Polybutene-1

Pipe Extrusion Guide

-1-

Disclaimer Unless otherwise agreed in writing, Basell disclaims any warranties with respect to the application of the information herein, its products or the safety or suitability thereof, or results obtained, whether express or implied, including, without limitation, any implied warranty of merchantability or fitness for a particular purpose and/or any other warranty. Buyers and users must determine the results to be obtained from the application of the information and the safety and suitability of the products for their own purposes. Buyers and users assume all risk, responsibility and liability whatsoever for any and all injuries (including death), losses or damages to persons or property arising from the application of the information or use of products, whether or not occasioned by sellers negligence or based on strict product liability or principles of indemnity or contribution. Basell neither assumes nor authorises any person to assume for it any liability in connection with the use of the information or products. Under no circumstances shall Basell be liable for special, consequential or incidental damages. The information provided in this document is provided as a service to polybutene-1 pipe customers and is based on general considerations, best estimates, practical experience and know-how collected over several years including other sources than Basell. It is intended for use only as general information for the production of unaltered PB 4237, PB 4235 and PB 4201 type materials. Although specific values may be given here they should be taken as guidelines only and may not be applicable for all systems, equipment and material grades to the same extent. The information provided is intended only for use as a starting point for the processing of Polybutene-1 pipes since modifications may be required in order to optimise for each particular customer, line or application. The information contained in this document may not be applicable for any type of pipe or system that utilises other material including all co-extrusion processes.

-2-

Table of contents 1. Description of PB-1 2. Properties of PB-1 pipe materials 2.1 2.2 2.3 2.4 2.5 2.6 Rheology Mechanical properties Impact resistance Compression set Abrasion and wear resistance Creep behaviour 2.6.1 2.6.2 2.6.3 2.7 2.7.1 2.7.2 2.7.3 3.1 3.2 General Creep performance at uniaxial load Practical consequences of creep Quick burst Creep rupture strength Flammability 5 10 10 11 13 13 13 13 13 15 15 17 17 17 20 20 21 22 22 22 22 23 23 24 24 25 28 28 28 28 General considerations Tooling estimation scheme Tooling for small and medium size pipe General considerations Equipment Physical properties
-3-

Pipe pressure performance

3. Pipe extrusion of PB-1 General extrusion techniques Extrusion equipment 3.2.1 3.2.2 3.2.3 3.2.4 3.2.5 3.2.6 3.2.7 3.2.8 3.2.9 3.2.10 3.2.11 3.3 Tooling 3.3.1 3.3.2 3.3.3 3.4 3.4.1 3.4.2 3.4.3 General considerations Feeding system Screw configuration Melt pump Breaker plate and screen pack Melt temperature and pressure sensors Die head Pipe sizing Materials of construction Pullers and coilers Cutters

28 29 34 36 36 36 36

Large diameter PB-1 pipe

3.4.4 3.5 3.6

Tooling for big pipe

38 39 40 40 40 41 41 42 42 42 42 43 surface 43 43 43 44 44 44 44 45 47

Grinding and reprocessing Troubleshooting 3.6.1 General procedure 3.6.1.1 3.6.1.2 3.6.1.3 3.6.2 3.6.2.1 3.6.2.2 3.6.2.3 3.6.2.4 3.6.2.5 3.6.2.6 3.6.2.7 3.6.3 Evaluation procedure 1 Evaluation procedure 2 Evaluation procedure 3 Melt sticking at pre-sizing water chamber faceplate or sizing sleeve Difficulty increasing rate of extrusion Longitudinal lines in pipe Pipe is not round (ovality) Poor appearance of (outside and inside) pipe

Miscellaneous problems

Elongation at break values below minimum Processing water quality, pressure and temperature Symptoms Possible causes Extrusion process Possible causes Raw material

Lot to lot variability in PB-1 pipe production 3.6.3.1 3.6.3.2 3.6.3.3

3.6.4

PB-1 pipe extrusion troubleshooting cross reference

4. Annex: List of standards relevant for PB-1 pipes

-4-

1.

Description of PB-1

Polybutene-1 (PB-1) is a thermoplastic polymer obtained by polymerisation of 1-butene using stereospecific Ziegler-Natta catalysts belonging to the family of polyolefins (Fig. 1). Due to its similar structure the properties resemble mostly those of polypropylene (PP) but because of the longer side chain there are some considerable differences. PB-1 is compatible with PP but not with PE.

H H l l CC Fig. 27: Sc H H n

H
l

H
l

CC l l H CH3 n

H H l l CC l l H CH2 n l CH3 Polybutene-1

Polyethylene

Polypropylene

Fig. 1: Structure of various polyolefins

PB-1 is a highly isotactic, partially crystalline homopolymer of high molecular mass. Highly isotactic means that nearly all C2 side chains are attached to the same side of the molecule. PB-1 must not be confused with the rubber-like polyisobutene (PIB) (Fig. 2).

C C C C C Butene-1 C C C

Isobutene C C C C C C C C C C C

C C C

P olyB utene-1 PB -1

PolyIsoButene PIB

Fig. 2: Polybuten-1 is not Polyisobutene

PB-1 crystallises upon cooling from the melt. During crystallisation the polymer chains fold to three-dimensional order in small regions, the crystallites. These crystallites are connected by tie-molecules and chain entanglements so that a single PB-1 molecule typically contributes to the structure of many crystallites. This physical network is the key for excellent mechanical properties of PB-1 pipe grades. The crystallites form superstructures, the so-called spherulites. The typical degree of crystallisation of Basell PB-1 pipe grades is about 50 %. The exact value of crystallinity as well as the size of crystallites and spherulites both depend strongly upon cooling conditions.
-5-

The crystallisation rate of PB-1 is considerably lower than PE or PP. Upon solidification from the melt PB-1 crystallises first to an 11/3-helix in a metastable tetragonal modification called form II which is kinetically favoured. In this stage PB-1 is a rather soft, mechanically weak material. Over several days the material hardens by transforming into form I which is a 3/1helix in hexagonal unit cell and which is thermodynamically favoured. This crystalline transformation can be observed by differential scanning calorimetry, or DSC, as shown in Figure 3.

Fig: 3: Transformation of crystalline form II -> I of PB 4237 measured by DSC

-6-

The transformation of form II to form I depends strongly on ambient temperature and pressure as demonstrated in Fig. 4. At atmospheric pressure (1 bar) the maximum rate of transformation occurs around 20 C but drops significantly by increasing or decreasing the temperature. If ageing is performed at lower or higher temperatures than 20 C only the time to achieve final properties is longer: the final performance of the material itself is not affected.

1.500 bar

1.200 bar

500 bar

1 bar

Fig. 4: Dependence of transformation of form II -> I of PB-1 on ambient temperature and pressure

As can be taken from Fig. 4, too, the crystalline transformation can be shortened from a few days to only a few minutes by application of hydrostatic pressure of up to 2 kbar using a suitable autoclave. Only in this final stage after termination of ageing PB-1 achieves its excellent high temperature mechanical strength which for pipe and piping system producers make the material a preferred candidate for all hot water applications.
-7-

Tab. 1: Characteristics of important crystalline forms and amorphous phase of PB-1 Crystalline Form Helix type I II amorphous 3/1 11/3 Crystal type twin hexagonal tetragonal Melt temperature 125 135 C 110 120 C Density 0.950 g/cm 0,900 g/cm 0,870 g/cm3

Provided the material is appropriately processed, pipe systems made of Basell PB-1 meet or comfortably exceed all national and international standards relevant for pipe applications. PB-1 combines the well-known properties of typical polyolefines, e.g. good chemical resistance, easy weldability and low noise emission, with a unique combination of outstanding creep resistance, excellent high temperature stress rating and high flexibility. The most prominent features of PB-1 pipe grades are:

high strength also at higher temperatures, excellent creep resistance, low modulus and high flexibility, little noise transmission, good weldability, strong wet abrasion resistance, resistant to most chemicals.

In principle, as a thermoplastic material, PB-1 is also recyclable. Basell Polybutene-1 is currently available in 3 pipe grades: Tab. 2: Available PB-1 pipe grades and their application Grade PB 4237 grey PB 4235 ivory PB 4201 black Strength class PB 140 PB 140 PB 140 Typical application Hot and cold water heating and plumbing Underfloor and radiator heating Cold water transport

Basell Polybutene-1 pipe grades are supplied as fully stabilised and coloured ready-to-use pelletised compounds. The main properties of Basell PB-1 pipe grades are summarised in Table 3.

-8-

Tab. 3: Typical properties of Polybutene-1 Homopolymer Resins for Pipe Applications MATERIAL PROPERTIES (a) PHYSICAL PROPERTIES
Melt flow rate MFR 190C/2.16 kg Density Hardness Shore D ISO 1133 ISO 1183 ISO 8608 dg/min g/cm 3

METHOD (b)

UNIT

PB 4201

PB 4235

PB 4237

0,35 0,928 53

0,35 0,939 53

0,35 0,939 53

MECHANICAL PROPERTIES (c)

Tensile strength at yield Tensile strength at break Elongation at break Flexural Elastic Modulus Notched Impact Strength at 20C Notched Impact Strength at 0C ISO R 527 ISO R 527 ISO R 527 ISO 178 ISO 180 ISO 180 MPa MPa % MPa kJ/m kJ/m 20,4 36,5 330 530 no break 40 20,4 36,5 330 530 no break 40 20,4 36,5 330 530 no break 40

THERMAL PROPERTIES
Melting point (Form I) Vicat Softening Temperature Coefficient expansion of liner
o

DSC (d) ISO 306 (A50)

o o

C C
o

130 120 1.3 x 10 0.19 -16

-4

130 120 1.3 x 10 0.19 -16

-4

130 120 1.3 x 10 0.19 -16

-4

thermal ASTM D696 ASTM C 177 DMTA (d)

cm/cm/ C W/mK C

Thermal conductivity (20 C) Glass transition temperature

SPECIFIC CHARACTERISTICS
Environmental Stress Cracking ASTM D 1693 (50C / 10 % Igepal C0630 solution) Wet abrasion (sand slurry test, 23C, 100 h) Suitability for potable applications h 15000, no failure

% various European water quality standards -

1 approved not for cold suitable water supply Black Ivory approved for hot and cold water supply Grey

Colour

a) Values shown are averages and not to be considered as product specifications. These values may shift slightly as more data is accumulated b) ASTM test methods are the latest under the current procedures. All specimens are prepared by injection (ASTM 2146) c) Tests performed on compression moulded specimens which were conditioned 10 days at 20C. d) DSC = Differential Scanning Calorimetry

-9-

2. 2.1

Properties of PB-1 pipe materials Rheology

During processing, the rheological behaviour of PB-1 in its molten state plays an important role. Processing characteristics like die swell and melt strength are determined by the rheology of the material. Also the heat generated by shear within the extruder is mainly governed by rheology.

10000

processing zone

1000

Shear viscosity (Pas)

LLDPE
100 ca. 100 s shear rate ca. 1000 s
-1 -1

LDPE PP

10

PB-1
1 1e+3 1e+4 1e+5 1e+6 1e+7

Shear stress (Pa)

Figure 5: Shear viscosity vs. shear stress

As for most other polymers the rheological behaviour of PB-1 is very non-Newtonian, too. This means that the melt viscosity will depend strongly upon the shear stress experienced during processing. In Fig. 5 the shear viscosity is plotted against shear stress for some polyolefins of similar MFR. As demonstrated in Figure 5, PB-1 is more sensitive to shear than other polyolefins. The practical consequence is that PB-1 needs less extruder drive power because of its lower viscosity at processing conditions. The relationship between shear stress and shear rate is given by the definitiion of viscosity which is

vis cos ity =

shear stress shear rate

- 11 -

10 5 Slope = -1,16

Shear stress Black: zero shear plateau Red: 20.000 Pa Blue: 80.000 Pa

10 4

h (Pas)
10 3

-1,04

-0,77

10 2

10 1 10 -1

10 0

10 1

10 2

Melt flow rate (g/10min)

Figure 6: Viscosity (at different stress levels) as a function of MFR at 190C. Homopolymer (pipe grades) 0,75 % Ethylene 2,2 % Ethylene Copolymers (specialty grades) 5,5 % Ethylene

Polybutene-1 can be extruded, injection moulded and compression moulded as required by the particular application. For all Basell PB-1 grades, there is a one-to-one relationship between the melt flow rate (MFR) and the steady state viscosity at a given shear stress level, as illustrated in Figure 6. When plotting viscosity values as a function of MFR, straight lines fit to the data points in a double logarithmic graph. The sensitivity is highest at small shear stresses, the slope of the line being equal to 1,16, and slightly decreases with increasing stress: the slope decreases until 1,04 at 20 000 Pa shear stress (about the stress level corresponding to conditions used for measuring MFR) and 0,77 at 80 000 Pa shear stress (approximately corresponding to processing conditions). At even higher shear stress or shear rate levels the slope further decreases. Using Figure 6, it can be calculated that 10% difference in MFR value corresponds to 12% difference in viscosity at low shear stress and to 8% at high shear stress. 20% difference in MFR would correspond to 19% and 13% difference in viscosity, respectively. 2.2 Mechanical properties

PB-1 is a partially crystalline polymer with high isotacticity and consequently high crystallinity. Generally, the crystalline part determines a number of intrinsic characteristics of the polymer. These include density, stiffness, hardness, creep resistance, abrasion resistance, temperature resistance and chemical resistance. On the other hand, the amorphous part influences other properties like mechanical strength, impact resistance, environmental stress cracking resistance and compression set properties.

- 12 -

As shown in the model depicted in Figure 7, the crystalline layers in PB-1 are connected by entangled tie-molecules. These tie molecules reside in the amorphous part. Because of the high molecular mass a large number of tie-molecules is generated and the relatively long C2H5 side groups prevent extensive slipping of entanglement chains. These two factors make the bonds between adjacent crystallites very stable. The crystalline lamellae form spherical superstructures, which are called spherulites. A strong 3-dimensional network of entangled crystallites is formed.

Crystalline parts

Amorphous part Entangled molecules

Figure 7: Chain entanglements between crystalline domains

Stress PB-1 ss

other polyolefins

Strain

Figure 8: Tensile behaviour of PB-1 vs. other polyolefins

The peculiar tensile behaviour of PB-1 is based mainly on these chain entanglements. PB-1 does not show the typical necking behaviour; instead it tends to support the load while it continues to stretch. This is sometimes referred to as ductile with work-hardening*. However, depending on the preparation of the test specimen and the conditions of measurement, PB-1 may exhibit a very little yielding (see Figure 8).

Turner, S., Mechanical Testing Of Plastics, 2 Ed, Longman Inc. New York, p.133, 1983 - 13 -

nd

2.3

Impact resistance

PB-1 has excellent impact toughness. The IZOD notched impact strength (ISO 180) of PB-1 is classified no break at room temperature. The material retains its flexibility even at temperatures below freezing point which strongly facilitates installation during cold seasons. The glass transition temperature determining the ductile / brittle transition of PB-1 lies at approx. 16C. 2.4 Compression set

The compression set of PB-1 is remarkable. PB-1 homopolymers are very flexible and soft materials. However, because of its network of strongly entangled crystallites it exhibits an excellent elastic recovery even though it is not cross-linked. Typically, the compression set at 23C is ca. 55 %, and at 70C ca. 64 %, when tested in accordance with ASTM D395-89, method B. 2.5 Abrasion and wear resistance

PB-1 has an excellent wet abrasion resistance, when tested in sand/slurry type conditions as shown in Figure 9. It performs as well as UHMW-PE which is well known for its outstanding abrasion and wear resistance. Therefore, pipes made of Basell PB-1 resins can also be used for transport of slurry, e.g. in the mining industry. In dry conditions, however, PB-1 behaves similarly to conventional polyolefins.

6 5 4 3 2 1 0 UHMW-PE PB-1 HMW-HDPE HDPE PP

Figure 9 : Sand-Slurry abrasion resistance of polyolefins

2.6 2.6.1

Creep behaviour General

All thermoplastic polymers show viscoelastic behaviour, i.e. their mechanical properties depend not only on stress and temperature but also on time. A particular, very important feature of viscoelastic materials is creep which means that the deformation of such materials at given temperature and load increases as a function of time. Figure 10 shows the time dependence of elongation at constant temperature and load of PB-1 compared to other polyolefins. This excellent creep performance is maintained even at elevated temperatures as shown in Figure 11.
- 14 -

32

24

D -H PE

-X PE

Elongation [%]

-Co PP

16

PP

PB-1
0 10
-2

10

10

10

10

Time [h]
Fig. 10: Creep behaviour of polyolefins in uniaxial tension at 23 C / 8 MPa

Elongation [%]

13,80 MPa @ 23C

4 6,60 MPa @ 60C 2 3,45 MPa @ 60C 3,45 MPa @ 23C 0 0,1 1 10 100 1000 10000

Fig. 11: Creep performance of PB-1 at elevated temperature and stress

- 15 -

2.6.2

Creep performance at uniaxial load

Two different experiments can be performed: retardation measurements in which the change of deformation e (t ) at constant stress (s = const.) is measured and relaxation experiments in which the change of stress s at constant deformation (e = const.) is monitored. As a result of retardation experiments the creep modulus can be obtained according to the equation Creep modulus E c (t ) =

s e (t )

(1)

This measurement can be performed in bending (flexural creep by three-point loading) according to ISO 6602 or in tension (tensile creep) according to ISO 899. Since in flexural bending defects of the outer fibre zone may disturb the result tensile creep is more reliable because of its uniform stress at whole cross section. It has to be taken into account that the measured value of creep modulus depends on the

400

Apparent modulus (MPa)

PP homopolymer at 60C and 2.75 MPa

300

200

nylon 12 at 80C and 2 MPa

PB-1 at 85C and 5.4 MPa

100

63 D copolyester at 100C and 5.5 MPa

0

10

100

1000

Time (hours)
Fig. 11: Creep modulus of PB-1 compared to other polymers at elevated temperatures

level of stress. 2.6.3 Practical consequences of creep

The creep performance / stiffness ratio of PB-1 is similar to engineering polymers like TPU, PA11 or PA12 as shown in Figure 13.

- 16 -

3000

Stiffness [MPa]

2500 2000

POM

PP
1500 1000

PA6/66

HDPE LDPE

500 0

PA11/12

PB-1

TPO

TPU

Creep Resistance

Figure 13: Stiffness vs. creep resistance of various polymers

Translated into pipe applications creep means 'blowing up' the pipe under constant pressure over time, i.e. increasing the diameter and at the same time decreasing wall thickness as illustrated in Figure 14, which leads to lower pressure performance at longer time. The excellent creep properties of PB-1 mean that the problem of creepis reduced to a minimum, even in hot water piping applications.

Creep
(Constant pressure over time)

Burst
(Further maintenance of pressure)

Fig. 14: Change of pipe dimensions and burst due to creep (schematic)
- 17 -

For calculating finished parts the properties obtained from long-term mechanical experiments are divided by a safety or design factor depending on application. Examples for such design factors can be found in relevant pipe standards like ISO 15876. 2.7 2.7.1 Pipe pressure performance Quick burst

Since final mechanical strength of PB-1 is only achieved after transformation of form II -> form I the quick burst performance of pipes depends on ageing time, too, as demonstrated in Fig. 15. Although 90 % of the final value is achieved after 5 days there is still some additional increase in quick burst and overall pipe performance even after months. However, an ageing time of 5 days is sufficient to meet all application requirements and the pipe is ready to use.

10,00

9,00

8,00

7,00

6,00

5,00

4,00

3,00

2,00

1,00

0,00 2 3 4 5 6 7 Time (days) 8 9 10 15 20

Fig. 15: Quick burst stress of PB 4237 pipes at 95 C as a function of ageing time (Ageing done at 23 C)

2.7.2

Creep rupture strength

More important than instantaneous strength like quick burst is the long time performance of PB-1 pipes up to and, for safety reasons, above the upper service temperature since PB-1 is intended for long-term use at elevated temperature and pressure. For most heating and plumbing applications an expected lifetime of 50 years and more is required. A full description of pipe performance as a function of time, temperature and pressure can be done via creep rupture strength diagrams according to ISO 9080 as shown in Figures 16 - 18 for PB 4237, PB 4235 and PB 4201.
- 18 -

Based on these diagrams a classification according to ISO 12 126 can be done. Starting point is the evaluation of creep rupture curves according to the Standard Extrapolation Method (SEM) as described in ISO 9080. This evaluation yields for the hoop stress at 20 C and 50 years lifetime the expected Long-Term Hydrostatic Strength (LTHS) and the 97,5 % Lower Probability Limit (LPL). This LPL hoop stress is classified according to the Renard 10 (R 10) number scheme as defined in ISO 3, which is a division of a logarithmic decade in 10 equal steps 1 1,25 1,6 2 2,5 3,2 4 5 6,3 8 10. Note: For extrapolated hoop stresses above 10 MPa the Renard 20 (R 20) number scheme is used, which divides the logarithmic decade in 20 equally spaced steps and thus yields a finer separation of MRS classification. The calculated LPL hoop stress at 20 C is then degraded to the next lower R 10 or R 20 number. The result is the Minimum Required Strength (MRS). Final estimation of the MRS class of current Basell grades is in progress. Preliminary data indicate that Basell PB-1 pipe grades will achieve at least a LPL hoop stress of 14 MPa. As a result of this, all current Basell PB-1 grades belong to MRS class PB 140.

Fig. 16: Creep rupture strength of PB 4237

- 19 -

Fig. 17: Creep rupture strength of PB 4235

Fig. 18: Creep rupture strength of PB 4201

- 20 -

Besides the determination of the MRS classification of the material creep rupture stress diagrams can also be used to evaluate the expected lifetime at any temperature and stress combination given.2 From the dimensional independent parameter hoop stress the corresponding pressure can be calculated according to the equation:

p=
with p (bar): s (MPa): e (mm): d (mm):

s e 20 d -e

pressure hoop stress wall thickness outer diameter

or by defining the Standard Dimension Ratio (SDR)

SDR =

d e

->

p=

s 20 SDR - 1

For practical purposes most often a safety or design factor of between 1,25 and 2 is considered in addition. A complete list of operational pressures dependent on application classes, pipe dimensions, temperatures, lifetimes and design factors can be taken from relevant pipe standards, e. g. ISO 15876 or DIN 16989. 2.8 Flammability

As other polyolefins, polybutene-1 is a material with normal flammability. Therefore, it belongs to building material class B2 according to DIN 4102-1. Polybutene-1 can be ignited by an open flame and continues to burn even after removal of the ignition source. Because of the generated heat the material melts with burning drips. The ignition is favoured by sharp edges and becomes easier for lower wall thickness. Typical combustion products are carbon monoxide, carbon dioxide and water but no corrosive or environmental harmful residues occur. For installation in buildings the use of suitable fire protected insulation materials like e.g. rockwool may be required as regulated by relevant local standards or other fire protection regulations. 3 Pipe extrusion of PB-1

Generally, PB-1 pipe materials can be extruded with standard extruder screws and die heads designed for polyolefins without major problems. As outlined in the previous section PB-1 crystallises relatively slowly in a kinetically favoured form II yielding a very soft product. Upon transformation to the thermodynamically stable form I the excellent properties of PB-1 pipe are achieved. At 20 C this ageing completes to more than 90 % within 5 days, but continues increasingly slowly later on. Even after months and years there is still some additional ageing. Because of this unique crystallisation and ageing behaviour some precautions during calibration and cooling of pipe processing have to be considered. The dimensions of fresh pipe have to be chosen slightly bigger to account for the shrinkage occurring during ageing. The storing conditions during ageing have to be controlled carefully in order to obtain good

In case of different temperatures or pressures a combined lifetime can be estimated using Miners Rule as described in ISO 13 760 which describes the cumulative load resulting from additivity of all individual loads at each particular temperature / stress combination. - 21 -

quality final pipe. The following guidelines could help to acquaint the processors with the handling characteristics of this unique material and the processing conditions required. 3.1 General extrusion techniques

The recommended processing melt temperature and melt viscosity of Basell polybutene-1 pipe compounds are very similar to other polyolefins, in particular to low and medium density polyethylene. The optimum melt temperature should be between 180 and 200 C. Use of higher than recommended melt temperatures can result in sticking of the extruded pipe in the sizing sleeve or presizer face plate or even in the extruder itself leading to problems in purging the extruder. Lower than recommended melt temperatures may cause excessive machine direction (MD) orientation resulting in poor pipe quality which may lead to reduced creep rupture performance and premature failure upon bending during installation of pipes. Depending on line and screw speed and screw design some additional shear heat may be generated leading to higher melt temperatures than set at the end of the die. Table 4 shows a typical temperature profile of extruder and die zones. Tab. 4: Typical extrusion temperature profile* Extruder Zone Temp 1 175 2 175 3 180 4 180 1 180 2 180 3 180 Die 4 180 5 180 6 185 190 Melt

Slight inevitable changes in MFR among different batches of PB-1 can be corrected very easily by simply adjusting the melt temperature accordingly. As a rule of thumb an increase of MFR (190/2,16) of 0,1 corresponds to a decrease in melt temperature of approx. 10 C. An example of corresponding MFR / melt temperature combinations is given in Table 5. Tab. 5: Change of melt temperature due to MFR variation MFR (190/2,16) Melt temp. (C) 0,25 202 0,30 196 0,35 190 0,40 185 0,45 181

By using a melt pump adjustments of melt temperature due to MFR variations can be avoided in most cases. As initially extruded polybutene-1 crystallises slowly into the phase II form, a soft, low modulus material. Upon ageing, polybutene-1 will change crystalline form within several days to phase I, a stiffer, higher modulus product exhibiting the final desired properties. The slow crystallisation rate of polybutene-1 requires direct water cooling prior to surface contact. A spray ring that provides a water film for quenching and lubricating the pipe surface without causing water marks should be used. In addition to water quenching it is recommended to use a water seal to presize the pipe to maintain uniform sizing and process stability. Due to the relatively slow crystallisation rate of PB-1 and individual characteristics of processing extruders various customers may use somewhat different conditions to produce PB-1 pipes. Some have found that starting with a lower melt temperature facilitates faster crystallisation from the melt and thus allows for easier pipe extrusion. For other customers the trade off between better processability obtained with lower melt temperatures and the
*

These temperatures are presented only as a guideline and should not be considered optimum for all extruders.
- 22 -

decrease in certain physical properties, like higher orientation in machine direction as measured by elongation at break, is not acceptable. Generally, melt temperatures between 180 C and 200 C combined with cooling water temperatures between 10 C and 12 C for spray ring, presizer and cooling baths may provide the best balance of pipe processability and physical properties for extrusion of small pipes of sufficiently high line speed. 3.2 3.2.1 Extrusion equipment General considerations

Any extruder suitable for processing of polyolefins can be used for extrusion of polybutene-1 pipe as well. Depending on size of pipes to be produced the appropriate size of extruder has to be chosen. For pipe sizes up to 25 mm O.D. an extruder having a maximum throughput of 120 - 150 kg/h will be sufficient. Depending on the design of the screw and feeding zone this is typically achieved with extruders having a screw diameter of 45 60 mm. For bigger pipes up to 110 mm O.D. a maximum throughput of 250 300 kg/h is recommended. In this case screw diameters up to 90 mm may be used. Length-to-diameter (L/D) ratios of 24 or greater are recommended to achieve sufficient plasticisation. Relatively low temperatures are applied to process polybutene-1 resins; however, heaters and controllers capable of efficient operation up to 260C are desirable. The extruder barrel should be divided into at least three, preferably five, independently controlled heating zones, each equipped with its own thermocouple and temperature indicating controller. Barrel air or water cooling systems are suitable for polybutene-1 pipe extrusion as long as adequate temperature control is achieved. Effective air cooling, however, might be acceptable. Water cooling of the throat section of the barrel should be used to prevent bridging and to increase throat-bearing life. Screw cooling and forced feeding are not required. Any of the drive systems normally employed for polyolefins may be used; however, good speed regulation (recommend 1 %) is essential. In contrast to other polyolefins, a polybutene-1 screw has a shallower feed zone and therefore requires higher screw speed (RPM) for maximum throughput. Polybutene-1, having a lower heat of fusion than lowdensity polyethylene (LDPE) requires less total energy per kilogram to process. 3.2.2 Feeding system

To increase throughput a grooved feeding zone can be used which has to be water cooled to ensure proper feeding and prevent blocking of the screw by partly molten pellets. Gravimetric feeding systems are recommended to have constant, uniform material supply. By using a dryer adsorbed moisture can be removed from pellets which otherwise may cause voids in pipe walls. 3.2.3 Screw configuration

Several commercial screw designs perform well with polybutene-1. These include conventional 2- or 3-stage screws as well as barrier type screws as shown in Fig. 19. In order to increase melt homogeneity the screw design may contain shear mixing sections, e.g. Maddox type. Tooth type mixing section are less suitable because they may introduce regions with higher residence time. A screw designed for polyethylene or polypropylene may also be acceptable. When purchasing an extrusion screw for the production of polybutene-1 pipe or tubing, the most sensible approach would be to consult an extrusion screw manufacturer. Considering individual requirements of the customer, the extrusion screw manufacturer will typically run rheology curves at different shear rates on the materials to be processed and will recommend a screw profile based on data generated by such experiments.
- 23 -

Fig. 19: Screw design: Standard 3-zone vs. barrier screw (Source: Fa. Battenfeld)

3.2.4

Melt pump

A melt pump, fitted to the particular extruder and processing conditions is strongly recommended because freshly extruded polybutene-1 pipe is extremely soft and thus very sensitive to even minor throughput changes which may result in surging and a concomitant unacceptable variation in pipe wall thickness and diameter. Output or melt pressure variations should be kept below 1 %. This will increase melt output and pipe extrusion rates (typically by at least 10 %), stability and allow for increased flexibility of the process. In addition to that the sensitivity of extrusion against variations of melt viscosity is greatly reduced. 3.2.5 Breaker plate and screen pack

A breaker plate and screen pack is recommended. Breaker plate holes should be streamlined for flow. Stainless steel screen packs containing a 20, 80, 40 mesh screens or a Dutch weave having similar mesh size are recommended to develop adequate backpressure for good mixing. Although the screens also act as a filter in the event foreign material is inadvertently introduced in the feed, precautions should be taken to avoid contamination. Resin feed stock and boxes of regrind should be kept closed whenever possible. As a further precaution, the use of a hopper magnet is suggested.
- 24 -

Note that the deliberate addition of processing aids, masterbatches or other additional material to the polybutene-1 being processed may invalidate the codes and standards as well as the relevant water authority approvals to which the material as supplied has conformance. 3.2.6 Melt temperature and pressure sensors

The extruder should be equipped with sensors for continuously monitoring temperature and pressure of the melt during extrusion. The melt temperature cannot be estimated from barrel temperatures since it may deviate considerably from the latter due to heat generated by shear, which varies with screw design, speed, and resin viscosity. The temperature sensor should be located downstream of the breaker plate. In order to obtain a more accurate measurement and to minimise the effect of any heat transfer from the heated metal surfaces, the temperature sensor should protrude into the melt stream. The tip of the sensor should extend at least 3 mm from the wall, but not further than the centerline of the flow channel. Extruder discharge pressure or head pressure should be monitored, preferably using a transducer type pressure gauge before and behind the melt pump, respectively. The use of pressure gauges provides information about the uniformity of extrusion conditions, continuous and sufficient melt supply and will detect such problems as surging. A further pressure sensor in front of the breaker plate will function as a safety device indicating clogging of the screen pack and, thus, prevent serious barrel overpressure. Normally, typical extrusion pressures for Basell polybutene-1 resins are low (80 120 bar). 3.2.7 Die head

The required pipe or tubing diameter and wall draw-down ratios depend upon extrusion rate and desired pipe size. Draw-down ratios of 5-20 % are typical, with larger profiles being at the upper end. Use of greater than recommended draw-down ratios can lead to poor quality pipes and high machine direction orientation. Appropriate tooling incorporating the recommended draw-down ratios for corresponding processing conditions is shown in the tooling section of this manual. Extrusion with inadequate draw-down ratio will result in difficulty in maintaining pipe dimensional control and quality.

Fig. 20: Basket Mandrel Die (Source: Fa. Battenfeld)

- 25 -

The optimum land length / annular gap (L/D) ratio also varies with line speed and pipe size. In general, (for pipe and tubing of 50 mm SDR 13.5 size and smaller), an L/D ratio of at least 8/1 is recommended to promote uniform extrudate and quality piping at economical rates of extrusion. Larger pipe sizes are less critical. Minimum disruption to material flow is desirable at this point avoiding formation of pronounced flow lines. Of the various die types available, the Basket Mandrel die shown in Figure 20 provides for the least interruption of material flow and therefore results in a more homogeneous material flow and pipe wall. However, other die design types like the spider mandrel die can be used as well provided a suitable temperature profile avoids formation of weld lines which may cause premature failure of pipes. 3.2.8 Pipe sizing

Because of its very low crystallisation speed compared to other polyolefines polybutene-1 pipes require some special measures during cooling and calibration. As shown in Figure 21, a spray ring and a pre-sizing water well are used before entering the usual calibrator forming the outer diameter of the pipe.

SPRAY RING DIE MELT

WATER WELL / PRESIZING CHAMBER

VACUUM CHAMBER WATER

SIZING SLEEVE

MOLTEN PIPE

PRESIZING FACEPLATE SPRAYED WATER SIZING SLEEVE FACEPLATE

Fig. 21: Precooling and calibration section of a polybuten-1 pipe line (schematic)

Immediately after having left the die head the polybutene-1 tube is quenched by means of a conical water film sprayed onto the pipe surface. The opening angle of this spray film should be approx. 45 degrees. A water head pressure of 2,5 3,0 bar at the spray ring with the valve open is typically used. Care must be taken to avoid damage of pipe surface by excessive water pressure or non-uniform spray pattern. Besides cooling this water film also
- 26 -

'lubricates' the outer pipe surface and thus prevents sticking of the still molten tube at the entrance of the water well faceplate. In addition to this immediate quenching, a water well equipped with a water seal faceplate having an entry angle of 40 to 45 degrees and a land length not greater than 0,8 mm should be provided to maintain uniform sizing and process stability. The water seal faceplate diameter depends on extrusion rates and tubing size. However, the seal ID should not be less than 7 % greater than the fresh tubing. The correct size is achieved when there is only a small gap (< 0,5 mm) between pipe surface and bore of water well faceplate. Typically, the water well is supplied with cooling water from the bottom having an overflow at its top side. Ideally, the water supply should be set in order to just balance the loss of water through the gap between pipe surface and bore of faceplate. If these conditions are met, this results in a slight, steady overflow of water. Generally, vacuum sizing is recommended for processing of polybutene-1 pipe. The vacuum sizing sleeve diameter should be 2,5 - 3 % greater than the in-line "fresh" tube diameter. The effective land length of the sleeve depends on extrusion rates being longer for higher line speeds. The sizing sleeve geometry for polybutene-1 differs somewhat from other polyolefins. A greater entry angle and sufficient length are required because of lower crystallisation rate of PB-1. At least for smaller pipes (up to 50 mm diameter) disc type calibrators are preferred. However, barrel type sizing sleeves containing holes or slits can be used provided their inner surface is not smooth but finely rifled to prevent sticking of the pipe at the metal surface. The key aim is to minimize the contact area between polybutene-1 and the metal surface of the sizing sleeve in order to prevent sticking. Spray rings and pre-sizing chambers are not typically used in the production of polybutene-1 tube in sizes over 70 mm diameter, however, it has to be checked whether a spray ring may help to maintain processing stability. Polybutene-1 generally requires much lower vacuum levels than other polymers because of its slow rate of crystallisation and low modulus. Very stable operation is achieved at vacuum levels as low as 40 80 mbar. It is therefore recommended that the sizing tank incorporates vacuum gauges calibrated in mbar. Only gauges providing a very stable vacuum should be used. In addition to that split vacuum tanks are preferred which allow to set 2 or 3 different vacuum levels along the pipe to increase dimensional stability and facilitate dimensional control. Contoured rollers are usually required to support PB-1 pipe in order to minimise pipe ovality for all pipe sizes. These rollers should be spaced every 0,5 m within the vacuum and cooling tanks and have to be installed below the pipe for spray cooling and above the pipe for flood cooling. The rollers in the vacuum tank should have the same inside diameter as the inside

Fig. 22: Contoured roller

- 27 -

diameter of the sizing sleeve. The rollers in the cooling tanks should be 4 5 % larger than the maximum fresh tubing radius to minimise out-of-roundness because of the very soft freshly extruded polybutene-1 pipe. In addition to this the rollers should have a land length of approx. 10 mm. For 75 m pipes and larger the radius should conform to the radius of the fresh tube. The first roller should be located approximately 50 75 mm from the sizing sleeve exit to maintain proper sizing and reduce distortion. A schematic drawing of a typical contoured roller is shown in Fig. 22. The contoured rollers can be made of any plastic material with sufficient stiffness and wet abrasive resistance such as polyethylene, polypropylene or nylon. Care should be taken to ensure that there is no significant friction of the roller bearings. Figure 23 gives a typical example of a contoured roller.

Fig. 23: Contoured roller for PB-1 pipe extrusion

The cooling tanks should be sized to have a length of 1 meter for each meter per minute of line speed. Spray cooling can be used as well as underwater cooling. Note that improper design or water pressure of spray dies may give rise to water markings on the pipe surface. Gaskets used to seal cooling tanks should be wide enough and made of very soft material in
- 28 -

order to avoid too much friction. Excessive friction will give rise to extra pulling force which can cause pipe pulsation. A processing water temperature of 10 12 C is recommended. 3.2.9 Materials of construction

In the molten state, Basell polybutene-1 resins are not corrosive to metals. Therefore, a general purpose grade steel typically used for plastics processing is adequate for extruder barrel and screw, melt pump, adapters, head and dies. Chrome plating of the extrusion dies is not required. They should be medium polished only, (0,3 m surface roughness). Chrome plated or highly polished surfaces can favour "stick-slip behaviour of the extrudate. The screw flight lands should be Stellite or surface hardened to prevent wear of the screw and to maintain the proper screw-barrel clearance. Chrome plating of the screw is not necessary. Pre-sizer and calibrator faceplate can also be made from brass. 3.2.10 Pullers and coilers

A continuous type puller with soft foam pads is recommended. The use of cleated pullers may be acceptable if the pads are constructed of soft rubber (i.e., Shore A hardness approximately 10) and do not present a discontinuity to the profile surface upon contact. Hard cleated pullers are not recommended since they will cause severe distortion of the initially soft polybutene-1 product. Tire type pullers are not recommended since inadequate contact is present that results in slippage. Also, excessive pressure causes profile flattening. Pullers may be pneumatically loaded but should be adjusted mechanically. The coiling diameter should be as large as practical to provide the optimum in finished product dimensional quality. The coiling tension should be as low as possible to avoid stretching. The minimum coiling diameters for polybutene-1 profiles and tubing are dependent upon diameter and wall thickness. It is recommended to maintain a coiling diameter of at least 40 times the pipe diameter, but not be less than 700 mm. Upon suitable recoiling in the opposite direction after ageing almost straight polybutene-1 pipe can be obtained on unwinding. During installation of polybutene-1 pipe bending diameters lower than 12 times the pipe diameter should be avoided to prevent excessive stress on outer pipe surface. It is recommended to use the highest bending ratio possible during application. 3.2.11 Cutters

For the production of small pipe up to 25 mm at higher line speeds (12 m/min and more) the use of fly wheel cutters is recommend to provide sufficiently fast cutting. For lower line speeds guillotine type or planetary saw cutters are acceptable, too. Since fresh polybutene-1 pipe is very soft, cutter blades should be sharpened or replaced regularly. 3.3 3.3.1 Tooling General considerations

Tooling dimensions to be used for extrusion of polybutene-1 pipe depend strongly on processing parameters like line speed, water temperature, melt temperature, etc. Other important factors for estimating correct tooling dimensions are pipe shrinkage during processing and subsequent ageing (form II-> form I transformation) as well as OD and wall thickness draw down ratio, i.e. ratio between die and freshly extruded pipe dimensions. These parameters in turn depend on pipe size.

- 29 -

3.3.2

Tooling estimation scheme

The following example demonstrates steps required for evaluating tooling dimensions for a given SDR 11 pipe of 20 mm (+ 0,3 mm) outside diameter (OD) and a wall thickness of 1,9 (+ 0,3 mm). Estimates provided in this example are based on calculations, premises and best estimates as well as practical experience. They are intended only as starting point guidelines for the production of polybutene-1 pipe of sizes below 40 mm OD. Some modifications may be required in order to optimise tooling for each particular line as well as for each particular set of processing conditions. All dimensions are in millimeters. Step 1: Determination of average freshly extruded (form II) outside diameter (OD-II) and mid-wall thickness (wall-II) of pipe First of all the dimensions (OD and wall thickness) of the aged pipe have to be defined. For this example of 20 x 1,9 mm pipe nominal values are: OD (OD-I) is 20 mm with a tolerance of + 0,3 mm whereas wall thickness (wall-I) is 1,9 mm +0,3 mm.

OD - I + (OD - I + OD tolerance ) OD - II = * (1 + OD shrink factor ) 2

OD-II OD-I OD tolerance OD shrink factor

Estimated mid-outside diameter of fresh 20,5 (form II) pipe Desired nominal outside diameter of aged 20,0 (form I) pipe Tolerance (+) of outside diameter of aged +0,3 pipe Estimated outside diameter shrinkage factor 0,017 (premise) for actual pipe size

wall - I + (wall - I + wall tolerance ) wall - II = * (1 + wall shrink factor ) 2

Wall-II Wall-I Wall tolerance Wall shrink factor

Estimated mid-wall thickness of fresh 2,07 (form II) pipe Desired nominal wall thickness of aged (form 1,9 I) pipe Tolerance (+) of wall thickness of aged pipe +0,3 Estimated shrinkage factor (premise) for 0,010 actual pipe size
- 30 -

Step 2: Determination of die inside diameter (DID) Fresh pipe size (OD-II): 20,5 Percent OD draw down ratio desired: 4,5 % Inside diameter of die (DID) is 4,5 % larger than outside diameter of freshly extruded (OD-II) pipe.

DID = OD - II * (1 + 0,045)
DID OD-II OD draw down ratio Estimated inside diameter of die 21,4

Estimated mid-outside diameter of fresh 20,5 (form II) pipe Estimated OD draw down ratio required 4,5 % (premise)

Step 3: Determination of die gap (DG) Fresh mid-wall thickness (wall-II) of pipe: 2,07 Percent fresh (wall-II) draw down ratio desired: 10 % Die gap (DID) is 10 % thicker than mid-wall thickness of freshly extruded (wall-II) pipe.

DG = wall - II * (1 + 0,100 )
DG wall-II wall draw down ratio Estimated die gap (die opening) 2,28

Estimated mid-wall thickness of fresh (form 2,07 II) pipe Estimated wall draw down ratio required 10 % (premise)

Step 4: Determination of outside diameter of pin (POD) Inside diameter of die (DID): 21,4 Die gap (die opening): 2,28

POD = DID - 2 * DG
POD DID DG Estimated outside diameter of pin Estimated inside diameter of die Estimated die gap (die opening) 16,9 21,4 2,28

- 31 -

Step 5: Determination of die land length (LL) The length of the parallel zone at the end of the die divided by the width of die opening or die gap (DG) should equal 10. This ratio is abbreviated L/D. Deviations from estimated land length can be tolerated as long as die swell and pipe surface remain acceptable.

LL = DG * L D
LL DG L/D Estimated land length Estimated die gap (die opening) 23 2,28

Ratio of length of parallel zone of die to die 10 gap (premise)

Step 6: Determination of inside diameter of sizing sleeve (SSID) Fresh outside diameter (OD-II) of pipe: 20,5 Percent processing shrinkage: 3% Inside diameter of sizing sleeve (SSID) is 3 % larger than fresh pipe size (OD-II).

SSID = OD - II * (1 + 0,030)
SSID OD-II Processing shrinkage Estimated sleeve inside diameter of sizing 21,2

Estimated mid-outside diameter of fresh 20,5 (form II) pipe Ratio of inside diameter of sizing sleeve to 3% outside diameter of fresh pipe (premise)

Step 7: Determination of sizing sleeve length (SSL) Inside diameter of sizing sleeve (SSID): 23 Desired ratio of sizing sleeve length to its inside diameter is 5/1. This estimates only the approximate length of the sizing sleeve. Depending on cooling intensity and line speed the actual length required may be somewhat longer or shorter.

SSL = SSID * 5

- 32 -

SSL SSID Sizing sleeve L/D ratio

Estimated length of sizing sleeve Estimated inside diameter of sizing sleeve

106 21,2

Ratio of inside diameter of sizing sleeve to 3% outside diameter of fresh pipe (premise)

Step 8: Determination of inside diameter of water well (presizer) faceplate (WSID) Fresh outside diameter (OD-II) of pipe: 20,5 Inside diameter of water well faceplate (WSID) is 13 % larger than fresh pipe size (OD-II).

WSID = OD - II * (1 + 0,130)

WSID OD-II Faceplate size ratio

Estimated inside diameter of water well 23,2 (presizer) faceplate Estimated mid-outside diameter of fresh 20,5 (form II) pipe Ratio of inside diameter of water well faceplate to outside diameter of fresh pipe 13 % (premise)

Step 9: Determination of inside diameter of water spray ring (SRID) Inside diameter of die (DID): 21,4 Inside diameter of water spray ring (SRID) is 50 % larger than inside diameter of die (DID).

SRID = DID * (1 + 0,50)

SRID DID Spray ring size ratio Estimated inside diameter of spray ring Estimated inside diameter of die 32 21,4

Ratio of inside diameter of spray ring to 50 % inside diameter of die (premise)

The inside diameter of the water spray ring is not very critical. As long as an adequate conical spray pattern is achieved at the pipe surface and there is no contact between pipe and spray ring even differently sized spray rings can be used. In some cases, it may be possible to use the same spray ring to produce several sizes of pipe having similar outside diameters.
- 33 -

Very important is the distance between spray ring and water well faceplate (typically 50 120 mm) as well as the distance between spray ring and die (typically 30 80 mm). By adjusting these distances, for which the values in brackets may serve as guideline, the effective die swell of the pipe can be adjusted. Although spray rings for pipe sizes of outside diameter greater than 63 mm are not absolutely necessary their use may improve the quality of the pipe surface.

Step 10: Estimate length of pre-sizing water chamber The pre-sizing water chamber is usually constructed from a tube or pipe with an inside diameter sufficiently greater than the pipe to be extruded. The preferred material for this tube would be a transparent plastic allowing the user to look into the chamber. The chamber has an inlet with a valve on the bottom in order to continuously add small amounts of water. A hole should also be present on top of the chamber to allow excess water to exit the chamber which during normal pipe production should be completely filled with chilled water (10 12 C). This pre-sizing water chamber is connected to the front of the vacuum tank and has a water seal (pre-sizing faceplate) attached at the other end. The distance between vacuum tank and water seal (pre-sizing faceplate) is the pre-sizing water chamber length. The function of the pre-sizing water chamber is to enhance the cooling of the slowly crystallising molten polybutene-1 tube and to pre-size the melt before final sizing takes place in the sizing sleeve. In order to correctly optimise the length of this chamber, it is necessary to know the line speed of pipe production. The length of the pre-sizing water chamber typically ranges from 50 to 125 mm being the longer the higher the line speed is. Line speed 3 m/min 10 m/min 17 m/min 23 m/min Estimated length of pre-sizing water chamber 50 mm 75 mm 100 mm 125 mm

The above mentioned estimates are valid for production of pipe sizes with an outside diameter of up to 63 mm only. Pre-sizing water chambers are not typically used for extrusion of big pipes.

- 34 -

3.3.3

Tooling for small and medium size pipe

Pre-sizing chamber Spray ring Pre-sizing faceplate (Water well) G A H C Sizing sleeve

F B

Vacuum tank E

50 80 mm 100 210 mm

Fig. 24: Schematic drawing of tooling for small PB-1 pipe

These tooling dimensions and drawings are based on calculations, premises and best estimates as well as practical polybutene-1 pipe experience. They are intended only as guidelines or starting points to assist in the production of polybutene-1 pipe. Some modifications may be necessary to optimize production for each particular system or when processing conditions like melt temperature, water temperature, line speed, draw down ratio, etc. deviate from these estimates. The production rate (line speed) estimates given in Tab. 6 are for experienced users and can only be achieved if the line used is suitably equipped to meet the needs for PB-1 extrusion. In addition to that it requires thorough understanding and developing sufficient expertise of PB-1 processing behaviour.

- 35 -

Tab. 6: Tooling dimension recommendations for small and medium size pipe

Tooling
Fresh pipe O.D. Fresh wall thickness Die I.D. Land length Pin O.D. Sizing sleeve I.D. Sizing sleeve length Pre-sizer faceplate I.D. Pre-sizer length Spray ring I.D. Line speed (m/min)

Diagram letter

12 x 1,3
12,3 1,46

16 x 1,5
16,4 1,67 16,9 18 13,2 16,9 200 18,5 120 25 20

16 x 2
16,4 2,17 16,9 24 12,1 16,9 200 18,5 110 25 18

17,9 x 2
18,3 2,17 19,0 24 14,2 18,9 200 20,7 100 30 16

20 x 1,9
20,5 2,07 21,4 23 16,9 21,2 200 23,2 100 35 16

21,9 x 2
22,4 2,17 23,5 24 18,7 23,2 180 25,4 90 35 14

25 x 2,3
25,6 2,54 26,8 28 21,2 26,5 150 28,9 80 40 11

27,9 x 2,5 32 x 2,9

28,6 2,74 29,8 30 23,8 29,6 150 32,3 75 50 9 32,7 3,15 35,2 35 28,3 33,9 180 37,0 70 60 8

63 x 5,8
64,4 6,24 72,8 69 59,1 66,7 300 72,8 50 120 3

A B C D E F G H

12,6 15 9,5 12,7 200 13,9 120 20 20

Pipe dimensions according to ISO 15876-2 All dimensions in mm

- 36 -

3.4 3.4.1

Large diameter PB-1 pipe General considerations

As the size of pipe increases, the line speed and die swell typically decreases and the need for spray rings and pre-sizing chambers becomes less apparent or beneficial to the extrusion process. Because the material will typically spend only a fraction of a second in the sizing sleeve when producing 16 mm pipe at 18 m/min, it is necessary to pre-cool and pre-size the pipe to facilitate the crystallisation and sizing process. When producing 160 mm pipe, the line speed is substantially reduced to about 0,6 m/min only. At that rate the material exits the die with much less die swell and could be subjected to surface cooling in the sizing sleeve for up to 25 seconds. The tooling calculations and premises that are used for smaller diameter pipe will not work with larger pipe sizes. 3.4.2 Equipment

Although larger extruders with increased output and/or lower line speeds are required the use of a melt pump is also recommended for large polybutene-1 pipe. Since pre-sizing water chambers are typically not used for large pipe the sizing sleeve will be closer (80 150 mm) to the die in order to maintain proper sealing of the vacuum tank. The use of a spray ring is not as important as for small pipe but can be helpful for big pipe, too, in order to enhance lubrication of the extrudate upon entering the sizing sleeve. For production of big pipe higher draw down ratios of 20 % or more are typically used. Because of higher wall thickness extended downstream cooling length is required despite much lower line speed used for large pipe extrusion, e.g. approx. 15 m for 110 x 10 mm pipe produced at 1,3 m/min. Preferred cutter type is a travelling or planetary saw with blade cooling to provide proper pipe cuts. Mostly straight pipes are produced. However, if coiled pipe is required, heavy duty coilers have to be used. 3.4.3 Physical properties Because of the much slower cooling speed of thick walled pipe a gradient of morphological and hence physical properties across the pipe wall becomes more prominent and makes the pipe more brittle and less flexible. As a result lower elongation at break will be achieved both in machine and transverse direction. A typical picture of obtained spherulite size distribution across pipe wall thickness is shown in Figure 25. By reason of the relatively fast cooling the spherulites at the outer surface are much smaller than at the slower cooled pipe inside. In addition to this there is an amorphous skin at the very outer pipe surface. As a consequence of this, elongation at break of thick walled pipe is considerably lower than that of thin walled pipe and shows a gradient across the pipe wall becoming even lower towards the inner surface. If available, inside cooling of the pipe could help a lot to improve this situation and to get a more uniform spherulite morphology across the wall with an amorphous skin at the inner surface, too. A schematic drawing of internal cooling is given in Fig. 26.

- 37 -

Crystal rich region Bigger spherulites

More amorphous region Smaller spherulites

Fig. 25: Spherulite morphology across pipe wall

Cooling tube with spray holes (0,5 1 mm)

Extension tube

Air or water inlet

Vacuum tank Solidified melt (pipe) Sizing sleeve Insulation

Polymer melt

Fig. 26: Schematic drawing of inside cooling during pipe extrusion

- 38 -

3.4.4 Tooling for big pipe

Sizing sleeve C

D B

Vacuum tank E

Fig. 27: Schematic drawing of tooling for big PB-1 pipe

Tab. 7: Tooling dimension recommendations for big pipes

Tooling
Fresh pipe O.D. Fresh wall thickness Die I.D. Land length Pin O.D. Sizing sleeve I.D. Sizing sleeve length Line speed (m/min)

Diagram letter

110 x 10
112,7 11,0

125 x 11,4
128,1 12,6 153,7 140 126,0 132,6 200 1

160 x 14,6
164,0 16,2 203,3 180 167,7 169,7 250 0,6

A B C D E

134,7 120 110,6 116,7 180 1,3

Pipe dimensions according to ISO 15876-2 All dimensions in mm

- 39 -

3.5

Grinding and reprocessing

While Basell does not recommend any particular type or style of grinder or granulator for use with polybutene-1, some general information on this type of equipment can be provided. Since polybutene-1 is a relatively soft, low modulus material with a somewhat low softening point temperature, some precautions have to be considered. The material has a tendency to deform or smear instead of being cut in a clean uniform manner. This is partly due to heat generation in the grinder or granulator caused by friction of the grinder blades trying to cut soft material. Generally, the longer polybutene-1 is aged after processing and the cooler the material is kept during regrinding, the easier it will be to cut it. While most heavy duty grinders will be able to handle polybutene-1, the following recommendations may help to make grinders perform more efficiently. 1. 2. 3. The grinder should have sufficient motor power to handle the volume and heat generation during grinding the material without burning up or seizing the motor. The grinder cutter blades should be kept sharp at all times to reduce frictional heat generation. The mesh size of the sieves should be chosen accordingly in order to prevent large particles to pass through and assure that the regrind material is of uniform size that the extruder can reprocess. Sometimes the performance of the grinder can be improved by removing some of the cutter blades in order to reduce frictional heat generation during the grinding process. Grinders with cooling options for cutter blades (chilled water or forced air) can be a benefit. The main purpose of a polybutene-1 grinder is to produce a clean material of small uniform size (approx. 3 5 mm) that can be readily fed into the extruder and processed in a consistent manner. Particle size of regrind and size of virgin pellets should match in order to avoid melt inhomogeneity caused by inconsistent feeding. Check MFR and OIT of regrind. MFR of regrind should match that of virgin material as close as possible to avoid extrusion instabilities due to different melt viscosity. OIT should remain above specification limit in order to make sure that no significant loss of stabiliser has occurred. Careful drying of regrind and virgin material is recommended to avoid problems caused by moisture. During collection of scrap and regrinding precautions should be taken to avoid contamination.

4. 5. 6.

7.

8. 9.

10. Based on current experience and best estimates not more than 10 % regrind should be used with not less than 90 % virgin material in order to avoid too much loss of performance and oxidative stability. These percentages are based on current experience and best estimates without giving any guarantee or accepting any liability. The above mentioned considerations are valid only for pure polybutene-1 material. Regrinding of barrier pipe is not considered.

- 40 -

3.6 3.6.1

Troubleshooting General procedure

First of all existing outside diameter and wall thickness variations of pipe have to be quantified. Then the root cause for excessive dimensional variations should be determined. This evaluation process of the pipe extrusion line can be done by segregating the system in the following three sub-systems: 1. 2. 3. Extruder / Adapters / Screen pack changer / Melt pump / Die Vacuum control / Cooling system Puller / Cutter

The procedure should start with isolation and evaluation of the sub-system most suspected to contribute to the problem. All sensors, gauges, transducers and thermocouples of the three sub-systems involved have to be calibrated. Before taking samples of pipes of approx. 1m length the extruder should be allowed to stabilise for at least 45 min after final adjustment to achieve target dimensions for the particular pipe size. At least 50 pipe samples should be collected. Pipe dimensions should be measured on each individual sample at least 5 days after production and measuring on a particular series should be completed within three days. The outside diameter is measured using a periphery tape with an accuracy of 0,05 mm. The wall thickness is measured using a spring-loaded micrometer with rounded ball ends at a minimum distance of 20 mm from the end with an accuracy of 0,02 mm. At least eight separate measurements should be taken at 45 angles around the pipe wall in order to determine the minimum value. Using all individual dimensions collected, minimum, maximum, mean value and standard deviation of outside diameter and wall thickness should be calculated. In addition to this dimensional check of the finished pipe there are some more tooling evaluations to be considered: a. b. The shape of the water film of the spray ring should be conical with an angle of 40 50 and centered at the pipe. Between pre-sizing water chamber faceplate and pipe there should be a small gap of not more than 0,5 mm. Bigger gaps will result in increased loss of cooling water and inconsistent water supply while contact between pipe and faceplate will cause sticking of the pipe leading which can lead to pulsation. Inappropriate pre-sizing chamber length or wrong sizing sleeve diameter itself will result in mismatch of pipe outside diameter and sizing sleeve inside diameter giving rise to sticking of pipe at sizing sleeve entrance if pipe diameter is too large or loss of vacuum if pipe diameter is too small. Tooling dimensions like pre-sizing chamber faceplate and length as well as sizing sleeve diameter will depend strongly on processing parameters like melt temperature, cooling water temperature, vacuum, line speed, etc. Evaluation procedure 1:

c.

d.

3.6.1.1

The feed throat cooling system should be checked to assure that there are no obstructions and sufficient cooling is provided to the feed throat. Systems utilising melt pumps should optimise differential pressure between melt pump input (suction) pressure and output (discharge) pressure. The pressure difference between these two points is typically maintained at approx. 70 bar, the discharge pressure being higher than
- 41 -

the suction pressure. Differences in material and processing conditions can affect the optimum differential pressure setting. In systems without melt pump screen packs or barriers in die head or adapter are normally used to develop head pressure. In these systems typical pressures are between 70 140 bar. a. The output consistency of the extruder should be evaluated at the rate (extruder speed) desired for the particular operation. This procedure should determine the amount of material fluctuation attributable to the extruder: The extruder should be run using standard barrel and die temperature profile at the desired output rate until processing parameters reach equilibrium, usually 30 min, and the material is pumped on the floor. After 30 min of operation samples of material should be collected using a spatula to cut away material from the die at 15 second intervals. Sample collection can be terminated after 10 min or 40 samples. The individual samples are weighed with an accuracy of 1 g and minimum, maximum and fluctuations are calculated.

b.

c. d.

Optimisation of this system can be done by appropriate adjustment of the temperature profile of barrel and die. Melt output consistency (surging) should be less than 1% when using a melt pump and can increase up to 10 % without melt pump (depending on material, screw configuration and temperature profile. A re-evaluation may be required whenever the material, screw or rate of extrusion is changed. Normal wear of screw and barrel may also call for re-evaluation of the system in order to maintain low levels of surging. 3.6.1.2 Evaluation procedure 2:

This describes the evaluation procedure of the vacuum control and water cooling system for adequate pressure and temperature control and consistency. a. Each vacuum compartment should be isolated from the other compartments (if the vacuum sizing system is equipped with multiple sizing compartments). Front and back openings are to be sealed with tape or other sealant. A small hole should be punched in the tape or sealant and the system should be run at typical operating conditions for 15 min with vacuum, temperature and pressure recorded every 10 seconds. Steps a. and b. are to be repeated for all vacuum compartments. By plotting results against time the control consistency of this sub-system is obtained.

b.

c. d.

Optimisation of this system could require repair or replacement of pumps, pump seals, vacuum valves or gaskets. Typical vacuum, temperature and pressure control is 2% of set point. 3.6.1.3 a. b. c. Evaluation procedure 3:

This describes the evaluation procedure of the puller and cutter system consistency. The puller should be operated at typical or desired speed for 15 minutes. A sufficiently long pipe is to be inserted at the entrance of the puller. The pipe should be marked at exactly the same location at 10 seconds intervals. This must be done with a high degree of precision. Alternatively a pipe cutter can be used that automatically cuts at specific time intervals with the same precision. By measuring the distance of markings or actual length of pipes cut differences in length indicate puller consistency.
- 42 -

d.

Optimisation of this sub-system could require re-calibration of the puller motor control, physical inspection of the mechanical linkage system that conveys motor speed to puller belts or slipping of the pipe as it is being pulled through puller belts. Possibly puller belts need to be replaced or puller belt pressure has to be adjusted. If a pipe coiler is used in the system, it should be checked that the coiler is not pulling the pipe through the puller belts. Eventually coiler tension has to be reduced. Besides inconsistency in pulling this could cause dimensional variations of pipe during processing as well as deformation (ovality) of pipe after it exits the puller. 3.6.2 3.6.2.1

Miscellaneous problems Melt sticking at pre-sizing water chamber faceplate or sizing sleeve

Inconsistent extruder output can cause stick / slip appearance of material entering the presizing chamber or sizing sleeve because during the higher volume output phase the material will stick or build up at those points. Spray ring and pre-sizing chamber water temperature and pressure are not optimised (10 12 C temperature and 3 bar pressure) or water temperature or pressure shows too much fluctuation. Position of spray ring with respect to die and / or pre-sizing chamber not optimised. Diameter and / or entrance angles of pre-sizing chamber faceplate and / or sizing sleeve not optimised. Increase length of pre-sizing chamber to allow for more melt cooling before pipe is sized. Incorrect vacuum level. Difficulty increasing rate of extrusion

3.6.2.2

Extruder should be capable of delivering consistent output at desired rate while operating at approx. 80 % of maximum throughput. Puller should be capable of delivering consistent speed at desired rate while operating at 80 % of maximum rating. Downstream water cooling length (1 m of cooling bath incl. vacuum tank for every m/min of line speed) and downstream water cooling temperature (10 C 14 C) should be adequate (temperatures of 10 C 12 C are recommended at spray ring and pre-sizing water chamber). The pre-sizing water chamber length may need to be increased (in 5 mm increments) as well as inside diameters of pre-sizer faceplate ( in 0,5 mm increments) and sizing sleeve (in 0,2 mm increments). Longitudinal lines in pipe

3.6.2.3

Burrs or scars on die, pin or sizing sleeve. Deposit on die / pin surface or sizing sleeve. Spider design not optimised, i.e. spider legs too wide or too cold. Contamination in die / pin or spider area causing polymer to flow around contaminated particle resulting in flow line. Tooling not optimised (die / pin land length typically between 10 20 L / D). Polymer melt temperatures too low (typically between 180 C 200 C). Insufficient back pressure in die / spider area (typically between 110 140 bar).

- 43 -

3.6.2.4

Pipe is not round (ovality)

Puller / haul-off belts are too hard (typically sponge type or soft rubber of Shore A hardness - approximately 10). Compression of puller belts on pipe is too strong. Cross-section of puller belt or belt pads not V-shaped. Downstream water cooling length or cooling water temperature is not sufficient, i.e. cooling length too short or water temperature too high, to cool pipe adequately before entering the puller / haul-off belts so that puller belts can deform the pipe after processing. No contoured rollers or rollers of wrong shape; typically a new set corresponding to the pipe size produced should be used, i.e. half-circle shaped approx. 5 % larger than the fresh outside diameter of the pipe with a land length of about 10 mm. Rollers should be spaced at 0,5 m intervals starting from the sizing sleeve along the entire length of the vacuum and cooling bath. Sizing sleeve or vacuum tank gaskets are not of correct size. Pipe coiling tension is too high. Poor appearance of pipe surface (outside and inside)

3.6.2.5

Burrs or scars on inside or outside of die / pin or sizing sleeve. Contamination of material, e.g. size, composition and cleanliness of regrind. Check proper shape of spray ring pattern and water temperature (10 C 12 C). Check screen pack integrity, cleanliness and mesh size (typically approx. 80 100 mesh). Moisture in extruder (from feed throat cooling condensation or on pellets. Temperature profile of extruder and die can be increased in order to get more shiny pipe. Elongation at break values below minimum

3.6.2.6

Extrusion rate too high. Too strong extension of pipe or draw-down ratio too high. Polymer melt temperature too low (typically between 180 C 200 C). MFR of polymer too low (can be compensated by higher melt temperature. Check proper shape of spray ring pattern and water temperature (10 C 12 C). The pre-sizing water chamber length may need to be increased (in 5 mm increments) as well as inside diameters of pre-sizer faceplate ( in 0,5 mm increments) and sizing sleeve (in 0,2 mm increments). Vacuum level too high (typically 40 80 mbar). Processing water quality, pressure and temperature

3.6.2.7

Dirty, contaminated (high mineral content) water could clog lines, pumps and spray ring and thus produce erratic flow. Water system treatments like rust inhibitors, pump lubricants, etc. that come into contact with pipe during processing are not recommended. Water pressure and volume (flow) should be adequate and consistent (particularly at spray ring and vacuum tanks) in order to maintain effective and uniform cooling and appropriate vacuum sizing.

- 44 -

3.6.3 3.6.3.1

Lot to lot variability in polybutene-1 pipe production Symptoms

Pipe outside diameter (O.D.) varies from original target or fluctuates during production. Pipe wall thickness varies from original target or fluctuates during production. Melt pressure or temperature at inlet to die varies upon feeding of new lot of material. Possible causes Extrusion process

3.6.3.2

Process water temperature or pressure changes or fluctuates during processing (seasonal changes or poor control). Material feed temperature or pressure changes or fluctuates during processing (seasonal changes or inconsistent control, i.e. cold / hot material from warehouse, improper drying, partial obstructions in feed throat, throat cooling temperature changes, condensation of moisture in feed section, etc.). Extrusion temperature profile or melt temperature varies from original setting during production (heater bands or controllers malfunction, inaccurate or malfunctioning temperature sensors, shear temperature changes due to screw or barrel wear, etc.). Extruder speed changes due to inconsistent motor speed control. Line speed (extrusion rate) varies during production (haul-off control inconsistent, haul-off belts worn, hardened or inconsistent contact / compression on pipe, etc.). Possible causes Raw material

3.6.3.3

MFR (melt viscosity) of material changes between lots Pellet density, shape or size changes between lots Pellet count (volume) of material changes between lots Variation of moisture/volatile content between lots Bulk density of material changes between lots Homogeneity of additive distribution changes between lots

Note: Basell PB-1 pipe grades are produced on a state-of-the-art polimerisation plant to a tight specification under a system certified to EN ISO 9002. The current product specification includes upper and lower limits on MFR, pellet size, moisture/volatile content and other important material properties.

- 45 -

3.6.4 PB-1 pipe extrusion troubleshooting cross reference Potential problem 1. Extruder surging Possible cause Wrong temperature profile Extruder speed (RPM) too high Insufficient back pressure 2. Poor vacuum control Extruder surging Stick-slip in sizing sleeve Poor water flow through vacuum tank Wrong size of vacuum tank gaskets 3. Wrong pipe O.D. Wrong tooling Wrong vacuum Wrong pre-sizing water chamber dimensions Wrong spray ring position Wrong melt temperature Wrong line speed 4. Pipe bambooing Extruder surging Variable vacuum Clogged vent port in pin Wrong pre-sizing water chamber dimensions Wrong pre-sizing water chamber faceplate angle Wrong melt temperature Wrong size of cooling bath gaskets Wrong spray ring position Wrong spray ring pattern Die swell too high Sizing sleeve too small 5. Wrong wall thickness Wrong tooling Wrong draw down ratio Wrong extruder speed Wrong puller speed 6. Poor pipe concentricity Poor die / pin adjustment Poor die design Wrong puller speed

- 46 -

7.

Oval pipe

Non-contoured rollers Puller compression / tension too high Coiler tension too high Wrong size of cooling bath gaskets

8.

Flow lines

Burrs or scars in pin / die, pre-sizer faceplate or sizing sleeve Melt temperature too low or wrong die temperature profile (spider lines) Land length too short Contamination of material Insufficient back pressure in die

9.

Crease lines

Die gap too large (too much material) Vacuum too low (pipe collapse)

10. Poor surface

Burrs or scars in pin / die, pre-sizer faceplate or sizing sleeve Wrong spray ring pattern or water pressure Volatiles (moisture) Dirty product Dirt in screen packs Melt temperature or line speed too low or too high (melt fracture)

11. Water spots

Wrong spray ring pattern or water pressure Wrong position or water pressure of spray dies in vacuum tank

12. Voids in pipe

Voids / volatiles in pellets Surface moisture (condensation of water) on pellets

13. Melt sagging

Melt temperature too high MFR too high Wrong tooling Tooling in wrong position

- 47 -

4.

Annex: List of standards relevant for PB-1 pipes

Characterisation of material ISO 1133 ISO 1183 ISO 8986 Plastics - Determination of the melt mass-flow rate (MFR) and the melt volume-flow rate (MVR) of thermoplastics Plastics Determination of density of non-cellular plastics Plastics - Polybutene (PB) moulding and extrusion materials - Part 1: Designation system and basis for specification; Part 2: preparation of test specimens and determination of properties Plastics - Differential scanning calorimetry (DSC) - Part 6: determination of oxidation induction time Plastics determination of environmental stress cracking (ESC) of polyethylene (PE) Full-notch creep test (FNCT)

ISO 11357-6 ISO FDIS 16770

Pipe related standards ISO ISO 161 ISO 497 ISO 1167 ISO CD 2505 ISO 3126 ISO 4065 ISO 4433 ISO 6259 ISO 6964 Thermoplastics pipes for the conveyance of fluids Nominal outside diameter and nominal pressure Guide to the choice of series of preferred numbers and of series containing more rounded values of preferred numbers Thermoplastics pipes for the conveyance of fluids - Resistance to internal pressure - Test method Thermoplastics pipes - Longitudinal reversion - Test methods and parameters Plastics piping systems Plastics piping components Measurement and determination of dimensions Thermoplastics pipes Table of wall thickness Thermoplastics pipes Resistance against chemical fluids Classification Thermoplastics pipes - Determination of tensile properties Polyolefin pipes and fittings Determination of carbon black content by means of pyrolytic degradation Test method and required values Plastics pipes and fittings - Opacity - Test method Plastics piping systems for the transport of water intended for human consumption - Migration assessment - Determination of migration values of plastics pipes and fittings and their joints
- 48 -

ISO CD 7686 ISO 8795

ISO 9080

Plastics piping and ducting systems - Determination of long-term hydrostatic strength of thermoplastics materials in pipe form by extrapolation Thermoplastic pipes Determination of creep behaviour Thermoplastic pipes Determination of ring stiffness Plastics pipes and fittings - Combined chemical-resistance classification table Thermoplastics pipes and fittings for hot and cold water systems Thermoplastics pipes for the conveyance of fluids - Dimensions and tolerances Thermoplastics materials for pipes and fittings for pressure applications - Classification and designation - Overall service (design) coefficient Polybutene (PB) pipes - Effect of time and temperature on the expected strength Thermoplastic pipes for the transport of fluids Determination of resistance against rapid crack propagation Laboratory test at small pipe samples (S4) Thermoplastic pipes for the transport of fluids Determination of resistance against rapid crack propagation Practical test (FST) Thermoplastic pipes for the transport of fluids Determination of resistance against crack propagation Test method for slow crack propagation of notched pipes (notch test) Plastics pipes for the conveyance of fluids under pressure - Miner's rule - Calculation method for cumulative damage Plastics piping systems for industrial applications - Polybutene (PB), polyethylene (PE), polypropylene (PP) - Specifications for components and the system Plastics piping systems for hot and cold water installations Polybutylene (PB) Part 1 - 7 Plastics piping and ducting systems - Method for exposure to direct (natural) weathering Method for the assessment of pigment or carbon black dispersion in polyolefin pipes, fittings and compounds

ISO 9967 ISO 9969 ISO/TR 10358 ISO 10508 ISO 11922 ISO 12162

ISO 12230 ISO 13477

ISO 13478 ISO 13479

ISO 13760 ISO 15494

ISO FDIS 15876-1 - 7 (formerly known as EN 12319) ISO DIS 16871 ISO FDIS 18553

- 49 -

CEN EN 496 EN 578 EN 712 Plastics piping and ducting systems - Plastics pipes and fittings Measurement of dimensions and visual inspection of surfaces Plastics piping systems - Plastics pipes and fittings - Determination of the opacity Plastics piping systems - End-load bearing mechanical joints between pressure pipes and fittings - Test method for resistance to pull-out under constant longitudinal force Plastics piping systems - Mechanical joints between fittings and polyolefin pressure pipes - Test method for leaktightness under internal pressure of assemblies subjected to bending Plastics piping and ducting systems - Thermoplastics pipes Determination of the longitudinal reversion Specification for installations inside buildings conveying water for human consumption Plastics piping systems for the transport of water intended for human consumption - Migration assessment - Guidance on the interpretation of laboratory derived migration value Plastics piping systems - Thermoplastics pipes - Determination of resistance to internal pressure at constant temperature Plastics piping and ducting systems - Plastics pipes and fittings Method for exposure to direct (natural) weathering Floor heating - Systems and components - Part 4: Installation Influence of organic materials on water intended for human consumption - Determination of odour and flavour of water in piping systems Plastics piping systems - Injection-moulded thermoplastics fittings, valves and ancillary equipment - Determination of long-term hydrostatic strength of thermoplastics materials used for injectionmoulded piping components Plastics piping systems - Thermoplastics pipes and fittings for hot and cold water - Method of test for the resistance of piping systems to thermal cycling Plastics piping systems for hot and cold water - Method of test for leaktightness under vacuum Plastics piping systems - Thermoplastics pipes and fittings for hot and cold water - Method of test for resistance of piping systems under pressure cycling

EN 713

EN 743 EN 806 ENV 852

EN 921 EN 1056 EN 1264-4 EN 1420

EN 12107

EN 12293

EN 12294 EN 12295

- 50 -

EN 12873

Influence of materials on water intended for human consumption Influence due to migration

DIN and other German standards and guidelines DIN 4102-1 DIN 4726 DIN 4727 DIN 16831-1 - 7 DIN 16887 DIN 16888-1 DIN 16889-1 DIN 16968 DIN 16969 DVGW W 270 Brandverhalten von Baustoffen und Bauteilen Teil 1: Baustoffe Begriffe, Anforderungen und Prfungen Warmwasser-Fubodenheizungen und Heizkrperanbindungen Rohrleitungen aus Kunstsstoffen Rohrleitungen aus Polybuten fr Warmwasser-Fubodenheizungen - Besondere Anforderungen und Prfung Rohrverbindungen und Formstcke fr Druckrohrleitungen aus Polybuten (PB) - PB 125 - Teile 1 - 7 Prfung von Rohren aus thermoplastischen Kunststoffen; Bestimmung der Zeitstand-Innendruckverhaltnis Bewertung der chemischen Widerstandsfhigkeit von Rohren aus Thermoplasten; Rohre aus Polyolefinen Bestimmung der chemischen Resistenzfaktoren an Rohren aus Thermoplasten; Rohre aus Polyolefinen Rohre aus Polybuten (PB); Allgemeine Anforderungen und Prfung Rohre aus Polybuten (PB) - PB 125 - Mae Technische Regel - Arbeitsblatt Vermehrung von Mikroorganismen auf Materialien fr den Trinkwasserbereich Prfung und Bewertung Technische Regel - Arbeitsblatt - Rohrverbinder und Rohrverbindungen Verbundrohre in der Trinkwasser-Installation; Anforderungen und Prfungen Technische Regel - Arbeitsblatt - Kunststoffrohre in der Trinkwasser-Installation; Anforderungen und Prfungen

DVGW W 534 DVGW W 542 DVGW W544 ASTM D 2581 Australia / New Zealand AS/NZS 2642.1-3 AS/NZS 3500

Standard specification for polybuylene (PB) plastics moulding and extrusion materials

Polybutylene pipe systems - Polybutylene (PB) pipe for hot and cold water applications Part 1 - 3 National plumbing and drainage code

- 51 -

AS/NZS 4020 Japan JIS K 6792 Korea KS M3363 Phillipines PNS 152 Spain UNE 53415-1 - 4 Thailand TIS 910-2532 UK BS 6920

Testing of products for use in contact with drinking water

Polybutene (PB) pipes for water works

Polybutylene (PB) Pipes

Specification for Polybutylene (PB) Pipes for Potable Water Supply

Plastic piping systems for hot and cold water installations Polybutylene (PB) Part 1 - 4

Polybutylene (PB) pipe and tubing for drinking water services

Suitability of non-metallic products for use in contact with water intended for human consumption with regard to their effect on the quality of the water

- 52 -