The problem
The Infineum Group of companies is a world-class petroleum additives enterprise. With its headquarters in the UK, it has regional business and technology centres in the UK, US and Singapore.
Infineum is a developer, manufacturer and marketer of lubricant additives, with its customers being oil companies and other lubricant and fuel marketers.
For motor oil to operate efficiently it has to have the correct consistency and achieving this may require the use of additives. Infineum produce specialist lubrication oils that contain inorganic chalk-like particles coated with a waxy detergent layer. Conventional analysis techniques were unable to determine the precise effect these additives were having on formulation so the optimum composition could not easily be determined.
The challenge
Infineum’s own techniques had provided only general data, insufficient to characterise the additives in detail, and thus their researchers were unable to ascertain the effect of adding or removing an ingredient to the formulation. CLiK Knowledge Transfer at Daresbury SIC were contacted to see if they could help.
A particular challenge was the response time - it had to be rapid so that modification could be made to the formulation without major loss of production time.
The solution
Researchers at the Synchrotron Radiation Source (SRS) at Daresbury Laboratory employed small angle X-ray scattering (SAXS) to examine a large number of formulations of particles and detergent composition in the oil. Typically the calcium and magnesium detergent particles are 2050 Å in size, a range that is easily accommodated by the SAXS method. In addition to providing information about particle size, SAXS also enables the particle shape and size distributions to be determined. The technique was operating at the limits of its sensitivity, and required considerable skill and experience from SRS staff to extract the subtle changes in the signal from the background noise. Only the high intensity of the X-rays produced by the synchrotron enabled this information to be obtained.
This characterisation of detergent additives in motor oil samples allowed quantification of process changes, control of rheological properties and performance characteristics of the finished product and prediction of the various interactions that can occur between detergent molecules and other additives in the finished oil. The results allowed Infineum to define a narrow range of formulations that gave optimum operating performance.


Benefits
- The problem was solved promptly and effectively due to the specialist equipment and expertise available through CLiK.
- The results allowed Infineum to define precisely the range of formulations it could tolerate to give best performance of its oilLoss of production time was kept to a minimum due to the rapid turnaround time between receiving the sample and reporting back the results
The problem
Innovia Films is the world's leading supplier of speciality Biaxially Oriented Polypropylene (BOPP) and cellulose films for speciality packaging, labelling, graphic arts and security products.
With a turnover of more than £400 million Euros, the business employs some 1,350 people worldwide. Total annual film capacity currently stands at more than 130,000 tonnes.
They requested evaluation of a coated polypropylene film used in food packaging, which degraded over a period of time resulting in increased opacity of the material when stored. The problem appeared to be related to the processing conditions under which the films had been manufactured.
The challenge
This particular challenge related to a film used in packaging food, in this particular case, for a company manufacturing and packaging potato crisps in transparent bags. Rapid turnaround time from receipt of samples to results of investigation was required to allow knowledge gained to be fed back into the manufacturing process.
The bags are manufactured from two polymer systems - a ‘core’ of polypropylene, which is coated on both sides by a 0.6 µm layer of a random copolymer of propylene and ethylene. Different parameters during manufacture and processing led to variations, both in the ‘haziness’ of the otherwise transparent films, and in how the transparency changes with time. The challenge facing Daresbury Laboratory was that either one of these constituent parts could have been causing the haziness.
The solution
The multidisciplinary facilities available on the Synchrotron Radiation Source allowed independent investigation of the bulk polymer and the surface layer.
Grazing incidence powder diffraction was used to look at the 0.6 µm surface layer – the diffraction patterns from all samples showed just three broad peaks, which corresponded exactly to the positions expected for pure polypropylene. Therefore, despite the presence of up to 10% ethylene in the copolymer, the molecular arrangement of polypropylene is being adopted in the coating layers’ crystallites. The peaks are sharper in the case of the ‘clear’ films, implying a higher level of molecular order within the crystallites.
Small angle X-ray scattering was used to look at the bulk polymer. Comparison of data recorded for ‘clear’ and ‘hazy’ samples revealed a subtle but significant effect. There was more scattering in the ‘hazy’ samples. It may be expected that there would be more crystallites in the ‘hazy’ samples – this information showed that the size of those crystallites is around 200 Å.


Grazing incidence X-ray Diffraction pattern of polymer surface layer for three samples. The samples range from "clear" to "hazy" in the order of red, blue and green respectively.
Benefits
- The crisp packet manufacturer was able to alter its production conditions to eliminate hazing
- The rapid solution of the problem allowed the manufacturer to demonstrate a proactive and trouble-shooting approach to its customers
- Loss of production was kept to a minimum, whilst the manufacturer’s brand reputation was enhanced