STRUCTURE FROM DIFFERENT POSITIONS ON
THE ANIMAL FOR OVINE LEATHER
5.1 Introduction
Leather is a natural product and as such is subject to a certain amount of variation, both across skins and between skins. In the previous chapter variations in the organisation of fibrillar collagen between skins was investigated. There were significant variations between the fibrillar collagen structure of skins and some of that variation could be related to tear strength. In this chapter variations in the fibrillar collagen structure across ovine skins will be investigated.
There are many reasons why studying the consistency of the collagen structure across skins is of interest. To determine if a skin meets the specifications for use in a particular
application, tests of the skin need to be undertaken. These tests are often destructive and therefore small samples are used. By determining the variation in properties across the skin, the importance of sampling position can be better understood, as some applications require large leather pieces which are consistent across their entirety.
There are many tests used to determine the strength of leather samples, including tensile and tear tests. Tongue-tear tests involve a square sample that is cut from the middle of one side through to the centre of the sample. This produces two ‘tongues’ which are pulled in
opposite directions, causing failure to occur along a single tear. Stitch-tear testing is used to determine the susceptibility of a material to tearing at a stitched seam. It involves cutting small holes, usually one or two, in one side of a sample and threading a metal wire through them. This wire and the side of the material opposite the holes are then clamped and pulled in opposite directions. Tearing does not necessarily propagate from the site of the holes in stitch tear testing.
Variation of physical properties of leather across cattle hides (Mann et al. 1951; Kanagy et al. 1952; Kanagy et al. 1952; Randall et al. 1952; Maeser 1960; Menkart et al. 1962), as well as kangaroo (Stephens and Peters 1989), mink and fox skins (Mantysalo et al. 1991) have
previously been investigated. These studies found significant variation in tensile strength, tear strength and elongation according to sample location and direction of measurement. Tongue-tear and stitch-tear strengths of bovine hides were found to vary with position, with strengths being lower in the butt and backbone areas and higher in the belly and shoulder regions (Kanagy et al. 1952; Kanagy et al. 1952; Randall et al. 1952). Tensile strength was found to be greatest in the belly region (Kanagy et al. 1952) and tensile strength measurements taken parallel to the backbone were found to be approximately 20% higher than those taken in the perpendicular direction (Randall et al. 1952).
Previous studies have investigated the variation in collagen fibre orientation across bovine leather hides (Osaki 1999), however, this study investigated the orientation only in the direction parallel to the surface, which has not been found to relate to strength (Basil-Jones et al. 2011). The aim of this chapter is to investigate if there is variation in the fibrillar collagen structure across ovine leather skins and how this relates to tear strength. To investigate this variation four positions across the skin were selected, the belly, butt, neck and OSP positions. An illustration of the location of these positions on the skin is provided in chapter 3. Skins were selected based on their tear strength at the OSP so that a range of strengths were represented.
Samples of cross-sections from 29 ovine skins were cut from 4 different positions; the belly, butt, OSP and neck. The belly and neck cross-sections were cut parallel to the backbone while the butt cross-sections were cut perpendicular to the backbone. OSP samples were cut in both directions. In addition samples in all directions; flat and cross- sections, were cut from each position on four skins. Samples were analysed using the methods and sample directions outlined in chapter 3.
5.2 Results
5.2.1 Thickness
The thickness of samples from all positions sampled was measured, with the results shown in Figure 5.1. The neck position was found to be thickest with an average thickness of 1.85 (with a standard deviation of 0.42) mm. The belly was the thinnest position with a
thickness of 1.08 (0.20) mm. The average thickness of the OSP was found to be 1.29 (0.22) mm for samples cut perpendicular to the backbone and 1.36 (0.24) mm for samples cut
parallel. The butt was found to have an average thickness of 1.57(0.39) mm, making it the second thickest position.
Figure 5.1: Thickness of leather taken from different positions on the ovine skin.
Statistical analysis found significant differences between the thicknesses of some of the different positions on the skin. The results of this statistical analysis are shown in Table 5.1. The neck was found to be significantly thicker than all other positions measured except the butt where the difference was not significant. The belly was found to be significantly thinner than all other positions measured except the OSP measured perpendicular to the backbone where the difference was not significant. The butt was also found to be significantly thicker than the OSP measured perpendicular to the backbone.
Table 5.1: The statistical significance of differences between the thicknesses of leather samples from different positions on the skin as determined by Tukey test.
Position Neck
Perpendicular Belly Perpendicular Butt Perpendicular OSP Perpendicular OSP Parallel Neck
Perpendicular Significant Not Significant Significant Significant Belly
Perpendicular Significant Not Significant Significant
Butt
Perpendicular Significant Not Significant
OSP
Perpendicular Not Significant
OSP Parallel
5.2.2 Tear Strength
The tear strength of all positions sampled was measured. The average absolute tear
strength was found to be highest for the neck with an average value of 50.7 (11.7) N. The OSP measured perpendicular to the backbone was found to have the lowest average tear strength with an average value of 35.5 (8.9) N. The belly position had a similar average absolute tear strength with a value of 35.6 (10.5) N. The butt and OSP measured parallel to the backbone had similar average tear strengths with average values of 43.6 (11.8) N and 42.1 (10.5) N respectively (Figure 5.2 a)).
In contrast, the average normalised tear strength was highest in the belly with an average value of 33.6 (9.7) N/mm. The second highest average normalised tear strength value was 31.3 (7.8) N/mm for the OSP measured parallel to the backbone. The remaining three positions had similar normalised tear strength with an average value of 28.1 (6.4) N/mm for the neck, 28.5 (7.2) N/mm for the butt and 28.2 (7.7) N/mm for the OSP measured perpendicular to the backbone (Figure 5.2 b)).
Figure 5.2: a) absolute tear strength and b) normalised tear strength of leather taken from different positions on the ovine skin.
Statistical analysis found significant differences between the absolute tear strengths of most of the positions measured. Results of this analysis are shown in Table 5.2. The only
positions that did not have significant differences between their absolute tear strengths were: the belly and OSP cut perpendicular to the backbone; the neck and OSP cut parallel to the backbone; and the butt and OSP cut parallel to the backbone.
A Friedman test found that the normalised tear strength of skin from belly position samples was significantly higher than that of skin from all other positions except the OSP measured parallel to the backbone where the difference was not significant. There was also a significant difference between the normalised tear strength of OSP samples measured in the different directions, with normalised tear strength being greater when measured parallel to the backbone.
Table 5.2: The statistical significance of differences between the tear strength’s of leather
samples from different positions of the skin as determined by Tukey tests. Bottom left side absolute tear strength and top right side normalised tear strength.
Position Neck
Perpendicular Belly Perpendicular Butt Perpendicular OSP Perpendicular OSP Parallel Neck
Perpendicular Significant Not Significant Not Significant Not Significant Belly
Perpendicular
Significant Significant Significant Not
Significant Butt
Perpendicular Significant Significant Not Significant Not Significant OSP
Perpendicular Significant Not Significant Significant Significant OSP
Parallel
Not
Significant Significant Not Significant Significant
Plots of the normalised tear strength of each position versus the average normalised tear strength of a skin were produced and are shown in Figure 5.3. Skins with a high average tear strength value were found to be consistently strong in all positions measured. This means that skins with a high average normalised tear strength are consistently strong in all positions sampled, as opposed to strong at some positions and weak at others. Trend lines were fitted to these plots with results provided in Table 5.3. These results indicated that the relationship was significant for all positions studied.
Table 5.3: Parameters for fitted regression lines of normalised tear strength of each position versus the average normalised tear strength of a skin data for each position sampled.
Slope r2 P-value (slope)
Neck 0.74 0.62 3.74x10-7
Belly 1.31 0.83 4.7x10-12
OSP 1.04 0.84 2.7x10-12
Figure 5.3: Normalised tear strength of position versus the average normalised tear strength of the entire skin for; a) neck, b) belly, c) OSP and d) butt.
5.2.3 Directionality of Normalised Tear Strength
Tear strength measurements were recorded for all four positions in both the parallel and perpendicular to the backbone direction for four skins with a range of tear strengths. The results are shown Figure 5.4. There was found to be a relationship between tear strengths measured parallel to the backbone and those measured perpendicular to the backbone for all positions measured, with tear strength measured in the parallel direction increasing linearly with that measured in the perpendicular direction.
Neck Belly
Figure 5.4: Perpendicular versus parallel tear strengths for neck - closed circle; belly - open circle; OSP - closed triangle; and butt - closed square, positions.
Regression analysis was performed on data from each position with results provided in Table 5.4. These results indicated that the relationship was significant for all positions studied.
Table 5.4: Parameters for fitted regression lines of perpendicular versus parallel tear strength data for each position sampled.
Slope r2 P-value (slope)
Neck 1.08 0.97 0.011
Belly 0.97 0.98 6.1 x 10-3
Butt 0.84 1.00 1.4 x 10-3
OSP 0.74 0.84 1.1 x 10-14
The tear strength at all the positions measured, except the OSP, was not significantly affected by whether the measurement was taken parallel or perpendicular to the backbone. The OSP was, however, affected by the direction of the measurement, with the tear strength values measured being lower when measured in the perpendicular direction.
5.2.4 Visual Variation in Structure across Cross-Sections
In order to allow greater understanding of how profiles of measured parameters across sample thicknesses relate to the SEM images of skin cross-sections, a SEM image of an
ovine leather cross-section is shown in Figure 5.4. As can be seen from this image, the grain-corium junction is located near the middle of the sample.
Figure 5.5: SEM image of a cross-section of ovine leather showing the approximate location of the grain-corium junction. Scale bar 1 mm.
5.2.5 Amount of Fibrillar Collagen
The amount of crystalline collagen was found to vary throughout the thickness of all samples of ovine leather as shown in Figure 5.6. All sampled positions have the same general profile, with higher concentrations of fibrillar collagen in the corium region than in the grain. It is known that corium is stronger than the grain and that fibrous collagen is the primary contributor to strength, therefore this finding supports this understanding.
The average profile does, however, differ between the positions. The profiles of the OSP cut parallel to the backbone and belly cross-sections are quite similar; the slight difference can be explained by the OSP having a greater thickness. This is understandable as the belly and OSP are quite close to each other. The cross-sections from the butt also have a similar profile to that seen for the belly and the OSP cut parallel to the backbone.
The OSP profile appears to vary significantly with sample direction, when cut
perpendicular to the backbone lower concentrations of fibrillar collagen across the entire
Grain edge Grain – corium junction Corium edge
profile are observed. The neck samples, which appear to have the greatest concentration of collagen in the corium and the thickest grain layer of all positions sampled, show the largest differences in profile compared to other positions.
Figure 5.6: Profiles of amount of crystalline collagen across sample thicknesses a) cut parallel to the backbone from the: neck - closed circle; belly - open circle; OSP - triangle, and b) cut perpendicular to the backbone from the: butt - closed square; OSP- open square.
Figure 5.7 showsthe average amount of collagen versus tear strength for samples from different positions for four skins. Statistical analysis found that there was no significant difference between the average amounts of fibrillar collagen in samples taken from different sample positions on the skin, despite obvious differences in cross-sectional profiles. Although the data appears to have a downwards trend, there was found to be no significant relationship between the amount of crystalline collagen and tear strength. A regression line fitted to all the data gave a slope of -0.035 arb. units.mm/N, r2 value of 0.13 and P-value of 0.09. This finding is consistent with that found in chapter 4 for samples from the OSP position. Similarly, regression analysis of samples of skin from different positions found there was no significant relationship between the amount of crystalline collagen and the tear strength in any of the positions studied.
Figure 5.7: Average amount of crystalline collagen versus tear strength for the: neck - closed circle; belly - open circle; OSP - closed triangle; and butt - open triangle.
5.2.6 d spacing
Ovine leather cross-sections display a characteristic d spacing profile with a dip in d spacing near the middle of the cross-section. The graphs in Figure 5.8 show that skin samples from the positions sampled all display this profile. As can be seen, the depth of the dip in d spacing varies between sample positions, with samples having a higher average thickness displaying a larger dip. The dip is most significant in the neck position, which is the thickest of all positions sampled. In contrast the dip is only very slight in the belly and butt
positions. The profiles for the OSP cut parallel and perpendicular to the backbone are quite similar, indicating that d spacing profile is independent of the direction of measurement.
Figure 5.8: Profiles of d spacing across sample thicknesses a) cut parallel to the backbone from the: neck - closed circle; belly - open circle; OSP - triangle; and b) cut perpendicular to the backbone from the: butt - closed square; OSP - open square.
Tear strength and d spacing were shown not to be related in any of the positions studied. Figure 5.9 shows the average d spacing for cross-sections of ovine leather from the
different positions. It can be seen from this figure that there is no correlation between tear strength and d spacing. This is consistent with the findings in chapter 4. There are,
however, differences between the average d spacing of the different positions.
Figure 5.9: Average d spacing versus tear strength for samples a) cut parallel to the backbone from the: neck - closed circle; belly - open circle; OSP - triangle; and b) cut perpendicular to the backbone from the: belly - closed square; OSP - open square.
Butt samples were cut perpendicular to the backbone while the other samples were cut parallel to the backbone. The analysis of the OSP position revealed that there is no significant difference (|t-stat|= 0.94, t-crit = 2.01, P = 0.35) between the d spacing of cross-sections cut parallel and perpendicular to the backbone and it was assumed that this trend is consistent across the entire skin. Analysis of the samples from different positions and analysed in both directions support this assumption (|t-stat|= 1.86, t-crit = 2.05, P = 0.07), although the sample size was quite small. It was therefore concluded that the results from samples cut perpendicular to the backbone could be compared with those cut in the parallel direction.
A Tukey test found that the neck had a significant lower average d spacing than that of all other positions measured. The only other significant difference in d spacing was between the belly and OSP cut perpendicular to the backbone (Table 5.5), with the average d spacing being higher in the belly. These differences could be explained by the variation in the d spacing profile with position. The average d spacing value was lowest (64.20 (0.25) nm) for the neck position which had both the largest variation in d spacing across its profile and the greatest thickness. The average d spacing value was highest for the belly
and butt positions (64.43 (0.20) nm and 64.38 (0.23) nm respectively) and showed the lowest variation in d spacing across its profile. The average value for the OSP was
64.31(0.22) nm in the parallel direction and 64.23 (0.62) nm in the perpendicular direction.
Table 5.5: The statistical significance of differences between the dspacing’s of leather
samples from different positions on the skin as determined by Tukey test. Position Neck
Parallel
Belly Parallel
Butt
Perpendicular OSP Parallel OSP Perpendicular Neck
Parallel
Significant Significant Significant Significant Belly
Parallel
Not
Significant Not Significant Significant Butt
Perpendicular Not Significant Not Significant
OSP Parallel Not Significant OSP Perpendicular
To investigate whether the variations in average d spacing with position was due to the extent of the variation in d spacing across cross-sectional thicknesses the variation in d spacing across the profile was calculated. The variation in d spacing across the profile of each sample was calculated by subtracting the minimum d spacing value recorded from the maximum d spacing value recorded and was used to approximate the extent of dip in the d spacing profile. The variation in d spacing was highest for neck samples with an average value of 1.12 nm. The variation in d spacing was lowest for the belly and butt samples with average values of 0.49 nm and 0.66 nm respectively. The average value for the OSP was 0.74 nm in the cross-sectional direction parallel to the backbone and 1.04 nm in the cross- sectional direction perpendicular to the backbone.
The variation in d spacing of the neck was found to be significantly higher than that of all other positions except the OSP cut perpendicular to the backbone where the difference was not significant (Table 5.6). There were also other statistically significant differences in the variation in d spacing with the value of the belly being lower than that of the OSP cut
in both directions and the value of the butt being lower than that of the OSP cut perpendicular to the backbone.
Table 5.6: The statistical significance of differences between the variation in d spacing across profiles of leather samples from different positions on the skin as determined by Tukey test. Position Neck Parallel Belly Parallel Butt
Perpendicular OSP Parallel OSP Perpendicular Neck
Parallel
Significant Significant Significant Not Significant Belly
Parallel
Not
Significant Significant Significant Butt Perpendicular Not Significant