1. Introduction

2. MATERIAL AND METHODOLOGY

2.3. Asphaltene Extraction Experimental Procedure

As illustrated in Figure 2, a specialized closed-chamber filtration apparatus was designed for asphaltene particle extraction. To initiate the procedure, a 22-micron Whatman filter paper was positioned in the apparatus, and its baseline weight was documented. In a subsequent step, 1 gram of crude oil was amalgamated with 40 cm^3 of heptane in a glass beaker. This mixture was then subjected to mechanical stirring at a rate of 200 rpm for a period of 60 minutes, facilitated by a magnetic stirrer. To mitigate the evaporation of heptane, the beaker was securely capped. Following agitation, the prepared sample was transferred to the filtration apparatus, which was hermetically sealed. The sample was allowed to undergo filtration for a 24-hour period. After this interval, the filter paper, now laden with asphaltene particles, was carefully removed (see Figure 3a) and exposed to open-air conditions for an additional 24 hours to achieve complete drying (see Figure 3b). The weight percentage of the extracted asphaltenes was subsequently determined according to Equation 1.

$$\mathrm{A}\mathrm{s}\mathrm{p}\mathrm{h}\mathrm{a}\mathrm{l}\mathrm{t}\mathrm{e}\mathrm{n}\mathrm{e} \mathrm{w}\mathrm{t}.\mathrm{\%}=\frac{{\mathrm{w}}_{\mathrm{w}\mathrm{e}\mathrm{t}}-{\mathrm{w}}_{\mathrm{d}\mathrm{r}\mathrm{y}}}{{\mathrm{A}}_{\mathrm{t}}}$$

1 

Where $w_{dry}$ is the weight of filter paper before filtration, $w_{wet}$ is the weight of filter paper after filtration and $A_t$ is the total weight of asphaltic crude oil.

Figure 1. Filtration Apparatus used for Asphaltene Extraction.

Figure 1. Filtration Apparatus used for Asphaltene Extraction.

Figure 2. Asphaltene Precipitation on Filter Paper (a) before drying, (b) after 24hrs.

Figure 2. Asphaltene Precipitation on Filter Paper (a) before drying, (b) after 24hrs.

The following calculation was done to obtain asphaltene weight percent (see Equation 1):

$$\mathrm{A}\mathrm{s}\mathrm{p}\mathrm{h}\mathrm{a}\mathrm{l}\mathrm{t}\mathrm{e}\mathrm{n}\mathrm{e} \mathrm{w}\mathrm{t}.\mathrm{\%}=\frac{{\mathrm{w}}_{\mathrm{w}\mathrm{e}\mathrm{t}}-{\mathrm{w}}_{\mathrm{d}\mathrm{r}\mathrm{y}}}{{\mathrm{A}}_{\mathrm{t}}}$$

1 

Where $w_{dry}$ is the weight of filter paper before filtration, $w_{wet}$ is the weight of filter paper after filtration and $A_t$ is the total weight of asphaltic crude oil.

3. Experimental Result and Discussion

3.1. Confocal images of Western Missouri oil

Figure 3a displays time-lapsed, processed confocal images for South-Western Missouri oil at a 5g/l asphaltene concentration, 60% heptane concentration, and 25°C. Initially, asphaltene flocs are observed within the 2 to 5-micron range. Post 90 minutes, the floc size expands dramatically, reaching up to 35 microns, but later contracts to a 2 to 20-micron range at the 300-minute mark. Figure 3b, keeping other parameters constant, highlights the processed images at 8g/l asphaltene concentration. At 5 minutes, the mean particle diameter varies between 2 to 18 microns. After 90 minutes, the particle size lies in the 2 to 30-micron range and extends up to 50 microns by 300 minutes. In Figure 3c, set at 10g/l, the initial particle size spans 2 to 8 microns, expanding to 22 microns at 90 minutes and 50 microns by 300 minutes. A noticeable increase in particle count over time is evident from Figure 3c. Figure 3d shows the processed image at 70 % heptane concentration, 10g/l asphaltene concentration, and 25 ^OC. the result indicates that at 5 minutes, the mean particle diameter is in the range of 2 to 15 micron. After the mean equivalent diameter increase from 3 to 36 microns while at 300 mean particle diameter increases from 3 to 60 microns. Figure 3e shows the processed image at a 100-rpm shearing rate with 10g/l asphaltene concentration, 60% heptane concentration, and 25 ^OC. The mean particle diameter range is between 2.5 to 11 microns at 5 minutes. After 90 minutes mean particle diameter increased and the range in between 4- and 55 microns. after 300 minutes, the mean asphaltene diameter range between 2 to 65 microns. Across all processed images, a consistent increase in particle count is also observed over time.

Figure 3. Processed images using MIPAR software (a) at asphaltene concentration 5g/l (b) at asphaltene concentration 8g/l, (c) at Asphaltene concentration 10g/l (d) 70:30 heptane to toluene ratio (e) 100 RPM shearing.

Figure 3. Processed images using MIPAR software (a) at asphaltene concentration 5g/l (b) at asphaltene concentration 8g/l, (c) at Asphaltene concentration 10g/l (d) 70:30 heptane to toluene ratio (e) 100 RPM shearing.

Results

Discussion

3.3. Cumulative Yield Percent Analysis using Centrifuge Experiments

There are three points of interest in cumulative asphaltene yield results. 1) Rate of aggregation 2) Changes in rate of aggregation at different time steps. 3) Any sharp increase or decrease in cumulative asphaltene yield. 4) total asphaltene yield.

Figure 5a shows the effect of the asphaltene concentration on the cumulative asphaltene yield in 60:40 and 70:30 Heptol ratio. Using 70:30 Heptane ratio (red line), two zones are observed. Asphaltene yield grows linear from 0 min to 90 min at the rate of 0.42 mg per min in zone 1. However, the rate of aggregation declines at 0.242 mg per minute from 90 to 300 minutes in zone 2. No sharp increase in cumulative asphaltene yield was observed. At 60:40 ratio (black line), three different zones are observed. From 0 to 30 minutes, 0.33 mg per minute of rate of cumulative yield. A sharp increase is observed from 30 to 45 minutes. After 45 minutes till 300-minute, 0.23 mg per min is observed. Total asphaltene yield at 70:30 is 92.5 mg while 89 gram at 60:40 Heptane to toluene ratio out of total 100 grams in both cases. The result indicates that increasing the heptane to toluene ratio has increases the asphaltene precipitation yield. The results are in agreement with J.A Duran, 2019 and Maqbool et al 2009. The result indicates the two different regions of rate of cumulative asphaltene yield are observed. The trends are in good agreement with Maqbool et al 2008 at 46.5 vol% and 50 vol % of asphaltene. However. any sharp increase in cumulative yield is not observed in their results. In the first zone, the rate of asphaltene yield is higher than in zone two. This could be due to increase in heptane solubility while decreasing the asphaltene solubility leading to continuous nucleation of large number of particles in zone 1 and second zone nucleation of asphaltene particles decline considerably but large flocculates are formed due to aggregation mechanism as shown in Figure 3e. Therefore, zone 1 is dominated by nucleation of particles and zone 2 is dominated by aggregation of particles. The sharp increase at 60:40 at 90 minutes is attributed to the aggregation mechanism which is caused by high π−π stacking, van der Waals (vdW) interaction, hydrogen-bonding interaction.

Table 5. Effect of HEPTOL on asphaltene mass yield 

Table 5. Effect of HEPTOL on asphaltene mass yield 

Parameter: HEPTOL	Rate of cumulative yield in Zone 1 (mg/min)	Rate of cumulative yield in Zone 2 (mg/min)	Total Cumulative Asphaltene Yield (mg)
60:40	0.33	0.23	89
70:30	0.42	0.242	92.5

Table 6. Effect of shearing rate on asphaltene mass yield 

Table 6. Effect of shearing rate on asphaltene mass yield 

Parameter: Shearing Rate	Rate of cumulative yield in Zone 1 (mg/min)	Rate of cumulative yield in Zone 2 (mg/min)	Total Cumulative Asphaltene Yield
No Shearing	0.33	0.23	89
100 RPM	0.33	0.24	91

Table 7. Effect of asphaltene concentration on asphaltene mass yield 

Table 7. Effect of asphaltene concentration on asphaltene mass yield 

Parameter: Asphaltene concentration	Rate of cumulative yield in Zone 1 (mg/min)	Rate of cumulative yield in Zone 2 (mg/min)	Total Cumulative Asphaltene Yield
10g/liter	0.33	0.23	89
8 g/liter	0.293	0.12381	70.5
5 g/liter	0.34	0.045238	40

Figure 5b shows the mean equivalent diameter for all given asphaltene concentrations at 23 C, no shearing and 60:40 heptane to toluene ratio. At 10g/liter (black line), three different zones are observed. From 0 to 30 minutes, 0.33 mg per minute of rate of cumulative yield. A sharp increase is observed from 30 to 45 minutes. After 45 minutes till 300-minute, 0.23 mg per min is observed. At 8 g/liter, three different zones are observed. From 0 till 75 minutes, the rate of cumulate yield is 0.293 mg per minute is observed. In zone two, A sharp increase in the yield is observed from 22 mg to 44.5 mg and in zone 3, from 90 min to 300 min, rate of cumulative yield of 0.12381 mg per min is observed. At 5g/liter asphaltene concentration, two zone are observed, in zone 1 from 0 to 90 min, the rate of cumulative yield is 0.34 mg per min. and in zone 2 from 90 to 300 minutes the rate of cumulative yield is 0.045238 mg per min. The result indicates the increasing the asphaltene concentration increases the cumulative asphaltene yield. The results are in good agreement with Rastegari H. et al. (2004). Furthermore, at 10g/liter and 8g/liter, a sharp incline is observed attributed to aggregation mechanism. However, such aggregation process starts earlier in the 10g/liter cases and later in 8 g/liter and at 5g/ liter no such aggregation process is observed. This indicates the increasing the asphaltene concentration causes quicker aggregation process and higher aggregation process. Furthermore, higher cumulative yield rate is attributed in zone 1 is attributed to higher nucleation and in zone 2m nucleation rate is reduced and aggregation of asphaltene flocs is increased. This implies that in zone 1 decreasing asphaltene solubility is the main mechanism while in zone 2 π−π stacking, van der Waals (vdW) interaction, hydrogen-bonding interaction are dominant forces since no new asphaltene flocs are formed. Figure 5c shows the cumulative asphaltene yield at different shear rates. At no shearing (black line), as mentioned in earlier cases, three different zones are observed. From 0 to 30 minutes, 0.33 mg per minute of rate of cumulative yield. A sharp increase is observed from 30 to 45 minutes. After 45 minutes till 300-minute, 0.23 mg per min is observed. At shearing of 100 rpm, similar trend was observed till 75 minutes, and after 75 minutes a sudden increase in particle size is observed from 36 mg to 58 mg. After that rate of cumulative yield is 0.24 mg per min. The result indicate the increasing the shearing rate will increase the asphaltene yield, The results are in good agreement with Nguyen et al 2021. This is due to better solubility of heptane due to high shearing. The result further records that sharp increase in cumulative yield attributed to aggregation process was observed multiple time at 100 rpm shearing rate. It is reflected that shearing the asphaltene could increase the forces such as π−π stacking, van der Waals (vdW) interaction, hydrogen-bonding interaction leading to higher aggregation process.

Figure 5. Cumulative asphaltene yield over time (a) At different Heptane-Toluene concentration (b) At different shear rates (c) At different asphaltene concentrations.

Figure 5. Cumulative asphaltene yield over time (a) At different Heptane-Toluene concentration (b) At different shear rates (c) At different asphaltene concentrations.

3.4. Correlation between asphaltene mass yield, asphaltene particle count and diameter range

In this study, the correlation between asphaltene mass yield, particle count, and diameter range is examined to address the existing gap in understanding the specific mass of asphaltene particles at various diameters. Given this gap, it's difficult to ascertain how the number of particles, based on their diameter, contributes to a specified mass yield. To tackle this, the study categorizes mean particle diameters into bins, each containing a range of mean equivalent diameters as detailed in Table 8. The study performs four distinct analyses: 1) comparing particle counts in early stages (0-90 minutes) to those in later stages (90-300 minutes) concerning mass yield; 2) focusing solely on early-stage particle counts in relation to mass yield; 3) examining particle counts only in later phases with respect to mass yield; and 4) observing overall trends in asphaltene mass yield over time.

Figure 6a illustrates the time-dependent asphaltene yield and particle count at a concentration of 10g/l asphaltene, complemented by Table 8, which presents the particle size distribution for all experimental cases. The data suggest that asphaltene mass yield can fluctuate over time, influenced by various factors. For instance, the mass yield was initially 5 mg at 5 minutes, decreased to 2 mg at 60 minutes, escalated to 21 mg at 240 minutes, and then declined to 15 mg at 300 minutes. It's noteworthy that an identical mass yield of 5 mg was observed at both 5 and 90 minutes; however, the particle counts were 1149 and 755, respectively. At the 5-minute mark, the mass is predominantly made up of larger, recently nucleated particles ranging from 2 to 9 microns in diameter, while at 90 minutes, particles had diameters ranging from 2 to 30 microns, as detailed in Table 8. At the 120- and 180-minute intervals, the mass yields were 8 mg and 7 mg with particle counts of 1647 and 1560, respectively, indicating minimal fluctuation in particle numbers. Conversely, in an earlier timeframe between 15 and 30 minutes, particle counts were 996 and 626, with similar diameters. These findings suggest that early-stage processes are dominated by nucleation and aggregation, while later stages see growth and aggregation as the prevailing mechanisms, even though fewer particles are nucleating compared to the early stages.

At an asphaltene concentration of 8g/l, Figure 6b shows the time-resolved asphaltene yield and particle count. The data indicate that the asphaltene mass yield fluctuates between 2.5 to 4.5 mg and 5.5 to 7.5 mg from 120 to 300 minutes, echoing the previously established notion that mass yield can vary over time. At the early stage, marked at 45 minutes, the particle count is 1734 with a mass yield of 4.5 mg, while at the later stage, specifically at 120 minutes, the count is nearly identical at 1732 but with a slightly higher mass yield of 5.5 mg. In the early phase, smaller particles dominate, falling within a diameter range of 2-15 microns. In contrast, the later stage displays a variety of processes—nucleation, growth, and aggregation—with particle diameters ranging from 2 to 19 microns. Moreover, particle counts of 259 and 411 were observed at 5 and 30 minutes, both correlating to a mass yield of 2.5 mg. This behavior aligns with the earlier case, reaffirming that the early stage is largely governed by nucleation events, characterized by a smaller mean equivalent diameter

Figure 6c illustrates the asphaltene mass yield and particle count at an asphaltene concentration of 5g/l. The data reveal that mass yield ranges from 2-4 mg during the initial 0-45 minutes and spikes to 9 mg at 60 minutes, while between 75 and 300 minutes, it stabilizes within the 3-4.5 mg range, reaching 7 mg at 120 minutes. Despite the time lapse, the mass yield does not show a significant increase, although evidence of severe particle aggregation is observed in both early and late stages. The particle size predominantly falls between 2 to 11 microns across these stages. Notably, nucleation persists even in later stages at 120 and 180 minutes, where particle diameters of 3-5 microns prevail, as detailed in Table 8, pointing to the dominance of nucleation and aggregation mechanisms.

Turning to Figure 6d, which focuses on a heptane concentration of 70, the asphaltene mass yield varies from 5.5 to 10.5 mg in the early stage (0-90 minutes) but then increases to range between 8.5 and 10.5 mg. This pattern contrasts with previous observations. Specifically, at 5 and 120 minutes, the mass yield stabilizes at 8.5 mg with particle counts of 1977 and 2809, respectively. Similarly, at 30 and 240 minutes, a mass yield of 10.5 mg is coupled with particle counts of 2185 and 3500, respectively. These observations suggest that nucleation not only dominates the early stage but also intensifies in the later stage, co-occurring with particle growth.

Figure 6. Asphaltene mass yield (mg) vs time, vs particle count (a) 10g/l, 25 ^o C, 60 % heptane concentration and no shearing (b) 8g/l, 25 ^o C, 60 % heptane concentration and no shearing (c) 5g/l, 25 ^o C, 60 % heptane concentration and no shearing (d) 10g/l, 25 ^o C, 70 % heptane concentration and no shearing.

Figure 6. Asphaltene mass yield (mg) vs time, vs particle count (a) 10g/l, 25 ^o C, 60 % heptane concentration and no shearing (b) 8g/l, 25 ^o C, 60 % heptane concentration and no shearing (c) 5g/l, 25 ^o C, 60 % heptane concentration and no shearing (d) 10g/l, 25 ^o C, 70 % heptane concentration and no shearing.

Table 8. Asphaltene particle size distribution over time. 

Table 8. Asphaltene particle size distribution over time. 

Bins	Counts
(a) Asphaltene concentration 8g/liter, 25 oC,
Particle Diameter Bin	5 mins	15 mins	30 mins	45 mins	60 mins	75 mins	90 mins	120 mins	180 mins	240 mins	300 mins
Total Counts
3-5	230	242	265	974	1134	1134	1705	1024	1089	1124	2167
5-7	7	29	71	221	196	196	312	317	760	820	720
7-9	7	34	56	240	120	120	135	249	621	516	461
9-11	5	25	13	111	46	46	31	84	116	316	116
11-13	3	3	5	86	31	31	12	36	51	51	55
13-15	4	0	1	44	20	20	1	17	25	4	12
15-17	2	1		31	12	12	0	3	3	3	3
>> 17-19	1			25	10	10	2	4	1	1	1
(b) Asphaltene concentration5g/liter, 25 oC,
Particle Diameter Bin	5 mins	15 mins	30 mins	45 mins	60 mins	75 mins	90 mins	120 mins	180 mins	240 mins	300 mins
Total Counts
3-5	33	70	826	643	1081	643	431	1411	1131	583	446
5-7	2	4	70	67	128	67	126	368	281	144	81
7-9	0	1	29	19	72	19	89	272	174	70	24
9-11		0	4	3	16	3	16	95	44	14	4
11-13		1	2	0	10	0	3	50	7	6	0
13-15		1	0	2	7	2	3	18	3	0	0
15-17			1	0	1		3	12	1		0
>> 17-30			1		5		1	9			2
>>30-40								1
>40-50				1		2		1
>50+						1
( c) Asphaltene concentration 10g/liter, 25 oC,
Particle Diameter Bin	5 mins	15 mins	30 mins	45 mins	60 mins	75 mins	90 mins	120 mins	180 mins	240 mins	300 mins
Total Counts		996
3-5	840	697	440	105	1508	2780	264	626		273	1928
5-7	174	173	99	8	180	497	109	279		131	480
7-9	107	101	71	5	76	410	118	279		128	466
9-11	17	17	12	0	17	166	71	154		43	187
11-13	7	3	4	0	6	123	57	113		36	119
13-15	1	2	0		1	65	38	78		24	48
15-17	3	3	0			48	36	52		16	27
>> 17-30						19	20			27	20
>>30-40						1				1
>40-50										1
>50+											1
(d) Asphaltene concentration 10g/liter, 70:30 HEPTOL Ratio , 25 oC, No shearing
Particle Diameter Bin	5 mins	15 mins	30 mins	45 mins	60 mins	75 mins	90 mins	120 mins	180 mins	240 mins	300 mins
Total counts
2.5	7	1285	1690	1690	3309	2737	1986	1986	2651	2668	7323
2.5-7.5	2	376	422	422	616	270	268	268	155	298	989
7.5-12.5		204	57	57	84	37	8	8	3	28	142
12.5-17.5		81	6		6	7	1	1	0	1	25
22.5		19	3		2	0	2	2		1	6
27.5		9			0	1	0			1	2
27.5 -50		3			2	1				1	2

4. Conclusion

5. Future Work

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