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ProLab Plus Manual The software package for method interlaboratory tests and proficiency tests Version 2.14

ProLab Plus Manual

The software package for method interlaboratory tests and proficiency tests

Version: 2.14

For Windows NT, Windows 2000, Windows XP, Windows Vista and Windows 7

December 2011

quo data GmbH Kaitzer Straße 135 D-01187 Dresden Germany

phone: +49 351 402 88 67 0

fax:

+49 351 402 88 67 19

Email: info@quodata.de www.quodata.de

Software development Dipl.-Ing. Norbert Schick Omri Teufert Robert Walther Daniel Rothmaler Sebastian Falk Dipl.-Phys. Christian Bläul PD Dr. Steffen Uhlig

Manual Dipl.-Math. Sabine Antoni Kirsten Simon Meike Schreitz PD Dr. Steffen Uhlig

The software described in this manual must only be used or copied according to the terms and conditions of the license agreement.

Copyright 1998-2011: PD Dr. Steffen Uhlig, Dresden

copied according to the terms and conditions of the license agreement. Copyright 1998-2011: PD Dr. Steffen

Contents

1 Introduction

5

2 Preparation

7

2.1 System requirements

7

2.2 Installation

7

2.3 Use of interlaboratory test data of older ProLab Plus versions

8

2.4 Hotline

8

3 Overview

9

4 General information

12

4.1 Mouse functions

12

4.2 Database handling

12

4.3 Important buttons

12

4.4 Overview of buttons in main window

13

5 Selecting ring tests

14

5.1

Putting ring tests in edit mode

14

6 File menu

16

6.1

Settings in reports, tables and charts

16

6.1.1 General settings

16

6.1.2 Report settings

17

6.1.3 Caption settings

18

6.2 Start report

19

6.3 Log info

19

6.4 New database

20

6.5 Change database

20

6.6 Backup file

21

6.6.1 Restore from file

21

6.6.2 Store database to file

21

6.6.3 Advice for long-term storage

21

7 Database menu

22

7.1 Ring test selection

22

7.2 Basic tables

22

7.2.1 How to work with the tables

22

7.2.2 Ring tests

27

7.2.3 Samples

28

7.2.4 Measurands

29

7.2.5 Laboratories

30

7.3 Structure of ring test

31

7.3.1 Laboratory allocation

32

7.3.2 Sample-measurand allocation

33

7.3.3 Sample-measurand-laboratory allocation

34

7.4 Encoding

37

7.4.1 Encoding laboratories

37

7.4.2 Encode test portions

38

7.5 Participating labs and data yet to be submitted

40

7.6 Characteristics of measurands

41

7.7 Test results

43

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7.8

Creation of corrected measurands

45

7.9 Analytical methods and sample preparations

46

7.10 Duplicate ring test

48

7.11 Export

48

7.11.1 Test results as CSV file

48

7.11.2 Laboratory files

50

7.11.3 Ring test

54

7.11.4 Email merges

55

7.12 Import

61

7.12.1 Import of structure with or without test results

61

7.12.2 Addresses, Measurands & samples, Analytical methods/Sample preparations

64

7.12.3 Ring test

64

8 Test on homogeneity and stability

65

8.1 Import test results

65

8.2 Encoding test portions

66

8.2.1 Uniform encoding of all test portions (for laboratories and for homogeneity analysis) and

66

8.2.2 Random selection of test portions for homogeneity test without encoding test portions for

random selection of homogeneity test portions

laboratories

69

8.2.3

Another example for encoding test portions

70

8.3 Test results

71

8.4 Computation

72

8.4.1 Assignment of test portions

72

8.4.2 Homogeneity

72

8.4.3 Stability

76

9 Data selection

79

9.1 Overview

79

9.2 Sample-measurand selection

79

9.3 Sample-measurand-laboratory selection

81

9.4 Save and load selection

83

10 Statistics

84

10.1 Overview

84

10.2 Ring test parameters

84

10.2.1 Option for DIN 38402 A 45: logarithmic calculation

87

10.2.2 Determine assigned value

88

10.2.3 Determine target

90

10.2.4 Variance function

91

10.3 Computation of Z-scores

92

10.3.1 Computation tab

92

10.3.2 Score values tab

95

10.3.3 Results tab

96

11 Charts and tables

98

11.1

Summary results

99

11.1.1 Right side bar

101

11.1.2 Menu Format

102

11.1.3 Menu Output

102

11.2 Survey of scores

104

11.3 Combination scores

106

11.3.1 Chart of RLP and RSZ

106

11.3.2 Laboratory assessment based on RLP

112

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11.3.3

Distribution of Z scores

118

11.3.4 Control chart and extended evaluation

11.4 Test on equivalence

123

123

11.4.1 Introduction

123

11.4.2 Define classes of methods

124

11.4.3 Recovery equivalence

126

11.4.4 Reproducibility equivalence

127

11.4.5 Repeatability equivalence

128

11.4.6 Sample specific method effects

128

11.4.7 Survey of methods

129

11.4.8 Export of results

129

11.5 Tolerance limits and rel. standard deviations

129

11.6 Youden plot

130

11.7 Histogram and normal plot

133

11.8 Chart of lab means and repeatability standard deviation

136

11.9 Kernel density estimator (KDE)

138

11.10 HORRAT trend

141

11.11 Principal Component Analysis (PCA)

143

11.12 Mandel’s h

& k statistics

145

11.13 Laboratory mean values

148

11.14 Further reports

149

12 Quick

start: The steps of statistical analysis

151

13 Some aspects of the statistical methods in ProLab Plus

156

13.1 When can the method of the Swiss food manual be applied?

156

13.2 When can Q/median, Q/Huber or DIN 38402 A45 be applied?

156

13.3 When can ISO 5725 and DIN 38402 A42 be applied?

156

13.4 When can the Horwitz function be applied?

156

13.5 When can the empirical Horwitz function be applied?

157

13.6 When can the nested design analysis according to ISO 5725-3 and ISO 5725-5 be

applied?

157

14 References

158

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ProLab Plus Manual . Introduction

5

1

Introduction

ProLab Plus is a software package specially conceived to facilitate a professional and effi- cient performance of the various tasks which arise in the context of interlaboratory tests, from statistical analysis to professional data handling. ProLab Plus can be used for the certifica- tion of reference materials, the evaluation of analytical methods and for the assessment of laboratories.

ProLab Plus will prove useful at every step of a proficiency test. It provides tools which will assist you right from the planning stage, to the realization of homogeneity tests, the automat- ic data input from laboratories, the application of statistical analysis and the generation of re- ports.

Several statistical methods are available:

- ISO 5725-2

- DIN 38402 A42 (German standard for method ring tests for water analyses)

- Swiss Food Manual

- Q-Method/Median (Robust statistical method)

- Q-Method/Huber (Robust method for proficiency tests used e.g. by the Ger- man co-operation for water analyses ‘LAWA’)

- DIN 38402 A45 (Robust Q-method and Hampel estimator)

- ISO 5725-5 (algorithm A+S)

- Nested Design 2x2 (ISO 5725-3/5)

- Nested Design (ISO 5725-3)

- (Empirical) Horwitz function

- ISO 13528

As for the assessment of laboratories, there are also several available protocols, such as the international Harmonized Protocol of IUPAC, ISO and AOAC 1 , ISO 13528, DIN 38402 A45,

CD

ISO 20612 and the LAWA 2 protocol. More specifically, the laboratories can be assessed

by

- Z scores, Z u scores, Zeta scores, Z’ scores

- Youden plots

- RSZ (Rescaled Sum of Z Scores)

- RLP (Relative Laboratory Performance)

- Percentage of successful measurements

ProLab Plus allows flexible data input, whether manual or through the import of digital files. The simple data entry program RingDat is provided which may be forwarded to the participat-

ing laboratories without extra charge. Additional information on the laboratories and the

methods can be entered into the system, such as addresses, the determination limit and the detection limit, the sample preparation method and the analytical method.

1 Michael Thompson and Roger Wood (1993), International Harmonized Protocol for Proficiency Testing of (Chemical) Analytical Laboratories. Journal of AOAC International 1993, Vol. 76, 926-940. 2 AQS der Länderarbeitsgemeinschaft Wasser für Wasser-, Abwasser- und Schlammuntersuchungen (Working Group on water issues of the federal states and the federal government)

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ProLab Plus Manual . Introduction

A powerful data selection program assists the user in the evaluation and the presentation of results, enabling him to sift data as convenient, to generate individual reports or reports for selections of laboratories, and to set up and save selection patterns. Up to four selection pat- terns per ring test can be saved.

All results are stored in the database. Comments can be saved for participants, measure- ments and within charts.

Numerous specialised chart-generating functions are provided to assist in the presentation of results, while a powerful report designer enables the generation of editable reports. Reports can be exported into the formats PDF, RTF (Word), XLS (Excel), HTML, Text and CSV. Charts can be converted into Bitmaps (BMP), Scalable Vector Graphics (SVG) and the Win- dows Meta File format (WMF).

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ProLab Plus Manual . Preparation

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2

Preparation

2.1 System requirements

The hardware and software requirements for ProLab Plus are listed in the following table.

Processor

RAM Hard disk Operating System

Intel Pentium or compatible with at least 1 GHz (> 2.4 GHz recom- mended) 512 MB > 300 MB free Windows NT (with service-pack 5), Windows 2000, XP Professional (not Windows XP Home Edition), Windows Vista and Windows 7.

ProLab Plus runs stable under Windows 7, and all calculations and reports work as ex- pected.

2.2 Installation

1. If you have an existing ProLab Plus version, please backup your current ProLab Plus program directory and your database before installing the new version into the current program directory. The path to the database is shown at the very top of the ProLab Plus window.

2. If you downloaded a setup program from our website, please run it now. If you want to in- stall ProLab using a CD, please put the CD into the drive. The setup program will start automatically. If not, please run setup.exe in the root directory of the CD.

3. Follow the installation dialogue and use the directories proposed. Upon successful instal- lation, a program group ProLab will be created, which contains ProLab, a help file for the Report Designer (Qrduser) and a program for direct input of data from laboratories (RingDat).

4. Run ProLab Plus.

5. After the first start you will see a registration dialogue with a registration number. You can phone quo data GmbH (+49 351 402 88 67 0) or send an email (info@quodata.de) and you will get the necessary key. After input of the key press “Save”.

Alternatively, you can proceed as follows. Close the program ProLab Plus. In the program directory you will find the file REGISTER.INI. Send this file via email to info@quodata.de. Within one working day, you will receive a new file REGISTER.INI with the key. This file must be copied into the program directory of ProLab, replacing the original file.

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ProLab Plus - Manual . Preparation

2.3 Use of interlaboratory test data of older ProLab Plus versions

Since ProLab 2003, a new database format is used (ADS, developed by Sybase which be- longs to SAP). The current version ProLab Plus 2.14 uses ADS 10. It is therefore not possi- ble to directly access older BDE databases. However, the conversion program „ProLabMigrator.exe" allows simple conversion of the old databases. Start this program, se- lect the directories for the BDE database and the ADS database and start the transfer.

2.4 Hotline

In case of problems use the hotline of quo data: +49 351 402 88 67 0 or send an email to:

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ProLab Plus Manual . Overview

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3

Overview

The main menu is the starting point of every evaluation using ProLab Plus. You are in the menu as soon as you successfully start ProLab Plus.

The main menu contains eight modules, which can be selected using the common Windows techniques (mouse, arrow keys or input of the corresponding character):

- File

- Database

- Homogeneity / Stability

- Selection

- Statistics

- Charts and tables

- Window

- Help

The modules are ordered in such a way that, in the performance and evaluation of a ring test, they are typically activated from left to right. One starts in the module File with the defini- tion of settings for reports and data base tables. That is followed by the description of the ring test, of the samples and measurands that are to be examined and evaluated, and of the en- coding of laboratories and samples. Once the results start coming in, they will thus be able to be imported or manually entered. All necessary functions for the latter procedure are located in the module Database. If required, a test of the homogeneity of the samples in preparation for the ring test can be conducted in the module Homogeneity / Stability, which also provides the necessary functions for any stability tests to be conducted later on. The Selection module provides all relevant tools for the selection of samples, measurands and laboratories to be included in assessment and analysis procedures or in the presentation of results. The evalu- ation, analysis and assessment procedures are then carried out in the module Statistics, while reports and charts in various layouts can be generated and displayed in the module Charts and tables. Each step within this sequence affects subsequent steps. All statistical re- sults obtained at any stage will be directly stored in the database. Earlier results of the same ring test will be overwritten automatically. If there are some modifications to implement ( e.g. in the calculation of Z scores) it is not necessary to create a new test: changing the data at the earliest relevant step is sufficient.

An overview of important functions in ProLab Plus is given in the following table.

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ProLab Plus Manual . Overview

File

Settings

Formats, general report settings and report designer

Generate database, change database, backup files

Database

Database and data input

Ring test selection

Basic tables: ring tests, samples, measurands (analytes), laboratories

Structure of ring test: assignment of laboratories and measurands

Encoding: Encoding of laboratories and samples

Participating labs and outstanding data

Characteristics of measurands: reference values, units, conversion factors et al.

Definition of analytical methods and sample preparations

Test results

Creation of corrected measurands

Duplicate ring test

Export: CSV files, laboratory files, ring test, email merge

Import: structure/test results, addresses, measurands & samples, analytical methods & preparations and ring tests

Homogeneity /

Import and analysis of homogeneity and stability test results

Stability

Import test results

Test portion encoding

Test results

Computation of homogeneity and stability

Selection

Selection of data for statistical analysis and the presentation of results

Selection of samples and measurands

Selection of samples, measurands and laboratories

Save and load selections

Statistics

Analysis and assessment

Calculation of statistical parameters of the ring test (lab means, lab s.d., overall mean, reproducibility s.d. and repeatability s.d., specification of target value and target s.d.)

Calculation of tolerance limits and single scores (Z scores, Z u scores, Zeta scores, Z’ scores)

Charts and

Charts and tables of the statistical analysis

Tables

Comprehensive presentation of results for each sample-measurand combination separately

Survey of scores

Combination scores and ring test-spanning analyses

Test on equivalence

Tolerance limits and rel. standard deviations

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ProLab Plus Manual . Overview

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Youden plot

Histogram and normal plot

Chart of repeatability standard deviations

Kernel density estimator (KDE)

HORRAT trend

Principal component analysis

Mandel’s h & k statistics

Laboratory mean values per sample and per measurand

Further reports: number of test results and labs, survey of test results, method characteristics, summary of outliers, individual reports

Help

Help function

Program update: check for new version

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ProLab Plus Manual . General hints

4 General information

4.1 Mouse functions

The main functions of the program can be activated by using the left mouse button. Some additional functions ( e.g. number of columns and column-width in tables) can be activated by using the right mouse button.

4.2 Database handling

In some forms, data sets ( e.g. measurands, ring tests, labs, samples, test results) can be accessed, edited, added or deleted. The following commands are available for this purpose:

Back

Forward

Insert

Delete

Save

Cancel

Go to the previous recordfor this purpose: Back Forward Insert Delete Save Cancel Go to the next record Insert new

Go to the next recordForward Insert Delete Save Cancel Go to the previous record Insert new record Delete selected record

Insert new recordSave Cancel Go to the previous record Go to the next record Delete selected record Save

Delete selected recordthe previous record Go to the next record Insert new record Save changes Cancel editing Please

Save changesto the next record Insert new record Delete selected record Cancel editing Please note that it

Cancel editingrecord Insert new record Delete selected record Save changes Please note that it is not possible

Please note that it is not possible to undo changes in the database. Therefore it is very im- portant to make a backup of the database at the beginning of each session, so the original database can be recovered. For the creation of the backup select File Backup file.

4.3 Important buttons

The following list explains some important buttons frequently used in the program:

Close

Closes current window.Close

Report

Click this button to display a report preview for the selected data. In many cases, it is also possible, by simultaneously holding down the SHIFT key  , to open a spreadsheet which allows data editing and storage in a way , to open a spreadsheet which allows data editing and storage in a way similar to the Excel program.

Help

Activates help for the current window.Help

Save

Click this button to save tables or charts as a file.Save

Print

Click this button to print out reports or charts.Print

Lab code

Click this button to turn switch between the laboratory name (LName) and the laboratory code (LCode) in charts and tables.Lab code

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ProLab Plus Manual . General hints

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4.4 Overview of buttons in main window

The buttons in the main-menu toolbar make it possible to easily activate the most important and commonly used functions. The following table offers an overview of these shortcuts.

Change ring test and define working mode

Change ring test and define working mode

Settings

Settings

Survey of test results

Survey of test results

Edit data of basic tables

Edit data of basic tables

Assignment of participating laboratories

Assignment of participating laboratories

Assignment of measurands to samples

Assignment of measurands to samples

Assignment of measurand-sample combinations to laboratories

Assignment of measurand-sample combinations to laboratories

Encoding laboratories

Encoding laboratories

Encoding test portions

Encoding test portions

Ring test-specific characteristics of measurands

Ring test-specific characteristics of measurands

Edit test results

Edit test results

Select sample / measurand for further use

Select sample / measurand for further use

Select sample / measurand / laboratory for further use

Select sample / measurand / laboratory for further use

Save selection

Save selection

Load previously saved selection

Load previously saved selection

Calculation of ring test parameters

Calculation of ring test parameters

Calculation of scores and laboratory evaluation

Calculation of scores and laboratory evaluation

Chart/table of laboratory mean values and standard deviations

Chart/table of laboratory mean values and standard deviations

Survey of scores

Survey of scores

Chart of tolerance limits and rel. standard deviations

Chart of tolerance limits and rel. standard deviations

Youden plot

Youden plot

Histogram und normal plot

Histogram und normal plot

Table of laboratory mean values and scores – per measurand

Table of laboratory mean values and scores per measurand

Table of laboratory mean values and scores – per sample

Table of laboratory mean values and scores per sample

Help

Help

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ProLab Plus Manual . Selecting ring tests

5 Selecting ring tests

Many features of ProLab Plus are specific to the selected ring test. Subsequently used mod- ules and functions always refer to the ring test previously selected in the selection box.

to the ring test previously selected in the selection box. Figure 1: Main menu There are

Figure 1: Main menu

There are two different working modes for a ring test. They can be selected from the main menu via the button Ring test or via the menu Database Ring test selection.

5.1 Putting ring tests in edit mode

If you want to work on a ring test, e.g. enter test results, carry out calculations etc., select the checkbox in the Access column for the relevant ring test and double click on the ring test, or close the window and select it from the selection box on the top of the main window.

select it from the selection box on the top of the main window. Figure 2: Database

Figure 2: Database Ring test selection

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ProLab Plus Manual . Selecting ring tests

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If you only want to view the results and prepare presentations, do not select the check box, but double click on the relevant ring test or select it from the selection box on the top of the main window. No data input or changes are possible in this mode.

If all ring tests should be included in a presentation, all of them need to be made accessible. Therefore click on the button Make all ring tests accessible. If you don’t want any of the ring tests in the edit mode, click on Make all ring tests read-only.

If a ring test is marked in red, it is currently opened on a different computer. You can also open it and make changes, but this may lead to inconsistencies in the database.

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ProLab Plus Manual . File Menu

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6 File menu

The File menu contains settings for reports and tables, the report designer and selection of the database.

6.1 Settings in reports, tables and charts

The Settings dialogue box allows you to choose different settings for how information will be displayed in the reports, tables and charts. This includes the specification of number formats and the name of the institution. Furthermore, the currently used logo is shown. It may be changed via the button Change.

Changes will be saved automatically upon closing the window or switching between tabs.

6.1.1 General settings

This tab enables you to enter general settings such as institution name, number format, crea- tion date, chart size and colours. If the check boxes for number format, date or default chart size are marked, these settings will apply to all tables, forms and graphics displayed.

will apply to all tables, forms and graphics displayed. Figure 3: File – Settings – General

Figure 3: File Settings General

The characters for formatting numerical values are:

.

Decimal separator

0

this digit must be a numeric character

#

this digit may be a numerical character

E+

exponential notation

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ProLab Plus Manual . File Menu

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By clicking on Reset chart settings all saved chart settings and profiles as well as information regarding size and colour are reset to the default setting. By clicking on Reset non-chart set- tings and confirming the list of configuration files to be deleted, all information regarding insti- tution, date and number format and many other settings stored by other ProLab windows are reset to the default setting.

By marking the checkbox Highlight outliers of type E in the summary results this option can

be selected. For further explanation of outliers of type E please refer to chapters 10.2 and

11.1.

6.1.2

Report settings

The tab Reports contains a comprehensive list of commonly used report templates. ProLab Plus offers a wide variety of templates, so the time-consuming task of designing reports can thereby often be avoided.

task of designing reports can thereby often be avoided. Figure 4: File – Settings – Reports
task of designing reports can thereby often be avoided. Figure 4: File – Settings – Reports

Figure 4: File Settings Reports

Select a report and click this button to open the Report designer module. Alternative- ly, a double click on the report will open the same module. Any changes become ef-

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ProLab Plus Manual . File Menu

fective upon saving the report in the Report Designer module. Customised report are highlighted in bold writing.

Since for some reports the data is missing in the templates, the report might look somewhat strange at first when using the preview. Upon input of data, however, you will find that the report looks fine.

Using this button will reproduce the original report template as created by the installa- tion program. This button is only relevant for reports highlighted in bold writing, that is to say, for customised report templates.of data, however, you will find that the report looks fine. Designing new reports is possible,

Designing new reports is possible, either directly or by using the Report Designer module.

This button opens the Report Designer for creating a new report. Report Designer for creating a new report.

This button allows you to edit existing reports.opens the Report Designer for creating a new report. User-defined reports can be accessed via the

User-defined reports can be accessed via the menu Charts and tables Further reports Own reports. The last column in the table shows the date of the last adjustment of the report template, not the date of the last time the report was used.

6.1.3 Caption settings

The Captions tab contains standard abbreviations for a number of names for titles and head- ers in charts and tables (e.g. column headers) and enables you to customise them. Please be aware that these settings will not become effective in every report. In some cases, the particular report has to be adjusted using the Report Designer.

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ProLab Plus Manual . File Menu

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ProLab Plus – Manual . File Menu 19 Figure 5: File – Settings – Captions 6.2

Figure 5: File Settings Captions

6.2 Start report

By choosing the menu item File Start report or pressing F8, you can determine the page number on which the next report you want to print will start. This is helpful when there are several reports to be compiled, i. e. you want to combine them into one report with succes- sive page numbers.

6.3 Log info

During a ProLab Plus session the following information is saved:

- Time of log in and log out

- User name

- Imported data

- Test results that have been changed

- Protocol of calculation of ring test parameters

- Protocol of calculation of scores.

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ProLab Plus Manual . File Menu

To access this information please choose Log info from the File menu. To open the report preview containing the information from all ProLab Plus sessions use the Report button.

from all ProLab Plus sessions use the Report button. Figure 6: File – Log info 6.4

Figure 6: File Log info

6.4 New database

Via File New database a new and empty database can be generated automatically in a new directory. This might be appropriate when different ring tests should be saved in differ- ent databases. Generally, saving ring tests in one and the same database might be reasona- ble, e.g. for an analysis spanning several ring tests; however, too many ring tests in the same database may slow down the program noticeably.

After selecting a directory from the list or entering a name for a new directory in the edit win- dow, the structures of the tables in the current database are copied to the target directory.

WARNING:

tained in these tables will be lost.

Existing tables in the target directory will be overwritten whereby any data con-

6.5 Change database

It is possible to change database directories, that is to say, to transfer a database with all the data relative to a ring test from one directory to another. Make sure that the new database di- rectory contains all required tables, otherwise your work may be compromised. This is best achieved by using the Backup file command or by copying the database directory outside of

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ProLab Plus Manual . File Menu

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ProLab Plus.

6.6 Backup file

This command allows backing up the entire database (all tables) in a compressed file and recovering it again from this file if necessary. LHARC is used as compression format. For saving your data, select a target folder and enter a file name. When quitting ProLab Plus you will be asked whether you want to create a backup copy of your database. Additionally, you can manually backup the database to a folder of your choosing by using the following tab.

to a folder of your choosing by using the following tab. Figure 7: File – Backup

Figure 7: File Backup file (Backup of database „Demo“)

6.6.1 Restore from file

In this window, all backup files that have been created so far (and still exist) are listed. In or- der to restore one of them, simply select it from the list and click the button Restore from file. Alternatively you can choose Select file… in the first row of the table and specify the LZH file you want to restore.

WARNING: Any existing data will be overwritten and thereby lost.

If you want to restore a database without overwriting existing data and tables, please create

a new database as described in section 6.4 before restoring.

6.6.2 Store database to file

In order to create a backup of your database, you have to select a target file first. Normally that will be a new file, which can be created via the first row Select file… Alternatively an ex- isting file from the list can be chosen. To start the process simply click Store database to file. Please note that any existing data will be overwritten and thereby lost.

6.6.3 Advice for long-term storage

Although there are several programs of other developers or Open Source communities which can open LZH files and/or the contained Advantage Database System files, this binary for- mat may not be the best choice for long-term storage of ring test data. It is recommended in- stead to export plain-text CSV files additionally (please refer to chapter 7.11.1).

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ProLab Plus Manual . Menu Database

7 Database menu

7.1 Ring test selection

Please refer to chapter 5.1, Putting ring tests in edit mode.

7.2 Basic tables

A ring test is defined by the samples, the measurands and the laboratories. Therefore, the

tables for the ring tests, samples, measurands and laboratories constitute the foundation of

the database. The basic tables can be reached via Database Basic tables. In these tables, all the information on samples, measurands and laboratories is entered, but no allocation ( e.g. e.g. which measurand is analysed by which laboratory on which sample) is carried out yet.

7.2.1 How to work with the tables

The data tables offer a powerful tool for working with the database. The data can be sorted and grouped in several ways, fields can be added and removed and whole tables or selec- tions can be saved in different formats.

In the following, several possibilities for working with the tables are described. However, it

must be noted that not all commands are available in all tables.

The most important buttons are

Save

Cancel

Add

Delete

Save changes

Cancel editing

Add new data

Delete selected data

New data ( e.g. ring tests or samples) can also be added by clicking into the first row of the respective table.

Please note that the names of the ring tests, the measurands, the samples and the laborato- ries are unique identification labels. Therefore they should not be changed later on. Name must only contain capital letters and numeric characters. Description can be filled and/or changed later. If the Description field is left empty, Name will be entered automatically.

When clicking with the right mouse button onto the column headers, a pop-up menu opens within which the available commands are in dark letters (see Figure 8). These commands will be explained in more detail in the following:

Reset table settings

All changes in the appearance of the table can be undone by choosing Reset table settings from the pop-up menu. You get there by a right click with the mouse onto any column head- er.

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Sorting

The tables can be sorted in ascending or descending order (with respect to a selected col- umn) either

- by left-clicking in the respective column header or

- by selecting the commands from the following pop-up menu, which opens by right- clicking into a column header.

menu, which opens by right- clicking into a column header. Figure 8: Pop-up menu after right

Figure 8: Pop-up menu after right mouse button click into column header

Add and remove columns, adjust order

The order of the columns can be changed by drag & drop: simply click in a column header and by keeping the mouse button pressed move the column to the desired position.

Unnecessary columns may be hidden by deselecting the respective column from the list that can be reached via the button Visible columns. A column may also be removed by clicking in the header and selecting Remove This Column from the pop-up menu. If formerly removed columns or further columns should be added to the table, simply select the column from the list under Visible columns or select the Field Chooser from the pop-up menu. From the field chooser, a column can be moved to the table by drag and drop.

In

order to add or remove several columns at once, right-click anywhere inside the table (not

in

the headers) and select Select columns from the pop-up menu while keeping the Shift key

pressed.

The column width can be adapted manually by moving the separators of a column. The best fit, i. e. the column width that enables to see the whole content of the column without wasting too much space, can be obtained by double clicking on a separator or by choosing Best Fit from the pop-up menu. An optimal width of all columns can be obtained via the command Best Fit (all columns) from the pop-up menu.

Grouping

A table can be grouped with respect to column entries and will thereby be divided into sub-

tables. Grouping can be done by marking the desired column and selecting Group By This

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Field from the pop-up menu. After selecting this command, a dark grey box will appear above the table indicating the column according to which the grouping is carried out. A further pos- sibility for grouping is to select the command Group By Box from the pop-up menu. The dark grey box then appears without any column header name. Now the column according to which the grouping should be carried out can be moved to the dark grey box via drag and drop.

In , the table grouping of measurands with regard to the column Category 2 is shown. As there are three entries in the Category 2 column, the grouped table now consists of three sub-tables, one for light metals, one for heavy metals and one for gasses. These sub-tables can be opened or closed via the + / - buttons.

Of course, a table can be grouped several times in succession. Thereby more and more sub- tables are generated. This grouping can be done again either by successively marking col- umn headers and selecting the command Group By This Field from the pop-up menu or by selecting the command Group By Box once and then successively dragging fields to the grey box above the table.

In both cases, the hierarchy of the grouping will be shown in the dark grey box.

of the grouping will be shown in the dark grey box. Figure 9: Basic table of

Figure 9: Basic table of measurands grouped by Category 2

Column width

Using the menu option Best Fit, the width of the columns will be adjusted according to the content. To adjust all columns at once the shortcut Ctrl + Addition (on the numerical key- board) can be used.

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Copy

Whole tables or selection thereof can be copied to the clipboard and, e.g., inserted into an Excel table. For this purpose use the right mouse button within the table (not in the headers). Then a pop-up menu will be displayed where you can select Copy table or Copy selection. With the first command, the whole table is copied. With the second command, only the row in which has been clicked is copied, along with the column header.

has been clicked is copied, along with the column header. Figure 10: Pop-up menu after right

Figure 10: Pop-up menu after right mouse button click into table

Save

All tables can be saved in different formats: text file, Excel file, XML file or HTML file. The ta- ble can be saved as a PDF or RTF file from within the report preview. For this purpose use the right mouse button within the table (not in the headers). Then a pop-up menu will be dis- played where you can select the desired saving format.

The information of a grouped table is always completely saved independently of the way it has been displayed in ProLab Plus, i. e. the information of sub-tables closed in ProLab Plus will be saved as well. Of course, the grouping is saved, too.

Search text

After clicking this menu item, a search bar will be shown. That bar can be opened by using the shortcut Ctrl + F alternatively. To close the bar, click on the cross on the left side or use the Esc key.

Select columns

This option opens a list with all columns that can be shown. There are three different types of lists:

1. In most windows, the default setting leads to a list with check boxes, which makes possible a swift selection of columns to show or hide.

2. If you decide to change the visibility of more than one column at once, hold the Shift

A window appears in

which you can show or hide all columns by using the keys ‘>>’ or ‘<<’. It is also possi-

key down while clicking on the menu option ‘Select columns’

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ble to show or hide single columns in this window. Some tables only offer this win- dow.

The third window can be reached by a right mouse click into a column header and se- lecting Field Chooser in the opening pop-up menu. The usage of that window is de- scribed above.

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7.2.2 Ring tests

The parent data for ring tests can be edited (entered, changed, deleted) in the Database Basic Tables dialogue box on the Ring tests page. The list comprises all open ring tests, i. e. all ring tests that are opened in the Edit mode (see section 5).

tests that are opened in the Edit mode (see section 5). Figure 11: Database – Basic

Figure 11: Database Basic Tables Ring tests

Name stands for the abbreviated name of the respective ring test. In the database it is usual- ly referred to as RName. To add a new ring test, either click in the box Add ring test or click

on

analysis, Report date, Cut-off date (unofficial deadline), Design and the number of Replicates in the respective cells of the table. Name may only contain up to eight capital letters and nu- merics.

For every ring test, a design can be selected from the scroll-down box, though this is not mandatory:

from the scroll-down box, though this is not mandatory: . Enter the name of the ring

. Enter the name of the ring test (Name) and, if necessary, the Description, the Date of

- Select single measurement if only one test result will be reported for every laboratory- sample-measurand combination.

- Select with replicates and enter the number of replicate measurement values for every laboratory-sample-measurand combination in the pop-up window. The number of repli- cates can be changed later if necessary. This will be used as default setting for the ex- port of laboratory files (7.11.2) and in the window for the input of test results. The com- putation of means and standard deviations however is not affected by that setting, as the number of actually available measurements is independently determined for these functions

- Select Nested design if you would like to work with a ring test design where e.g. two measurement values belong to one day and two values belong to another day (see ISO 5725-3).

The selection of the design will affect the window for entering the test results, however the design can always be changed again later, if need be. If no design is selected, the number of replicates can be defined later on, in the test results window.

Further information (e.g. year, organizer) regarding the ring test can be entered in the field Group. This may be helpful for a later grouping of the ring tests.

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Warning: If you delete a ring test, please note that this operation will also delete any data in other tables that refer to this ring test ( e.g. samples, ring test-sample-measurand combina- tions, test results, lab codes). It does not delete measurand and laboratory data in the basic tables.

7.2.3 Samples

To enter a new sample or change information regarding existing samples, please select the tab Samples in the dialogue box Database Basic Tables.

After selecting the corresponding ring test, a sample can be added either by clicking in the

button. Afterwards Name and Description can be entered in the

corresponding fields. The name of the sample (in the database referred to as SName or PName) is a unique identification, therefore it should not be changed later on. Name must only contain capital letters and numerics.

box Add sample or on the

capital letters and numerics. box Add sample or on the Figure 12: Database – Basic Tables
capital letters and numerics. box Add sample or on the Figure 12: Database – Basic Tables

Figure 12: Database Basic Tables Samples

For an easier selection of samples in the calculations, two categories are available under which distinguishing features of the samples can be entered. The button Sorting opens a new window, where the samples can be sorted by drag & drop or according to defined fields. Please be aware that changes can only be made if the ring test is opened in the Edit mode. Entering a new sample requires the existence of a ring test, as samples (other than measur- ands or laboratories) are always subordinated to a ring test.

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Warning: Please note that deleting a sample will also delete any data in other tables that re- fer to this sample ( e.g. ring test-sample-measurand combinations, test results, test portion codes). Deleting a sample does not however delete ring tests, measurands or laboratory da- ta in the basic tables.

7.2.4 Measurands

The parent data for measured measurands can be edited (entered, changed, deleted) in the Database Basic Tables dialogue box on the Measurands tab. Changes are only possible, if the corresponding ring test is opened in the Edit mode. If the ring test is opened in the Read mode, the measurand data can be read, but not changed.

To add a measurand, either click in the box Add measurand or click on

measurands is independent from the ring test and the sample. The necessary allocation will be carried out later.

In the form you can enter the name of the measurand (Name in the database referred to as MName), the description of the measurand and if desired further distinguishing features under two categories and the number format for the test results. The restriction of using only capital letters and numerics for Name applies here as well.

. The table of

and numerics for Name applies here as well. . The table of If you want to

If you want to change the order in which measurands appear elsewhere in ProLab, please click the Sorting button. A pop-up window will appear where you can choose how the meas- urands should be sorted: by name, description or category (or manually via drag and drop).

description or category (or manually via drag and drop). Figure 13: Database – Basic Tables –

Figure 13: Database Basic Tables Measurands

Warning: Please note that deleting a measurand will also delete any data in other tables that refer to this measurand ( e.g. ring test-sample-measurand combinations, test results). Delet- ing a measurand does not however delete ring tests, samples or laboratory data in the basic tables.

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7.2.5 Laboratories

The parent data for laboratories can be edited (entered, changed, deleted) in the Database Basic Tables dialogue box on the tab Labs as Table. To add a laboratory click in the box Add

laboratory or on the

The table of laboratories is independent from the ring test and the sample. The necessary al- location will be carried out later. Changes are only possible if the respective ring test is opened in the Edit mode. If the ring test is opened in the Read mode, the laboratory data can be read, but not changed.

You can enter the name of the laboratory, a description, the address and if desired fur- ther information such as contact person, email address, telephone numbers etc. Email ad- dresses and contact persons are of special importance if you want to use the email merge module of ProLab Plus (see also section 7.11.4). More than one address can be specified by using spaces or semicolons as delimiters. Furthermore, up to two categories can be speci- fied for each laboratory that allows for a later selection of sub-groups of laboratories.

Please note, that for Name only capital letters and numerics are allowed. If the Description field is left empty or contains only space characters, the laboratory name will be entered au- tomatically, since different reports and graphics use the description to specify the laboratory.

To show a tabular summary of all laboratories click the Report button.

summary of all laboratories click the Report button. button in the lower part of the window.

button in the lower part of the window.

the Report button. button in the lower part of the window. Figure 14: Database – Basic

Figure 14: Database Basic Tables Labs as Table

Displaying all information on a laboratory in a table often leads to a confusingly high number of columns that can hardly be displayed at once. Therefore, on the tab Labs as Cards there is also the option to show all laboratory information as business cards.

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ProLab Plus – Manual . Menu Database 31 Figure 15: Database – Basic Tables – Labs

Figure 15: Database Basic Tables Labs as Cards

As the address structure varies from one country to another, it is possible to enter all address information in the additional fields Additional 1 to Additional 6 instead of the fields Street, ZIP and City. This offers the possibility to create, for example, address labels with the correctly arranged address. Thus (see also Table 1), for a German address the additional name of the laboratory could be entered in the field Additional 1, the street with number in Additional 2 and the postal code and city in Additional 3. For the UK the additional name of the laboratory could be entered again in the field Additional 1, the street with number in Additional 2, the city in Additional 3, the county in Additional 4 and the postal code in Additional 5.

Germany

USA

UK

short name of lab

short name of lab

short name of lab

1 additional name

1 additional name

1 additional name

2 Street + No

2 No + Street

2 No + Street

3 ZIP City

3 City State/ZIP

3 City

Country

Country

4 County

5 ZIP

Country

Table 1: Examples of addresses

Warning: You may delete laboratories, but please note that this operation will also delete any data in other tables that refer to this laboratory ( e.g. ring test-sample-measurand combina- tions, test results, lab codes). Deleting laboratories does not however delete ring tests, sam- ples or measurands in the basic tables.

7.3 Structure of ring test

After the basic tables have been filled, it still has to be determined which samples were ana- lysed by which laboratories with respect to which measurands. Hence it is necessary to as-

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sign the investigated measurands to the samples and the laboratories to the respective sam- ple-measurand combinations.

Therefore select the command Structure of ring test in the menu Database or the buttons:

of ring test in the menu Database or the buttons: for the laboratory allocation for the

for the laboratory allocation

for the sample-measurand allocation

for the sample-measurand-laboratory allocation.

7.3.1 Laboratory allocation

In the window Laboratory allocation all laboratories that take part in the ring test can be se- lected.

In order to assign a laboratory to the ring test, double click into the column that is indicated by a lighter background colour. If there are more ring tests in the database, they are shown as well, so you can compare with previously organised ring tests. The current ring test is al- ways shown in the first column and indicated by a lighter background. All remaining ring tests follow in chronological order. By selecting rectangular sections of the column you can easily choose several laboratories at once and either assign them to the ring test by clicking on the button Include selected laboratories or delete them by clicking on Exclude selected laborato- ries. If you want to allocate all laboratories to the ring test, simply click on Include all labora- tories.

Warning: Please note that deleting the allocations of laboratories will also delete the corre- sponding test results!

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ProLab Plus – Manual . Menu Database 33 Figure 16: Database – Structure of ring test

Figure 16: Database Structure of ring test Laboratory allocation

By marking the checkbox Participating laboratories first, the laboratories that participate in the corresponding ring test are listed first followed by the laboratories (if applicable) that do not participate.

The table can be sorted by name, description or category by clicking in the respective co- lumn headers.

A list of all participating laboratories can be displayed by clicking on the Report button.

You can select the columns to be displayed, define the width of the columns and copy parts or the whole table to the clipboard for further use, e.g. in Excel, with a right mouse button click into the table.

7.3.2 Sample-measurand allocation

Select the menu Database Structure of ring test Sample-measurand allocation to specify which samples have been or will be analysed with respect to which measurands.

To assign a measurand to a sample, check the corresponding cell by double-clicking. By se- lecting rectangular sections of the table you can easily choose several measurands at once and either assign them to samples by clicking on the button Include selected combinations or delete them by clicking on Exclude selected combinations. If you want to allocate all measur- ands to all samples, simply click on Include all combinations.

The current assignment table can be viewed as a report by clicking on the Report button. You can select the columns to be displayed and define the width of the columns with a right

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mouse button click in the table. Furthermore, the whole table or sections of it can be copied to the clipboard and pasted to e.g. Excel.

Warning: Please note that deleting the assignments of measurands will also delete the cor- responding test results!

will also delete the cor- responding test results! Figure 17: Database – Structure of ring test

Figure 17: Database Structure of ring test Sample-measurand allocation

7.3.3 Sample-measurand-laboratory allocation

Select the menu Database Structure of ring test Sample-measurand-laboratory allocation to assign samples and measurands to the laboratories of the ring test.

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ProLab Plus – Manual . Menu Database 35 Figure 18: Database – Structure of ring test

Figure 18: Database Structure of ring test Sample-measurand-laboratory allocation (per sample)

You can now determine which samples are sent to which laboratories to investigate which measurands. This can be accomplished by assigning laboratories one sample at a time, one measurand at a time, for all measurands, or for all samples. The default setting when open- ing the window is per sample (i. e. one sample at a time).

If you choose one of the options per sample or per measurand, simply select the sample or the measurand from the table on the right side and assign the laboratories to each measur- and or sample by double-clicking in the respective cell. By selecting rectangular sections of the table you can easily choose several samples or measurands at once and either assign them to laboratories by clicking on the button Include selected combinations or delete them by clicking on Exclude selected combinations. If you want to allocate all samples or all measurands to all laboratories, simply click on Include all combinations.

It is also possible to assign laboratories to all measurands or all samples. If you choose across all measurands, any specifications will refer to all measurands, i. e. they will apply to all measurands that have been assigned to the particular sample under consideration.

If a laboratory does not analyse a certain sample, there will be no entry in the corresponding field.

If only some of the measurands have been assigned to a laboratory (through the sample un- der consideration), the symbol % will be displayed in the field.

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If all measurands have been assigned to a laboratory (through the sample under considera- tion), an X will be displayed in the field.

You can create new assignments or delete existing ones. Any such changes will, however, from now on affect all measurands that have been assigned to the sample in question.

that have been assigned to the sample in question. Figure 19: Database – Structure of ring

Figure 19: Database Structure of ring test Sample-measurand-laboratory combinations (across all samples)

By selecting rectangular sections of the table you can easily choose several samples at once and either assign the combination of these samples and all measurands to laboratories by clicking on the button Include selected combinations or delete them by clicking on Exclude selected combinations. If you want to allocate all combinations of samples and measurands to all laboratories, simply click on Include all combinations.

If you choose across all samples, any specifications will refer to all samples, i. e. they will apply to all samples that have been assigned to the respective measurand. Again the sym- bols % and X are used to indicate that only some of the samples have been assigned to the respective laboratory or that all samples have been assigned, respectively.

You can select the columns to be displayed and define the width of the columns with a right mouse button click in the table. Moreover, the whole table or sections of it can be copied to the clipboard and pasted to e.g. e.g. Excel.

The sample-measurand-laboratory combinations can be displayed as a report by clicking on

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the Report button.

Warning: Please note that deleting laboratory assignments will also delete the corresponding test results!

7.4

Encoding

If the identity of the laboratory must not be revealed, the laboratory name must not appear in the evaluation reports and has to be encoded in a suitable way. Apart from encoding the la- boratories you can also encode the samples. This is useful if it is suspected that the laborato- ries may exchange their analytical results.

7.4.1 Encoding laboratories

All test results contained in the database are registered under an addressconsisting of the four components ring test, sample, measurand and laboratory. To make sure that all data can be correctly attributed at any time, this address must not change 3 , i. e. the particular la- boratory always has to be indicated by LName. If, however, the identity of the laboratory should not be revealed, LName must not appear in the evaluation reports and has to be en- coded in a suitable way. The encoding can be done via Database Encoding Laboratories

can be done via Database – Encoding – Laboratories or by clicking onto the button in

or by clicking onto the button in the main menu.

Any code can be entered in the Code field or laboratory codes can be generated automati-

Code field or laboratory codes can be generated automati- cally by clicking onto this button .

cally by clicking onto this button . Existing codes are thereby deleted irrevocably. Please note that the encoding only applies to the currently selected ring test.

3 This means that, for example, in order to execute an evaluation over various ring tests, a physical laboratory should have the same value for LName in each ring test. If you change LName in the basic tables the allocation will not be disturbed, as LName will be changed for all ring tests and all secondary windows.

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38 ProLab Plus – Manual . Menu Database Figure 20: Database – Encoding – Laboratories 7.4.2

Figure 20: Database Encoding Laboratories

7.4.2 Encode test portions

Apart from encoding the laboratories you can also encode the test portions. This is useful if it is suspected that the laboratories may exchange their analytical results. You can get to the

may exchange their analytical results. You can get to the encoding via Database – Encoding –

encoding via Database Encoding Test portions or by clicking the button in the main menu. Test portion codes are composed of up to 8 alphanumeric characters without special characters and spaces.

Therefore the following notations are introduced: Sample denotes different kinds of samples as water sample or soil sample. From each sample, test portions are produced which will be sent to the laboratories or used for the homogeneity analysis.

Encoding can be performed

- manually

- automatically, without homogeneity test portions

- automatically, taking into account the homogeneity test portions (see section 8.2)

Manual encoding

In order to encode the test portions an existing ring test structure is essential, i. e. data for every sample-measurand-laboratory combination of the current ring test must exist. A code can be assigned to each laboratory-sample combination. To encode the test portions unam- biguously, any combination of test portion code and LName must exist only once. A violation of this rule will prompt an Index Error, which can be adjusted by assigning a new code to the

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test portion. Please note that same samples in different laboratories may have same test por- tion codes.

Example:

SName LName Test portion code

Soil2

L01

Sample2

ok

Soil2

L02

Sample2

ok, because Sample2 differs in LName

Soil3

L02

Sample2

invalid, because Sample2 has already been assigned to Soil2/L02

The test portion codes are entered via a matrix having the samples as columns and the la- boratories as rows. In case of an invalid entry, an error message will be displayed upon leav- ing the edited field and the original value will be restored.

Automatic encoding

For convenience, the test portion codes can be generated automatically. First define the number of test portions that will be generated per sample. If there are as many test portions as participating laboratories, simply enter the number of laboratories. If there are more test

portions generated than participating laboratories ( e.g. if a homogeneity and/or stability test

is planned or if the remaining test portions will serve as reference material after the ring test),

simply enter the total number of test portions that are generated. By clicking on the button

, test portions of every sample are randomly assigned to each participating laboratory, and

a unique four-digit code is generated for every sample-laboratory combination. If you require the test portion codes to be greater than a certain minimum value, enter this desired mini- mum value in the field First value for test portion code.

If the number of test portions per sample is less than the number of participating laboratories (which should be the minimum number of test portions to generate), ProLab Plus generates the codes on the basis of this minimum number.

If a homogeneity test is carried out, the respective test portions can be encoded by means of the tab Homogeneity test portion encoding or later on under the menu item Homogenei- ty/Stability.

If originally no homogeneity test portions were included in the number of test portions per

sample, but homogeneity and/or stability test portions are nevertheless needed, it is recom- mended to enter the corrected total number of test portions per sample (i. e. the number of test portions for the laboratories + the number of test portions for the homogeneity test + the number of test portions for the stability test) and repeat the encoding of the test portions for the laboratories in order to ensure a random ordering of all test portions.

In the rows Prefix und Suffix additional tokens can be entered, that will precede the code or be attached to the end of the code, respectively.

tokens can be entered, that will precede the code or be attached to the end of

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40 ProLab Plus – Manual . Menu Database Figure 21: Database – Encoding – Test portions

Figure 21: Database Encoding Test portions

Additionally there is the possibility to display a table with the test portion codes as a report and to print labels with laboratory and sample specifications and optionally a barcode (where ring test name, lab code and test portion code are coded). In order to do this, the label forms in File Settings Reports 75 Label / 77 Label with barcode must be adapted to the re- quired label format.

barcode must be adapted to the re- quired label format. Figure 22: Label for test portions

Figure 22: Label for test portions with and without barcode

7.5 Participating labs and data yet to be submitted

In the menu Database Participating labs and data yet to be submitted the following infor- mation is stored automatically or can be entered manually:

- Date of sample arrival in laboratories

- Date of measurements

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- Date of the ring test organiser’s receipt of test results (reporting date)

- Date of importing test results in ProLab

- Persons involved

- Comments.

test results in ProLab - Persons involved - Comments. Figure 23: Database – Participating labs and

Figure 23: Database Participating labs and data yet to be submitted

All information can be viewed for the currently opened ring test or all ring tests that have been made accessible (see section 5). Select Current ring test only or All unlocked ring tests.

If all that is required is an overview of the laboratories for which no test results have been imported, check Only laboratories with data yet to be submitted.

A report with an overview can be generated listing either all laboratories or only those labora-

tories with results yet to have been received or imported.

7.6 Characteristics of measurands

After the ring test structure has been defined, the Characteristics of measurands dialogue box allows further specification of the measurands analysed in the ring test. Reference val- ues, reference standard deviations, measurement units and appertaining multiplication fac- tors can be entered. Additionally two fields Rel. s.d. min and Rel. s.d. max for minimum or maximum values of the relative standard deviations (in %) are available. In mode “L = lim- ited” (see section 10.2.3) these values for the relative standard deviations will be used in the assessment of the laboratories.

will be used in the assessment of the laboratories. Using the button all values – except

Using the button all values except for the reference value and reference s.d. are as-

for the reference value and reference s.d. – are as- signed to the selected measurand in

signed to the selected measurand in all samples of the ring test. Using the button all values except for the reference value and reference s.d. are assigned to all measurands

of the current sample. Using the button

to all measurands of the current sample. Using the button all values – except for the

all values except for the reference value and

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reference s.d. are assigned to all measurands in all samples of the ring test.

assigned to all measurands in all samples of the ring test. Figure 24: Database – Characteristics

Figure 24: Database Characteristics of measurands

If the database already contains units, they can simply be selected from the scroll-down menu. The multiplicator, if included in the database, will automatically be selected by ProLab Plus. New units must always be created via the window Characteristics of measurands. Please click the button next to the Unit field to open the Units window. In the table, the new unit with its corresponding multiplicator can be entered. Please make sure to always leave one “empty” unit, so the declaration of a unit can be suppressed if necessary.

The multiplication factor (multiplicator) is the factor, by which the test results have to be mul- tiplied to obtain the concentration values. The multiplication factor for the measurement unit µg/kg, for instance, is 10 -9 = 1E-9, the multiplication factor for the measurement unit % is 10 -2 = 1E-2. The entry of this multiplication factor is indispensable to guarantee the correct calculation of the standard deviation according to Horwitz.

factor is indispensable to guarantee the correct calculation of the standard deviation according to Horwitz. quo

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ProLab Plus – Manual . Menu Database 43 Figure 25: Database – Characteristics of measurands –

Figure 25: Database Characteristics of measurands Units

7.7 Test results

To enter the test results, open the Test results dialogue box from the Database menu. You can choose between entering the test results in a detailed form or in a table.

Depending on the ring test design that was selected under Database Basic tables Ring tests the corresponding number of fields for entering test results is shown.

If no specific design was defined, the number of replicates can be manually determined in the present window. The field Show test results makes it possible to define the number of replicates (1 to 32) and, accordingly, the number of input fields for the test results.

If the ring test is of nested design the corresponding specific order of the test results must be respected. For example, if for three different days two measurement values are available, the design should be nested 3 x 2. There is a maximum of six test results per laboratory, the first two belong to day 1, test results 3 and 4 to day 2 and test results 5 and 6 to day 3. The test results need to be entered in this order.

Besides the fields for the test results, there are State fields as well. You can choose between the following entries in these fields

NN

=

not detectable,

NB

=

not determinable,

GL

=

greater than (Greater Limit),

NA

=

not available

These can be used for the assessment of a laboratory. However, a State entry is not re- quired, even when there are no test results available.

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44 ProLab Plus – Manual . Menu Database Figure 26: Database – Test results – Detailed

Figure 26: Database Test results Detailed form

In the detailed form, the following shortcuts have been implemented, for the sake of conven- ience:

[Ctrl]+ [P]

previous sample

[Alt] + [P]

next sample

[Ctrl]+ [M]

previous measurand

[Alt] + [M]

next measurand

[Ctrl]+ [L]

previous laboratory

[Alt] + [L]

next laboratory

Apart from the test results, the limit of detection, the limit of determination, the upper limit of the measuring range, the measurement uncertainty and the sample preparation and analyti- cal method can be entered as well. In order to assign the sample preparation and/or analyti- cal method for the measurements, they must have been defined beforehand. This is carried out under Database Definition of analytical methods and sample preparations (see section

7.9).

In the detailed form, additional information on the measurands ( e.g. Unit, multiplicator,) as entered under Characteristics of measurands (see section 7.6) are also shown. This infor- mation can be changed, but please be aware that these changes are specific to the measur- and and will affect the test results of all laboratories.

to get to the table view. The fields for the test results are named M 1, M 2, …, and

Click

the fields for state entries are named S 1, S 2,… by default. In order to adjust the layout to your needs, you can click the option Visible columns.

2,… by default. In order to adjust the layout to your needs, you can click the

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ProLab Plus – Manual . Menu Database 45 Figure 27: Database – Test results – Table

Figure 27: Database Test results Table view

In the status bar at the bottom edge of the ProLab window, the description of the current la- boratory, that of the sample and, if applicable, the test portion code are shown at all times.

7.8 Creation of corrected measurands

With ProLab Plus, it is possible to correct the measurement values and to generate a new measurand (the old ones will not be overwritten) in the three following ways:

1.measurand

2.measurand

3.measurand

100

correction value

100

(100

correction value

correction value)

The correction value may either be an already existing measurand or a constant that has to be entered manually.

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46 ProLab Plus – Manual . Menu Database Figure 28: Database – Creation of corrected measurands

Figure 28: Database Creation of corrected measurands

Enter a name for the new, corrected measurand and click on the Start button to generate the new measurand. A pop-up window will appear where you can enter a description of the new measurand. After saving this description, a second pop-up window will appear where the characteristics of the new measurand, such as unit, multiplicator, reference value, s.d., and minimum/maximum rel. s.d. can be entered.

value, s.d., and minimum/maximum rel. s.d. can be entered. Figure 29: Pop-up windows after generating a
value, s.d., and minimum/maximum rel. s.d. can be entered. Figure 29: Pop-up windows after generating a

Figure 29: Pop-up windows after generating a new, corrected measurand

7.9 Analytical methods and sample preparations

Data on the sample preparation (SP) and the analytical method (AM) can be entered in the database in case the influences of SP and AM are to be included in special statistical evalua- tions. Under Database Definition of analytical methods and sample preparations all possi- ble methods can be entered in two tables. An allocation to the actual measurements is car- ried out when entering the test results (see section 7.7).

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Both tables allow entry of a code (ID, only numbers are allowed), an abbreviation (Name, used in the Summary results chart) and a full name (Description).

When defining new methods, click in the first row of the table and enter the corresponding data. ProLab Plus will automatically provide missing entries, so it is sufficient to enter, for in- stance, only the description.

To generate a printable overview, click the Report button above the table; with a right mouse click into the table, other available exportation means can be accessed.

table, other available exportation means can be accessed. Figure 30: Database – Definition of analytical methods

Figure 30: Database Definition of analytical methods and sample preparations Analytical methods

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7.10 Duplicate ring test

Under Database Duplicate ring test, a copy of the currently opened ring test can be gene- rated. It is possible to choose between copying only the structure of the ring test or the whole ring test including the test results. This feature is especially helpful when a ring test with the same structure is carried out several times. The name (8 digits) of the new ring test must be entered in the appropriate window. A more detailed description can be specified in the Basic tables afterwards.

can be specified in the Basic tables afterwards. Figure 31: Database – Duplicate ring test 7.11

Figure 31: Database Duplicate ring test

7.11 Export

ProLab Plus offers several export functions:

- Export the whole ring test including the test results as a CSV file

- Create laboratory files that can be filled in by the laboratories

- Export the whole ring test as an LZH file

- Contact laboratories by emails with attachments from ProLab Plus.

All functions are described in more detail in the following sections.

7.11.1 Test results as CSV file

Open the Database Export CSV file dialogue box to export test results and laboratory da- ta. The export of data is recommended if the data is to be further processed in another pro- gram, such as EXCEL, or if a backup copy in ASCII format is to be created, that can later be re-imported if necessary. The export is always carried out for the current ring test, unless the box All ring tests is activated.

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ProLab Plus – Manual . Menu Database 49 Figure 32: Database – Export – CSV files

Figure 32: Database Export CSV files

If only the selected data records should be exported, check Show selected data only. This will reduce the number of lines in the exported file. (Of course, the desired fields need to be selected.)

The following data are always exported: ring test name (RName), sample name (SName = PName), measurand name (MName) and laboratory name (LName).

If All fields (columns) is checked, all information of the ring test(s) will be exported. If it is not checked, fields such as laboratory mean (M), laboratory standard deviation (s.d.), Score, the quantification limit (QL), detection limit (DL), the upper limit (GL), outlier values, additional comments, sample preparation (SP), analytical method (AM), measurement unit, laboratory and test portion codes, measurement uncertainty (MU) and recovery rate can be selected. If the measurement results and corresponding state fields of the ring test should be exported as well, click the button Measured valuesto specify which of the results should be export- ed.

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50 ProLab Plus – Manual . Menu Database Figure 33: Selection of measured values to be

Figure 33: Selection of measured values to be exported

After making your selection, click on the button Export to start the data export. A dialogue box will appear, and you will be asked to enter the path and name of the export file. The file generated by ProLab Plus can be imported into EXCEL in the CSV format. By de- fault, the semicolon is used as column (field) separator so that the exported test result table can easily be re-imported into ProLab Plus. For other applications it might be more appro- priate to choose another field separator character from the list on the left of the export button.

7.11.2 Laboratory files

To avoid a laborious and therefore error-prone manual input of the laboratorial data, ProLab Plus provides a function for automatic data transfer via CD or email (using appropriate secu- rity tools) between the participants and the organizer.

In order to prepare the data transfer, specific files can be created using the menu Database Export Laboratory files (for RingDat). These are then filled in by the participating laborato- ries with the help of a special program called RINGDAT3. The data set for each laboratory contains a FILENAME.LA2 file and a FILENAME.LAB file. The latter is an ASCII file with the columns sample name (SName) / test portion code (SCode), Measurand name (MName) and measurement unit. The columns containing the individual test results are added in the RingDat3 program. FILENAME.LA2 is a configuration file that contains information on the ring test, instructions and other parameters. The content of this file can be viewed in any text editor; changes should, however, be avoided.

Besides the laboratory files, the participants also need to receive the following files, which are located in the sub-directory RingDat3 in your current ProLab directory (the folder where ProLab is installed):

- RingDat3.EXE,

- RingDat_English.HTML

- translations\English.xml

As experience has showed that sending exe-files via email may cause problems, there is the

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possibility for the ring test participants to download all three files from the quo data homep- age. Please contact us (info@quodata.de) to receive login data for the download.

In addition, ProLab Plus offers the possibility of creating individual laboratory files for each laboratory and to save these on different storage devices ( e.g. CD, pen drive). To do this, click on Copy labwise to storage device in the Create laboratory files (for RingDat) window. It is now possible to select a laboratory and the drive (storage device) you would like to copy the files to. Upon clicking copy or pressing F5, ProLab Plus saves the files FILENAME.LAB, FILENAME.LA2, RingDat3.EXE, and RingDat_Englisch.HTML to the selected drive (see

7.11.2.1).

Furthermore, we can supply a customized online input tool for participants, thus circumvent- ing the need to use RingDat for laboratory files.

The laboratory files are usually created lab-wise, though it is sometimes advantageous to create one single file for all laboratories. If the check box per laboratory has been marked, one set of data will be created for each laboratory. In this case FILENAME corresponds to LName. If the check box is not marked, only one set of data with the RName as FILENAME will be created. If the boxes per laboratory and Lab code are marked, additional files where the FILENAME corresponds to the lab code are created. While the lab-wise option is easier to fill out for the participants, the option for all laboratories simplifies the distribution of the empty files to the laboratories and the following import.

If the check box Export selected combinations only is marked, only those files are exported which correspond to the selected combinations of sample, measurand and laboratory (see also section 9). If laboratories should specify the date of analysis, please mark the corre- sponding check box. The number of measurement values needs to be specified in order to have sufficient fields available in the RingDat file. If it is required that a laboratory enter a value in each field, please mark All data are needed. If the field Addresses is checked, there will be an additional tab in RingDat, where every participant can see and edit his address in- formation. If changes have been made, they will be highlighted during the import (see 7.12.2) and can be incorporated into the Basic tables if desired.

When creating lab-wise files while the option Test portion code is enabled, a test portion code has to exist for each laboratory and each sample. If the test portion code is missing, the corresponding sample-measurand combination will not be displayed! When creating one file for all laboratories only the names of the measurands and the measurement units will be included in the file. The test portion code has to be added by the laboratory.

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52 ProLab Plus – Manual . Menu Database Figure 34: Database – Export – Laboratory files

Figure 34: Database Export Laboratory files (for RingDat)

To transfer information about the analytical methods and sample preparations, please acti- vate the check box Analytical methods and sample preparations. In this case two additional tabs will be displayed. On the tab Select AM and SP the analytical and sample preparation methods to be made available in the program RINGDAT3 can be selected. If the list of avail- able analytical methods is long and unwieldy, but not all analytical methods are meaningful for any particular measurand, there is the possibility to deselect meaningless analytical methods on the tab Allocation of AM to measurands.

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ProLab Plus – Manual . Menu Database 53 Figure 35: Database – Export – Laboratory files

Figure 35: Database Export Laboratory files (for RingDat): Allocation of AM to measureands

A text box is available for entering information for the laboratories (General information for

laboratories). RINGDAT3 will display the contents of this text box at the bottom of the Meas- ured values tab. Furthermore, in RingDat there is the possibility to print a protocol of the test results. It is possible to enter information for the laboratories to be displayed on these proto-

cols as well. This information will be shown on the header on the left and/or on the right. Make sure, the box Include general information in protocol is checked.

Before exporting, the order in which the combinations of samples and measurands are sort- ed in RingDat must be determined: according to the samples first and then the measurands

or vice versa.

Finally, via the Export button and the dialogue box which appears, all lab files can be saved

in the folder you select

urement values can be entered.

The *.lab files can now be opened with RingDat3.exe and meas-

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54 ProLab Plus – Manual . Menu Database Figure 36: Lab file for laboratory L005 opened

Figure 36: Lab file for laboratory L005 opened with RingDat3

Copy labwise to storage device

In this tab you can select a laboratory from the list on the left, a target drive (e.g. a pen drive) from the drop-down menu on the right and click on the Copy button. When the pen drive is removed from the computer, the input field Target drive will be empty. If Windows uses the same target drive letter again, as soon as a new pen drive is plugged in, the list in ProLab will show it again. If there are more than one pen drives plugged in, Win- dows will choose a different drive letter for each one. ProLab will store the creation date of the files copied onto the pen drive for each laboratory. That information can be seen via Database Participating laboratoriess and data yet to be submitted as well. On the sidebar there is a list of files to be copied onto the storage device. You can add your own files by clicking onto the list using the right mouse button.

7.11.3 Ring test

Besides the export of certain data (especially structure of ring test and test results) into an ASCII file, there also exists the possibility to save a ring test as a complete database. In or- der to do this, copies are generated of all important tables in the current database. These ta- bles contain only data of the selected ring test. They are denoted by the prefix ‘~’ and saved in an LZH table. Importing a ring test is carried out via Database Import Ring test (LZH compressed). Thereby it is possible to archive data of a ring test, delete the ring test from the current database and import it at a later point in time.

Please take note of the advice on long-term storage.

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7.11.4 Email merges

In ProLab Plus there is the possibility to send email merges to the participants of the ring test. The email merge module can be found under Database Export Email merge.

This is applicable for sending e.g.

- General information emails, such as announcements of meetings, delays and other ad- ministrative information

- Deadline reminder emails

- Single laboratory files including RingDat

- Downloads

- Analysis results and certificates

An important prerequisite for using the email merge module in ProLab Plus is the entry of email addresses in the basic tables of the database. More than one address can be specified by using spaces or semicolons as delimiters. Additional data fields, such as laboratory name, laboratory description, and the title of the contact person, are relevant as well.

and the title of the contact person, are relevant as well. Figure 37: Database – Basic

Figure 37: Database Basic tables Labs as Table: Enter relevant information

The first tab of the email merge window is called Compose email and this is where the email text can be entered, and the attachments specified. This is also where it is possible to deter- mine which laboratories should receive the email.

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56 ProLab Plus – Manual . Menu Database Figure 38: Database – Export – Email merge:

Figure 38: Database Export Email merge: Compose email

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Template files

There is the possibility to import and use templates for a email merge. To do so, specify the path of the file (.txt or .rtf) after clicking Import text file. In this text file, the only requirement is that the first line contains the subject of the email. The main body of the email then starts in the second line, typically beginning with the addressee’s title and name before proceeding with the content of the email.

and name before proceeding with the content of the email. Figure 39: Import of individual templates
and name before proceeding with the content of the email. Figure 39: Import of individual templates

Figure 39: Import of individual templates from a text file

After selecting a template (see example in Figure 39), the text file is transferred to the edita- ble text window. It is also possible to insert macros, that is to say, variables that stand for in- formation that changes from laboratory to laboratory and that is then entered in the email au- tomatically for each participant; for example, the addressee’s name and title, or the laborato- ry’s code, In order to insert a macro, mark the section in the email text where the it should appear and select the macro from the box Macro selection.

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Attachments

Attachments can be included as static attachments, which are the same for all laboratories, or as dynamic attachments, that is to say, attachments with laboratory-specific information that are only sent to the corresponding laboratories.

that are only sent to the corresponding laboratories. In order to include a file as a

In order to include a file as a static attachment, click on the button Add file ( ) below the At- tachments field and select the desired file. This static file is then sent to all laboratories, e.g. the final report which all laboratories should receive. The selected path appears under At- tachments.

A precondition for the attachment of dynamic files is, of course, that these laboratory files, which differ only in their laboratory name or description, have to be available. These different, laboratory-specific files will also have laboratory-specific names, or laboratory-specific paths.

laboratory-specific names, or laboratory-specific paths. To start, select one such file via the Add file button

To start, select one such file via the Add file button ( ). The corresponding path is now shown in the Attachments field. If you click on it, it will appear in the Edit field (orange) below the Attachment field. In the next step, mark the section in the file path where the macro should be inserted. Finally, select the desired macro from the box Macro selection.

Single attachments or all of them can be deleted via the buttons Remove selected file and Clear attachment.

the buttons Remove selected file and Clear attachment . Figure 40: Attaching a dynamic file to

Figure 40: Attaching a dynamic file to the email

Of course, the laboratories which should receive the email need to be selected as well. This

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is done in the right part of the tab Compose email. In this box, all laboratories that were sup- posed to participate in the current ring test are shown, i. e. all laboratories that were selected for participation. However, it might be that not all of these laboratories have submitted data. Thus, it is possible that not all of these laboratories should receive a particular email with at- tachments. For example, a report with individual results will not be available if a laboratory has not submitted any data.

Laboratories to which emails should be sent can be selected manually by marking the re- spective boxes. Alternatively, all laboratories can be selected in one step (Select all labs).

It is also possible to base the selection of laboratories on the existence of PDF files. In order to do this, there must be a folder with PDF files whose names refer to laboratory names. For example, one PDF file could be called Labmean (Merkmal) L001.pdf(see Figure 41). Using the button Selection by serial PDF files and choosing the relevant folder will lead to a selec- tion of only those laboratories referred to in a PDF file name in the chosen folder.

referred to in a PDF file name in the chosen folder. Figure 41: Selecting laboratories by

Figure 41: Selecting laboratories by PDF files

On the tab Preview, the email merges are displayed. All inserted macros are replaced by the corresponding data. The preview window shows one email after another with the individual attachments.

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60 ProLab Plus – Manual . Menu Database Figure 42: Preview of email merge The details

Figure 42: Preview of email merge

The details regarding the email server are displayed on the last tab Settings. Appropriate set- tings should be carried out by the administrator.

Before the emails are sent, an automatic data consistency check (e.g. the existence of all files to be sent as attachments) is carried out. It is also possible to carry out such a con- sistency check manually in the Compose email tab by using the button with the magnifier. ProLab Plus will tell you if the check was successful or not.

To send the emails, there are two possibilities: either (1) all emails are first saved in the out- box of the email program (Outlook, Thunderbird etc.) or (2) all emails are directly sent via the mail server of the provider. The first option has the advantage that all mails can be checked again with the email program and are listed in the Sent folder after they have been sent.

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ProLab Plus – Manual . Menu Database 61 Figure 43: Database – Export – Email merge:

Figure 43: Database Export Email merge: Settings

7.12 Import

ProLab Plus allows the import of

- The structure of the ring test with or without ring test results

- Laboratory addresses

- Measurands & samples with all characteristics

- Analytical methods & sample preparations

- Ring tests (LZH compressed)

Click in the menu item Database Import and select the type of data to be imported. In the following, the import of measurement data will be described in detail. The import procedure of addresses or information on the measurands and samples is similar.

7.12.1 Import of structure with or without test results

Almost all data that can be entered manually into the database may also be imported from EXCEL or CSV files.

The general structure of the import files is always the same: each column has to be assigned to a field in the database. The import procedure comprises the following steps:

1. select type of data to be imported,

2. open the import file or paste the data into the import window,

3. assign columns in the import file to database fields,

4. start transfer of the file into the database.

Click on

4. start transfer of the file into the database. Click on to open the import file.

to open the import file. In the opening dialogue box select the correct directory,

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file type (*.db, *.csv, *.lab, *.txt, *.xls, *.xlsx) and name of the import file. Excel files need to be saved as EXCEL 97 or above. The file to be imported must not be opened or used by an- other program. Alternatively, input via copy & paste is possible by either clicking into the empty table and pressing the key combination Ctrl + V, or by right-clicking and selecting the option Paste from the opening menu.

Subsequently the individual columns are assigned to the database fields. In order to select these fields, please click on the arrow in the top row of the relevant column. A list will appear where you can select the database fields. The fields M 1, M 2, …, M 32 correspond to the test results 1, 2, …, 32.

If the ring test is of nested design a certain order of the test results to be entered needs to be respected. For example if for three different days two measurement values are available, the design should be nested 3 x 2. Thus, in total there are up to six test results, the first two be- long to day 1, test results 3 and 4 to day 2 and test results 5 and 6 to day 3. The test results must be entered in that order.

Columns that are already assigned to database fields are highlighted in blue.

already assigned to database fields are highlighted in blue. Figure 44: Database – Import – Structure/ring

Figure 44: Database Import Structure/ring test results

Before the data is transferred into the database, all rows that do not contain valid mea- surements (e.g. the headline) should be deleted. This can be done by clicking with the right mouse button on the cell, column or row and selecting Delete.

If the first row contains the headers that should not be imported, simply check the box Ignore first line on the right side of the window.

The correct decimal delimiter in accordance with your data has to be chosen on the right side of the window before starting the transfer.

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The imported test results are always assigned to the currently selected ring test. If test re- sults should be imported into a new ring test, please create a new ring test in the menu Da- tabase Basic tables and select it for editing. Afterwards test results may be imported as de- scribed above.

If the import file only contains one laboratory, no column for lab names is required. In this case, mark the check box Laboratory on the right side of the window and enter the name of the laboratory. Proceed analogously if the import file only contains pertaining to one sample or measurand. The name of the laboratory or sample is entered into the corresponding field. This name is then assigned to all datasets of the file in question.

It is further to be noted that there are two columns each for sample, measurand and laborato- ry in the basic tables. Those columns refer to name and description. As the name must con- sist of no more than eight characters (alphanumerical or underscore), the import into ProLab Plus works as follows:

1. A name for each dataset is created by reducing the already existing text to eight characters, after removal of all characters that are not allowed.

2. If there is no already existing sample (or measurand or laboratory) with this name, it is applied. In this case, and in this case only, the entire original text will be used as de- scription.

3. If the name of a sample (or measurand or laboratory), that has already been imported during the current process, is the same as the newly generated one, ProLab Plus de- termines whether it corresponds to the same text. For example, since “A+” and “A-are assigned the same new name “A”, they would be treated as the same sample (or measurand or laboratory). In case of such a collision the user will be asked if both samples can be assumed to be identical.

It is recommended to use the semicolon as column (field) separator. Depending on the Win- dows setting, the use of comma or point is recommended as decimal separator.

After checking the plausibility of the table with respect to correct column assignment, start the transfer of data by clicking on the button Transfer data. Now all columns that contain val- ues attached to a database field (highlighted in blue) are entered successively in the data- base. Since an automatic comparison of the different tables is performed at the same time, the import of the file may take a few minutes. The changes within the database and error messages will be listed in the log window and the log file (see chapter 6.3).

Please note: Be aware that wrong names or column assignments for the laboratories, sam- ples, measurands or ring tests may have serious consequences for the database, and that restoring the original database or repairing the damage may take great effort. It is therefore important to thoroughly check the names and the assignment of the columns before starting the import. Moreover all tables of the database should be backed up first. For example, if a laboratory with name “001” has been defined in the Basic tables but, in the process of import- ing data, the name of the lab is changed to “1”, ProLab Plus will interpret this as a new labor- atory and will not assign the values to laboratory “001”. Thus, make sure the right format is defined in the Excel table (showing leading zeros etc…)

You can also import data if the corresponding laboratories, ring tests, samples and measur- ands have not yet been defined. In this case ProLab Plus will ask you if a cross-check of the

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tables should be performed. Click the All button to cancel the enquiry, which will otherwise reappear at every new entry.

Remember that descriptions cannot be entered in the Import menu, but only manually in the Basic Tables menu.

If there is a space character in between two separators, ProLab Plus will interpret this as a column that contains a NULL value.

Test results that contain invalid characters will result in a warning.

Test results with the character '<' will be interpreted as results below the limit of quantifica- tion. In this case the test result will be set to NULL and obtain the state NB. The actual value will be entered as the limit of quantification.

Test results with the character '+' will be interpreted as results above the “greater limit”. In this case the test result will be set to NULL and obtain the state GL. The actual value will be entered as “greater limit”.

7.12.2 Addresses, Measurands & samples, Analytical methods/Sample preparations

The import of laboratory addresses, samples and measurands, and of analytical methods and sample preparations is analogous to the procedure described in section 7.12.1.

7.12.3 Ring test

The basis for importing a ring test is an LZH-file that has been created earlier by exporting a ring test via Database Export Ring test (LZH compressed).

Please note that already existing data with identical names (whether ring tests, sam- ples, measurands or laboratories) will be overwritten after confirmation is given. The confirmation prompt will appear even if there are no values in the actual database but the fields are already defined.

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8 Test on homogeneity and stability

8.1 Import test results

This window allows the import of homogeneity and/or stability test results from an Excel file. The import is carried out as described in section 7.12.1.

If you want to enter the homogeneity test results manually you need first to encode the test portions (see section 8.2).

If only a test on homogeneity should be carried out, the Excel table has to contain columns for the sample name, the measurand, the test portion code and the test results. If a stability test should be carried out as well, an extra column for the date is necessary in order to dis- tinguish homogeneity and stability measurements.

Sample

Measurand

Test portion code

M 1

M 2

tuna

As

1

2.83

3.14

 

     

At first, the Excel table needs to be opened in ProLab Plus. Accordingly, it must not be al- ready opened with another program. The data may also be entered via copy & paste. In the next step, the columns need to be assigned and further import specifications need to be car- ried out before the import can be started.

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Plus – Manual . Test on homogeneity and stability Figure 45: Homogeneity/Stability – Import test results

Figure 45: Homogeneity/Stability Import test results

8.2 Encoding test portions

The window Test portion encoding offers the possibility to encode all test portions and select homogeneity test portions randomly.

For the sake of clarity, the following terminology is introduced: sample denotes different kinds of sample, such as water sample or soil sample. From each sample, test portions are pro- duced which are sent to the laboratories, used for the homogeneity analysis or kept behind as retain test portions or for stability analysis.

Furthermore, it has to be determined if the test portions for the laboratories (i. e. for the ring test) and for the homogeneity analysis are to be encoded uniformly, or if the test portions for the homogeneity analysis should be encoded separately.

Uniform encoding of all test portions (for laboratories and for homogeneity analysis) and random selection of homogeneity test portions

Encoding of all test portions is carried out in two main steps. First codes are generated for all test portions and then some of these test portions are assigned randomly to the laboratories and others to the homogeneity analysis. These encoding and selection steps are not per- formed in the menu Homogeneity/Stability but in the menu Database Encoding Test por- tions, because it is necessary to include the homogeneity test portions in the encoding from

8.2.1

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the beginning or else a random selection of these test portions cannot be ensured. If the ho- mogeneity test portions have not been considered from the beginning, the whole encoding including that for the laboratory test portions should be repeated (see also section 7.4.2).

If there are several kinds of sample available, there is the possibility to assign the codes in such a way that it is impossible to identify the kind of sample by means of the codes. If for example 100 test portions are produced for each of two samples, all 2 x 100 codes can be assigned to the test portions randomly over both samples instead of assigning codes 1 - 100 to the first sample and codes 101 - 200 to the second sample.

Via the menu Database Encoding Test portions, codes are generated at first for all pro- duced test portions, for the laboratories as well as for the homogeneity analysis the homo- geneity test portions are selected later on. The codes may be generated manually or auto- matically.

The individual steps are:

1. Enter the total number of test portions produced per sample, e.g. 95 test portions of which 80 (= number of laboratories) are shipped to the laboratories, 10 are used for the test on homogeneity and the remaining 5 test portions serve as retain test portions

2. Generate codes for test portions for the laboratories on the tab Test portion encoding:

for the laboratories on the tab Test portion encoding : 3. After encoding the test portions

3. After encoding the test portions for the laboratories, the test portions for the homogenei- ty test have to be encoded. To do so, select the tab Homogeneity test portion encoding or the menu item Homogeneity/Stability Test portion encoding.

4. Enter the number of test portions for which the homogeneity analysis will be carried out, e.g. 10 of the 95 test portions of each sample;

5. Generate the codes for the test portions of the homogeneity analysis via the button

;
;
test portions of the homogeneity analysis via the button ; Figure 46: Database – Encoding –

Figure 46: Database Encoding Test portions: Steps 1 and 2 for encoding test portions

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After the codes have been generated, labelling of the test portions can be carried out. The labels should be printed beforehand, as should the overview of the assignment of labels to test portions. The labels can be edited individually before printing.

For each sample, the assignment overview as well as the labels are sorted in ascending or- der according to their code. Then, for the sample in question, labels can now be affixed suc- cessively to randomly selected test portions. The labelled test portions can then be sorted according to whether they are to be shipped to the laboratories or are meant for the homo- geneity analysis.

be shipped to the laboratories or are meant for the homo- geneity analysis. Figure 47: Assignment

Figure 47: Assignment overview

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8.2.2 Random selection of test portions for homogeneity test without encoding test portions for laboratories

ProLab Plus allows the random selection of homogeneity test portions from all produced test portions without having to encode all of them. This is done under Homogeneity/Stability Test portion encoding. First, the total number of test portions (per sample) needs to be speci- fied, as well as the number of homogeneity test portions. In the case that more than one sample are being tested, the codes will be spread randomly over all samples.

The proceeding is as follows:

1. Enter the total number of test portions (per sample), e.g. 100

2. Enter number of test portions per sample used for the homogeneity analysis, e.g. 10

3. Generate the codes for the random selection of the test portions for the homogeneity

the codes for the random selection of the test portions for the homogeneity analysis via the

analysis via the button .

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Plus – Manual . Test on homogeneity and stability Figure 48: Homogeneity/Stability – Encoding test

Figure 48: Homogeneity/Stability Encoding test portions: Steps 1, and 2 for encoding test portions

test portions: Steps 1, and 2 for encoding test portions Figure 49: Homogeneity/Stability – Test portion

Figure 49: Homogeneity/Stability Test portion encoding: Step 3 for encoding test portions

The test portions for the homogeneity test can now be selected according to the randomly generated codes. Ideally, all produced test portions already have a unique number ( e.g. or- der of production) so that all that remains to be done is to select the test portions with the corresponding numbers. If there is no such numbering, the selection may be made simply by counting.

8.2.3 Another example for encoding test portions

Ring test organiser’s situation 100 laboratories will participate in the ring test. For these participants there are 115 test por- tions containing 230 g of material and another 100 test portions containing 700 g of material,

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which can be used as reference material at the end of the test. So in total there are 215 test portions. For the test on homogeneity 20 of those 215 portions should be selected. For the first group (with test portions containing 230 g material) a maximum of 15 test portions may be randomly selected, otherwise there would not be enough test portions for all participants left.

Solution using ProLab Plus In the first step the number of test portions in the window Database Encoding Test por- tions Test portion encoding will be determined as 115. When clicking on the button with the little key, the 100 test portions for the laboratories will get a randomly selected code in the range from 1 to 115. After that using the tab Homogeneity test portion encoding the total number of test portions will be raised to 215. In the next encoding step the test portions for homogeneity tests will be randomly selected out of the remaining 15 portions containing 230 g and the remaining 100 portions containing 700 g.

8.3 Test results

Test results for the homogeneity and/or stability test may be entered manually in the window Homogeneity/Stability Test results. At the top of the window you can choose the sample and measurand. You can enter up to 32 test results for each test portion. If it is necessary to distinguish between homogeneity and stability results, a date must be entered.

homogeneity and stability results, a date must be entered. Figure 50: Homogeneity/Stability – Test results quo

Figure 50: Homogeneity/Stability Test results

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8.4

Computation

8.4.1 Assignment of test portions

If data for both the test on homogeneity and the test on stability have been imported, it is necessary to determine which data belong to the homogeneity analysis and which to the sta- bility analysis. This is accomplished by specifying date ranges for both kinds of samples.

If no stability analysis has been carried out, no date range needs to be defined in order to carry out the analysis of the homogeneity test results. In this case, simply all available data are used in the statistical analysis. For the stability test, however, a date range always needs to be defined. In that case it is absolutely necessary to include dates in the database.

it is absolutely necessary to include dates in the database. Figure 51: Specifying date ranges for

Figure 51: Specifying date ranges for analysis of homogeneity samples and stability samples (in this ex- ample, the homogeneity analysis has been carried before 31 st July 2010, whereas the stability samples have been analysed after 30 th September 2010)

8.4.2 Homogeneity

For the test on homogeneity, the following statistical methods are available:

- F test:

- ISO 13528:

- Harmonized Protocol: Test on significant heterogeneity 4

Check for significant heterogeneity

Check for sufficient homogeneity

4 M. Thompson, S. L. R. Ellison and R. Wood: Pure Appl. Chem., Vol. 78, No. 1, pp. 145196, 2006.

doi:10.1351/pac200678010145

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The necessary parameters for the test on homogeneity are the analytical precision s(analytical) (standard deviation within the test portions) and the heterogeneity standard de- viation s(samples) (standard deviation between the test portions).

All standard deviations can be displayed and used in the calculations as absolute or as rela- tive quantities. The selection is done in the upper left part of the window.

The F test is used to determine whether the heterogeneity standard deviation s(samples) de- viates significantly from zero to a significance level of 5 %, i. e. if it can be assumed that the difference between the mean values are caused by measurement deviations only. If the latter is the case, the assumption of sample homogeneity is accepted. If not, it can be concluded that the sample is not suitable for a ring test.

For the method according to ISO 13528 and to the Harmonized Protocol, a target standard deviation s(target) is necessary.

In ISO 13528, the heterogeneity standard deviation is compared to the target standard devia- tion. The samples can be considered sufficiently homogenous if the heterogeneity standard deviation is not greater than 0.3 x target standard deviation. The motivation of the factor 0.3 is the fact that in the case of agreement between the target standard deviation and the re- producibility standard deviation (here, the heterogeneity standard deviation), the latter in- creases due to the sample heterogeneity by 10 % at most.

According to the Harmonized Protocol (2006), the hypothesis that the sample is sufficiently homogenous is checked. In a first step, the analytical precision is analysed. This must be smaller than 0.5 x target standard deviation. An insufficient analytical precision may conceal significant sample heterogeneity. In a second step, the heterogeneity standard deviation is analysed. If the latter exceeds the allowable quantity of 0.3 x target standard deviation to a significance level of 5 %, the hypothesis is rejected, and the sample is deemed unsuitable.

The Harmonized Protocol does not make heavy demands regarding the sample homogenei- ty. Even if the heterogeneity standard deviation is significantly larger than zero and lies within the range of 50 % of the target standard deviation, the samples might be accepted.

In ProLab Plus, at first the mean value, the analytical precision and the heterogeneity stand- ard deviation are displayed in a table for each sample-measurand combination. The result of the F test is shown as well: “OK” means that there is no significant heterogeneity; “Not OK” means that there is significant heterogeneity.

For the test according to ISO 13528 and the Harmonized Protocol, the target standard devia- tion needs to be specified at first. This has to be carried out for each sample-measurand combination. The following modes are available:

- Horwitz: calculation of the target standard deviation according to Horwitz

- Corrected Horwitz: if the relative target standard deviation according to Horwitz is grea- ter than 22 %, it is truncated to 22 %

- Manual: fixed quantity for target standard deviation, e.g. 10 %

- Target standard deviation from ring test: applicable after analysing a ring test, i. e. after the data of the ring test have been analysed statistically

For the calculation of the Horwitz standard deviation, a so-called multiplicator corresponding to the measurement unit is necessary. Therefore, before calculating the Horwitz standard

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deviation, a unit and the respective multiplicator need to be specified for each measurand. This is done under Database Characteristics of measurands (see also section 7.6).

The Horwitz standard deviation as well as the corrected Horwitz standard deviation may be further adjusted by the Horwitz Ratio (HORRAT). The HORRAT value is the ratio between the reproducibility standard deviation of a ring test and the Horwitz standard deviation. A HORRAT value smaller than 1 shows that the reproducibility standard deviation of the ring test is smaller than the respective Horwitz standard deviation. HORRAT-corrected standard deviations may be calculated by multiplying the Horwitz standard deviation by the HORRAT value. This HORRAT-corrected Horwitz standard deviation may be used as an estimation for the reproducibility standard deviation expected in the current ring test. If the current repro- ducibility standard deviation is larger than the HORRAT-corrected Horwitz standard deviation computed on the basis of data from a former ring test, it may be an indication that specific analytical difficulties have appeared which may have been caused by a different sample ma- trix.

The specification of the mode of the target standard deviation is carried out via the scroll- down menu in the column Mode s(target). If a HORRAT value is available, it can be entered manually in the column HORRAT. As soon as a value is entered that differs from 1, the HORRAT-corrected target standard deviation is calculated automatically. In the mode Ma- nual the target standard deviation needs to be entered manually in the corresponding col- umn.

Example:

The procedure is explained by the example in Figure 52:

For the measurand Arsenic the mode Horwitz has been selected and a HORRAT value of 0.75 has been specified. The relative target standard deviation is 0.75 x 13.69 % = 10.27 %.

For the measurand Copper the mode Manual has been selected and a relative target stand- ard deviation of 20 % has been specified manually.

For the measurand Lead the mode Horwitz has been selected and the relative target stand- ard deviation equals 17.78 %.

After the specification of the target standard deviation, the results of the test on homogeneity according to ISO 13528 and the Harmonized Protocol are displayed.

- ISO 13528

o

OK = sufficient homogeneity

o

Not OK = insufficient homogeneity

- Harmonized Protocol

o

OK = no significant heterogeneity

o

Not OK = significant heterogeneity

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