Bsi bs en 01423 2012 (2013)

54 Annex J normative Test method to determine glass beads and antiskid aggregates ratio in mixtures of the two .... The main changes incorporated in this revision are: a Modification of

BSI Standards Publication

Road marking materials — Drop on materials — Glass beads, antiskid aggregates and mixtures of the two

This British Standard is the UK implementation of EN 1423:2012, incorporating corrigendum February 2013 It supersedes BS EN 1423:1998 which is withdrawn.

The start and finish of text introduced or altered by corrigendum is indicated in the text by tags Text altered by CEN corrigendum February 2013 is indicated in the text by 

The UK participation in its preparation was entrusted by Technical Committee B/509, Road equipment to Subcommittee B/509/2, Horizontal road markings and road studs

A list of organizations represented on this subcommittee can be obtained on request to its secretary

This publication does not purport to include all the necessary provisions

of a contract Users are responsible for its correct application

© The British Standards Institution 2013

Published by BSI Standards Limited 2013ISBN 978 0 580 82420 3

Amendments/corrigenda issued since publication

Date Text affected

30 June 2013 Implementation of CEN corrigendum February 2013

NORME EUROPÉENNE

English Version

Road marking materials - Drop on materials - Glass beads,

antiskid aggregates and mixtures of the two

Produits de marquage routier - Produits de saupoudrage -

Microbilles de verre, granulats antidérapants et mélange de

ces deux composants

Straßenmarkierungsmaterialien - Nachstreumittel - Markierungs-Glasperlen, Griffigkeitsmittel und

Nachstreugemische

This European Standard was approved by CEN on 17 December 2011

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member

This European Standard exists in three official versions (English, French, German) A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom

EUROPEAN COMMITTEE FOR STANDARDIZATION

C O M IT É E U R O P É E N D E N O R M A LIS A T IO N EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2012 CEN All rights of exploitation in any form and by any means reserved

Incorporating corrigendum February 2013

Contents

Foreword 5

1 Scope 6

2 Normative references 6

3 Terms and definitions 6

4 Requirements 7

4.1 Glass beads 7

4.1.1 Surface treatments of glass beads 7

4.1.2 Visibility characteristics 7

4.1.3 Granulometry 8

4.1.4 Dangerous substances 10

4.1.5 Durability aspects  Resistance to chemicals: water, hydrochloric acid, calcium chloride and sodium sulphide 10

4.2 Transparent antiskid aggregates 10

4.2.1 pH value 10

4.2.2 Granulometry 10

4.2.3 Dangerous substances 12

4.2.4 Durability aspects  Resistance to fragmentation (friability) 12

4.3 Non transparent antiskid aggregates 12

4.3.1 pH value 12

4.3.2 Visibility characteristics 12

4.3.3 Granulometry 13

4.3.4 Durability aspects  Resistance to fragmentation (friability) 14

4.4 Mixtures of glass beads and antiskid aggregates 14

4.4.1 General 14

4.4.2 Durability aspects 15

5 Testing, assessment and sampling methods 15

5.1 General 15

5.2 Sampling 15

5.3 Glass beads 16

5.3.1 Surface treatments of glass beads 16

5.3.2 Visibility characteristics 16

5.3.3 Granulometry 16

5.3.4 Dangerous substances 16

5.3.5 Durability  Resistance to chemicals: water, hydrochloric acid, calcium chloride and sodium sulphide 16

5.4 Transparent antiskid aggregates 16

5.4.1 pH value 16

5.4.2 Granulometry 17

5.4.3 Dangerous substances 17

5.4.4 Durability  Resistance to fragmentation (friability) 17

5.5 Non transparent antiskid aggregates 17

5.5.1 pH value 17

5.5.2 Visibility Characteristics 17

5.5.3 Granulometry 17

5.5.4 Durability  Resistance to fragmentation (friability) 17

5.6 Mixture of glass beads and antiskid aggregates 17

6 Evaluation of conformity 18

6.1 General 18

6.2 Initial type testing and type testing 18

6.2.1 General 18

6.2.2 Test samples, testing and compliance criteria 19

6.2.3 Test reports 21

6.3 Factory Production control (FPC) 21

6.3.1 General 21

6.3.2 Requirements 21

6.3.3 Product specific requirements 25

6.3.4 Initial inspection of factory and FPC 26

6.3.5 Continuous surveillance of FPC 26

6.3.6 Procedure for modifications 26

7 Marking 27

Annex A (normative) Test method to determine the refractive index of the glass beads 28

A.1 General 28

A.2 Principle 28

A.3 Equipment and materials 29

A.4 Procedure 30

A.5 Expression of the results 30

Annex B (normative) Test methods to determine the resistance of the glass beads to the effects of water, hydrochloric acid, calcium chloride and sodium sulphide 31

B.1 Resistance to the effects of water 31

B.2 Resistance to the effects of hydrochloric acid 31

B.3 Resistance to the effects of calcium chloride 31

B.4 Resistance to the effects of sodium Sulphide 31

Annex C (normative) Glass bead defects 33

C.1 Oval glass beads (see Figure C.1) 33

C.2 Satellites (see Figure C.2) 33

C.3 Tear shaped glass beads (see Figure C.3) 33

C.4 Glass beads fused together (see Figure C.4) 34

C.5 Roundish glass beads (see Figure C.5) 34

C.6 Opaque glass beads (see Figure C.6) 34

C.7 Milky glass beads (see Figure C.7) 35

C.8 Gas inclusions (see Figure C.8) 35

C.9 Grains (see Figure C.9) 35

C.10 Foreign particles 36

Annex D (normative) Test method to determine maximum weighted percentage of defective glass beads  Procedure 37

D.1 General 37

D.2 Results of counting 38

Annex E (normative) Test method to determine the presence of the moisture proof coating 40

E.1 Procedure A 40

E.2 Procedure B 41

Annex F (normative) Test method to determine the presence of floatation coating 42

F.1 General 42

F.2 Principle 42

F.3 Apparatus and reagents 42

F.4 Procedure 42

F.5 Results 42

Annex G (normative) Test method to determine the friability index of the antiskid aggregates 43

G.1 General 43

G.2 Apparatus 43

G.3 Material to be tested 43

G.4 Procedure 44

G.5 Expression of results 44

G.6 Precision 45

Annex H (informative) Alternative test methods to determine maximum weighted percentage of defective glass beads 46

H.1 General 46

H.2 Visual test method 46

H.3 Automatic test method 47

Annex I (normative) Test method to determine the presence of dangerous substances 53

I.1 Reference method 53

I.2 Quick alternative method 54

Annex J (normative) Test method to determine glass beads and antiskid aggregates ratio in mixtures of the two 55

J.1 General 55

J.2 Equipment and material 55

J.3 Procedure 55

J.4 Alternative methods 55

Annex ZA (informative) Clauses of this European Standard addressing the provisions of the EU Construction Products Directive 57

Bibliography 70

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights This document supersedes EN 1423:1997

This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essential requirements of EU Directive(s)

For relationship with EU Directive(s), see informative Annex ZA, which is an integral part of this document The main changes incorporated in this revision are:

a) Modification of the definitions to clarify better the different products glass beads antiskid aggregates and mixtures of the two;

b) Update of the standard to the new technologies that allow lower defects on glass beads with diameter equal or bigger than 1 mm;

c) Addition of the essential characteristic of dangerous substances for glass beads and transparent antiskid aggregates in glass;

d) Addition of test method to determine presence of dangerous substances;

e) Addition of test method to determine glass beads and antiskid aggregates ratio in mixtures of the two; f) Modification of the order of paragraphs to comply to the template for European Standards;

g) Addition of Clause 6 “Evaluation of conformity”;

h) Modification of parts of Annex ZA to comply to the template for product standard

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom

1 Scope

This European Standard specifies the requirements applicable to glass beads, anti-skid aggregates, and the mixture of the two, which are applied as drop-on materials on road markings products (i.e paints, cold plastics and thermoplastics)

Glass beads and/or anti-skid aggregates, or their mixture, applied during the process of manufacturing other road marking products are not covered by this European Standard

2 Normative references

The following referenced documents are indispensable for the application of this document For dated references, only the edition cited applies For undated references, the latest edition of the referenced document (including any amendments) applies

EN ISO 787-9, General methods of test for pigments and extenders — Part 9: Determination of pH value of

aqueous suspension (ISO 787-9)

ISO 565:1990, Test sieves — Metal wire cloth, perforated metal plate and electroformed sheet — Nominal

sizes of openings

ISO 2591-1, Test sieving — Part 1: Methods using test sieves of woven wire cloth and perforated metal plate ISO 7724-2, Paints and varnishes — Colorimetry — Part 2: Colour measurement

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply

3.1.2

antiskid aggregate

hard grain of natural or artificial origin, used to provide antiskid qualities for the road markings

NOTE This product is defined by the following characteristics:

− transparent antiskid aggregates: granulometry, resistance to fragmentation (friability); in addition, for transparent antiskid aggregates in glass, content of dangerous substances;

− non-transparent antiskid aggregate granulometry, resistance to fragmentation (friability) chromaticity co-ordinates and luminance factor

3.1.3

mixture of glass beads and antiskid aggregates

product which is a combination of here above product criteria and their relative ratio

3.2

intermediate bulk container

IBC

container with a capacity of up to 1 300 kg, used as an intermediate solution in between bags and tins (25 kg

to 50 kg) and bulk transport

4 Requirements

4.1 Glass beads

4.1.1 Surface treatments of glass beads

4.1.1.1 General

Special coatings may be applied to the surface of the glass beads to enhance their properties

4.1.1.2 Moisture proof coating

Moisture proof coating is added to avoid that the glass bead absorb air humidity When tested in accordance with 5.3.1.1, the presence of moisture proof coating shall be declared as Pass” or “Fail”

4.1.2 Visibility characteristics

4.1.2.1 Refractive index

The refractive index or index of refraction of a substance is a measure of the speed of light in that substance

It is expressed as a ratio of the speed of light in vacuum relative to that in the considered medium

The refractive index n of glass beads, shall be determined in accordance with 5.3.2.1 It shall comply with the

following classes:

• Class A n ≥ 1,5;

• Class B n ≥ 1,7;

• Class C n ≥ 1,9

4.1.2.2 Maximum weighted percentage of defective glass beads

In a collection of glass beads, maximum weighted percentage of defective glass beads is used to identify the

percentage of glass beads that are not perfectly spherical

The reference method for the determination of the maximum weighted percentage of defective glass beads is

described in 5.3.2.2 Glass beads defects are listed in Annex C

Once the reference method has been applied and only one defect per bead has been taken into

consideration, the maximum weighted percentage of defective beads shall be 20 % including a maximum of 3

% of grains and foreign particles (see Table 1) If a granulometry includes beads with diameters lower than 1

mm and diameters equal to or greater than 1 mm they shall be separated by means of a sieve with nominal

sizes of openings of 1 mm and checked separately

Table 1  Maximum weighted percentage of defective glass beads

Diameter of glass beads

mm

Maximum weighted percentage of defective glass

beads

%

Maximum weighted percentage of grains and foreign particles

%

During the separate checking of the glass beads with diameters lower than 1 mm and diameters equal to or

greater than 1 mm, the maximum weighted percentage of defective glass beads of each fraction shall be

recorded separately in the results of counting

4.1.3 Granulometry

Granulometry is the measure of the size gradation of a collection of glass beads

The granulometry of the glass beads shall be declared giving the minimum and the maximum percentages by

mass of the cumulative retained glass beads on metal wire cloth test sieves sizes R 40/3 according to

ISO 565:1990, using the test sieving procedure defined in ISO 2591-1

Granulometries of glass beads shall be described by selecting sieves in accordance with the following rules

(see also Table 2):

− the upper safety sieve shall retain 0 % to 2 % of the total mass of the antiskid aggregates;

− the upper nominal sieve shall retain 0 % to 10 % of the antiskid aggregates;

− if necessary, intermediate sieves shall be added to limit the ratio between the nominal sizes of

openings of two successive sieves to a maximum of 1,7 : 1;

− for each of the intermediate sieves, the range by mass between the minimum N1 % and the maximum

N2 % of the cumulative retained percentages shall be not more than 40 % (N2 - N1 ≤ 40);

− the lower nominal sieve shall retain 95 % to 100 % of the beads

Table 2  Selecting sieves for glass beads

The range of possible granulometries is defined in this clause and by Table 2 above

Many granulometries are acceptable dependent on customer requirements and manufacturer specifications The examples showed in Table 3 and Table 4 are given to demonstrate proper interpretation of the standard Granulometries of glass beads are not only restricted to the two examples of Table 3 and Table 4

Table 3  Example 1: 425-90 microns

lower nominal 95 to 100

4.1.4 Dangerous substances

Glass beads are manufactured mainly from recycled glass from industrial and domestic consumers

Historically, glass manufacturers used some dangerous substances (arsenic, antimony and lead) as a colouring and refining agent, but improved furnace technology has enabled glass manufacturers to eliminate these toxic additives in their production processes It is important to control the content of those dangerous substances because glass beads in their intended use are spread into the environment

In order to check the content of arsenic, lead and antimony, the glass beads shall be tested in accordance with 5.3.4

Each element (As, Pb, Sb) shall be separately classified into one of the following two classes:

− Class 0: no value requested;

4.2 Transparent antiskid aggregates

4.2.1 pH value

The pH value of the antiskid aggregates shall be determined in accordance with 5.4.1 The pH value shall be not less than 5 and not greater than 11 The result shall be declared as “Pass” or “Fail

4.2.2 Granulometry

Granulometry is the measure of the size gradation of a collection of grains

The granulometry of the transparent antiskid aggregates shall be described giving the minimum and the maximum percentages, by mass, of the cumulative retained particles on metal wire cloth test sieves ISO 565:1990 - sizes R 40/3 - using the test sieving procedure defined in ISO 2591-1

Granulometry of transparent antiskid aggregates shall be described by selecting sieves in accordance with the following rules (see also Table 5):

− the upper safety sieve shall retain 0 % to 2 % of the total mass of the antiskid aggregates;

− the upper nominal sieve shall retain 0 % to 10 % of the antiskid aggregates;

− if necessary, intermediate sieves shall be added to limit the ratio between the nominal sizes of openings

of two successive sieves to a maximum of 1,7 : 1;

− for each of the intermediate sieves, the range by mass between the minimum N1 % and the maximum

N2 % of the cumulative retained percentages shall be not more than 40 % (N2 - N1 ≤ 40);

− the lower nominal sieve shall retain 95 % to 100 % of the beads; antiskid aggregates;

− the lower safety sieve shall retain 99 % to 100 % of the aggregates; this sieve shall not be lower than

90 µ

Table 5  Selecting sieves for aggregates

Sieves ISO 565:1990 Cumulative retained

mass

Upper safety 0 to 2 Upper nominal 0 to 10 intermediate N1 to N2

Lower nominal 95 to 100 Lower safety 99 to 100

The range of possible granulometries is defined in this clause and by Table 5 above

Many granulometries are acceptable dependent on customer requirements and manufacturer specifications The examples showed in Table 6 and Table 7 are given to demonstrate proper interpretation of the standard Granulometries are not only restricted to the two examples of Table 6 and Table 7

Table 6  Example 3: 710-150 microns

Sieves ISO 565:1990 Cumulative retained

The granulometry of the antiskid aggregates shall be determined in accordance with 5.4.2

4.2.3 Dangerous substances

Transparent anti-skid aggregates in glass are manufactured mainly from recycled glass from industrial and domestic consumers Historically, glass manufacturers used some dangerous substances (arsenic, antimony and lead) as a colouring and refining agent, but improved furnace technology has enabled glass manufacturers to eliminate these toxic additives in their production processes; it is important to control the content of those dangerous substances because antiskid aggregates in their intended use are spread into the environment

For transparent anti-skid aggregates in glass, in order to check the content of arsenic, lead and antimony, the glass aggregates shall be tested in accordance with 5.4.3

Each element (As, Pb, Sb) shall be separately classified into one of the following two classes:

− Class 0: no value requested;

− Class 1: ≤ 200 ppm (mg/kg)

4.2.4 Durability aspects  Resistance to fragmentation (friability)

Resistance to fragmentation is indicated by the friability index

The friability index of transparent antiskid aggregates shall be determined in accordance with 5.4.4 and the maximum value of the friability index shall be declared

The compliance with the durability test is presumed to retain the performances stated for the requirements

4.3 Non transparent antiskid aggregates

The colour of non transparent antiskid aggregate shall be defined by chromaticity co-ordinates (x,y)

The chromaticity co-ordinates shall be determined in accordance with 5.5.2.1 and shall lie inside the region defined by the corner points given in Table 8

Table 8  Corner points of the chromaticity regions for non transparent antiskid aggregates

4.3.3 Granulometry

Granulometry is the measure of the size gradation of a collection of grains

The granulometry of non transparent antiskid aggregates shall be described giving the minimum and the maximum percentages, by mass, of the cumulative retained particles on metal wire cloth test sieves ISO 565:1990 - sizes R 40/3 - using the test sieving procedure defined in ISO 2591-1

Granulometry of non transparent antiskid aggregates shall be described by selecting sieves in accordance with the following rules (see also Table 9):

− the upper safety sieve shall retain 0 % to 2 % of the total mass of the antiskid aggregates;

− the upper nominal sieve shall retain 0 % to 10 % of the antiskid aggregates;

− if necessary, intermediate sieves shall be added to limit the ratio between the nominal sizes of openings

of two successive sieves to a maximum of 1,7 : 1;

− for each of the intermediate sieves, the range by mass between the minimum N1 % and the maximum

N2 % of the cumulative retained percentages shall be not more than 40 % (N2 - N1 ≤ 40);

− the lower nominal sieve shall retain 95 % to 100 % of the beads;

− the lower safety sieve shall retain 99 % to 100 % of the aggregates; this sieve shall not be lower than 90

µ

Table 9  Selecting sieves for aggregates

Sieves ISO 565:1990 Cumulative retained

mass

R 40/3 % Upper safety 0 to 2

Upper nominal 0 to 10 intermediate N1 to N2

Lower nominal 95 to 100 Lower safety 99 to 100

The range of possible granulometries is defined in this clause and by Table 9 above

Many granulometries are acceptable dependent on customer requirements and manufacturer specifications The examples showed in Table 10 and Table 11 are given to demonstrate proper interpretation of the standard Granulometries are not only restricted to the two examples of Table 10 and Table 11

Table 10  Example 3: 710-150 microns

Sieves ISO 565:1990 Cumulative retained

The granulometry of non transparent antiskid aggregates shall be determined in accordance with 5.5.3

4.3.4 Durability aspects  Resistance to fragmentation (friability)

Resistance to fragmentation is indicated by the friability index

The friability index of non transparent antiskid aggregates shall be determined in accordance with 5.5.4 and the maximum value of the friability index shall be declared

The compliance with the durability test is presumed to retain the performances stated for the requirements

4.4 Mixtures of glass beads and antiskid aggregates

4.4.1 General

The characteristics of a mixture of glass beads and anti-skid aggregates and their requirements, together with their test methods and the way of expression their results, shall be determined separately for glass beads and antiskid aggregated in the following way:

− for glass beads: according to entire 4.1;

− for transparent antiskid aggregates: according to entire 4.2;

− for non transparent antiskid aggregates according to entire 4.3

Table 10 — Example 5: 710-150 microns

Table 11 — Example 6: 1 000-150 microns

4.4.2 Durability aspects

In a mixture of glass beads and antiskid aggregates durability shall be conducted separately for glass beads transparent antiskid aggregates and non transparent antiskid aggregates:

− for glass beads durability shall conform to 4.1.5;

− for transparent antiskid aggregates durability shall conform to 4.2.4;

− for non transparent antiskid aggregates durability shall conform to 4.3.4

5 Testing, assessment and sampling methods

5.1 General

Test methods for glass beads, antiskid aggregates and mixtures of the two are listed in the following clauses NOTE Reference to the test method standards should be made to allow the selection of a suitable representative sample

5.2 Sampling

In order to test glass beads, antiskid aggregates and mixtures of them a representative sample of the material

to be tested shall be taken as follows

The drop on material sample shall be taken from at least three bags or one Intermediate Bulk Container (IBC) When M, in kilograms, is the mass of the drop on material to be tested, at least 1,5 kg of the material shall be taken by inserting an appropriate probe in the full height of a certain number 'S' of bags, or inserting the probe

S times in the whole height of an IBC The probe shall be driven to the bottom of the bag, in an upright position, or into the IBC containing the material to be tested

Another possibility to take a representative sample from the S bags is to use a 1/1 splitter

S is calculated by the formula:

150

M

S =

A representative sample shall be obtained by mixing the material taken with the S insertions of the probe in

the bags The representative sample shall be split by means of a 1/1 splitter in the number of samples necessary for the tests

NOTE A test probe can be constructed from a tube of 28 mm to 34 mm diameter and 1 000 mm to 1 200 mm in length The end of the probe which reaches the bottom of the bag or the IBC should be fitted with a plugging system After penetration of the probe to the full depth of the bag or the IBC, the plug is inserted and the probe removed The contents

of the probe represent a single sample of the material to be tested

When sampling into the IBC, if the test probe cannot go to the full depth of the container, the following alternative method shall be used:

• a quantity of 20 kg ± 1 kg shall be removed from the IBC in a bucket;

• the content of the bucket shall be split by means of a 1/1 splitter in the number of samples necessary for the tests

5.3 Glass beads

5.3.1 Surface treatments of glass beads

5.3.1.1 Moisture proof coating

When the manufacturer declares the presence of a moisture proof coating the glass beads shall be tested in accordance with Annex E When procedure A of Annex E is used 80 % of the glass beads shall pass the test showing the presence of the moisture proof coating When procedure B of Annex E is used the glass beads shall pass the test without any flow stoppage When procedure A fails procedure B shall be used

5.3.1.2 Floatation coating

The presence of a floatation coating on the surface treated glass beads shall be established by testing glass beads in accordance with Annex F When procedure of Annex F is not applicable, then an alternative test method shall be declared by the manufacturer

The refractive index n of glass beads, shall be determined in accordance with Annex A

5.3.2.2 Maximum weighted percentage of defective glass beads

The maximum weighted percentage of defective glass beads for glass beads shall be determined as described in Annex D; some alternative test methods are described in Annex H

When alternative test methods are used as in Annex H, the correlated values shall be applied Method described in Annex D (normative) shall always be considered as the reference test method

The resistance shall be determined in accordance with Annex B

5.4 Transparent antiskid aggregates

5.4.1 pH value

The pH value of the antiskid aggregates shall be determined in accordance with EN ISO 787-9

5.4.4 Durability  Resistance to fragmentation (friability) 

The resistance to fragmentation expressed as friability index of the antiskid aggregates shall be determined in accordance with Annex G

5.5 Non transparent antiskid aggregates

NOTE Modification of the sample preparation in accordance with ISO 7724-2 is proposed since the grains of the antiskid aggregates are not fine enough to form a tablet, when pressed without a binder

5.5.3 Granulometry

The reference method to determine the granulometry of the antiskid aggregates shall be ISO 2591-1

5.5.4 Durability  Resistance to fragmentation (friability) 

The friability index resistance to fragmentation of the antiskid aggregates shall be determined in accordance with Annex G

5.6 Mixture of glass beads and antiskid aggregates

The test methods to determine characteristics of a mixture of glass beads and anti-skid aggregates and the way of expressing their results shall be executed separately for glass beads and for the antiskid aggregates and shall be in accordance:

− for the part of glass beads: according to 5.3, and all subclauses;

− for the part of anti-skid aggregates: according to 5.4 and / or 5.5 and all their sub-clauses

The reference method to determine the relative ratio between glass beads and antiskid aggregates in a mixture is described in Annex J

6 Evaluation of conformity

6.1 General

The compliance of drop on materials with the requirements of this standard and with the stated values shall be demonstrated by:

− initial type testing and type testing;

− factory production control by the manufacturer, including product assessment

The manufacturer shall always retain the overall control and shall have the necessary means to take responsibility for the product

6.2 Initial type testing and type testing

Tests previously performed in accordance with the provisions of this standard may be taken into account provided that they were made to the same or a more rigorous test method, under the same system of attestation of conformity on the same product or products of similar design, construction and functionality, such that the results are applicable to the product in question

NOTE 1 Same system of attestation of conformity means testing by an independent third party under the responsibility

of a product certification body

For the purposes of testing, the drop on materials are grouped into families, where it is considered that the results for one or more characteristics from any one product within the family are representative for that same characteristics for all drop on materials within that same family

NOTE 2 Products may be in different families for different characteristics

The only characteristics where the grouping in families are allowed are:

− for glass beads: surface treatment; refractive index, resistance to water, hydrochloric acid, calcium chloride and sodium sulphide, dangerous substances;

−

− for non transparent antiskid aggregates: pH value, chromaticity co-ordinates and luminance factor friability index

Type Tests or Initial Type Testing shall be performed for all characteristics included in the standard for which the manufacturer declares performances:

− at the beginning of the production of a new or modified glass beads, antiskid aggregates and admixture of the two (unless a member of the same family); or

− at the beginning of a new or modified method of production (where this may affect the stated properties); or

− they shall be repeated for the appropriate characteristic(s), whenever a change occurs in glass beads, antiskid aggregates and mixtures of the two design, in the raw material or in the supplier of the components, or in the production process (subject to the definition of a family), which would affect significantly one or more of the characteristics

Where components are used whose characteristics have already been determined, by the component manufacturer, on the basis of compliance with other product standards, these characteristics need not be re-assessed The specifications of these components shall be documented, as shall be included in the inspection scheme for ensuring their compliance

Products marked in accordance with appropriate harmonized European specifications may be presumed to have the performances stated with that marking, although this does not replace the responsibility on the glass beads, antiskid aggregates and mixtures of the two designer to ensure that the beads, antiskid aggregates and mixtures of the two as a whole is correctly designed and its component products have the necessary performance values to meet the design

6.2.2 Test samples, testing and compliance criteria

The number of samples of glass beads, antiskid aggregates and mixtures of the two to be tested/assessed for Initial type testing shall be in accordance with Table 12:

Table 12  Number of characteristics, number of samples and compliance criteria

Type of

drop-on

Assessment method

Number of samples /tests

by product or family

Compliance criteria

Refractive index 4.1.2.1 5.3.2.1 2/family a 4.1.2.1 Maximum weighted

percentage of defective glass

beads 4.1.2.2 5.3.2.2 1/product granulometry 4.1.2.2

Granulometry 4.1.3 5.3.3 1/product granulometry 4.1.3

Dangerous substances 4.1.4 5.3.4 2/family a 4.1.4 Resistance against chemicals:

water, hydrochloric acid,

calcium chloride and sodium

Granulometry 4.2.2 5.4.2 1/product granulometry 4.2.2

Dangerous substances (for

Resistance to fragmentation

a As long as there is only one product in the family only one sample has to be tested for ITT From 2 products

on a second product has to be sampled to carry out an ITT of this characteristic to show the results for this characteristic are representative for all drop on material within this same family

6.2.3 Test reports

All Type Tests, Initial Type Tests and their results shall be documented in test reports

All test reports shall be retained by the manufacturer for at least 10 years after the last date of production of the glass beads, transparent antiskid aggregates non transparent antiskid aggregates or mixtures, to which they relate

6.3 Factory Production control (FPC)

6.3.1 General

The manufacturer shall establish, document and maintain an FPC system to ensure that the products placed

on the market comply with the declared performance of the characteristics

The FPC system shall consist of written procedures, regular inspections and tests and/or assessments and the use of the results to control raw and other incoming materials or components, equipment, the production process and the product

All the elements, requirements and provisions adopted by the manufacturer shall be documented in a systematic manner in the form of written policies and procedures

This production control system documentation shall ensure a common understanding of conformity evaluation and enable the achievement of the required product characteristics and the effective operation of the production control system to be checked

Factory production control therefore brings together operational techniques and all measures allowing maintenance and control of the compliance of the product with this technical specification

6.3.2 Requirements

6.3.2.1 General

The manufacturer is responsible for organizing the effective implementation of the FPC system

Tasks and responsibilities in the production control organization shall be documented and this documentation shall be kept up-to-date

The responsibility, authority and the relationship between personnel that manages, performs or verifies work affecting product conformity, shall be defined This applies in particular to personnel that needs to initiate actions preventing product non-conformities from occurring, actions in case of non-conformities and to identify and register product conformity problems Personnel performing work affecting product conformity shall be competent on the basis of appropriate education, training, skills and experience for which records shall be maintained

In each factory the manufacturer may delegate the action to a person having the necessary authority to:

− identify procedures to demonstrate conformity of the product at appropriate stages;

− identify and record any instance of non-conformity;

− identify procedures to correct instances of non conformity

The manufacturer shall draw up and keep up-to-date documents defining the factory production control The manufacturer's documentation and procedures should be appropriate to the product and manufacturing process

The FPC system should achieve an appropriate level of confidence in the conformity of the product This involves:

a) the preparation of documented procedures and instructions relating to factory production control operations, in accordance with the requirements of the technical specification to which reference is made;

b) the effective implementation of these procedures and instructions;

c) the recording of these operations and their results;

d) the use of these results to correct any deviations, repair the effects of such deviations, treat any resulting instances of non-conformity and, if necessary, revise the FPC to rectify the cause of non-conformity

Where subcontracting takes place, the manufacturer shall retain the overall control of the product and ensure that he receives all the information that is necessary to fulfill his responsibilities according to this European Standard

If the manufacturer has part of the product designed, manufactured, assembled, packed, processed and/or labeled by subcontracting, the FPC of the subcontractor may be taken into account, where appropriate for the product in question

The manufacturer who subcontracts all of his activities may in no circumstances pass these responsibilities on

to a subcontractor

Manufacturers having an FPC system, which complies with EN ISO 9001:2008 and which addresses the requirements of this European Standard are recognized as satisfying the FPC requirements of the Council Directive 89/106/EEC

6.3.2.2.3 Raw materials and components

The specifications of all incoming raw materials and components shall be documented, as shall the inspection scheme for ensuring their compliance

In case supplied glass beads are used, the attestation of conformity level of these glass beads shall be that given in this harmonised standard In case supplied antiskid aggregates are used for the production of mixtures, the attestation of conformity level of the antiskid aggregate shall be that given in this standard or the manufacturer of the mixture shall test the antiskid aggregates according to Table 13 and Table 14

Table 13  Transparent anti-skid aggregates FPC

Property Clause Minimum frequency of tests

fragmentation (friability) 4.2.4 every delivery

Table 14  Non transparent anti-skid aggregates

Property Clause Minimum frequency of tests

pH value 4.3.1 1 test/year/supplier

Chromaticity

co-ordinates (x,y) 4.3.2.1 every delivery

Luminance factor 4.3.2.2 every delivery

Granulometry 4.3.3 every delivery and at least every 10 t

6.3.2.2.5 Traceability and marking

Individual batches of glass beads antiskid materials and mixtures of the two shall be identifiable and traceable with regards to their production origin The manufacturer shall have written procedures ensuring that processes related to affixing traceability codes and/or markings are inspected regularly

6.3.2.2.6 Controls during manufacturing process

The manufacturer shall plan and carry out production under controlled conditions

6.3.2.2.7 Product testing and evaluation

The manufacturer shall establish procedures to ensure that the stated values of the characteristics he declares are maintained

The characteristics, and the means of control, are described in Table 15, Table 16 and Table 17

Table 15  Glass beads FPC final testing minimum frequency

Characteristic Clause Minimum frequency of tests

Surface treatment 5.3.1 Every batch and at least every 5 t

Refractive index 5.3.2.1 1 test / year

Maximum weighted

percentage of defective

glass beads

5.3.2.2 Every batch and at least every 5 t

Granulometry 5.3.3 Every batch and at least every 5 t

Dangerous substances

(Pb, As, Sb) 5.3.4 Every 1 000 t and at least once a month

Resistance to chemicals:

water, hydrochloric acid,

calcium chloride and

sodium sulphide

5.3.5 1 test/year

Table 16  Transparent Anti-skid aggregates FPC final testing minimum frequency

Property Clause Minimum frequency of tests

fragmentation (friability) 5.4.4 1 test/year

Table 17  Non transparent anti-skid aggregates FPC final testing minimum frequency

Property Clause Minimum frequency of tests

Chromaticity co-ordinates

(x,y) 5.5.2.1 1 Test/month or every 100 t

Luminance factor 5.5.2.2 1 Test/month or every 100 t

Granulometry 5.5.3 every 10 t

Resistance to

fragmentation (friability) 5.5.4 1 test/year

6.3.2.2.8 Non complying products

The manufacturer shall have written procedures which specify how non-complying products shall be dealt with Any such events shall be recorded as they occur and these records shall be kept for the period defined

in the manufacturer’s written procedures

6.3.2.2.9 Corrective action

The manufacturer shall have documented procedures that instigate action to eliminate the cause of conformities in order to prevent recurrence

non-6.3.2.2.10 Handling, storage and packaging

The manufacturer shall have procedures providing methods of product handling and shall provide suitable storage areas preventing damage or deterioration

6.3.3 Product specific requirements

The FPC system shall:

− address this European Standard; and

− ensure that the products placed on the market comply with the stated performance characteristics The FPC system shall include a product specific FPC, which identifies procedures to demonstrate compliance

of the product at appropriate stages, i.e.:

a) the controls and tests to be carried out prior to and/or during manufacture according to a frequency laid down in the FPC test plan; and/or

b) the verifications and tests to be carried out on finished products according to a frequency laid down in the FPC test plan

If the manufacturer uses only finished products, the operations under b) shall lead to an equivalent level of compliance of the product as if FPC had been carried out during the production

If the manufacturer carries out parts of the production himself, the operations under b) may be reduced and partly replaced by operations under a) Generally, the more parts of the production that are carried out by the manufacturer, the more operations under b) may be replaced by operations under a)

In any case the operation shall lead to an equivalent level of compliance of the product as if FPC had been carried out during the production

NOTE Depending on the specific case, it can be necessary to carry out the operations referred to under a) and b), only the operations under a) or only those under b)

The operations under a) refer to the intermediate states of the product as on manufacturing machines and their adjustment, and measuring equipment etc These controls and tests and their frequency shall be chosen based on product type and composition, the manufacturing process and its complexity, the sensitivity of product features to variations in manufacturing parameters, etc

The manufacturer shall establish and maintain records that provide evidence that the production has been sampled and tested These records shall show clearly whether the production has satisfied the defined acceptance criteria and shall be available for at least three years

These records shall be available for inspection

Where the product fails to satisfy the acceptance measures, the provisions for non-conforming products shall apply, the necessary corrective action shall immediately be taken and the products or batches not conforming shall be isolated and properly identified

Once the fault has been corrected, the test or verification in question shall be repeated

The results of controls and tests shall be properly recorded The product description, date of manufacture, test method adopted, test results and acceptance criteria shall be entered in the records under the signature of the person responsible for the control/test

With regard to any control result not meeting the requirements of this European Standard, the corrective measures taken to rectify the situation (e.g a further test carried out, modification of manufacturing process, throwing away or putting right of product) shall be indicated in the records

Individual products or batches of products and the related manufacturing documentation shall be completely identifiable and retraceable

6.3.4 Initial inspection of factory and FPC

Initial inspection of FPC shall be carried out when the production process has been finalized and in operation The factory and FPC documentation shall be assessed to verify that the requirements of 6.3.2 and 6.3.3 are fulfilled During the inspection it shall be verified:

a) that all resources necessary for the achievement of the product characteristics required by this European Standard are in place and correctly implemented, and

b) that the FPC-procedures in accordance with the FPC documentation are followed in practice, and c) that the product complies with the Initial Type Testing / Type Testing samples for which compliance with this European Standard has been verified

All locations where final assembly or at least final testing of the relevant product is performed, shall be assessed to verify that the above conditions a) to c) are in place and implemented

If the FPC system covers more than one product, production line or production process, and it is verified that the general requirements are fulfilled when assessing one product, production line or production process, then the assessment of the general requirements does not need to be repeated when assessing the FPC for another product, production line or production process

All assessments and their results shall be documented in the initial inspection report

6.3.5 Continuous surveillance of FPC

The surveillance of the FPC shall include a review of the FPC test plan(s) and production processes(s) for each product to determine if any changes have been made since the last assessment or surveillance The significance of any changes shall be assessed

Checks shall be made to ensure that the test plans are still correctly implemented and that the production equipment is still correctly maintained and calibrated

The records of tests and measurement made during the production process and to finished products shall be reviewed to ensure that the values obtained still correspond with those values for the samples submitted to Type Testing/Type Testing and that the correct actions have been taken for non-compliant devices

6.3.6 Procedure for modifications

If modifications are made to the product, production process or FPC system that could affect any of the product characteristics required by this standard, then all the essential characteristics for which the manufacturer declares performance, which may be affected by the modification, shall be subject to Initial Type Testing/Type Testing, except as described in 6.2.1

Where relevant, a re-assessment of the factory and of the FPC system shall be performed for those aspects, which may be affected by the modification

All assessments and their results shall be documented in a report

7 Marking

The manufacturer shall provide the following information to accompany the product

Technical data sheet of the product mentioning the granulometry with all the sieves and specifications as defined in 4.1.3, 4.2.2 and 4.3.3

Each packaging of the product shall contain the following identification:

− the last two digits of the year in which the product was manufactured;

− the presence of a surface treatment;

− the batch number;

− product identification: Name (e.g commercial name or other unique identification of a granulometry);

− content of the packaging

Where the above information is also required as part of regulatory marking, compliance with the requirement for regulatory marking shall be deemed to satisfy the requirements of this clause without the need for repetition

A.2 Principle

Viewed under the microscope, transparent solids which are immersed in a liquid give an image bounded by dark or luminous bands The appearance will vary, depending upon the difference between the refractive indices of the two bodies, according to their dispersing capacity and illumination

Under axial lighting conditions index differences are perceptible; but they become considerably more pronounced under oblique lighting, due to the fact that under such conditions the bands become sharper on one side than on the other Their position is determined by the direction of the incident beam and by the difference between the index of the solid under examination and that of the liquid in which it is immersed

+ refractive index for the body higher than that for the liquid Shadow on screen side

= refractive index for the body equal to that for the liquid No shadow, coloured edging

- refractive index for the body lower than that for the liquid Shadow on the opposite side to the screen

Key

1 cardboard or screen

2 dark part of the field

Figure A.1  Schematic diagram showing the technique for determining the refractive index

NOTE The position of the shaded part of the field may be reversed, depending upon the microscope setting Only the position of the screen should therefore be taken into account

Where devices are fitted with an image rectifier (magnifiers and certain microscopes), the phenomenon is reversed If there is any doubt as to the properties of the device which is being used, a test should be carried out with water, since glass beads always have a higher refractive index This will reveal how the phenomenon appears

When preparing in advance a series of liquids with known indices and immersing the test objects in them one after the other, it shall be determined either that there is a liquid with the same index or that the index for the test object falls between the indices for two liquids, one higher and one lower

A.3 Equipment and materials

A.3.1 General

In order to perform the test, the following equipment and materials are required:

 a microscope;

 liquids with a known refractive index;

 a concave microscope slide;

 a piece of black board, measuring approximately 10 cm x 15 cm

A.3.3 Liquids with known refractive index

In order to obtain liquid scales graduate indices, either pure bodies with a constant known refractive index or, alternatively, mixtures may be used

Examples of liquids used for glass beads having the following refractive indices at 20 °C:

 place the concave slide in the specimen holder of the microscope;

 turn the condenser to the maximum setting;

 open the iris to the full aperture;

 light the specimen from below;

 slip the board with the straight edges in below the condenser, so as to obscure half of the field visible through the eye piece, which will give angled illumination of the remaining visible part of the field;

 observe the glass beads in the illuminated area of the field in view through the eye piece;

 compare observations with the diagram in Figure A.1;

 depending upon the conclusions reached, repeat the above procedure and continue to repeat this procedure, using liquids with different refractive indices, until a liquid is found with a refractive index identical to that of the glass beads; or until two liquids are found with close refractive indices, as listed in A.3.3, which sandwich the index for the glass beads

A.5 Expression of the results

The index found or the indices for the two liquids on either side of the index for the test subjects, shall be given, specifying also the temperature at which the test was carried out and quoting references for the glass beads which have been examined

B.1 Resistance to the effects of water

In a distillation flask fitted with a glass tube at the top, this tube to serve as a reflux condenser, boil

10 g ± 0,1 g of glass beads for 60 min ± 10 s in 100 g ± 1 g of CO2 free water After the test objects have been boiled for the required period, filter the glass beads, cool the liquid to room temperature and then add two drops of phenolphthalein solution as an indicator

Using a solution of hydrochloric acid, titrate the liquid until the phenolphthalein changes colour A blank test shall be carried out in parallel

Note any changes which appear in the surface using the microscope at an enlargement of between 20× and 50×; note also the quantity of HCl used

B.2 Resistance to the effects of hydrochloric acid

Immerse 10 g ± 0,1 g of glass beads in 100 ml ± 0,1 ml of dilute hydrochloric acid solution, buffered to give a

pH of 5,0 to 5,3, for 90 h at a temperature of 20 °C ± 3 °C

With the help of a microscope with 20× to 50× magnification, note any changes which may have appeared on the surface after the glass beads have been rinsed in distilled water and dried

B.3 Resistance to the effects of calcium chloride

Immerse 10 g ± 0,1 g of glass beads in 100 ml ± 0,1 ml of a normal solution of calcium chloride for 3 h at a temperature of 20 °C ± 3 °C

With the help of a microscope with 20× to 50× magnification note any changes which may have appeared on the surface after the glass beads have been rinsed in distilled water and dried

B.4 Resistance to the effects of sodium Sulphide

B.4.1 Apparatus and reagents

B.4.1.1 Microscope, with minimum magnification of 10

B.4.1.2 50 ml bottle with a glass stopper

B.4.1.3 Distilled water

B.4.1.4 A saturated solution of sodium sulphide in distilled water at 20 °C with the addition of 2,0 %

anionic wetting agent

B.4.2 Procedure

Take 10 g ± 0,1 g of glass beads from a representative sample

Place the glass beads in a stoppered bottle and cover with the solution containing the sodium sulphide and allow to stand for 1 h Pour off the solution containing the sodium sulphide and rinse three times with distilled water

Dry the glass beads in an oven at 100 °C ± 5 °C and, using the microscope, compare these with an untreated sample

B.4.3 Results

When compared with an untreated sample the glass beads shall not be darker

Annex C

(normative)

Glass bead defects

C.1 Oval glass beads (see Figure C.1)

When the ratio of the major diameter D to the minor diameter d is greater than 1,3 (D/d >1,3), the oval glass

bead shall be considered defective

Figure C.1  Oval glass bead

C.2 Satellites (see Figure C.2)

When a glass bead supports more than two smaller glass beads, called satellites, or when, in the case of two

satellites, the ratio of the diameter d of the major of them to the diameter D of the supporting glass bead is greater than 0,25 (d /D > 0,25 ), the glass bead shall be considered defective

Figure C.2  Satellite

C.3 Tear shaped glass beads (see Figure C.3)

When the ratio of the major dimension L to the minor dimension l is greater than 1,3 (L /l>1,3), the glass bead

shall be considered defective

Figure C.3  Tear shaped glass bead

C.4 Glass beads fused together (see Figure C.4)

When the ratio of the major dimension D2 to the minor dimension D1 is greater than 1,3

(D2/D1> 1,3), the particle shall be considered a defective glass bead

Figure C.4  Two glass beads fused together

C.5 Roundish glass beads (see Figure C.5)

When the ratio of their major dimension L to the minor dimension l is greater than 1,3 (L /l > 1,3), the glass

bead shall be considered defective

Figure C.5  Roundish glass bead

C.6 Opaque glass beads (see Figure C.6)

Opaque glass beads shall always be considered defective

Figure C.6  Opaque glass bead

C.7 Milky glass beads (see Figure C.7)

The milky appearance is due to gaseous inclusions in part or in the whole volume of the bead Milky glass beads shall always be considered defective

Figure C.7  Milky glass bead

C.8 Gas inclusions (see Figure C.8)

When the ratio of the sum of the projected area of the bubbles inside a glass beads Σsi to the projected area

of the glass bead S is greater than 0,25 (Σsi /S > 0,25), the glass bead shall be considered defective

Figure C.8  Gas inclusions

C.9 Grains (see Figure C.9)

Glass particles which present one or more sharp angles shall be considered defective glass beads