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The proposed method of crack resistance testing of constructional materials in corrosive media provides determination of the electrochemical condition at the tip of not only a steady but also of a propagating crack. The values of pH andϕ at the tip of the crack change with growth of it.
"1. A polymer composition for the manufacture of pipes having a design stress of at least 9.0 MPa (PE112) and a slow crack propagation resistance of at least 1000 hours at 4.9 MPa loop [sic] stress at 80ºC temperature, measured according to ISO 13479:1997, comprising 92-99%wt of a bimodal ethylene polymer and 1-8%wt of carbon black, said composition being characterised by having MFR5 measured according to ISO 1133 in the range 0.15 to 0.30 g/10 min and a density in the range 955 to 965 kg/m**(3), said polymer being composed of 42-55%wt of a low molecular weight ethylene homopolymer having MFR2 measured according to ISO 1133 in the range 350 to 1500 g/10 min and 58-45%wt of a high molecular weight copolymer of ethylene with 1-hexene, 4-methyl-1-pentene, 1-octene and/or 1-decene.
- Standard ISO 13479:1997 (D11) which according to claim 1 was used to measure the slow crack resistance at 4.9 MPa only referred to PE 80 and PE 100 resins whereas the patent related to PE112 grade resins. Since D11 stated in Annex A that the test was applicable to other polymer materials, the argument of the patent proprietor that the skilled person would know how to develop test parameters and specifications for PE112 resins was accepted.
- Although only a single example (example 4) met the product requirements of claim 1 and showed a slow crack propagation resistance of at least 1000 hours, the evidence of the patent as well as the explanation in D16 strongly suggested that the amount of comonomer together with other properties such as MFR5 and density were essential in order to obtain the required combination of design stress and slow crack propagation resistance. The application as filed together with general knowledge of the field put the skilled person into a position to understand these aspects.
"A pipe having a design stress of at least 9.0 MPa (PE112) and a slow crack propagation resistance of at least 1000 hours at 4.9 MPa hoop stress at 80ºC temperature measured according to ISO 13479:1997, formed of a polymer composition comprising 92 to 99 wt.-% of a bimodal ethylene polymer and 1 to 8 wt.-% of carbon black, wherein said polymer composition being characterized by having MFR5 measured according to ISO 1133 in the range of 0.15 to 0.30 g/10min, an FRR21/5 of at least 38, and a density in the range 955 to 965 kg/m**(3), and wherein said bimodal ethylene polymer which has a density of at least 953 kg/m**(3) is composed of 42-55 wt.-% of a low molecular weight ethylene homopolymer having MFR2 measured according to ISO 1133 in the range of 350 to 1500 g/10min and 58-45 wt.-% of a high molecular weight copolymer of ethylene with 1-hexene, 4-methyl-1-pentene, 1-octene and/or 1-decene."
(b) Examples 3 and 4 failed to disclose how the polymers had been prepared beyond a teaching that these polymers had been prepared under "slightly different" conditions to those of "Example 1" (by which it was assumed that "Example 2" was meant since Example 1 related to preparation of the catalyst, not to a polymer). The polymer composition of Example 2 had an MFR5 falling outside the scope of the claim but nevertheless resulted in a pipe with the required slow crack propagation resistance at 4.9 MPa hoop stress. In contrast example 3 having a MFR5 value within the scope of the claim resulted in a pipe with slow crack propagation resistance at 4.9 MPa of 965 hours, i.e. below the limit of 1000 hours given in the claim. Arguments of the respondent that 965 hours would be considered as equivalent to 1000 hours by rounding were not consistent with the fact that in the patent the slow crack propagation resistance data was reported to a precision of four significant figures. 2ff7e9595c
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