Introduction to the subject

QUALITY IN THE ANALYTICAL

LABORATORY

3rd level in chemistry

Introduction to the subject

Subject 6 ECTS: 150 h (60 h P + 90 h NP)

LECTURES: 12 hours
• Group 1: Montserrat Hidalgo Núñez
• Group 8: Antonio Canals Hernández

LABORATORY: 39 hours: Block 1 (21 hours) + Block 2 (18 hours)

Montserrat Hidalgo Núñez (L1)

Block 1 Miguel Ángel Aguirre Pastor (L2)
Ignacio Solaberrieta Gonnet (L3)
• Groups L1+L2+L3:
Montserrat Hidalgo Núñez (L1)
Block 2 Miguel Ángel Aguirre Pastor (L2)
Ignacio Solaberrieta Gonnet (L3)

SEMINARS: 3 hours
• Group S1: Montserrat Hidalgo Núñez
• Group S8: Antonio Canals Hernández

TUTORIALS: 6 hours
• Group T1: Montserrat Hidalgo Núñez
• Group T8: Antonio Canals Hernández
Introduction to the subject

TUTORSHIP: Monday and Wednesday, from 9:00 to 11:00 am. Prof. office at
3rd floor of Sciences II building (ask in advance tutorship by “campus
virtual”)

Sciences II building
Analytical Chemistry Dptm
3rd floor
 Introduction to the subject

Theory syllabus
2 February – 10 March
Theoretical program

ü CHAPTER 1: Quality in the analytical laboratory: Introduction

ü CHAPTER 2: Traceability of measurement results
ü CHAPTER 3: Uncertainty of measurement: Principles
ü CHAPTER 4: Single laboratory validation of measurement
ü CHAPTER 5: Inter-laboratory comparison exercises

Application of concepts: 22 March

S1/S8: Traceability, validation, uncertainty budget: Practical case

Out of class:

EVC: Traceability, validation, uncertainty budget: Practical case

 Introduction to the subject

Theoretical concepts
Theoretical program

TrainMiC Programme
Training in metrology in chemistry
(msc-euromaster.univ-lyon1.fr)

Goal
To provide training about quality
assurance for analytical measurements
to assist to interpret and implement the
technical requirements of ISO-IEC-
17025 for chemical and bio-analytical
measurement
 Introduction to the subject

Theoretical concepts
Theoretical program

Application of concepts:

Seminars S1/S8 to study a practical case: Traceability,

validation, uncertainty budget (informatics classroom)

Mr. Alfredo Sánchez Agulló

Graduate in Chemistry. External evaluator
of ENAC (freelance)
Public healthcare laboratory of Alicante Last day of lectures (10th of March,
tentative)
2 hours
 Introduction to the subject

Practicals in lab

XXII Interlaboratory comparison exercise for Analytical

Practical program

Chemistry students

Students from different Spanish Universities

analyze the same material

Results of all students are statistically compared

The exercise Organizer submits a final report.

Students could compare their results obtained in
the exercise
 Introduction to the subject

INTERCOMPARISON EXERCISE (INTER-LABORATORY COMP.)

Practical program

Organization, performance and evaluation of measurements or

tests on the same or similar tests items by two or more
laboratories in accordance with predetermined conditions

Goal

To assess the quality of results obtained by the labs

(to demonstrate their aptitude - PT)

Laboratory: To demonstrate its Learning

competence

• “Yourself” (inside your laboratory)

• To direct customers
• To third parties
 Introduction to the subject

Teaching/learning goals
Practgical program

üTo motivate the students about the need to get reliable results in the
analytical labs

üTo contribute to the acquisition of competences and fundamental skills

for future professional development

üTo promote the critical point-of-view of the students to assess the

analytical results and propose corrective actions if necessary

üTo apply a tool for the evaluation and improvement of teaching quality
of Analytical Chemistry

ü To familiarize students with the official methods of analysis

 Introduction to the subject

PARTICIPATING UNIVERSITIES
Practical program

ü IES Mateo Alemán (Alcalá de Henares)

ü Universidad de Alicante (Alicante)
ü Universitat de Barcelona (Barcelona)
ü Universidad de Cádiz (Cádiz)
ü Universitat de Girona (Girona)
ü Universidad Autónoma de Madrid (Madrid)
ü Universidad de Málaga (Málaga)
ü Universidad del País Vasco (San Sebastián)
ü Universidad de Salamanca (Salamanca)
ü INS Escola del Treball (Barcelona)
ü CIFP Avilés (Avilés)
ü Universidad de Extremadura (Badajoz)
ü IES Juan Carlos I (Murcia)
 Introduction to the subject

HOW IS AN INTERLABORATORY COMPARISON EXERCISE ORGANIZED?

Practical program

Realization of the exercise

• Distribution of samples among the participants by the

Organizer of the exercise (University of Barcelona)
• Analysis of samples by the participants
• Reporting by participants to the Organizer

Exercise assessment

• Evaluation of results by the Organizer

• Reporting the results by the Organizer to participants
• Draw conclusions (Laboratories - corrective actions)
 Introduction to the subject

REPORT FROM THE ORGANIZER

Practical program

Statistical treatment of results

 Introduction to the subject

HOW ARE LABORATORY PRACTICES ORGANIZED?

Practical program

Available samples (Reference Materials – RM) and

parameters to determine:
• Ground soil: pH, conductivity, removable K and assimilable P
• Pharmaceutical preparation: acetylsalicilic acid and paracetamol
contents
• Solid milk: ashes, calcium and zinc (refered to dry sample)
• Beer: ethanol, total acidity and pH

Organization
• Groups of three/four students
• Some groups of students will receive the same sample type, but
with different reference code
• The reference code of sample “must be indicated” in the final
report
 Introduction to the subject

DEVELOPMENT OF PRACTICE

Procedure
Practical program

(1) Preliminary information supplied

• Type of sample to analyze
• Parameters to determine and how to give the results

(2) Information searching TC (TNP)

• Bibliographic searching of analytical methods to get
the parameters Report TB

(3) Selection of analytical method 1st Tutorial

• Discussion about the “best” method

(4) Block 1
Training period
• The selected method is applied to some test samples Report 1
2nd Tutorial
(5) Interlaboratory comparison exercise Block 2
• The tested method is used to analyze a RM
Report 2
 Introduction to the subject
DEVELOPMENT OF PRACTICE

(4) – Training period

Practical program

The selected method is tested with a real sample:

• Ground soil: soil from the Alicante area (supplied)
Block 1 • Analgesic: pharmaceutical preparation “Actrón” (supplied)
23 March - 31 March • Solid milk: commercial solid milk (supplied)
• Beer: commercial beer (no supplied)

Preparation of the working protocol

Method application to replicates of test samples Modifications to

Getting results improve the
quality of the
Statistical analysis and interpretation of results results

Establishment of the method to be applied

Report 1 2nd Tutorial: discussion of results Block 2

 Introduction to the subject
DEVELOPMENT OF PRACTICE

(5) – Interlaboratory comparison

Practical program

Block 2 The tested method is used to analyze a

2 - 4 May RM supplied by the Organizer

The previously tested method is used

Statistical analysis of replicates (mínimum 3)

Getting results

Reporting results (IC exercise) Report 2

3rd Tutorial: results discussion and 5 of May

reporting to the Organizer (method/results)

Reporting the results (and method) to the Organizer Results of 3

independent
Quality assessment of obtained results determinations
 Introduction to the subject

INFORMATION ABOUT THE SAMPLES (RM)

Practical program

Preparation and spreading out of samples:

RM are specially prepared by the laboratory “Mat Control” of
Analytical Chemistry Department (Universidad Barcelona).
This laboratory studies the uniformity and stability of RM and
organizes the IC exercise.

Establishment of reference values:

Organizing committee composed of several educational
centers (Universidad Complutense de Madrid, Universidad
del País Vasco, Universitat Jaume I y Universitat de
Barcelona). It establishes the reference values of
parameters investigated in the IC exercise.
 Introduction to the subject

INFORMATION ABOUT THE SAMPLES (RM)

Practical program

Samples and parameters to determine

RM Beer: 250 mL/unit (supplied by San Miguel (Lleida), same manufacturing lot)

- Ethanol (% weight) Analytical methods suggested (Official Method

- Total acidity (% lactic acid) of Analysis and/or any other method
- pH previously tested)
Will be stated after the bibliographic searching

RM Ground soil: 150 g/unit (agricultural ground soil from the area of Barcelona)

- pH Analytical methods suggested (Official

- Conductivity (µS/cm) Method of Analysis and/or any other method
- Moisture (%) previously tested)
- Assimilable P (mg/kg, s.m.s) Will be stated after the bibliographic
- Removable K (mg/kg, s.m.s) searching
 Introduction to the subject

INFORMATION ABOUT THE SAMPLES (RM)

Practical program

Samples and parameters to determine

RM Solid milk: 30 g/unit (commercial: La Lechera, Nestlé, prepared mixing

different units from the same production lot)
- Moisture (%) Analytical methods suggested (Official Method
- Ashes (%) of Analysis and/or any other method previously
- Calcium (%, s.m.s) tested)
- Zinc (mg/kg, s.m.s) Will be stated after the bibliographic searching

RM Analgesic: 5 g/unit (prepared from: pure substances – acetylsalicilic acid and

paracetamol – matrix of sacarose, with similar composition to commercial
products)

- Acetylsalicilic acid (%) Analytical methods suggested (Official Method

- Paracetamol (%) of Analysis and/or any other method previously
tested)
Will be stated after the bibliographic searching
 Introduction to the subject
ASSESSMENT

Bibliographic
search
Assessment

Report of results
Practical lab
45%
and reports Work performance and
attitude
TNP – Similar to the one done
Exercise 5%
on seminars

Theoretical questions and/or

Final exam 50%
problems (theory + practical)

Attendance to in-class activities is mandatory (³ 80%

lectures/seminars)
Attendance to the assigned lab sessions is mandatory (³ 80 %)
Minimum threshold (4.0 lab and 4.0 final exam) to compute
Second option: only for the final exam
 Introduction to the subject
ASSESSMENT

Quality of presentation
Contents (tested methods, tests
Assessment

Report 1 performed, … ) 100%

The information collected through Calculations, expression of results
bibliographic search (bibliografic Conclusions
work) and justification of the
method(s) choiced will be taken
into account Quality of presentation, contents,
calculations, expression of results
70%
Uncertainty budget
Report 2 Conclusions
If applicable
Results of IC exercise 30%
Performance assessment (option 1)*

≤2 Satisfactory (3 points)
x lab - X ass
zeta score: x= |x| > 2 but ≤ 3 Questionable (2 points)
2 2
u +u
lab ass Unsatisfactory (1 point)
>3
% RSD > % RSD mean of all participant results (- 1 point)

(*) if the Organizer supplies the certified values (UA statistical treatment)
 Introduction to the subject
ASSESSMENT

Quality of presentation
Contents (tested methods, tests
Assessment

Report 1 performed, … ) 100%

The information collected through Calculations, expression of results
bibliographic search (bibliografic Conclusions
work) and justification of the
method(s) choiced will be taken
into account Quality of presentation, contents,
calculations, expression of results
70%
Uncertainty budget
Report 2 Conclusions
If applicable
Results of IC exercise 30%
Performance assessment (option 2)*

≤2 Satisfactory (3 points)
Z score:
𝑥!"# − 𝑋"$$ Questionable (2 points)
Organizer (Barcelona) 𝑍= |Z| > 2 but ≤ 3
𝑠 Unsatisfactory (1 point)
>3
UA % RSD > % RSD mean of all participant results (- 1 point)

(*) if the Organizer does not supply the certified values (Organizer statistical treatment + UA
correction)
 Introduction to the subject
BIBLIOGRAPHY

Books
Bibliography

• COMPAÑÓ, Ramón; RÍOS, Ángel, “Garantía de la calidad en los laboratorios analíticos”, Ed. Síntesis,
Madrid (2002)
• VALCÁRCEL, Miguel; RÍOS, Ángel, “La calidad en los laboratorios analíticos”, Ed. Reverté, Barcelona
(1992).
• MILLER, James M. ; MILLER, Jane Charlotte, “Estadística y quimiometría para química analítica”, Ed.
Prentice Hall, Madrid (2005).
• VALCÁRCEL, Miguel, et al., “Foundations of Analytical Chemistry: A teaching-learning approach”,
Springer International Publishing, 2018.

Web sites
http://www.eurachem.org/
http://www.eurachem.org/index.php/publications/guides/mv ® (Validation)
http://www.eurachem.org/index.php/publications/guides/quam ® (Uncertainty)
http://www.eurachem.org/index.php/publications/guides/trc ® (Trazeability)
http://www.eurachem.org/index.php/publications/guides/usingpt ® (Inter-lab/Proficiency testing )
http://www.eurachem.org/index.php/publications/guides/usingrm ® (Reference materials)
http://www.european-accreditation.org/publications
 Introduction to the subject

TENTATIVE DATES TO PRESENT REPORTS

Dates

Bibliographic search Analytical methods 6 March

1st lab report Block 1: Training 24 April

2nd lab report Block 2: IC exercise 10 May

Practical exercise
Exercise 28 April
resolution
 Introducción a la asignatura
Formación de grupos y asignación de muestras

Prácticas = Grupo castellano + Grupo inglés

Grupos de laboratorio

- Se formarán 14 grupos de prácticas

- Habrá 3 o 4 grupos por cada tipo de muestra, dependiendo de la muestra:
4 suelo / 4 leche en polvo / 3 cerveza / 3 preparado farmacéutico
- Cada grupo estará formado por 3 alumnos, con las siguientes excepciones:
• 2 grupos de suelos estarán formados por 4 alumnos
• 2 grupos de leche en polvo estarán formados por 4 alumnos

- La composición de los grupos será libre (los alumnos pueden elegir su agrupamiento - 3
personas máximo, con las excepciones indicadas arriba)
- Una vez decidida la composición del grupo, uno de sus integrantes lo comunicará a la
coordinadora de la asignatura (Montserrat Hidalgo) mediante tutoría por campus virtual,
indicando también la muestra elegida (leche en polvo, preparado farmacéutico, suelo o
cerveza)
- La asignación de la muestra a un determinado grupo, y la aceptación de la composición del
grupo, se hará por orden de recepción de la tutoría. En caso de que no sea posible asignar la
muestra y/o composición solicitada a un determinado grupo (por exceder el máximo de
grupos permitidos por muestra, o el máximo nº de alumnos), se le comunicará al grupo
solicitante, indicando también qué muestras quedan libres para elegir y el nº de alumnos
permitido