INFLUENCE OF LOCAL GELATION DEGREE

ON THE FREQUENCY OF BREAKS OF

PVC PRESSURE PIPES

H. Muschik*, H. Dragaun*, P. Valenta**

*
Federal Testing Centre – TGM,
Plastics Technology and Environmental Engineering

** Pipelife Austria GmbH. & Co KG.Austria

Budapest 2008

Federal Testing Centre – TGM, Plastics Technology and Environmental Engineering

 ABSTRACT

• Assessment of homogeneity of plastification:

e.g. standardized method by immersion in Dichlormethane (DCMT)

• Round Robin Tests revealed low reliability of DCMT method

• Alternative methods to assess homogeneity are in discussion and

content of this presentation

• Investigated samples: uPVC pipes

- Pb stabilized and
- OBS stabilized

• Methods of investigation:
- DCMT: gelation (chemical attack/no attack)
- DSC: gelation/onset temperature
- Fracture toughness test: creep behaviour (C-ring test)
- Tensile test: tensile strength, elongation at break

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 Advantage of DCMT ÖNORM EN 580: 2003

• Requires Dichlormethane (DCMT) section

at “technical
1 purity”

• End of pipes are milled (A) or turned (B) to have

a defined surface for exposition to chemical attack
section 3

of DCMT (typical storage conditions are 30min at 15°C)

section 3

• G = Proportion of non attacked surface to total exposed

surface

• Advantage: quick method, good overview

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 “Reliability” of DCMT

attack
Both chamfers of the left pipe were prepared
by turning in the same way but stored in DCM
of different suppliers (both commercial
technical quality).

no attack chamfer made by

milling
(strong attack)

The chamfer of the upper pipe

section was milled, the lower one
was turned. Immersion in the same chamfer
DCM-bath. made
by turning
(attack)

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 Background

Determination of gelation G by DSC:

• ISO 18373-1:2007, ISO 18373-2:2008

– Onset temperature Tons (= processing temperature)
– Gelation degree G (proportion of enthalpy change A to total consumed
enthalpy A+B).

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 Program

Following aspects were examined:

• Constancy of DCMT–attack along direction of extrusion

• Distribution of onset temperature and gelation degree

along wall thickness

• Comparison between Pb- and OBS-stabilization

• Comparison of different quality of pipes

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Constancy of DCMT–attack along direction of extrusion

section 1
section 1

section 2

section 2

section 3

section 3

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 Onset temperature along extrusion direction

Onset temperatur (Tons) mid of pipe wall in extrusion direction

positions of DCM-attack and no DCM-attack

192,0
dn110 PN12,5; Pb-Stab. DCM-attack

dn110 PN12,5; Pb-Stab. DCM-attack; single meas.

190,0
dn110 PN12,5; Pb-Stab. no DCM-attack

188,0 dn110 PN12,5; Pb-Stab. no DCM-attack; single meas.

.

186,0
Tons [°C]

184,0

182,0

180,0

178,0 0,5 1,5 2,5 3,5

Section 1 Section 2 Section 3

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 Gelation degree along extrusion direction

Gelation degree (G) mid of pipe wall in extrusion direction

positions of DCM-attack and no DCM-attack

100,0

95,0

90,0

85,0
G [%].

80,0

75,0
dn110 PN12,5; Pb-Stab. DCM-attack

dn110 PN12,5; Pb-Stab. DCM-attack; single meas.

70,0
dn110 PN12,5; Pb-Stab. no DCM-attack
65,0 dn110 PN12,5; Pb-Stab. no DCM-attack; single meas.

60,0 0,5 1,5 2,5 3,5

Section 1 Section 2 Section 3

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 Onset temperature along wall thickness

Onset temperature Tons along wall thickness

positions of DCM-attack and no DCM-attack in circumference
194,0

192,0

190,0 Pb-stab.
188,0
strong attack no attack
186,0

184,0
Tons [°C] .

182,0

180,0 OBS-stab.
178,0

176,0

174,0 dn225 PN10; OBS-Stab. DCM-attack

dn225 PN10; OBS-Stab. No DCM-attack
172,0
dn315 PN6; Pb-Stab. DCM-attack
170,0 dn315 PN6; Pb-Stab. No DCM-attack
168,0 0,5 1 1,5 2 2,5 3 3,5

inside pipe wall mid pipe wall outside pipe wall

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 Mechanical properties and gelation degree

• At the breaking line from internal pressure tests no

DCMT-attack could be seen
Æ Therefore a systematic damage analysis was
carried out: the breaking area of pipes broken in
internal pressure tests were compared with those
positions of the opposite side by:

Æ Determination of Tons and G

break
Fracture toughness test
Viscosity number
Light microscopy

„break line“

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 Mechanical properties and onset temperature

Onset temperature (Tons) along wall thickness

positions of "break line" and on the opposite position

205,0

200,0

195,0
.
Tons [°C]

190,0

185,0
dn 110 PN20, Pb-stab. "break line"

dn 110 PN20, Pb-stab. "break line"; single meas.

180,0
dn 110 PN20, Pb-stab. opposite "break line"

dn 110 PN20, Pb-stab. opposite "break line"; single meas.

175,0 0,5 1,5 2,5 3,5

inside pipe wall mid pipe wall outside pipe wall

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Federal Testing Centre – TGM, Plastics Technology and Environmental Engineering

 Mechanical properties and onset temperature

Onset temperature (Tons) along wall thickness

positions of "break line" and on the opposite position

200,0
dn225 PN10; OBS-Stab. "break line"
198,0 PN 16
dn225 PN10; OBS-Stab. opposite "break line"
196,0
dn225 PN16; OBS-Stab. "break line"
194,0 dn225 PN16; OBS-Stab. opposite "break line"
192,0
Tons [°C] .

190,0

188,0

186,0 PN 10
184,0

182,0

180,0

178,0

176,0 0,5 1 1,5 2 2,5 3 3,5

inside pipe wall mid pipe wall outside pipe wall

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Federal Testing Centre – TGM, Plastics Technology and Environmental Engineering

 Fracture toughness test

• ISO/FDIS 11673:2005 (E)

• Notches have been milled in

line of breaking and in
opposite position

• Samples have to resist at

least 15 min testing time
until break (for modern pipe
production no problem)

• Elongation at 100 h testing

time was recorded

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 Fracture toughness test

Relative elongation εrel (opposite position / "break line")

(mean of 3 single measurements)
160,0

140,0 "break linie"

opposite position

120,0

100,0
εrel [%] .

80,0

60,0

40,0

20,0

0,0 1

Pb-stab. dn
1 110 PN20 OBS dn 2225 PN10 OBS dn3225 PN16

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 Tensile test

Elongation at break (εB)

(samples at "break line" and in opposite position)

200

"break line"
180
opposite position
160

140

120
εB [%]

100

80

60

40

20

0
Pb-stab dn 160 PN10 Pb-stab. dn 160 PN16 OBS dn 225 PN 16 OBS dn 225 PN10

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 Viscosity number/Light microscopy

OBS-Stab. bubble
• Viscosity number at positions
of breaking line and opposite
position showed no significant
difference
(no molecular degradation) 1000 µm

• Light microscopy of breaking

areas showed bubble formed Pb-Stab.
areas (10 to 200 µm)

• Damage area = locally too high bubble

processing temperature 1000 µm

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 Summary

• Applied stabilizers Pb and OBS show no substantial

influence on the gelation degree

• Except very high gelation degrees DSC analysis and

DCMT are in good correlation

• Distribution of gelation degree in circumference

(attack/ no attack) showed to be constant in direction
of extrusion obviously deriving from extrusion
conditions
• Due to shear rate a higher gelation degree was found at
the pipe surface compared with the pipe wall center
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Federal Testing Centre – TGM, Plastics Technology and Environmental Engineering

 Summary

• Along „break line“ from internal pressure tests very

high gelation degrees (“over gelation”) and locations of
bubbles could be found (but no molecular degradation)

• In fracture toughness test in the area of „break line“

a lower creep rate was found than at the opposite
position

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 Information

For further information see

www.kunststoff.ac.at

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