The Sixth International Proficiency Testing Conference

(03)04th − 06th October 2017

Cristina Stancu, Mariana Coarna

CEPROCIM S.A., Blvd. Preciziei, no. 6, Sector 6, Bucharest, Romania

ABSTRACT
The aim of this paper is to present the results of eight yearly rounds of a proficiency testing program for laboratories (called Interlaboratory Test) testing two of the most important properties of an
adhesive for ceramic tiles: initial adhesion strength according to the standard EN 1348 art. 8.2 (test used in all 8 editions) and tensile adhesion strength after water immersion according to EN 1348 art. 8.3
(test used only in last 2 editions).
In the last 8 years between 9 and 38 Institutes/ Laboratories of research and Adhesive for ceramic tiles manufacturers from nineteen European countries joined our program. The participation at this
scheme is useful in the evaluation of the laboratories performance and to identify the eventually problems, if is the case. The goal of every participant is to obtain “satisfactory” results, meaning that
there is capable to provide reliable results. The condition of obtain “satisfactory” results is one of the necessary requirements for the authorised or accredited laboratories. Robust statistical procedures
according to ISO 13528 were used to calculate the z-scores and the statistical parameters. About 94% of the test results provided by the participant laboratories were framed as “satisfactory”, having
IzI ≤ 2, according to EN ISO/CEI 17043, both for initial adhesion strength and tensile adhesion strength after water immersion.

INTRODUCTION
Interlaboratory tests represent the means by which each laboratory can evaluate its competence and establish a common language regarding the values obtained for the technical characteristics of the
tested products. Interlaboratory test represents also a requirement for all accredited laboratories, or in course of accreditation, which must conform to the requirements of EN ISO/IEC 17025:2005 +
EN ISO/ IEC 17025:2005/AC:2006 for participation in interlaboratory comparisons or proficiency testing programmes.
Besides the main purpose of performance evaluation, it is estimated that Interlaboratory tests have other roles such as: identification of possible problems during the determinations, training personnel, conferring
an increased customer confidence in the results provided by the laboratory, a tool for regulatory bodies in the certification process (e.g. bodies for evaluation and verification of constancy of performance).
In this general context, CEPROCIM initiated in 2008 an Interlaboratory tests program yearly carried out on cementitious adhesives for ceramic tiles, aiming to assess laboratories’ ability to competently perform the
initial adhesion strength and tensile adhesion strength after water immersion according to EN 1348:2008 and, the present paper summarises the obtained results of five rounds, between 2008 and 2016 .

ORGANIZING THE INTERLABORATORY TEST PROGRAM

 Samples send to the participants
Every year were prepared a number of about 30 ÷ 60 parcels, rising from a edition to another, containing a bag with adhesive, 30 pieces of ceramic tiles EN 1348 and two pieces of concrete slabs in the
first 6 editions/ a piece of concrete slab for the last 2 editions. Through the eight editions of the Interlaboratory Tests on Adhesives for ceramic tiles different types of adhesives according to EN 12004
produced by different manufacturers from Romania were use (i.e. C2FTE, C2TE, etc.).
Establish the samples homogeneity
The test used for all the eight editions of the Interlaboratory tests on Adhesives for ceramic tiles for establishing the homogeneity of the adhesive for ceramic tiles was determination of 0.250 mm residue.
Establish the assigned value and the standard uncertainty of the assigned value. Evaluation of the results using the «z»-score
For the statistical calculation, algorithm A in Annex C from the standard ISO 13528:2015 was applied. This implies an iterative calculation of the robust values for mean and standard deviation based on
all the participants’ results, including CEPROCIM’s results. The value obtained after the last iteration represents the assigned value (X) chosen to be the consensus value. In the z-score calculation
program the assigned value and the standard deviation associated to the assigned value have been used as they result from calculation without being round.

RESULTS AND DISCUSSIONS

Table 1. The evolution of the statistical parameters for all 8 editions of Interlaboratory Test on adhesives for ceramic tiles
Statistical parameters
Edition
p x min x max x* s* X s uX V
Ist edition Initial adhesion strength ILC provider's concrete slabs 18 0.5 2.8 1.1 0.7 1.5 0.9 0.3 59
IInd edition Initial adhesion strength ILC provider's concrete slabs 22 0.7 2.7 1.1 0.4 1.1 0.3 0.1 28
IIIrd edition Initial adhesion strength ILC provider's concrete slabs 26 0.7 2.8 1.4 0.3 1.5 0.4 0.1 29
IVth edition Initial adhesion strength ILC provider's concrete slabs 34 0.6 1.8 1.2 0.3 1.2 0.3 0.1 24
Vth edition Initial adhesion strength ILC provider's concrete slabs 43 1.6 5.1 2.0 0.2 2.0 0.2 0.0 12
ILC provider's concrete slabs 28 1.2 2.6 2.2 0.4 2.1 0.4 0.1 19
VIth edition Initial adhesion strength
Participant own concrete slab 25 1.3 2.6 2.0 0.4 1.9 0.4 0.1 22
ILC provider's concrete slabs 26 0.2 2.0 0.8 0.2 0.8 0.2 0.1 29
Initial adhesion strength
VIIth edition Participant own concrete slab 24 0.1 1.8 0.8 0.1 0.8 0.2 0.1 29
Tensile adhesion strength after water immersion Participant own concrete slab 25 0.4 2.0 0.6 0.1 0.6 0.2 0.1 30
ILC provider's concrete slabs 38 0.8 4.2 1.7 0.3 1.6 0.3 0.1 20
Initial adhesion strength
VIIIth edition Participant own concrete slab 35 0.8 2.6 1.6 0.4 1.6 0.4 0.1 25
Tensile adhesion strength after water immersion Participant own concrete slab 35 0.6 1.9 1.1 0.3 1.1 0.3 0.1 25

3 3 3

2 2
2
1
1 1
z-score

0
z-score
z-score

0 0
-1
-1 -2 -1

-2 -3
-2
-4 1 2 3 4 5 6 7 8 9
-3 10 11 12 13 14 15 16 17 18
1 2 3 4 5 6 7 8 9 19 20 21 22 23 24 25 26 27
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 28 29 30 31 32 33 34 35
10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26
19 20 21 22 23 24 25 26 27 28 27 28 29 30 31 32 33 34
29 30 31 32 33 34 35 36 35 36
37 38 No. participants No. participants
No. participants
1st edition 2nd edition 3rd edition 4th edition 5th edition 6th edition 7th edition 8th edition 6th edition 7th edition 8th edition 7th edition 8th edition
Fig. 1. The z-score results for determination of initial Fig. 2. The z-score results for determination of initial adhesion Fig. 3. The z-score results for determination adhesion
adhesion strength on concrete slabs given by the strength on participant own concrete slab strength after water immersion strength on participant
organizers own concrete slab

CONCLUSIONS
 Beginning with the year 2008 CEPROCIM had yearly organized the Interlaboratory test program on adhesives for
1.85 %
1.57 %
1.88 %
INSTITUTES/
LABORATORIES OF
94.44 %
2.78 %
INSTITUTES/
LABORATORIES OF
ceramic tiles. At this scheme, a group of 9 - 38 laboratories representing institutes/laboratories of research and
93.73 % 3.45 % RESEARCH
4.63 %
2.82 % 0.93 %
RESEARCH
adhesive for ceramic tiles manufacturers from all over Europa took part at least once.
ADHESIVE

1.25 %
1.57 % MANUFACTURERS 0.93 % ADHESIVE  Beginning with the first edition of the scheme the determination subjected to the program was initial adhesion
MANUFACTURERS
strength according to EN 1348 using all materials send by the provider.
 Starting with the VIth edition, we have expanded our area by introducing the possibility for the participants to
Satisfactory Questionable Unsatisfactory Satisfactory
Institutes/ Laboratories Questionable
of research AdhesiveUnsatisfactory
manufacturers participate in the schema with the results obtained using a concrete slab of their own, too.
a) b)  Since VIIth edition we have expanded the area even more by introducing the adhesion strength after water
immersion test, too.
Fig. 4. The evaluation of the results obtained by all participants at the  Over 94% of the test results provided by the participant laboratories could be framed as “satisfactory”
Interlaboratory Test on the Adhesive for the determination of: (having IzI ≤ 2) according to EN ISO/CEI 17043, which proves that overall the participating laboratories performed
a) initial adhesion strength; b) adhesion strength after water immersion well and tend to improve their working procedure.