1

"TECHNICAL PERFORMANCE REQUIREMENTS OF BLACK PRESSURE PIPES -

THE CRITICAL ROLE OF SPECIALTY P-TYPE CARBON BLACKS IN
COMPOUNDS AND MASTERBATCHES."

ABSTRACT
Carbon Black is an important constituent in polyethylene compounds used in the
manufacture of pressure pipes for the distribution of potable water and gas. The use
of specialty P-Type carbon blacks provides for the most cost effective means of
achieving the necessary level of UV stabilisation without compromising the ultimate
performance requirements of these pressure pipes.
This paper will review the critical properties of carbon blacks used in the manufacture
of pressure pipe masterbatches and compounds and how a range of specialty high-
performance carbon blacks, widely referred to as "P-Type" carbon blacks have been
developed and commercialised by Cabot to meet the ever-increasing long term
performance and reliability requirements of pressure pipes.
Additionally, the use of both masterbatches and direct carbon black addition in the
manufacture of compounds will be critically reviewed.

CARBON BLACK IN PRESSURE PIPE COMPOUNDS

Carbon black, a fine particulate filler is widely used in the production of
masterbatches and compounds used in the manufacture of polyethylene pressure
pipes. The reason for its widespread usage is because carbon black provides for the
most cost efficient means of providing the required level of UV weathering protection
to polyethylene.

There are many types of carbon black, produced by a variety of manufacturing

methods, resulting in large differences in their morphologies, physical properties and
degree of chemical cleanliness and purity. This means that the ultimate performance
of polyethylene compounds used in the manufacture of pressure pipes can vary
considerably depending on the type of carbon black used. Some will have excellent
performance, others not so.

Over the past 40 years or so, extensive industrial experience has shown that the
selection of the most suitable types of carbon most for use in black pressure pipes
can be broadly specified in terms of five key performance criteria, namely;
• Particle size,
• Microscopic dispersion,
• Compound moisture absorption,
• Chemical impurities,
• Dispersability.

These parameters represent the key performance indicators, although there are
secondary performance parameters which, depending on the method of pipe making
require consideration for optimal results. Viscosity of the masterbatch and of the
compound would be one such secondary performance parameter, colour strength
would be another.

The various regulatory bodies, standards institutions and water and gas utilities
companies and service providers have formulated a set of performance requirements
for all types of pressure pipe including PE63, PE80 or PE100.
These performance requirements are based on the above mentioned five key
performance criteria.

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These requirements in simplified format can be summarised in the table below:

BLACK COMPOUND REQUIREMENTS EN12201, NF114 & EN13244

PROPERTY: LIMIT: TEST METHOD:

Manufacturers method and
Carbon Black Particle Size <=25ηm.
ASTM D-3849
Carbon Black Content 2.0 – 2.6% ISO 6964

Carbon Black Dispersion <=3 ISO/FDIS 18553

Density >=930Kg.m-3 ISO 1183

Melt Flow Rate 190°C/5Kg. 0.2 – 1.1g/10min ISO 1133

Oxidative Induction Time
>20 minutes EN 728
200°C.
Water Content <=300ppm. EN 12118

Volatiles <=350GJm-2 EN 12099

UV Weathering Exposure >=3.5GJm-2 ISO 1056 and ISO 4607

On pipes:Tensile, pressure and
Mechanical Properties
crack propagation.
Drinking Water Quality National Regulations.

A full set of these requirements is tabulated in APPENDIX 1

Cabot Specialty P-Type Carbon Blacks for Pressure Pipe Usage

For more than 30 years Cabot has been working closely with polymer producers,
compound makers and standards committees in the development and
commercialisation of specialty carbon blacks developed specifically for use in
polyethylene pressure pipe applications.
In the early years, Cabot launched VULCAN ® P which quickly became an industry
standard. Subsequently two further grades were introduced; ELFTEX ® TP and
ELFTEX ® 254. ELFTEX ® TP has now replaced VULCAN ® P as the industry
standard.
Recently a new specialty P-type carbon black has been successfully commercialised;
ELFTEX ® P100 offering improvements in compound moisture absorption ("CMA")
and dispersability.

These specialty P-type carbon blacks comply with the following specifications:

PROPERTY TEST METHOD LIMIT

Total Ash ASTM D-1506 < 0.10%
Toluene Extract ASTM D-1618 < 0.03%
Total Sulfur CTM 15.71 < 0.1%
Particle Size ASTM D-3849 < 25 nm
325 Mesh Residue ASTM D-1514 < 20 ppm

These specifications are stipulated for pressure pipe applications to satisfy the
various industry standards across the world.

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The Star Diagram is a visual and useful means of comparing differing types of
carbon black for their relative suitability for use in pressure pipe applications.
The star diagram shown below compares the performance of Cabot specialty P-type
carbon blacks together with a typical conventional or general purpose grade of
carbon black commonly used for non-critical performance applications.

Particle Size

Compound Moisture
Ease of Dispersion
Absorption

Microscopic Dispersion Chemical Impurities

Elftex P100 Elftex TP Conventional Black

Details on the Five Key Performance Criteria

Particle Size
The efficiency of carbon black as a UV absorber primarily depends on the primary
particle size. At a constant loading in polyethylene, carbon black aggregates, based
on fine primary particles will present a proportionately larger surface area to incident
UV - and hence a superior UV absorbing efficiency - than that of a coarser grade of
carbon black.

Primary
particle Primary particle size
(typically 15 to 60 nm)

Carbon black aggregate

Figure 1 shows that P-type blacks widely improve mechanical properties and
weathering performance versus conventional carbon black.
The appropriate loading level depends on the part thickness, exposure conditions and
type of carbon black. Usual loading to impart optimum UV protection vary between
2 and 3% (it should be noted that these carbon black levels correspond to 5 to 7.5%
masterbatch, as typical carbon black loading is about 40%).

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 Figure 1. Effect of carbon black primary particle size on UV weathering
performance

Accelerated Weathering - ATLAS*

55 µm LDPE films with 2.5% CB
125
Less than 25 nm Particle
Retained Elongation at Break, %

60 nm Particle
100

75

50

25

0
0 250 500 750 1000 1250
Exposure time (hours)
Fig.2 shows that P-type carbon blacks efficiently protect pressure pipes against UV
induced degradation. Most of the national and international industry standards for
pressure pipes, such as BS6730, NFT54-072 and ISO/FDIS8779, recognise the
importance of particle size with respect to UV stability. For that purpose, they specify
a carbon black particle size of below 25 nm with a carbon black concentration of 2.0-
2.5 weight%.

Fig. 2 – Effect of loading levels on ultraviolet light absorption

600

< 25 nm particle size

500
60 nm particle size
(Kilo Abs.Units/meter)
Absorption Coefficient

400

300

200

100

0
1 1.25 1.5 1.75 2 2.25 2.5 2.75 3 3.25 3.5

% Carbon Black in LDPE films

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Microscopic Dispersion
The most commonly used Microscopic Dispersion test is the so-called "press-out
method", because it involves examination of thin hot-pressed compound samples
under an optical microscope using transmitted light. A rating or grade is defined
based on the size and number of undispersed carbon black agglomerates.

The presence of undispersed carbon black agglomerates in the pipe wall can lead to
premature failure of the pressure pipe. Apart from the high cost of replacement and
repair, a premature cracking of a gas conduit under pressure is also an obvious
safety hazard.
The surface smoothness of the inner and outer wall of the pipe is also a very
important performance criteria, both for aesthetics and for fluid flow properties.
The majority of the national and international industry standards for pressure pipes
recognise this importance and specify a compound microscopic dispersion rating of
<= 3 (according ISO/FDIS 18553).

6.
Microscopic Dispersion

5.

4.

3.

2.

1.

0.
Elftex ® P100
Elftex ® 254

Competitive

Conventional
Elftex ® TP

Black

Black

The level of compound microscopic dispersion that can be achieved using

ELFTEX ® 100 is excellent. ELFTEX ® TP shows a slightly lower level of compound
microscopic dispersion than ELFTEX ® P100, which is significantly superior to a
conventional black.

Chemical Cleanliness
There are very strict requirements on the chemical cleanliness of compounds that are
used to make pressure pipe for potable water. These requirements for potable water
pressure pipes have been defined according to the industry knowledge of the factors
that affect the drinking water taste and odour, well known in the industry as
‘organoleptic’ properties. These organoleptic requirements have been further
translated into low sulphur impurity, ash, and toluene extract requirements by these
industry regulatory agencies.

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 12000

Chemical Cleanliness, ppm

10000

8000

6000

4000

2000

0
Toluene Sulfur Ash

Elftex P100 Elftex TP Conventional Black

P-Type CB are especially characterised by very low contents of both sulphur and
toluene extract. As shown above ELFTEX ® P100 and ELFTEX ® TP have very small
amounts of sulphur impurities, ash, and toluene extract levels compared to a
conventional black.

Compound Moisture Absorption

0.80
Compound Moisture Absorption, %

0.70

0.60

0.50

0.40

0.30

0.20

0.10

0.00
Elftex P100 Elftex TP Conventional
Black

Compounds containing carbon black usually absorb some moisture upon exposure to
air. This moisture absorption, or compound moisture absorption (CMA) as it is known
in the plastics industry can create processing problems (e.g. die drool), surface
defects or internal cavities in the finished part. This is due to the migration of
entrapped moisture through the compound during the extrusion process in cases
where the compound is not sufficiently dried. The high purity of these specialty
P-type Blacks makes it possible to achieve low levels of CMA in compounds, which in
turn makes the need for a thorough pre-drying of the compound prior to pipe
extrusion both less critical and energy intensive.

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 Dispersability
Carbon black dispersability indicates the ease with which the P-type black can be
wetted with the resin and subsequently de-agglomerated. This performance measure
is dependent primarily on the fundamental characteristics of the carbon black.
Considering the physics of nano particles, it represents the Van der Waals attractive
force needed to separate the agglomerates into discrete carbon black aggregates.
This measure is independent of the polymeric system used to disperse the P-type
black. It is also an indicator of the relative yields that can be achieved on the
compounding equipment with the different carbon black grades. ELFTEX ® P100
has a superior dispersability than ELFTEX ® TP, which is itself is greatly superior to
the dispersability of a conventional black.

Poor Dispersability Excellent Dispersability

(partial de-agglomeration) (full de-agglomeration)

cross section cross section

The photomicrographs above illustrate how dispersability of the carbon black affects
the de-agglomeration and polymer wetting. It is easier to achieve full de-
agglomeration and wetting with specialty P-type blacks.

PIPE COMPOUND MANUFACTURE

Two methods are used for the production of black pressure pipe compound;
• Compounding using direct addition of carbon black,
• Compounding using a ready-formulated masterbatch

PIPE COMPOUND MANUFACTURING FLOW CHART

IN HOUSE

POLYMER CRUMB OR PELLET BLACK MASTERBATCH

94% 6%

COMPOUNDING

I. Represent 80% of all compounds. 100%

II. Line capacity from 1mt up to +30 mt/hr

Each method has its advantages and disadvantages, regarding capital outlay,
manufacturing costs, productivity BLACK
and compound quality and performance.
PIPE COMPOUND

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Each method has its advantages and disadvantages, regarding capital outley,
manufacturing costs, productivity and compound quality and performance.
The masterbatch route offers greater flexibility of manufacture; Can be both "in-line"
and "off-line", using either polymer reactor crumb or polymer pellets, whereas the
direct addition of carbon black route is nearly always "in-line" involving the use of
HPDE reactor crumb.
In some cases, where the compounder uses polymer reactor crumb a micronised
masterbatch is preferred. Having both materials in the same form offers benefits in
the form of better & more consistent compound dispersion quality and output.

A comparison of the two methods is shown below.

Installation & Equipment Requirements.

Direct Carbon Black Addition: Use of Masterbatch:

Bulk silo.
Bulk silo conveyencing and piping.
Dust separator for bulk silo.
Pre-Blender. (optional)
Dust separator for pre-blender.
(optional)
Additives dosing and metering
equipment. (optional)
Compounding extruder materials feed
system.
Also required but can be smaller and
therefore lower cost.
Also required but can be simplified and
therefore lower cost.
Not required.
Also optional but not required if fully
formulated masterbatch is used.
Not required.
Also optional but not required if a fully
formulated masterbatch is used.
Also required but simpler and
therefore lower cost.

Compounding and Compound Properties.

The use of masterbatch compared to the use of direct addition of carbon black shows
the following benefits:
• Greater production flexibility, in terms of campaign size, start-up, shut-down and
shorter, simplified clean-downs.
• Other coloured compounds, such as yellow/orange gas pipe and blue/purple
potable water pipe compounds can readily be produced on the same
compounding equipment. Clean downs and equipment purging is both easier and
shorter- Remember carbon black is a fine powder and even a few ppm. can pose
a serious contamination risk.
• Compounding can be optimised using less shear and lower specific energy input,
resulting in better control and consistency in physical and organoleptic properties.
This results in less polymer chain scission, degradation and a reduction in taint-
odour related problems together with improvements in stress crack resistance.

Financial - Capital investment Costs.

Direct addition of carbon black has higher costs associated with:
• Installation of dust separators on both the bulk silo and pre-blender.
• Probable need for additives dosing equipment.
• Higher maintenance costs.
• Higher costs for scrap and waste disposal.
• Additional and more extensive cleandown times resulting in lower productivity
and service income.

• The one positive for using direct addition of carbon black is lower raw materials
costs, essentially meaning the difference between the relative price of carbon
black and masterbatch.
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Safety, Health & Environmental Issues.
The IARC Hazard Rating of carbon black was recently changed from Class 3 to 2B.
Likewise the Airborne Dust Exposure Rating changed from 3mg per cubic metre to
1mg per cubic metre.

Thus adopting the masterbatch route has distinct benefits:

• Safer working environment for operators and technicians.
• No risk of environmental pollution and spills caused by carbon black.

Compound Quality & Consistency.

Using the masterbatch compounding route offers important advantages to the
pressure pipe compound maker.
• The carbon black is predispersed in a suitable polymer carrier.
• The masterbatch supplier assumes the responsibility of providing a masterbatch
suitable for use in this compounding application, both in terms of the
concentration and type of carbon black [a specialty P-type], the dispersion
quality, rheology and viscosity.
• The masterbatch used can be fully formulated to include all thermal stabilisers
[antioxidants], metal scavengers and if required, processing aids.
• A reputable supplier of masterbatch will offer a warranty related to the quality &
consistency of the masterbatch supplied. This in turn means that the compound
maker can be assured of compound uniformity and consistency leading to a
reduction in QA testing and test equipment costs.

MASTERBATCH CHARACTERISTICS AND PROPERTIES

Polymer carrier. This can be LDPE, LLDPE or HPDE, although the use of LDPE is
nowadays limited to production of PE63 & some PE80 potable water pipe compounds.
LLDPE is used for both PE80 & PE100. The use of HDPE as a carrier is limited to
PE100 compound production.

Type of carbon black. To comply with the requirements laid down in the Standards
and Norms, only specialty P-type carbon blacks should be used.

Concentration of carbon black. This can vary between 35% to 45% by weight but
40% is the most common.

Dispersion quality. This should be at least in compliance with the Standards &
Norms and should ideally be better. An average ISO Rating of 3 is considered
acceptable.

Rheology and Melt Viscosity. This needs to be balanced to provide for a

masterbatch which has sufficient rheology so as not to have a negative impact on
the compound physical properties, yet is not so viscous as to prove difficult to
homogenise and dilute easily in the natural HDPE.
As carbon black has a reinforcing, viscosifying effect in polymer, it is not practical to
use a PE80 or PE100 natural HDPE as the base carrier for the masterbatch and an
HDPE with a higher Melt Flow Rate is invariably used.

Addition of thermal stabilisers and other functional additives. This is optional,

however it is commonplace for pressure pipe compound makers to specify a black
masterbatch incorporating antioxidants [primary and secondary/ phenolics and
phosphite]. Sometimes the inclusion of metal scavengers and process aids is also
specified.

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PRESSURE PIPE INDUSTRY –TRENDS AND CHALLENGES

Trends.
• The number of compound producers is growing, increasing the level of
competition which in turn puts pressure on suppliers to better manage costs and
try to differentiate themselves by providing better performing pressure pipe
compounds.
• Less use of direct carbon black addition during compounding; Some established
producers have or are switching to the use of fully formulated masterbatches.
Switching to masterbatch use enables producers to more fully utilise existing
equipment and realise significant gains in productivity an compound quality
without the need for further capital investment.
• Increasing use of micronised masterbatch to further improve compound quality
and consistency.

Challenges.
From the pipes utilities and service providers.
• Ongoing demands for improvements in organoleptic properties, ESCR
performance and stress crack resistance. The goal here being to further improve
the reliability of infrastructure and ultimately extend the working lifetime of
pressure pipes.

From the compound manufactures.

• Ongoing requirement for productivity improvements and higher quality more
consistent compounds.

It is demonstrated that these improvements can be realised by the selection of

specialty P-type carbon blacks preferably used in conjunction with the masterbatch
compounding route, in either pellet or micronised forms.

SUMMARY
Polyethylene pressure pipes and fittings are highly engineered components designed
to satisfy the stringent requirements of the potable water and gas pipe utilities
companies and service providers.
There are many differing grades and families of carbon black each with vastly
differing properties in terms of morphology, chemical cleanliness and purity.
It is shown that the selection of the appropriate grade or family of carbon black is
critical in the manufacture of black compounds for pressure pipes.
For this reason the various industry standards committees and regulatory bodies
have put in place detailed specifications defining both the morphological and
chemical cleanliness of carbon blacks to be use in these applications.
In response to this Specialty P-type carbon blacks have been developed and
successfully commercialised to meet the requirements of the pressure pipes industry.
- These requirements can be satisfied 100% of the time by the use of specialty P-
type carbon blacks such as ELFTEX ® P100 and ELFTEX ® TP.

Furthermore, it is shown that for optimum pipe performance only the compound
route should be followed and that the use of a suitable masterbatch during the
compound making process can offer distinct advantages in terms of compound
quality and consistency.

The Author.
Chris Sidebottom is presently Regional Marketing and Sales Manager for Polymer
Producers Pacific-Asia. He has over 31 years experience in the plastics processing
industry; all served with Cabot in various business, market development and
technical roles. He gained his BSc. in Physics at The University of Manchester,
England.
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 APPENDIX 1. TABLE OF NF/EN/ISO NFT NORMS - REQUIREMENTS FOR
PRESSURE PIPES

Black Polyethylene Compound Requirements.

Norm : NF114 (review15, Jan01) prEN 12201-1 ISO4437

Plastics piping system for water
short title : supply (PE) Buried PE pipes for …gaseous
Limit Test Method Limit Test Method Limit Test Method
CB particle size − - -
CB content 2.0-2.6 % NFT51-140 2.0-2.5% ISO6964 2.0-2.5% ISO6964
CB dispersion ≤3 NFT51-142 ≤3 ISO11420 ≤3 ISO11420
ISO1872/1, ≥ 930 kg/m³ (base
Density ≥ 925 kg/m³ NFT51-063 ≥ 930 kg/m³ ISO1183 (D) polymer) ISO1183, 1872/1
value measured
±20% (of
MFI 190°C on base ISO1133 (5kg for ISO1133 MFR: ±20% (of ISO1133
nominated value)
compound ±10% PE100,80,63) nominated value)
OIT 200°C > 20min EN728 ≥ 20min EN728 > 20min ISO/TR10837
Water content − ≤ 300mg/kg EN12118 ≤ 300mg/kg ASTM D-4019
Volatiles − ≤ 350mg/kg EN12099 ≤ 350mg/kg annex A
Weathering − -
on pipes : tensile, pressure, crack on pipes : crack on pipes : crack
Mechanical tests propagation,… propagation. propagation
Water quality − -
"Buried PE pipes for the supply of
NF114 p.21 table2:"Specification "Plastics piping system for water gaseous fuels -spec." p.6
Title :
for Pipes" supply -(PE) - Part 1 : General" table1:"Characteristics of the PE
compound"

norm : NF T 54-065 ISO/FDIS 8779

short title : PE pipes for …gaseous combustible PE pipes for irrigation laterals
Limit Test Method Limit Test Method
CB particle size - 0.010µm - 0.025µm
CB content 2.0-2.6% NFT51-140 2.25 ± 0.25% ISO6964
CB dispersion ≤3 NFT51-142 ≤3 ISO11420
Density ≥ 925 kg/m³ NFT51-063, ISO1872/1
±20% (of MFR: ±30% (of
MFI 190°C NFT51-016
nominated value) nominated value) ISO1133
OIT 200°C > 20min NFT54-075
Water content −
Volatiles ≤ 350mg/kg annex D
Weathering -
Mechanical tests -
Water quality -
"PE pipes for gaseous combustible
distribution networks -spec." p.6
Title : "PE pipes for irrigation laterals -spec." p.2
table1:"Specification for the base
composition"

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APPENDIX 1 Continued.

Carbon Black Requirements.

BS6730 NFT54-072
Black PE pipes …. for potable water Tubes en PE "5"
Cabot definition of "P-type" CB
325 mesh residue (ppm) < 20 − −
Ash (%) < 0.1 − −
Total sulphur (%) < 0.1 − −
Particle size (nm) < 25 Particle size (nm)* : 0.010-0.025µm Particle size (nm) : 0.010-0.025µm
Toluene extract (%) < 0.03 Toluene extract : 0.10% max Toluene extract : 0.10% max
Extension coefficient : 0.10 max Density : 1500-2000 kg/m³
Volatil matter : 2% max Volatil matter : 9% max
* or Iodine number : ≥110mg iodine/gr.CB
"Black polyethylene pipes up to nominal size
"Tubes en Polyéthylène "5" (5MPa) -
63 for above ground use for cold potable water
Spécifications"
-Table 4"

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APPENDIX. 2

THE PRESSURE PIPE COMPOUND VALUE CHAIN

INDUSTRY
REQUIREMENTS

1 PIGMENT Carbon Black Particle Size

<=25mm
80% 20%

MASTERBATCH Microscopic
2 PRODUCER Dispersion

CEN/TS155
3 COMPOUNDER ISO/DIS4427
POLYMER PRODUCER ISO/CD4437

4 TRANSFORMER LNE/BENOR
KIWA/AENOR

5 INSTALLER LNE/BENOR
KIWA/AENOR

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