, video acquisition area, history
record area, result area, etc., as shown in (Figure 2).
[Link].1 Menu bar: Work spectrum, qualitative analysis, analysis report, language,
help.
[Link].2 Toolbar: Halogen, Continuous Measurement History, Connect Instrument,
Initialize, Stop, Start, Store Name
Rules, standard library, suppliers, parameter configuration, preheating.
[Link].3 Status bar: equipment, working curve, working spectrum, qualitative
analysis.
[Link].4 Working area: There are six working areas, and different working areas
are selected for different samples.
[Link].5 Spectrum display area: displays the currently tested or opened spectrum.
[Link].6 History Record Area: Displays information of the tested spectra.
[Link].7 Video acquisition area: set video, obtain sample images, etc.
[Link].8 Result display area: displays measurement results or calculation results.
Document No.
41QAD-WI-111
XRF Device Work Instructions Document Number
Version
B2
Revision Number
XRF Instrument Operating page number
5of 17
Sheet Number
Instructions Effective
22 -Nov-202
Date
Effective Date 3

Figure 2
5.4 Splitting of XRF test samples:
5.4.1 Principles for sample splitting: The samples to be tested must be split into materials with
uniform components or multi-component materials that cannot be disassembled, degraded or
split into different materials by mechanical operations (such as twisting, cutting, punching,
grinding, filing).

[Link] Split the surface material, peel off the backing paper of the surface material, and
measure the backing paper; measure the surface material after peeling off the
backing paper; measure the surface material without glue.
[Link] Split the backing paper and measure directly with the measuring side facing downwards.
[Link] To separate the glue, peel off the backing paper of the glue and place the measuring side facing
downwards.
[Link] To disassemble the protective film, peel off the bottom film of the protective film and place the
measuring surface downward.
[Link] Split the ink and pour the ink into a special sample cup for measurement to carry out
measurement.
[Link] To split the finished product, peel off the backing paper on the finished product and place the
measuring surface facing downward.

[Link] Split the carbon ribbon and measure it directly with the measuring side facing downwards.
[Link] For Macallan projects, ink and glue (liquid) need to be dried before testing. UV ink is
applied on the glass to simulate the UV energy lamp of the production line for ink drying
and testing. Ordinary ink and glue are applied on the glass to simulate the production
line oven temperature of 85℃ for 15 minutes and then tested. If there are special
requirements, the baking time is extended until the ink and glue are dried, and after
drying, they are peeled from the glass for testing.

5.5 XRF instrument operating instructions


5.5.1 Turn on the power switch and the power switch on the instrument in sequence, and start the
program.
5.5.2 Preheat the instrument.
5.5.3 Operation mode setting.
5.5.4 Initialization and testing.
5.5.5 After the test, turn off the instrument power switch, the power switch, and the program.
5.6 Operation mode setting
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[Link] measuring instrument has seven operating modes


[Link] Determination of CrCI in plastics,
[Link] Determination of CrCdPbHg in steel
[Link] Determination of CrCdPbHg in non-ferrous metals
[Link] Measurement of CrCdPbHg in solder
[Link] Testing plastics and others
[Link] Determination of CrCdPbHc in magnesium and aluminum

[Link] Titanium content measurement CI

5.6.2 Select one of the seven operating modes by clicking on the program.
[Link] Determination of CrCI in plastics Used to measure the CrCI element,
[Link] Determination of CrCdPbHg in steel Used to measure CrCdPbHg elements.
[Link] Determination of CrCdPbHg in non-ferrous metals Used to measure CrCdPbHg
elements,
[Link] CrCdPbHg in solder is used to measure CrCdPbHg elements.
[Link] Plastic glue and other elements used to measure CrAsBrCdHgPb,
[Link] Determination of CrCdPbHc in magnesium and aluminum is used to measure the
CrCdPbHc elements.
[Link] Titanium content measurement CI measurement is used to measure CI elements.
Note: Conventional tests include [Link] for testing plastics and others and [Link] for testing
titanium and Cl.

5.6.3 Select the operation mode according to the properties of the material (Figure 3)

Figure 3

5.7 XRF control specifications, refer to " XRF test judgment warning standards" ( unit: ppm)
5.8 Measurement device
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5.8.1 Measurement-specific pure silver calibration sheet, used to initialize the instrument
5.8.2 When measuring raw materials containing glue, the special test film must be replaced after
the measurement.
5.8.3 Special sample cup for measurement. The sample cup is used to measure liquids and
particles. Pour the liquid or particles into the sample cup for measurement and end the cleaning.
Sample cup
5.9 Measurement stroke setting
5.9.1 The measurement time is set to 200s
5.9.2 When the measurement is completed, the program stops automatically and the measured
material is taken out.
5.10 Sample preparation before measurement:
5.10.1 Sample conditions. Ideally, the sample to be tested should meet the following conditions:
[Link] Have sufficient thickness (3mm-5mm or more for plastics, 1MM or more for metals, and 15mm or
less for liquids.
[Link] The size of the sample must be >3CM*3CM.
[Link] Samples that are too thin need to be stacked to a certain thickness before measurement.
[Link] The specimen is uniform.
[Link] The surface should be flat, smooth and free of cracks.
[Link] If the client or applicant has special requirements, XRF testing shall be carried out in
accordance with the client or applicant’s requirements.
5.11 XRF measurement steps
5.11.1 Connection

[Link] First check the connection between the power supply, computer and instrument to make sure
they are correct.
5.11.2 Instrument preheating
[Link] Turn on the machine, put in any sample, and click the "Preheat" button (Figure 4).
Set the preheating time (30 minutes), and click "OK" (Figure 5).

Figure 4
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Figure 5

5.11.3 Initialize the instrument

[Link] Click the "Initialize" button in the toolbar (Figure 6), place the pure silver standard
into the sample chamber according to the prompts, and click
“OK” (Figure 7).

Figure 6

Figure 7
[Link] After the initialization is successful, it will prompt that the initialization is successful
(Figure 8), otherwise it will prompt that the initialization failed (as shown in Figure 9).
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Figure 8 Figure 9

Note: Initialization is a very important step before testing the sample spectrum. Initialization can
restore all aspects of the instrument to their proper settings and restore all elements to the
correct energy channel.

5.12 Select Workspace


5.12.1 Select the correct working area according to the sample type (Figure 3)
5.13 Measurement
5.13.1 Place the sample in the measuring area of the instrument (the rubber surface cannot touch
hands or other materials). You can check whether the sample is within the measuring range
of the instrument through the sample diagram (Figure 10). You can also observe the sample
during the test.

Figure 10

5.13.2 Click the Start Test button (Figure 11)

Figure 11
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5.13.3 Enter the relevant information of the measurement sample in the following dialog box, and

then click OK (Figure 12)


Figure 12

Note: Please do not start the sample name with “* / \ ? | < > :”.

[Link] If the sample name you input has the same name as an existing spectrum line, the system will
pop up a prompt (Figure 13)

Figure 13

[Link] If you need to replace, click "OK" and then start the test; if you do not need to replace, click
"Cancel" and re-enter
Sample name.
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5.14 After the test is completed, the current test is completed (Figure 14)

Figure 14
5.14.1 The test results can be seen in the test results column and the history column (Figure 15)

Figure 15
5.14.2 The test result column shows PASS. If the test result is unqualified, it will show Fail. The tester should
Select the corresponding standard procedure to test again, and the test result shall be subject to the result of
the retest.
_ _ _ means the content is less than 2ppm or does not contain this element, ''_ _ _'' means the element has
not been tested.
fruit.
5.15 Print & Save Report
5.15.1 Click on the analysis report and save it successfully (Figure 16)

Figure 16
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5.15.2 Open the report, write the operator's name in the operator column, and print it out (Figure 17)

Figure 17

5.15.3 Open the analysis report, the save path is usually set to the public disk by default, you

can edit it if necessary, click the small icon '' '' to confirm (Figure 18)
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Figure 18

5.15.4 Above, the XRF operation process is completed and the instrument is turned off.
5.16 Data Judgment Principles
5.16.1 If the content is less than the specification value, it is judged as qualified. The machine
automatically judges (see Figure 17)
5.16.2 If the content is greater than the specification value, it is judged as unqualified and the machine
automatically judges (Figure 17)
5.16.3 Each customer’s XRF has been set up in the XRF machine in accordance with each
customer’s specifications as defined in the “Prohibited Substances XRF Control Specifications”.
5.17 Management and requirements of XRF test records;
5.17.1 Define the <Hazardous Substance Analysis Report> in the XRF system, which must include
the sample name, supplier batch, tester, limit value, measurement
Results, graphs.
5.17.2 Save the <Hazardous Substance Analysis Report> to the public disk in the path X:\QA\Shared\
SQA\01 IQC\16 Hazardous Substance Test
Test report.
5.17.3 When the XRF test result fails, the sample needs to be retested. The retest OK result and the first
test result are saved in the same file for easy traceability. If the retest fails, the abnormality
must be reported to the supervisor and HSF specialist immediately.
5.18 Maintenance and annual calibration of XRF testing equipment,
The instrument needs to be externally calibrated once a year; the standard block used for self-
calibration needs to be calibrated once a year.
5.19 For daily inspection, please refer to "PSD-QP-06-001 A Equipment Preventive Maintenance
Inspection Daily Record Form"
5.19.1 Is the machine turned on? (Yes√, NoX)
5.19.2 Check all parts for abnormalities
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5.19.3 Turn on the power and check whether the indicator lights are normal.
5.19.4 The machine must be turned on and preheated for 30 minutes on the day of testing.
5.19.5 Are there any abnormalities during the trial run?
5.19.6 Do not block the heat dissipation holes of the instrument or hinder the heat dissipation of the
instrument
5.19.7 Standard block self-calibration data
Cr 100±10
As 29.1±10
Br 770±77
Cd 137±13.7
Hg 23.7±10
Pb 98±10
Cl 666±66.6
5.19.8 Complete cleanup after shutdown
5.20 Notes:
5.20.1 During sampling and splitting of samples, personnel must wear PE gloves or use tweezers to
pick up samples.
5.20.2 The instrument protective cover must not be opened during the test;
5.20.3 During the cleaning process, it is strictly forbidden to use hands or other materials to touch
and contaminate the X-ray tube and detector window;
5.20.4 Do not place flammable items near the instrument
5.20.5 Do not block the heat dissipation holes of the instrument or hinder the heat dissipation of
the instrument
5.20.6 The preheating process is essential for the instrument when it is just turned on. Preheating
can help the instrument enter the working state better.
To ensure the stability of the instrument test state and the reliability of the test results
5.20.7 If any abnormality is found in the instrument during daily equipment inspection and daily
operation, the test should be stopped immediately, and the abnormality should be reported
to the superior and handled in accordance with the "Monitoring and Measuring Equipment
Control Procedure". At the same time, the product should be handled in accordance with
the "Non-conforming Product Control Procedure".
5.20.8 XRF sample storage: storage temperature 23±5 ℃ , humidity 50±20%, shelf life is project EOL+1
year. Samples are stored in PE bags, liquid samples are stored in PP cans , and each
sample is marked with the material number , test time, and material batch information on
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the PE bag or PP can .


5.21 Verification of XRF operation accuracy. The accuracy of XRF detection is 30%.
5.21.1 When IQC tests new materials, it is necessary to compare them with the third-party test
reports. If the deviation of the test results exceeds 30%, the supplier must be required to
adjust the test intensity of the XRF tester to ensure that the test deviation does not exceed
30%.
5.22 Self-calibration operation method
5.22.1 Use the EDXRF software and log in as an administrator;

Figure 19
5.22.2 Select the corresponding curve to measure plastic and others, put in the Ag sheet, and
initialize;

Figure 20
5.22.3 After successful initialization, insert EC681K, click Start and create a new name for testing;
5.22.4 After the test is completed, click on the working curve to edit the data and find the newly
created test sample name and enter it in sequence
Apply to open the chart and observe the curve. If the curve is generally upward, it means that the
instrument is measuring
If the measurement is accurate, press OK and the self-calibration is finished.
Document No.
41QAD-WI-111
XRF Device Work Instructions Document Number
Version
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Revision Number
XRF Instrument Operating page number
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Instructions Effective
22 -Nov-202
Date
Effective Date 3

Figure 21

Figure 22

Figure 23
5.22.5 If the measurement curve is not upward as a whole, it means that the instrument is faulty and
the abnormality should be reported to the superior.
At the same time, the products are handled in accordance with the "Non-conforming Product Control
Procedure".

6.0Reference Documents:
6.1 QAD-SOP11 Hazardous Substance Management Standards
6.2 QAD-SOP03 《 Measurement and Monitoring Equipment Management Procedure 》
6.3 41QAD-QP-03 "Non-conforming Product Control Procedure"

7.0Related Records:
7.1 41QAD-WI-111-001 [Hazardous Substance Analysis Report]
7.2 41QAD-WI-111-002 [Raw material XRF test record]
Document No.
41QAD-WI-111
XRF Device Work Instructions Document Number
Version
B2
Revision Number
XRF Instrument Operating page number
17of 17
Sheet Number
Instructions Effective
22 -Nov-202
Date
Effective Date 3

7.3 QR-41QAD-WI-111-03 [Raw material X RF test record sheet_Flexo ]


7.4 QR-41QAD-WI-111-04 【 Ink XRF Test Record_Flexo 】

8.0Reference Records:
8.1 QR-MSD-SOP01-04 < Declaration of Environmentally Controlled Substances >

9.0Process Flow Charts:


N/A

10.0 Appendix:
N/A

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