Qazi HAA, J Environ Sci Curr Res 2019, 2: 008

DOI: 10.24966/ESCR-5020/100008

HSOA Journal of
Environmental Science: Current Research
Research Article

Study of Qualification of Coating hesion strength test, impact test and cathodic disbondment test. All
testing were evaluated to check compliance against the standard
Procedure Specifications as Per DIN 30670 requirements and coating procedure specifications.
Keywords: Cathodic disbondment test; Chloride content test; Coat-
Din 30670 for 3lpe Coating of 8 ing procedure qualification; Coating procedure specifications; Corro-
sion protection; Dew point; DIN german institute for standardization;
Inch Diameter Erw Pipe Elongation test; Holiday test; Impact test; Indentation Test; Peel Ad-
hesion; Surface preparation; Thickness measurement; Three layer
polyethylene coating (3LPE).
Hafiz Abdul Ahad Qazi*

Department of Quality Control Health and Safety Environment Engineer,

Kotri, Pakistan Introduction
Since the advancements in piping technology for oil and gas trans-
Abstract portation, three layer polyethylene coating have been in use for not
only giving corrosion protection to the pipelines but also enhancing
In present study qualification of 3 layer polyethylene coating pro- the service life of it. 3LPE (Three Layer Polyethylene) systems con-
cedure is discussed which is adopted for the corrosion protection sists of first functional layer: a high performance Fusion Bonded Ep-
of API 8 Inch ERW line pipes. API monogrammed bare pipes were
oxy (FBE) an anticorrosion layer, followed by second functional layer
supplied by the local manufacturer while coating was performed as
a copolymer adhesive which makes bond between epoxy and polyeth-
per DIN 30670 standard. Raw materials including surface prepara-
tion and coating raw materials steel grit, acid and chromate, epoxy, ylene and third functional layer an outer layer of high density poly-
adhesive, HDPE and bare pipes were tested and compared with the ethylene which provides tough and durable protection. 3LPE coating
manufacturer testing certificate for specification compliance check, systems provide the most efficient pipeline protection for small and
results are presented in tables 1-4. Physical inspections of bare large diameter pipelines with moderately operating temperatures from
pipes were carried out before assigning unique identification number -40ºC up to 80ºC which is comparatively higher range.
to each pipe. Surface preparation including pre-heating of pipes at
least 3ºC above dew point temperature, steel grit blasting of pipes Prior to start of regular coating production of each order, a proce-
to get the desired Sa 2.5 surface with 50 to 80 microns profile, acid dure qualification trial is adopted for each pipe diameter range, Inch,
washing of pipes to remove excess chloride ions, Rinsing of pipes for each combination of coating material, and for each plant, to set up
after acid washing with RO water, drying of pipes through blowers, that plant, materials and coating procedures resulting quality of finish
induction heating of pipes up to the epoxy manufacturer recom- product confirming to the properties of the material, relevant stan-
mended temperature which is 200 to 220 degree celsius, first layer dards, specifications and material manufacturer’s recommendations.
epoxy powder application through electrostatic spray gun technique, In current study, coating procedure qualification is performed for 8
second layer of adhesive and third layer of Polyethylene film appli- inch diameter ERW pipe, four test pipes are selected for coating pro-
cation through side extrusion process, quenching of coated pipes,
cedure qualification. Out of four test pipes, one pipe coated with adhe-
full length coating holiday inspection and in the end Final inspection
sive, one pipe coated with epoxy, one pipe coated with polyethylene
of coated pipes. Four test pipes were selected for coating procedure
qualification. Out of these 4 test pipes, First pipe coated with adhe- and one pipe coated with all three layers. Properties of the starting raw
sive layer for adhesive layer thickness measurement, Second pipe materials as mentioned in test certificates supplied by the respective
coated with epoxy layer for epoxy layer thickness measurement, manufacturers is compared with the standard specifications raw mate-
third pipe coated with Polyethylene layer for polyethylene layer thick- rials include client supplied bare pipes which are manufactured as per
ness measurement along with sampling for indentation hardness API 5L 45th edition. Surface preparation raw materials which include
test, fourth pipe coated with all three layers and tested for thickness steel grit, phosphoric acid and chromate. Coating raw materials which
measurement of combined three layers, holiday detection, peel ad- include epoxy powder, copolymer adhesive and high density polyeth-
ylene.
*Corresponding author: Hafiz Abdul Ahad Qazi, Department of Quality Control
Health and Safety Environment, Pakistan, Tel: +923448344723, Email: ahadqa- Surface Preparation Materials Properties
[email protected]
Seen from tables 1-3.
Citation: Qazi HAA (2019) Study of Qualification of Coating Procedure Spec-
ifications as Per Din 30670 for 3lpe Coating of 8 Inch Diameter Erw Pipe,
Pakistan. J Environ Sci Curr Res 2: 008.
Methodology
Received: March 15, 2019; Accepted: April 17, 2019; Published: April 25, 2019 Client supplied bare pipes were visually inspected for surface de-
fects dents, pits, bevel and root damage, straightness, surface contam-
Copyright: © 2019 Qazi HAA. This is an open-access article distributed under the
terms of the Creative Commons Attribution License, which permits unrestricted ination etc., QC cleared pipes sent for surface cleaning process while
use, distribution, and reproduction in any medium, provided the original author rejected pipes sent for re-working or replacement. Detailed coating
and source are credited. process steps are presented in flow diagram below (Figure 1).
Citation: Qazi HAA (2019) Study of Qualification of Coating Procedure Specifications as Per Din 30670 for 3lpe Coating of 8 Inch Diameter Erw Pipe, Pakistan.
J Environ Sci Curr Res 2: 008.

• Page 2 of 7 •

Manufacturer C% Mn% Si% S% P% Hardness (HRC) Microstructure Density (g/cm3)

Steel Grit Thomas Abrasive 0.97 0.91 0.88 0.018 0.02 47-52 Tempered Martensite 7.4

Manufacturer and Type Density (g/cm3) Color

Phosphoric Acid Chemetall, Oakite 33 1.310 Light Yellow

Manufacturer and Specific Gavity

Appearance PH @ 20ºC Hexavalent Cr. As g/l CrO3 Hegmann Gauge Test
Type @ 20ºC
Chromate
Chemetall, Accomet No Particle exceeding 12
Dark Brown Liquid 1.91 2.3 97
PC microns

Table 1: Properties of steel grit, phosphoric acid and chromate as per manufacturer test certificate.

Thermal
Cathodic
Char-
Disbondment
Particle Particle acter- Flexibility Test
Manufacturer and Moisture Density Radius of Impact
Fusion Size % 150 Size % 250 stics- In- Water Soak at 3 Degree @
Type Content % (G/L) Disobondment Resistance
Bonded Microns Microns flection 30ºC
(-3.5 V, @ 65ºC,
Epoxy Point
24 hours)
(J/G)
Jotun JotaPipe
0.19 2 0.2 1455 39.7 1 mm >1.5 Joule Rating 1 No Cracking
1003-21S

Table 2: Properties of fusion bonded epoxy as per epoxy manufacturer test certificate.

* Epoxy raw material tests done by the manufacturer as per CSA-Z245.20-10 standard.

Density @ Melt Flow Rate Ultimate Ten- Vicat Softening Flexural Tensile Im-
Manufacturer Hardness Melting Water Absop-
23ºC (Kg/ (g/10 min) @ 190 sile Strength Point (A50, Modulus pact @ 20 ºC
Adhesive and Type (Shore-D) point (ºC) tion (%)
cm3) ºC & 2.16 Kg (MPa) 10N), Unit (ºC) (MPa) (J/cm3)
Lushan, L-5R 929 1.81 19.6 60 101.9 125.4 280 12.6 0.06

Table 3: Properties of Copolymer Adhesive as per adhesive manufacturer test certificate.

* Adhesive raw material tests performed by the manufacturer as per ASTM relevant standards.

Melt Index @ 190ºC & Density Compound Carbon Black Oxidation Induction Time @ Moisture Content Total Volatiles
Polyeth- 2.16 Kg load (g/10 min) (Kg/m3) Content (%) 210ºC Al Pan (Minutes) (ppm) (ppm)
ylene
0.49 954 2.18 52 10 110

Table 4: Properties of Copolymer Adhesive as per adhesive manufacturer test certificate.

* Polyethylene raw material tests performed by the manufacturer as per ISO relevant standards.

First step is the surface preparation of pipes prior to coating appli- Second step is the coating application. Surface treated pipes are
cation. To do so first pipes are passed through gas furnace for preheat- subjected to induction heating of pipes upto the epoxy manufactur-
ing of pipes above dew point temperature thereafter pipes are sub- er recommended temperature which 200-220ºC. Epoxy powder is
jected to steel grit blasting using centrifugal blasting technique where sprayed on pipes through electrostatic spray gun technique after some
all the rust on pipes surface is removed,. In steel grit blasting, pipes seconds of epoxy layer application second layer of copolymer adhe-
sive and third layer of polyethylene is applied on pipes through side
are cleaned up to white metal surface appearance Sa2.5 with required
extrusion process there after pipes are passed through Quenching tank
surface profile. Using acid spraying technique, pipes are sprayed with
where cold water is sprayed on as coated pipes where soft coated
phosphoric acid solution which reacts with chloride ions present on pipes are converted to hard coated form. In the end of second stage
pipe surface and rinsing the pipes with RO water flash them out of the coated pipes are subject to full length holiday detection where flaw in
pipe surface. In the end of first step quality inspection is performed. coating is detected.

Volume 2 • Issue 1 • 100008

J Environ Sci Curr Res ISSN: 2643-5020, Open Access Journal
DOI: 10.24966/ESCR-5020/100008
Citation: Qazi HAA (2019) Study of Qualification of Coating Procedure Specifications as Per Din 30670 for 3lpe Coating of 8 Inch Diameter Erw Pipe, Pakistan.
J Environ Sci Curr Res 2: 008.

• Page 3 of 7 •

one sample pipe No.4 was selected from the batch on which following
tests were marked and performed: full length holiday inspection, 3
Layer Polyethylene thickness measurement as can be seen from figure
9, visual inspection, Cathodic disbondment test at 60ºC as can be seen
from figure 10, impact test figures 11 and 12, Peel adhesion test as can
be seen from figures 13 and 14, indentation hardness test of PE sheet
as can be seen from figures 15 and elongation test of polyethylene
sheet as can be seen from figures 16 and 17.

Figure 1: Schematic diagram of 3 layer polyethylene coating process.

Third step involves removal of coating up to the specific length

from both ends through cutback brush rollers thereafter in the final
stage coated pipes are inspected for thickness measurement, coating
bevel, cutback length, marking, and other quality control testing. The Figure 2: Showing dry bulb and wet bulb temperature.
testing results discussed in the results and discussion chapter.

Results and Discussion

In current study four pipes are selected as sample, Pipe Numbers
01 to 04 was selected from the batch all the measurements were re-
corded on these pipes. Dew point was calculated first to identify the
temperature required to be set for preheaters. In current study dew
point measured was 9.2ºC as can be seen from the figure 2 hence the
temperature of preheaters were set accordingly the temperature mea-
sured after preheaters was 39ºC as can be seen from figure 3 which
is quite higher than the dew point. Steel grit blasting of pipes carried
out using centrifugal shot blasting technique, the surface profile mea-
sured 75 microns using testex tape and foil thickness gauge (replica Figure 3: Temperature before shot blasting.
method) refer figure 4 and satisfactory surface cleanliness level which
is under the standard specifications as can be seen from figure 4, chlo-
ride content test using digital titration method performed before acid
washing on blasted pipes which was measured 48 PPM which is high-
er than the client specifications (<20PPM) hence acid washing with
10% phosphoric acid +90% RO water solution was performed the
chloride ions value after acid washing and RO rinsing was record-
ed 5 PPM which is under the client specified limit as can be seen
from figure 5. As 200-240ºC temperature before epoxy application
is a requirement of first layer application, bare pipes passed through
induction heating process the temperature measured using contact
thermometer just before first layer epoxy application was 206 Degree
Celsius which met the epoxy manufacturer recommendation as can
Figure 4: Shows shot blasted pipe surface profile.
be seen from figure 6. Application of all three layers were visually
witnessed all production parameters including Pipe temperature, No.
of epoxy guns, pressure of epoxy spray, adhesive and Polyethylene
extruders melt temperature, pressure and RPM of driving screw and
coating speed were recorded. For qualification testing, first adhesive
layer is applied on bare pipe subsequent to cooling thereafter dry film
thickness of adhesive layer measured which is 286-345 microns using
dry film thickness calibrated gauge the adhesive layer sample reading
was found under the client specifications (250 Microns Min. to 450
Microns Max.) as can be seen from figure 7. Thereafter epoxy layer
qualification performed the thickness measured on epoxy cured film
was 243-270 microns which met the client specifications (200 Mi-
crons Min.) as can be seen from figure 8. After both layer qualification Figure 5: Shows chloride content test value after acid wash.
performed normal production was started at the qualified parameters

Volume 2 • Issue 1 • 100008

J Environ Sci Curr Res ISSN: 2643-5020, Open Access Journal
DOI: 10.24966/ESCR-5020/100008
Citation: Qazi HAA (2019) Study of Qualification of Coating Procedure Specifications as Per Din 30670 for 3lpe Coating of 8 Inch Diameter Erw Pipe, Pakistan.
J Environ Sci Curr Res 2: 008.

• Page 4 of 7 •

Figure 6: Shows chloride content test value after acid wash.

Figure 10: Cathodic disbondment test piece after test.

Figure 7: Pipe temperature before epoxy application.

Figure 11: Shows impact test at fixed height of 1 meter.

Figure 12: Holiday detection at 25 KV after impact test.

Figure 8: Shows epoxy cured film thickness 243 microns.

Figure 13: Shows peel adhesion test.

For qualification of coating procedure specifications some of the

tests were performed on production floor and results evaluated at the
same time while some of the tests were performed in laboratory under
controlled temperature. Table 5 shows the qualification tests results
for surface preparation, table 6 shows testing results conducted on
Figure 9: Shows 3 Layer thickness measured value 2.585 mm.
shop floor whereas table 7 shows testing results conducted in labora-
tory.

Volume 2 • Issue 1 • 100008

J Environ Sci Curr Res ISSN: 2643-5020, Open Access Journal
DOI: 10.24966/ESCR-5020/100008
Citation: Qazi HAA (2019) Study of Qualification of Coating Procedure Specifications as Per Din 30670 for 3lpe Coating of 8 Inch Diameter Erw Pipe, Pakistan.
J Environ Sci Curr Res 2: 008.

• Page 5 of 7 •

Figure 14: Shows peel adhesion value which is 240 N/cm. Figure 16: PE Sheet Elongation Test Specimen.

Figure 15: Indentation test of PE sheet @70ºC. Figure 17: PE sheet Elongation Measurement

Chloride Content Chloride Content Pipe Temperature Pipe Tempera-

Preheating Grit Blasting Grit Blasting
Dew Point Preheating Tem- Test on grit blasted Test on grit blasted Requirement ture Measured
Temperature Profile Require- Profile Mea-
Measured perature Measured pipe surface pipe surface Mea- Before Epoxy Before Epoxy
Requirement ment sured
Requirement sured Application Application
> 3ºC of Dew
9.2ºC 39ºC 50- 80 Microns 75 Microns <20 PPM 5 PPM 200-220ºC 206ºC
Point

Table 5: Testing Results related to surface preparation prior to coating application.

*Chloride Content test as per standard ISO 8502-2

Thickness Online Impact Resistance

Thickness Thickness Thickness Thickness Online Peel Peel Impact Resistance
Epoxy Thickness Holiday at 23ºC subse-
First Lay- Adhesive 3 Layer 3Layer Holiday Strength Strength at 23ºC subsequent
First Second Layer Test at quent to Holiday
er Epoxy Layer 3LPE 3LPE Test at 25 @ 25ºC @ 25ºC to Holiday Detec-
Layer Adhesive Req. 25 KV Detection at 25
Req. Measured Req. Measured KV Result Req. Measure tion at 25 KV Req.
Measured Req. KV Result
>200 243-270 250-450 286-345 2.5-3.1 > 150 N/ 240 N/
> 2.5 mm No Spark No sparks No Spark No spark
Microns Microns Microns Microns mm Cm cm

Table 6: Qualification testing results the testing was performed and evaluated on production floor.

*Thickness of all three layers measured as per Annex A of DIN 30670

* Holiday Detection as per Annex E of DIN 30670
* Peel adhesion strength as per Annex D of DIN 30670
* Impact Resistance test as per Annex H of DIN 30670

Cathodic Disbondment Test @ Cathodic Disbondment Test @ Indentation Test @ (i) 23ºC Indentation Test @ (i) 23ºC Elongation Test Elongation Test
60ºC, -3.5 V, 24 hours Requirement 60ºC, -3.5 V, 24 hours Result @ (ii) 70ºC Requirement @ (ii) 70ºC Measured @23ºC Requirement @23ºC Measured
(i) < 0.2 mm (i) 0.07 mm
Radius of Disbondment < 7 mm Radius of Disbondment 3 mm > 400% 733%
(ii) < 0.4 mm (ii) 0.1 mm

Table 7: Qualification testing performed and evaluated in laboratory at controlled temperature.

* Cathodic disbondment test at 60ºC as per ASTM G42

* Indentation hardness test as per Annex I of DIN 30670
* Elongation test as per Annex F of DIN 30670 and standard ISO 527-1 to 527-3

Volume 2 • Issue 1 • 100008

J Environ Sci Curr Res ISSN: 2643-5020, Open Access Journal
DOI: 10.24966/ESCR-5020/100008
Citation: Qazi HAA (2019) Study of Qualification of Coating Procedure Specifications as Per Din 30670 for 3lpe Coating of 8 Inch Diameter Erw Pipe, Pakistan.
J Environ Sci Curr Res 2: 008.

• Page 6 of 7 •

Conclusion References
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the manufacturing specifications and DIN 30670 hence the coating sile properties of plastics. Touchstone Research Laboratory, West Virginia,
procedure specifications found satisfactory and approval is given for USA.
normal routine coating production.

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