Lynne Wong's PhD thesis

Lynne Wong's PhD thesis Lynne Wong's PhD thesis

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Sample Table 4.5. Reproducibility of Brix-free water determinations on fibre samples. Mass of Mass of bottle Mass of bottle + sample Mass of Mass of dis. H 2O/g Brix before Mean p 1 Brix after Mean p 2 Adjusted blank (b) bottle/g empty sample/g + 110 g distilled + water/g sample/g w 1 w 2 p 1 p 2 p 2w 2w 3/(w 1w 4) 1b Rind fibre 225.48 231.24 342.47 5.76 111.23 0.00 0.00 0.00 0.000 0.01 0.01 0.01 0.010 0.009 2b Rind fibre 5.76 111.23 0.009 3b Rind fibre 5.76 111.23 0.009 4b Stalk fibre 226.13 231.45 344.88 5.32 113.43 0.00 0.00 0.00 0.000 0.01 0.01 0.02 0.012 0.012 5b Stalk fibre 5.32 113.43 0.012 6b Stalk fibre 5.32 113.43 0.012 7b Top fibre 202.07 208.02 319.60 5.95 111.58 0.00 0.00 0.00 0.000 0.07 0.06 0.07 0.067 0.061 8b Top fibre 5.95 111.58 0 0 0 0.064 9b Top fibre 5.95 111.58 0.064 10 Green leaf 11 b fibre Green leaf 12 b fibre Green leaf b fibre Sample 220.77 226.34 340.25 5.57 113.91 0.00 0.00 0.00 0.000 0.03 0.03 0.04 0.033 0.039 5.57 113.91 0 0 0 0.035 5.57 113.91 0.036 Mass of bottle Mass of bottle Mass of bottle + sample Mass of Mass of soln./g Brix before Mean p 3 Brix after Mean p 4 net p Brix-free water Standard + + sample/g empty/g sample/g 110 g 10º Brix solution/g w 3 w 4 p 3 p 4 p 4 - b [100w 4(1-p 3 p -1 )]/w 3 deviation 1 Rind fibre 226.29 231.40 344.72 5.11 113.32 9.97 9.98 9.98 9.978 10.07 10.06 10.06 10.067 10.05 17.56 2 Rind fibre 212.64 217.74 326.96 5.10 109.22 5 9.978 10.07 0 10.07 5 10.08 5 10.073 10.06 8 18.30 3 Rind fibre 216.80 222.05 337.42 5.25 115.37 9.978 10.07 0 10.07 0 10.07 0 10.070 10.06 4 18.10 0.383 4 Stalk fibre 216.30 221.49 333.15 5.19 111.66 9.978 0 0 0 10.07 10.07 10.07 10.072 10.06 1 17.49 5 Stalk fibre 225.36 230.53 340.71 5.17 110.18 9.978 5 10.08 10.09 10.09 10.087 10.07 0 20.45 6 Stalk fibre 214.09 219.49 333.30 5.40 113.81 9.978 10.08 10.09 10.08 10.085 10.07 5 19.85 1.565 7 Top fibre 180.48 186.20 303.13 5.72 116.93 9.74 9.74 9.75 9.745 5 9.890 9.900 9.910 9.900 3 9.839 19.50 8 Top fibre 175.38 181.10 292.88 5.72 111.78 0 5 0 9.745 9.900 9.910 9.915 9.908 9.844 19.72 9 Top fibre 178.31 184.33 301.07 6.02 116.74 9.745 9.900 9.910 9.915 9.908 9.844 19.48 0.133 10 Green leaf fibre 11 Green leaf fibre 12 Green leaf fibre 183.50 189.69 298.29 6.19 108.60 9.745 9.87 9.875 9.885 9.877 9.838 16.55 165.85 171.86 288.55 6.01 116.69 9.745 9.86 9.875 9.865 9.867 9.832 17.09 180.63 186.87 305.25 6.24 118.38 9.745 9.87 9.875 9.88 9.875 9.839 18.14 0.809 126

In order to test for homogeneity of samples, fibres of various components of cane were extracted from 15 kg of cane. After removing and discarding the nodes, the rind was separated from the stalk. Fibres were extracted from the rind and the stalk, washed free of sucrose and dried as per the method described in Chapter 3 (Sections 3.4.3.1 and 3.4.3.2). Fibres were separated from the fines/pith as much as possible to obtain four well-separated fractions: stalk fibre (620 g), pith (1175 g), rind fibre (1240 g) and rind fines (830 g). There were also two mixtures: stalk with pith weighing 250 g and rind fibre with fines weighing 915 g. No effort was made to further separate these two mixtures as they would serve to see to what extent reproducible results could be obtained from them. Each of these six fractions was tested in five replicates and one blank determination was effected. Drying was effected in a vacuum oven at 80 °C for 3 hours. To 6 g of sample when cool were added 110 g of 10° Brix sucrose solution. A contact time of one and a half hours was allowed during which period, the sample was shaken every ten minutes. The Brix-free water results are shown in Table 4.6, which indicate that the fractions of stalk fibre, rind fibre, rind fibre + fines, and rind fines were homogeneous, despite such a small sample (6 g) taken from a large sample, e.g. 1240 g, in the case of rind fibres. For the stalk fibre + pith mixture and stalk pith sample, results were not reproducible, probably because of the difficulty associated with drying the pith. Hence the drying condition prior to analysis needed investigation. 4.4.5 Drying conditions prior to analysis When more of the samples which had been examined previously (results shown in Table 4.3) were analysed again two days later for their Brix-free water content under the same analytical conditions and incorporating the blank value, significantly higher results (P < 0.05) were obtained (see Table 4.7). This would indicate that the samples were drier on the second occasion than when first examined, and took up more water to satisfy their Brix-free water capacity. Thus, the overnight vacuum drying at 65 °C so far adopted needed to be re-examined. One green leaf fibre sample was well mixed, and sub-samples of 6 g were weighed into separate bottles. Samples were dried at 65 °C under vacuum of 875 mbar for 2, 4, 6 and 16 hours. The Brix-free water results (Table 4.8) show increasing values from 2, 4, 6 hours reaching the highest value at 16 hours, implying that drying under these conditions for less than 16 hours is insufficient to drive off the moisture originally present in the sample. 127

Sample<br />

Table 4.5. Reproducibility of Brix-free water determinations on fibre samples.<br />

Mass of Mass of bottle Mass of bottle + sample Mass of Mass of dis. H 2O/g Brix before Mean p 1 Brix after Mean p 2 Adjusted blank (b)<br />

bottle/g empty sample/g + 110 g distilled + water/g sample/g w 1 w 2 p 1 p 2 p 2w 2w 3/(w 1w 4)<br />

1b Rind fibre 225.48 231.24 342.47 5.76 111.23 0.00 0.00 0.00 0.000 0.01 0.01 0.01 0.010 0.009<br />

2b Rind fibre 5.76 111.23 0.009<br />

3b Rind fibre 5.76 111.23 0.009<br />

4b Stalk fibre 226.13 231.45 344.88 5.32 113.43 0.00 0.00 0.00 0.000 0.01 0.01 0.02 0.012 0.012<br />

5b Stalk fibre 5.32 113.43 0.012<br />

6b Stalk fibre 5.32 113.43 0.012<br />

7b Top fibre 202.07 208.02 319.60 5.95 111.58 0.00 0.00 0.00 0.000 0.07 0.06 0.07 0.067 0.061<br />

8b Top fibre 5.95 111.58<br />

0 0 0<br />

0.064<br />

9b Top fibre 5.95 111.58 0.064<br />

10 Green leaf<br />

11 b fibre Green leaf<br />

12<br />

b fibre<br />

Green leaf<br />

b fibre<br />

Sample<br />

220.77 226.34 340.25 5.57 113.91 0.00 0.00 0.00 0.000 0.03 0.03 0.04 0.033 0.039<br />

5.57 113.91<br />

0 0 0<br />

0.035<br />

5.57 113.91 0.036<br />

Mass of bottle Mass of bottle Mass of bottle + sample Mass of Mass of soln./g Brix before Mean p 3 Brix after Mean p 4 net p Brix-free water Standard<br />

+<br />

+<br />

sample/g<br />

empty/g sample/g 110 g 10º Brix solution/g w 3 w 4 p 3 p 4 p 4 - b [100w 4(1-p 3 p -1 )]/w 3 deviation<br />

1 Rind fibre 226.29 231.40 344.72 5.11 113.32 9.97 9.98 9.98 9.978 10.07 10.06 10.06 10.067 10.05 17.56<br />

2 Rind fibre 212.64 217.74 326.96 5.10 109.22<br />

5<br />

9.978 10.07 0 10.07 5 10.08 5<br />

10.073 10.06 8<br />

18.30<br />

3 Rind fibre 216.80 222.05 337.42 5.25 115.37 9.978 10.07<br />

0<br />

10.07<br />

0<br />

10.07<br />

0<br />

10.070 10.06<br />

4<br />

18.10 0.383<br />

4 Stalk fibre 216.30 221.49 333.15 5.19 111.66 9.978<br />

0 0 0<br />

10.07 10.07 10.07 10.072 10.06<br />

1<br />

17.49<br />

5 Stalk fibre 225.36 230.53 340.71 5.17 110.18 9.978<br />

5<br />

10.08 10.09 10.09 10.087 10.07 0<br />

20.45<br />

6 Stalk fibre 214.09 219.49 333.30 5.40 113.81 9.978 10.08 10.09 10.08 10.085 10.07<br />

5<br />

19.85 1.565<br />

7 Top fibre 180.48 186.20 303.13 5.72 116.93 9.74 9.74 9.75 9.745<br />

5<br />

9.890 9.900 9.910 9.900<br />

3<br />

9.839 19.50<br />

8 Top fibre 175.38 181.10 292.88 5.72 111.78<br />

0 5 0<br />

9.745 9.900 9.910 9.915 9.908 9.844 19.72<br />

9 Top fibre 178.31 184.33 301.07 6.02 116.74 9.745 9.900 9.910 9.915 9.908 9.844 19.48 0.133<br />

10 Green leaf<br />

fibre<br />

11 Green leaf<br />

fibre<br />

12 Green leaf<br />

fibre<br />

183.50 189.69 298.29 6.19 108.60 9.745 9.87 9.875 9.885 9.877 9.838 16.55<br />

165.85 171.86 288.55 6.01 116.69 9.745 9.86 9.875 9.865 9.867 9.832 17.09<br />

180.63 186.87 305.25 6.24 118.38 9.745 9.87 9.875 9.88 9.875 9.839 18.14 0.809<br />

126

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