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Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 1

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Subject PP-R-001 in Spirdane D60

Author O.J.P. Post

Date 2013-11-27

Document number STM 20130315

Project number 4001824

Distribution Customer

R.C.J. Millet 

B. Fischer 

M. van der Schuur 

P. Dijkgraaf 

A.G. Talma

J.P.F.M. van Hertrooij

J. Nuysink

G. Nagelhout

H.J. Edelijn

M.A.D. Davidsson

Product Safety File

Secretary FC, Archive

1 Product Safety Investigation Form SI-3

Drafted by

Name O.J.P. Post Date 2014-01-28

Function Safety Engineer Signature

Approved by

Name H.J. Edelijn Date 2014-01-28

Function Manager Safety Testing & Modeling Signature
Product Safety Investigation Form SI-3 of PP-R-001 in Spirdane D60

STM 20130315

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 2

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Chemical name : PP-R-001

Assay : ≈ 40 %

Act.O : 7.2 %

Solvents : Spirdane D60

Carriers : --

Appearance : Clear liquid

Formula : 

Product no. : --

Laboratory notebook : 4619, 4213, 4887, 4234, 

 4227, 3118

BU : Functional Chemicals

Res. Proj. no. : --

Res. Task no. : 4001824

Batch no. : RCM13-101

Applying section : --

SI-1 reference : --

SI-2 reference : STM20120273

1.1 Preliminary conclusions

Thermal stability : high (low – medium – high)

SADT : ≥ 110 °C (indicative)

Flashpoint : 56 °C

SHV : not high (not high – high)

Estimated deflagration : no (slowly/no – rapid)

Auto-ignition : class T3 (T1 – T2 – T3 – T4 – T5 – T6)

Expected sensitivity to dust explosion : n.a. (not sensitive – sensitive – very

sensitive – extremely sensitive)

Increase in hazard due to physical

changes at low temperatures : no (no – yes)

Increase in hazard due to concentration : no (no – yes)

Hazard : low (low – high)

1.2 Preliminary advice

Approved for SI-4 : yes (no – yes – to be discussed)

(Further) Phlegmatizing is : not required (required – not required)

Storage temperature : 20°C (max.); 0°C (min.)

1.3 Remark

Detonation data known : no (no – to be determined – yes, Ref.....)
Product Safety Investigation Form SI-3 of PP-R-001 in Spirdane D60

STM 20130315

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 3

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Detailed test results

1. Mini-HAST (mini-Wärmestau), see appendix

Conditions : temperature : 110 °C

intake : 50 g

Observations : self-accelerating decomposition after: hours

or

maximum temperature rise of : 2.2 °C after : 24 hours

Result : Thermal stability is high (low – medium – high)

SADT : ≥ 110 °C (indicative)

Preliminary Tstorage : 20 °C

2. Flashpoint (liquids only)

Method : Setaflash (ISO 3679), EU test A9

Result : Flashpoint is 56 °C

3. Koenen test (Stahl Hülsen Verfahren, SHV), (Ref.1)

Method : UN test E1

Conditions : orifice : 2.0 mm (3 tests performed; other 2 tests: fragmentation type A)

Observations : negative (negative – positive)

 type of fragmentation : type B

t1 : 30 s

t2 : 11 s

Result : Koenen is not high (not high – high)

4. Propagation of deflagration (from SI-4), see appendix

Method : Deflagration in a 48 mm Dewar vessel, UN test C2 (Ref.2)

Conditions : test temperature : 50 °C

 Observations : deflagration rate : 0.019 mm/s

 Result : no (no – yes, slowly – yes, rapidly)
Product Safety Investigation Form SI-3 of PP-R-001 in Spirdane D60

STM 20130315

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 4

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

5. Auto-ignition temperature (exploratory test)

Method : DIN 51794, EU test A15, only screening

Observation : n.a. (decomposition peroxides) °C (ref.3)

Result : Temperature class is T3 (as a standard)

6. Dust-explosion test (exploratory test for powders only)

Method : MIKE-3, see PCS test method C-SR-036

Conditions : concentrations : 4 trials at 500 g/m3, 750 g/m3 and 1000 g/m3 each

 Particle size : μm

Observation : 3 mJ : n.a. (negative – positive)

100 mJ : n.a. (negative – positive)

1000 mJ : n.a. (negative – positive)

Result : Expected sensitivity to dust explosion is :

 (not sensitive – sensitive – very sensitive – extremely sensitive)

7a. Cold storage test (lab code: NUK13112)

Conditions : sample : RCM13-087 (Active Oxygen=7.45%) in Spirdane D60

temperature : -25°C (seeded with pure cyclic trimer MEK peroxide)

tube : 28 mm (ID)

duration : 5 days (stirred) + 3 days (not stirred)

Observations : solidification : no (no – yes)

crystallization : no (no – yes)

phase separation : no (no – yes)

Result : Increase in hazard due to physical

changes at low temperatures : n.a. (no – yes)

7b. Cold storage test (lab code: NUK13118)

Conditions : sample : RCM13-101A (Active Oxygen=8.34%) in Sprirdane D60

temperature : -27°C (3 times seeded with pure cyclic trimer MEK peroxide)

tube : 28 mm (ID)

duration : 7 days

Observations : solidification : no (no – yes)

crystallization : no (no – yes)

phase separation : no (no – yes)

Result : Increase in hazard due to physical

changes at low temperatures : no (no – yes)
Product Safety Investigation Form SI-3 of PP-R-001 in Spirdane D60

STM 20130315

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 5

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

8.a Evaporation/concentration test, sample in Spirdane D60 (phlegmatized products only) , see appendix

Method : Concentration followed by PVT

Conditions : temperature : 20 °C

intake : 50.02 g

Observations : weight loss :4.14 g ( - 8.3% )

PVT with 10 g at 9 mm : n.a. (weight loss<10%) (negative – positive)

Result : Increase of hazard due to concentration : no (no – yes)

Weight loss (g) Active Oxygen, ref 4 (%)

RCM13-101 (start) -- 7.2 %

PTO13112601 (after 24h) 4.14 g 7.8 %

PTO13112602 (after 48h) 7.42 g 8.3 %

PTO13112603 (after 120h) 15.72 g 10.1 %

Note:

The criterion for increased hazard due to concentration is a weight loss of > 10% during the test period of 

24 hours. The conclusion according to this definition is: no increased hazard.

However, by evaporation of all solvent, a peroxide with a very high active oxygen content will be formed (18%). 

Therefore the ideal solvent for this formulation will be a solvent with a higher molecular mass / low vapor 

pressure.

This evaporation/concentration experiment is repeated with Isopar-M as solvent, see appendix:

8.b Evaporation/concentration test,, sample in Isopar M (phlegmatized products only) , see appendix

Method : Concentration followed by PVT

Conditions : temperature : 20 °C

intake : 50.00 g

Observations : weight loss :3.17 g ( - 6.3% )

PVT with 10 g at 9 mm : n.a. (weight loss<10%) (negative – positive)

Result : Increase of hazard due to concentration : no (no – yes)

Weight loss (g) Active Oxygen, ref 5 (%)

RCM13-091 (start) --- 7.2 %

PTO13121101 (after 24h 3.17 g 7.4 %

PTO13121102 (after 48h) 5.52 g 7.6 %

PTO13121103 (after 120h) 10.25 g 7.8%

From evaporation point of view, Isopar M is a much better solvent than Spirdane D60.
Product Safety Investigation Form SI-3 of PP-R-001 in Spirdane D60

STM 20130315

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 6

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

2 References:

1. STM 20130223: Heating under Confinement (Koenen Test) of PP-R-001 in Spirdane 

D60/Isopar L, O. Post, October 2013

2. Recommendations on the transport of dangerous goods, Manual of Tests and Criteria, 

5th revised edition, 2009

3. PGS-8, Storage of Organic peroxides, December 2011

4. ECG-MAS A20131045, Determination of the total Active Oxygen content in cyclic 

peroxides, December 2013

5. ECG-MAS A20131086, Determination of the total Active Oxygen content in cyclic 

peroxides, December 2013
Product Safety Investigation Form SI-3 of PP-R-001 in Spirdane D60

STM 20130315

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 7

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

3 Appendix

Result of mini-HAST at 110°C

Result of Deflagration test PP-R-001 (batch RCM13-101)
Product Safety Investigation Form SI-3 of PP-R-001 in Spirdane D60

STM 20130315

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 8

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Result evaporation experiment of PP-R-001 in Spirdane D60 at 20°C 

Mass loss after 24 hours: 8.3%

Result evaporation experiment of PP-R-001 in Isopar-M at 20°C

Mass loss after 24 hours: 6.3%