ISO 15360-2:2015
(Main)Recycled pulps — Estimation of Stickies and Plastics — Part 2: Image analysis method
Recycled pulps — Estimation of Stickies and Plastics — Part 2: Image analysis method
ISO 15360-2:2015 specifies a method to estimate Stickies and Plastics in all grades of recycled pulp. It applies the principles for the separation of Stickies and Plastics described in ISO 15360‑1. The visualization and counting techniques described in ISO 15360‑1 are replaced here by image analysis. ISO 15360-2:2015 permits the use of different laboratory screening devices as well as screens of different sizes when applying the specified method. It is impracticable to define more closely the equipment or screen sizes to be used, because of the wide range of Stickies and Plastics found in recycled pulps, and the various screening devices which are being successfully used for their measurement. NOTE This method will only estimate those Stickies and Plastics which are tacky and which are retained on the screen of a given slit size under the temperature and pressure conditions of this test method. It is important to note that this will probably not be the total amount of Stickies and Plastics that are actually present in a given pulp sample.
Pâtes recyclées — Estimation des matières collantes et des matières plastiques — Partie 2: Méthode par analyse d'image
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Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 15360-2
Second edition
2015-11-01
Recycled pulps — Estimation of
Stickies and Plastics —
Part 2:
Image analysis method
Pâtes recyclées — Estimation des matières collantes et des
matières plastiques —
Partie 2: Méthode par analyse d’image
Reference number
ISO 15360-2:2015(E)
©
ISO 2015
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ISO 15360-2:2015(E)
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ISO 15360-2:2015(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Apparatus and equipment . 2
6 Reagents . 4
6.1 For marking the Stickies by metallic powder adhering to the Stickies . 4
6.2 For marking the Stickies by coating particles pulled out from a coated paper . 4
7 Sampling . 4
8 Adjustment and calibration of the image analysis system . 4
9 Pretreatment of the sample . 4
10 Procedure. 5
10.1 Processing the sample through the screening device . 5
10.2 Distribution of the separated Stickies or Plastics on the filter paper . 5
10.3 Determination of Stickies by marking with metallic powder . 6
10.3.1 Heat setting. 6
10.3.2 Dyeing. 6
10.3.3 Recording of Stickies . 6
10.4 Determination of Stickies by marking with white coating particles . 6
10.4.1 Heat setting. 6
10.4.2 Filter paper washing . 7
10.4.3 Drying . 7
10.4.4 Recording of Stickies . 7
10.5 Determination of Plastics . 7
10.6 Calculation of Stickies and Plastics . 7
11 Calculations. 8
11.1 Number of Stickies and Plastics . 8
11.2 Area of Stickies and Plastics . 8
12 Test report . 8
Annex A (normative) Laboratory screening equipment .10
Annex B (normative) Comparison chart .11
Annex C (informative) Precision .12
Bibliography .14
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ISO 15360-2:2015(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 6, Paper, board and pulps.
This second edition cancels and replaces the first edition (ISO 15360-2:2001), of which it constitutes
a minor revision by moving the precision statement to an informative annex. It also incorporates the
technical corrigendum ISO 15360-2:2001/Cor 1:2007.
ISO 15360 consists of the following parts, under the general title Recycled pulps — Estimation of Stickies
and Plastics:
— Part 1: Visual method
— Part 2: Image analysis method
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ISO 15360-2:2015(E)
Introduction
This part of ISO 15360 is complementary to ISO 15360-1, which concerns estimation of Stickies and
Plastics in recycled pulp by visual examination. ISO 15360-2 is particularly useful for pulps having a
high content of Stickies or Plastics or both where visual inspection is very time-consuming to carry out.
Two alternatives are given for the estimation of Stickies, while there is only one procedure for the
estimation of Plastics.
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INTERNATIONAL STANDARD ISO 15360-2:2015(E)
Recycled pulps — Estimation of Stickies and Plastics —
Part 2:
Image analysis method
1 Scope
This part of ISO 15360 specifies a method to estimate Stickies and Plastics in all grades of recycled
pulp. It applies the principles for the separation of Stickies and Plastics described in ISO 15360-1. The
visualization and counting techniques described in ISO 15360-1 are replaced here by image analysis.
This part of ISO 15360 permits the use of different laboratory screening devices as well as screens
of different sizes when applying the specified method. It is impracticable to define more closely the
equipment or screen sizes to be used, because of the wide range of Stickies and Plastics found in recycled
pulps, and the various screening devices which are being successfully used for their measurement.
NOTE This method will only estimate those Stickies and Plastics which are tacky and which are retained on
the screen of a given slit size under the temperature and pressure conditions of this test method. It is important
to note that this will probably not be the total amount of Stickies and Plastics that are actually present in a
given pulp sample.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 638, Paper, board and pulps — Determination of dry matter content — Oven-drying method
ISO 4119, Pulps — Determination of stock concentration
ISO 5263 (all parts), Pulps — Laboratory wet disintegration
ISO 5269-2, Pulps — Preparation of laboratory sheets for physical testing — Part 2: Rapid-Köthen method
ISO 7213, Pulps — Sampling for testing
ISO 8486-1, Bonded abrasives — Determination and designation of grain size distribution — Part 1:
Macrogrits F4 to F220
DIN 54516, Testing of paper and board — Determination of plybond resistance
TAPPI T 541 om-89, Internal bond strength of paperboard (z-direction tensile)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
Stickies
diverse group of materials that are retained on a laboratory screen of given slit aperture (100 μm or
150 μm) and which adhere to objects that they touch
Note 1 to entry: Stickies can adhere to objects at ambient conditions or they can adopt adhesive characteristics
when subjected to elevated temperature, elevated pressure or change pH.
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ISO 15360-2:2015(E)
Note 2 to entry: The following is a non-exhaustive list of Stickies: products derived from residues of materials
such as inks, tars, hot melts, waxes, and multivalent metal ion soaps or different types of pressure-sensitive
adhesives (tapes).
Note 3 to entry: A Stickie particle can be a composite of adhesive material together with non-adhesive plastic
fragments and cellulosic fibres.
3.2
Plastics
non-adhesive polymers that are retained on a laboratory screen of a given slit aperture (100 μm or
150 μm), but excluding cellulosic materials
Note 1 to entry: The following is a non-exhaustive list of Plastics: polymeric materials derived from such sources
as polyethylene, polypropylene, polyester, UV-cured coatings and polystyrene.
4 Principle
A sample of pulp in disintegrated form is washed through a laboratory screen of a given slit aperture
until the filtrate is clear. The material is removed and transferred to a filter paper. The Stickies are
marked either with white aluminium oxide powder or by particles of coating that they pull out from
a special coated paper. The Plastics are highlighted by dyeing the filter paper black and hiding the
Stickies with black silicon carbide powder. The Stickies and Plastics are measured using an image
analyser. The total numbers of Stickies and Plastics are determined and reported. Other report formats
are possible, including the numbers of Stickies and Plastics of various areas, or a histogram showing the
area distribution.
5 Apparatus and equipment
5.1 Disintegrator as specified in ISO 5263 (all parts).
5.2 Laboratory screening equipment, fitted with a screen complying with the specification as
described in Annex A.
NOTE For the purpose of this method, a screen is that part of the laboratory screening equipment which
separates the Stickies and Plastics from the cellulose fibre. Various laboratory screening equipment can use
different terminology to describe the separating medium (e.g. “slots” instead of “slits”).
5.3 Image analyser system for illuminating, viewing, and detecting images. The image analyser
system used shall be capable of scanning or viewing the total area of the filter paper upon which the
Stickies or Plastics are collected (20 cm diameter or larger). The image analyser system incorporates the
following components.
5.3.1 Specimen stage, generally consisting of a flat plate on one side of which the specimen illuminant
and detector are located. The specimen stage shall be shielded to prevent influence from ambient light.
The prepared specimen is a piece of filter paper upon one side of which the Stickies and Plastics have been
collected. The side of the prepared specimen upon which the Stickies and Plastics have been collected
faces the illuminant and image detector. The exact configuration of the specimen stage will depend upon
the image detector used.
5.3.2 Image detector, either a scanner or camera-based image detector, with at least 256 grey levels
of sensitivity and a physical pixel resolution below 50 μm/pixel such that four contiguous pixels will have
2
a combined area of 0,01 mm or less. The image detector shall view the specimen normal to its surface.
5.3.3 Illuminant, un-polarized with wavelength concentrated in the visible portion of the spectrum,
such that 95 % of the light reflected from a white surface will be between 380 nm and 750 nm. The most
preferred illuminant provides illumination that is diffuse or axially symmetric with an incident angle
of 45° ± 5°. As a minimum, the illuminant shall consist of two members providing illumination at an
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ISO 15360-2:2015(E)
incident angle of 45° ± 5°. The illumination from the two members shall oppose each other at an angle of
180°. A preferred illuminant consists of four members each providing incident illumination at 45° ± 5°,
placed such that the four members oppose one another at angles of 90°. The uniformity of illumination
over the area of the specimen stage before any software corrections shall be within ±4 %.
5.3.4 Image analysis software, capable of determining the average intensity (“grey level”) of a
detected image, for example, a Stickie or piece of Plastic, as well as the average background intensity
surrounding the speck when examining the picture elements of a digitized Stickies or Plastics speck
[1][2][3][4] 2
using a “centre-surround” filtering technique. The normal size of the software filter is a 1,0 mm
area centred on the Stickie or Plastic. The software shall be capable of adjusting this area as required to
completely surround the detected image of a Stickie or Plastic. The detection threshold is 10 % of the
100 % contrast scale on the comparison chart (Annex B). The detection threshold is applied between the
contrary and the average background intensity as defined by the centre surround filter.
5.4 Calibration chart as shown in Annex B. The chart is a film with a series of black and grey spots
of different shapes, areas and contrasts. The chart is used for checking the performance of the image
analyser system. For the purpose of this part of ISO 15360 only the spots of 100 % contrast are used.
NOTE The calibration method uses dark spots on a white background but this test detects light contraries
on the dark background. The effect of this difference is yet unknown.
5.5 Büchner funnel with a sintered glass filtering base of 20 cm diameter or larger. The funnel may be
substituted by a Rapid-Köthen sheet former (ISO 5269-2).
5.6 White or black filter paper, comprised of 100 % cellulose fibres, qualitative, medium fast grade,
to fit the funnel or sheet former (5.5).
5.6.1 White filter paper for marking the Stickies by metallic powder.
5.6.2 Black filter paper for marking the Stickies by coating particles pulled out from a coated paper.
5.7 Release paper, silicone coated.
5.8 Oven capable of maintaining a temperature of 105° ± 2°.
5.9 Heated press capable of applying a pressure of 95 kPa ± 5 kPa at 94 °C ± 4 °C for 10 min. A Rapid-
Köthen sheet dryer operated at these conditions is suitable (ISO 5269-2).
5.10 Shallow glass dish, approximately 25 cm × 20 cm. The exact size of the glass dish is unimportant,
provided the smaller dimension is greater than the diameter of the filter paper.
5.11 Metal plates, the top plate of which is circular with a diameter of 28 cm ± 1 cm and a mass of
6,0 kg ± 0,1 kg (5.6.1), and the bottom plate of which is the same size as the top plate or larger. The
bottom plate may be of any convenient shape, for example circular with a minimum diameter of 28 cm,
square with a minimum length of 28 cm, or other shape as desired.
5.12 Filter washing device (see 10.4.2) to wash the filter with a gentle stream of water at a pressure of
about 0,1 MPa (1 bar), flow rate of about 10 l/min and distance of delivery tip from filter of about 180 mm.
5.13 Water resistant black felt pen.
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ISO 15360-2:2015(E)
6 Reagents
6.1 For marking the Stickies by metallic powder adhering to the Stickies
6.1.1 White powdered aluminium oxide, purified Al O with a grain size distribution of F220
2 3
according to ISO 8486-1.
6.1.2 Aqueous solution of a black dye which is substantive to cellulose. Commercial black inks have
been found suitable.
6.1.3 Black powdered silicon carbide, SiC, with a grain size distribution of F220 according to
ISO 8486-1.
6.2 For marking the Stickies by coating particles pulled out from a coated paper
2
6.2.1 Coated paper as specified in the following: wood-free sized base paper, grammage about 70 g/m
to which is added a coating consisting of calcium carbonate and a synthetic binding material on one side
2 2
of 50 g/m to 55 g/m , brightness (ISO) 85 % ± 3 %, plybond resistance of coating 2,0 kN/m ± 0,5 kN/m
tested according to DIN 54516 or 5,5 kPa ± 1,5 kPa tested according to TAPPI T 541 for a total sheet
2 2
grammage of 120 g/m to 125 g/m , size large enough to completely cover the black filter paper carrying
the Stickies. When placed in contact with Stickies under the temperature and pressure specified in 5.9,
the coating adheres to the Stickie particle, causing it to appear white in colour. To verify coating plybond
resistance under the conditions of this test, the coated sheet may be processed according
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