Softening point and Penetration Index of

bitumen from parts of Southwestern
Olugbenga A. Ehinola, Olugbenga A. Falode and G. Jonathan
The softening point (SP) and penetration index (PI) of bitumen from parts of southwestern Nigeria are
important properties needed for better design and optimization of the upgrading process of Nigerian
bitumen. This study was carried out to design and fabricate a cost effective and efficient softening point
tester to classify bitumen into grades.
The Ring and ball equipment was fabricated locally according to the American Society for Testing and
Materials (ASTM) and was utilized to determine the SP of bitumen samples collected from four locations
namely: Agbabu (AB), Iluburin (IB), Loda (LB) and Ode-Omode (OB). Two disks of bitumen, cast in shouldered
brass rings, were heated at a controlled rate in a liquid bath while each supports a steel ball. The SP was
reported as the mean of the temperatures at which the two disks soften enough to allow each ball, enveloped
in bitumen, to fall a distance of 25 mm. The SP values obtained were used to compute the various
penetration indices and to predict the grade of bitumen.
The SP results for AB, IB, LB and OB are 30, 48, 48.10 and 38.10 °C respectively while that of PI results are
-3.8, -1.3, -1.1, and -1.6 respectively. The bitumen grades predicted for the four locations are: temperature
susceptible bitumen for AB (250/330 Grade) and conventional paving bitumen for OB, IB and LB (50/70 and
160/220 Grade). The OB, IB and LB samples are therefore suitable for road pavement, while the AB sample
can be modified for industrial use.

Key words: Nigeria,softening point, bitumen, penetration index

1. INTRODUCTION asphaltenes and aromatics. This in turn produces an en-
Bitumen is an oil based non-crystalline solid or viscous vironment of heavy component and a decrease of API
substance derived from petroleum that exists in the nat- gravity so that heavy oil devoid of light component is the
ural or as a by-product of refinery processes; has adhe- end result (bitumen).
sive properties, and substantially soluble in carbon The other process of bitumen formation is known as
disulphide. It is a mixture of organic liquids that are biodegradation, which occurs when oxygen charged me-
highly viscous, black, sticky, and composed primarily of teoric water carry aerobic bacteria from the surface to
highly condensed polycyclic aromatic hydrocarbons. Bi- the accumulation in the reservoir trap, then
tumen is obtained by removing the lighter fractions (such biodegradation occurs. These aerobic bacteria attack
as liquid petroleum gas, petrol and diesel) by distillation mainly the normal alkanes, although it can also attack
of blends of heavy crude oil during the refining process. the other oil components on a smaller scale. The mete-
The vast majority of refined bitumen is used in construc- oric water must have dissolved oxygen content of at least
tion industry. Bitumen's primary use is as a constituent 0.8 g/litre. It must contain nutrient and be free of hydro-
of products used in paving and roofing applications. Ap- gen sulphide (H2S) which will poison the bacteria.
proximately 85% of all the bitumen produced worldwide In shallow oil accumulation near the edges of the basin
is used as the binder in asphalt for roads and it is also where the reservoir best continue to surface outcrop, a
used in other paved areas such as airport runways, car combination of water - washing and bacteria biodegrada-
parks and footways. tion can also convert very heavy large amount of oil into
Natural Bitumen forms from oil which are already gen- heavy tar or bitumen, an example is the deposit of bitu-
erated and migrated into reservoirs and are subjected to men in the Dahomey basin south-west Nigeria.10 The out-
other effects as well as normal maturation processes, crop belt of the tar sands lies within the Nigerian sector
these additional changes occur when the continuity of the of the Benin Basin which is a marginal pull-apart10 or
reservoir horizons permit either up-deep or down deep marginal sag basin.9 The eastern ward limit of the Benin
gas to come in contact with the oil accumulation, one of basin is marked by the Okiti-pupa High while the basin
such processes is known as water washing, which occurs extends westwards into Togo and the Volta Delta
when the reservoir trap is in contact with moving mete- (Ghana). The basin contains about 3 000 m of sediments
oric water. The process is simply the flushing away of the and the stratigraphy has been described.13,2 Omatsola
lighter hydrocarbon compound in amount proportional and Adegoke13 recognized three formations belonging to
to their solubilities. The result is a big decrease in gaso- the Abeokuta Group. These are: Ise Formation
line range hydrocarbon content and decrease in light (Neocomian -Albian) consisting essentially of continental

NAFTA 63 (9-10) 319-323 (2012) 319

MATERIAL AND METHODS Brass rod of 23mm by 9mm was used to fabricate the The bitumen samples were collected from four study lo. well sorted. The 2. Ring holder sulphur.. in order to ascertain their grades. Unlike some substances (e. thick films. 2. The kinetic parameters and temperature range for the pyrolysis of asphaltene fraction of Nigerian oil sand bitu. moderately to Fig. cuses on the determination of the softening point and (c) Bench-:This involved the use of a hacksaw and penetration index of bitumen from southwestern Nigeria file to shape out the edges into dimension. FABRICATION OF APPRATUS and andalusite some of which could be economically ex- ploited. The Araromi Forma- tion (Maastrichtian-Paleocene) conformably overlies the Afowo Formation and consists of sands. 1. as the temperature rises. the sands range from fine to coarse-grained.. Sample was collected from a sand grains are sub-angular to sub-round in shape. holes. Instead. ball centering guides.. Ilubirin (IB). such as joint and 2nd drill-19 mm diameter drill was used to expand the crack fillers and roofing materials. minor and trace elements in ried out according to the American Society for Testing the Nigerian tar sands with concentrations ranging from and Materials (ASTM). tion was brass and the specification of the apparatus are tent of the tar sands is 12-14 wt% and compares favour.Maastrichtian) con- sisting of coarse to medium grained sandstones with interbeds of shale. zircon. has particular significance for materials which are to be used as pavement material.OLUGBENGA A. positively skewed Sl. bituminous materials do not have a definite 25 mm (thickness). staurolite. among others. garnet 3. with some illite. sands also contain some heavy minerals which include opaques. 1. The physical and chemical characteristics of the oil sands have been summarized5. overlain by dark-grey shales with interbeds of lime- stones and marl. grits and siltstones. sands. Overlying the Ise Forma- tion is the Afowo Formation (Turonian. Tap / wrench. EHINOLA. nickel and vanadium contents. melting point. stated in Figure 2. Agbabu (AB). smectite and mixed layer clays. OLUGBENGA A. Karta lokacija na kojima su prikupljeni uzorci and mesokurtic and represent deposits of high energy environ- ments (e. sample was collected from a drilled well (I) Tap / Die. The ball centering guides were drilled These include: and machined to the required size. 320 NAFTA 63 (9-10) 319-323 (2012) . except for its lower 1. Die / Wrench. 5 The fabrication of the softening point apparatus was car- The presence of 22 major. rutile. SOFTENING POINT AND PENETRATION INDEX OF. LATHE MACHINE. men to release more oil-like liquid has been carried (iii) Centre Punch: Used to make mark on the out. tourmaline.12 The bitumen con.5 ppm have been reported. Die / with metal casing. Ball centering guide 2. The 4. FALODE .g.6 mm diameter drill was used to liquid fuel. Loda (LB).3.. water which changes from solid to liquid Brass plate of 89 mm (length) by 30 mm (breadth) by at 0 °C). overlying the basement com- plex. siltstones and clay. these (a) Marking out-: This involve using the following materials slowly change from brittle or very thick and tools slow-flowing materials to softer and less viscous liquids. The temperature at which bitumen softens make five holes out of the length. (ii) Steel Tool: Used for measurement. The present study fo. Texturally.g beaches) which have been reworked. this was achieved with the aid of a cations from Southwestern Nigeria (Fig. clay content of the sands (2-7%) is essentially kaolinite 3. (i) Scriber: used to make lines. sample was collected from tar sand. ably with the Athabasca tar sands. Ode-Omode Mile 2 (OB).14 This information is needed for better design and measured line optimization of upgrading process of Nigerian bitumen to (b) Drill-:1st drill--5. The drilled well with metal casing. Map showing the sample locations. The material used for the fabrica- 17 to 35. 1. Stud. 1). sample was collected from tar sand.

The Sl.5 °C per P = Penetration at temperature T minute. (III) Cutting Tools used-: Knife edge. FALODE . OLUGBENGA A. The pouring temperature and the room tempera. Fabricated Ring and ball Apparatus (ASTM D36-95 tered with a sieve to remove impurities while pouring. Several equations exist ature susceptible bitumens to around +7 for highly that define the way that the viscosity (or consistency) blown low temperature susceptible (high PI) bitumen. asphalt binders with high penetration num- bers (called "soft") are used for cold climates while as. Izraðeni ureðaj s prstenom i kuglicom (ASTM D36-95 rings and assembly and two ball bearings.. The temperature at which each bitumen speci. Some of the samples were fil. the specification) samples were then allowed to set for 30 minutes. 2. OLUGBENGA A.. 2. Pfeiffer and Van Doormaal developed an equa- tion for the temperature response that assumes a value 5. Bottom plate This was drilled the same way as the ring holder. is plotted against measurements at two temperatures..50±0. the following processes were used to achieve this: (I) The rod was turned to the required size. 5. changes with temperature. that: The values of A and PI can be derived from penetration If the logarithm of penetration. T. (III) It went through a drilling process. Fig.T1 and T2 using the temperature. EXPERIMENTAL PROCEDURES Specimens were prepared exactly as specified in ASTM D36-95 in precisely dimensioned brass rings and main- tained at a temperature of not less than 10 °C below the expected softening point (SP) for at least 30 minutes be- fore the test.PI of the response of bitumen to variation in temperature.05 g) was A = The temperature susceptibility centered on each specimen and heat was then applied to the beaker so as to raise the temperature by 5±0. P. were then opis) placed in a liquid bath filled to a depth of 600±3 mm and the whole system maintained at a temperature of 5±1 °C for 15 minutes (Freshly boiled distilled water was used log P = AT + K (1) for the bitumen softening point). 20(1 . K = Constant men touches the base plate was recorded to the nearest The value of A varies from 0.25 A ) PI = (3) phalt binders with low penetration numbers (called 1 + 50 A "hard") are used for warm climates. it is possible to predict its behavior in an application.. Therefore. where A 9. = 50 A (2) 10 + PI Knowing the penetration index of particular bitumen. they become softer when The value of PI ranges from around -3 for high temper- heated and harden when cooled.001 5 to 0. Drill and Boring Tool were used.5 mm steel ball bearing (weighing 3. (II) The rod was then stepped turned. there may be considerable difference in temperature re- ture were recorded. (IV) Then it went through boring and step boring. PENETRATION INDEX (PI) of about zero for road bitumen. sponse. For this reason they de- COMPUTATION fined the penetration index (PI) as: The penetration index represents a quantitative measure 20 . a straight line is obtained such that: equation: NAFTA 63 (9-10) 319-323 (2012) 321 . All bitumen display thermoplastic properties i. 4. (II) Milling machine/dividing head-:This was used to make holes on the centering guide and also to make sure the holes were equal to each other.06 showing that 0. 4. Shouldered rings A brass rod of 23 mm by 9 mm was used to fabricate the shouldered rings. EHINOLA.2 °C.e. 3. or explicitly. The preparation involved heating the bitu- men samples until it boiled and was able to be poured (pouring temperature). Screws 2BA Screw and 2BA Tap were used.SOFTENING POINT AND PENETRATION INDEX OF. One of the best known is that The PI is an unequivocal function of A and hence it may developed by Pfeiffer and Van Doormaal which states be used for the same purpose.

1 Conventional paving bitumen. but Agbabu (AB) 330 0. its sulphur Agbabu (AB) 250/330 -3. improving its workability when hot Ilubirin (IB) 50/70 -1. SOFTENING POINT AND PENETRATION INDEX OF. Table 1..3 Conventional paving bitumen.046 lected can be applied successfully on road construction in the tropics. 3. FALODE .10 110 30 Water 8 0. and 4). Agbabu A= (4) T1 .log 800 A= (5) T1 . Results of the softening point from the study area Softening Point Temperature Pouring Temperature Room Temperature Time Sample Source Bath Liquid (°C) (°C) (°C) (min. 6. Sul- phur usually reduces the high tem- Ode-Omode Mile 2(OB) 160/220 -1. Results of penetration and sulphur content from the study area on the SP and PI results.. OB. sented in tables 1 and 2 respectively.64 0.64 wt% (Table 2).6 Conventional paving bitumen. log pen at T1 . OB.log pen at T2 The bitumen grade is summarized in Table 3.T2 (AB) sample flows at room temperature and are usually best applied for pavement in temperate regions of the Pfeiffer and Van Doormaal (year) found that most bitu- men had a penetration of about 800 dmm ( deci-milli- metre) at the ASTM softening point temperature. However.106 men.120 Equations (3) and (5) were applied in this study to cal- culate first for A (temperature susceptibility of bitumen) and PI (penetration index).040 temperature susceptible bitu- Loda (LB) 65 0.42 0.softening point .20 softening point PI = (6) 50 log pen .Three of the four samples col- Ode-Omode (OB) 170 0.45 0. Poloeni stupèani grafikon s toèkama razmekšanja i ranged from 30 to 48. thereby making it com- pacting. and its deformation to resistance when cold. Sample AB could be categorized as Ilubirin (IB) 60 0.392 this can only be achieved after they must have been upgraded.OLUGBENGA A.500 log pen .42 and 0. RESULTS AND DISCUSSION Fig 3. OB and LB samples meet the requirement for Penetration Sulphur content ( Cobalt/Nickel ratio Locations (decimillimetre) weight %) (weight %) conventional pavement bitumen. the result of the sulphur content shows Table 3.. The sulphur contents are between 322 NAFTA 63 (9-10) 319-323 (2012) .) AGBABU (AB) 30 104 30 Water 1 ILUBIRIN (IB) 48 110 30 Water 8 ODE-OMODE (OB) 38. LB and IB.ASTM softening point Substituting equation (5) in equation 3 and assuming a penetration test temperature of 25 °C gives: 1952 . These were calculated from the measured softening point temperatures and penetra- tions. Loda (LB) 50/70 -1.. for bitumen to be used as Bitumen location Grade Penetration index Best possible use road pavement material. Based Table 2. Bar chart showing softening point and penetration The SP and PI results for the bitumen samples are pre- index plot of AB.52 0. The SP results Sl. Replacing T2 in the above equation by the ASTM soften- ing point temperature and the penetration at T2 by 800 they obtained equation (5): log pen T1 . perature viscosity of bitumen.8 Temperature susceptible bitumen content should be between 4-6%. In fact. OLUGBENGA A.10 °C and the PI ranged from 60 to indeksom penetracije za AB. IL.10 102 30 Water 4 LODA (LB) 48. LB i IB 330 mm (Figs. EHINOLA. The predictive Grade of Bitumen that all the samples have low sulphur.

resins (responsible for adhesion and ductility) and oils (low molecular weight. Falode. OLUGBENGA A. "Offshore Stratigraphy and Paleontology of the Dahomey (Benin) Embayment. ASTM (1978): "Standard Tests Method for Resistance to Plastic Flow of Bitu- minous Mixtures using Marshall Apparatus. E. (1985): "Chemical Composition of Bitumen Extracted from tumen are also applied in industrial processes. PP.425 -433. Los Angeles. Ibadan. pp. Aho. Klemme. 1981. 1992. The Nigerian Min- ing and Geoscience Society.. Fig 4. R and Ehinola. Egashira. 3. Uni- versity of California. and Adegoke. NAPE Bull.G.. pp. viz. W. Judson (eds). Depart- ment of Geology.105-110. Petroleum and Global Tec- Sl. p. Poloeni stupèani grafikon s toèkama razmekšanja tonics. "Global Basin Classi- fication System AAPG. Ago-Iwoye. Ekweozor.Pyrolysis study of Nige- widely used method of measuring the consistency of a bi. LB are Conventional pavement grades and Sample AB is temperature susceptible grade. Monismith. The particular kind of grade applied in the construction of road goes a long way to determine the durability or fail- ure of the road. C. and Enu. 18(1): 130-137. U.R. Ekweozor. 3.A. C. Heatflow and Hydrocarbon in minutes Recovery". 54. H. O. tively these bitumen reserves can be cracked to get other 13. (stupnjeva) nasuprot vremena u min. 7. O. California. (l.379.A. NJ. 44:65-81. CONCLUSION The ring and ball apparatus has shown that the bitumen samples from the study area are not the same but of two grades. FALODE . Princeton University Press: Princeton.P. Proceedings. Energy and Environmental Research Group. (1968) "Application of the Indirect Tensile to Stabilized Materials.Properties. 1975. In: A.94. References 1. Ehinola. University of Ibadan. University of Ibadan. De- partment of Geology. Fischer and S.235. 251-304. The low sulphur content would have defi- nitely affected the SP and PI of the bitumen and study on v the sulphurisation of Nigeria bitumen would possibly Authors: help to improve the grade." Annual Book of ASTM Stan- dards. It is a means of classification rather than a measure of quality (The en- gineering term consistency is an empirical measure of the resistance offered by a fluid to continuous deforma- tion when it is subjected to shearing stress). I." Highway Research Record No. "Tectonic Evolution and Creta- petroleum products. I. 5. Bull. .. 4. Ibadan. H. M. Low grade bi. Nigeria. tuminous material at a given temperature. Nafta. University of Ibadan. Olugbenga A. M. O. Energy and Environmental Research Group.. and Nwachukwu.S. Bilman. Kennedy. 200284." Proceedings.. Part 15. alterna. T. and Hudson.D. 2003. E. 67:2175-2193. ehinola01@yahoo. 200284.. Third International Conference on Heavy Crudes and Tar Sands.. 7(2):121-130. De- partment of Petroleum Engineering. Highway Re- search Board. world but not in tropic regions like Nigeria. "Textural Characteristic of the Nigerian Tar Sands". P. 82 .Editors. Enu. 6. PP 44-64 8. (1989): "The Origin of Tar Sands of South-Western Nigeria. Nigerian Tar Sands"..A.I. Olugbenga A. W. The type and amount of these constituents are determined by the source petroleum and the method of processing at the refinery. 1985. A. Bulletin 4." Nigerian Association of Petroleum Exploration. ria bitumen and its fractions. 200284. F.135-138 7. Kingston. no. (1990): "Geochemistry of Oil Sands of Southwestern Nige- ria. pp. John Read and David Whiteoak(2003): The Shell Bitumen Book. The consis- tency is a function of the chemical constituents of bitumen. R. C. Oluwole. 2. Samples OB. A. U. responsible for strength and stiffness). 1983. the relative proportions of asphaltenes (high molecular weight. and Williams. D.14 ceous Stratigraphy of the Dahomey Basin".. Geol. 11. Nige- ria. J. M. John Read and David Whiteoak(1995): The Shell Bitumen Industrial Book. pp. The penetration of bituminous material is the most 14. Min. 9. West Africa". Design and Performance. J.36 -48.S. Berkeley.A. ehinola01@yahoo. Nigeria George Jonathan. IL. Sonibare." The Institute of Transportation and Traffic NAFTA 63 (9-10) 319-323 (2012) 323 .G. S. C. Oyo State. responsible for viscosity and fluidity). 4. 373.SOFTENING POINT AND PENETRATION INDEX OF. A bar chart of softening point (degrees) against time 10. Oyo State. "Geothermal Gradients. I. vol. 12. Dishroon.D. pp. Sedimen- tary Geology. Energy and Environmental Research Group. 81-88. Oyo State. Omatsola.O. Oil and Gas Journal. B. Ibadan. First Workshop on Nigerian Tar Sands. OLUGBENGA A.961): "Asphalt Paving Mixtures .