3.1 Results and Discussions of Experiments on Distilling Liquor
The measurement results of the degree, volume and speed of the liquor are shown as the follow tables.
Table.1 The result of water distillation of A
Time interval(min)
|
4
|
4
|
4
|
8
|
8
|
8
|
8
|
8
|
Volume(mL)
|
120
|
140
|
120
|
120
|
156
|
138
|
98
|
46
|
Degrees(vol)
|
25
|
28
|
43
|
50
|
38
|
10
|
5
|
3
|
Speed(mL/s)
|
30
|
35
|
30
|
15
|
20
|
18
|
12
|
6
|
Table.2 The result of steam distillation of A
Time interval(min)
|
Volume(mL)
|
Degrees(vol)
|
Speed(mL/s)
|
10
|
60
|
45
|
6
|
10
|
55
|
42
|
5.5
|
10
|
109
|
14
|
10.9
|
It can be seen from the Table.1 that the volume, degree and speed of the first and middle stages are the best. The degree and speed decrease significantly in the last stages. From the Table.2, we can know that the highest degree of liquor that is 45 degrees, which belong to the first stage. And then the degree gradually decreased.
As a general rule the degree of head liquor is often the highest in the initial stages during the distillation. Table 1 shows that head liquor’s degree is slightly lower. It is speculated that the firepower of the induction cooker is so larger that the liquid evaporation in the kettle speed up, and the cooling water was not replaced in time.
ffect of A is no And the area and the temperature of the cooling device can’t guarantee the timely condensation of alcohol vapor. Therefore, the power of the induction cooker was adjusted in the following experiments on distilling liquor. Large fire was used at the beginning and the end of the experiment, and small fire was used when the condensate flowed out.
Compared with water distillation and steam distillation of A, if the low tail liquor was not included, In the water distillation experiment, consumed 800g of raw, produced 396 mL liquor, which exclude the first section and the last section distilling liquor with low degree. The liquor yield is 49.5%, and the average degree of liquor is 43 degrees. In the steam distillation experiment, consumed 250g of rice, obtained liquor 115 mL, the liquor yield was 46%, and the average degree of liquor is 43.6 degrees. It can be seen that the yield of alcohol and alcohol degree are almost the same whether distilled in water or distilled on water. The distillation eless than the distiller in modern folk workshops. The results show that A can distill liquor effectively, and it is undoubtedly a distiller.
Table.3 Volume and degree of liquor by water distillation of B
Time interval(min)
|
Volume(mL)
|
Degrees (vol)
|
Speed (mL/s)
|
10
|
20
|
30
|
2
|
10
|
35
|
24
|
3.5
|
>10
|
104
|
15
|
< 10
|
Table.4 Volume and degree of liquor by steam distillation of B
Time interval(min)
|
Volume(mL)
|
Degrees (vol)
|
Speed (mL/s)
|
4
|
30
|
22
|
7.5
|
4
|
40
|
16
|
10
|
4
|
56
|
10
|
14
|
>4
|
110
|
5
|
|
It can be seen from table.3 and table.4 that the degree of head liquor by water distillation and steam distillation is the highest, and then gradually decreases. Table.3 shows that in the experiment of water distillation, the highest degree of liquor is 30 degrees. If the liquor below 15 degrees in the end section is not included, the rice is 300g, the volume of the liquor is 55 mL, the liquor yield is 18.3%, and the average degree of liquor is 26.2 degrees. Table.4 shows that distillation on water, the highest alcohol is 22 degrees. If the liquor below 15 degrees is not included, consumed 175g of rice, the volume of the liquor is 70mL, the liquor yield is 40%, the average degree of liquor is 19 degrees. Either way, the liquor yield and alcohol degree are not high. In this regard, we think it is mainly due to the lack of imitation. The experimental results still show that B indeed a distiller.
From the perspective of the structure of the utensil, the cooling area of B is much larger than that of A, but the cooling effect is not as good as that of A, which is related to the position cooling water. The steam of A touches cooling water and then condenses. Although the interlayer of B is filled with water, the main cooling effect is still the cover, which mainly depends on air. It is speculated that if the interlayer changes the cooling water continuously, the cooling effect will be better. In addition, the height and width of B is nearly half of the original, so the area of the cover is 1/4 of the original, the surface area of the inner cylinder wall with water as the cooling medium is 1/4 of the original, which means that the cooling area of B is only 1/4 of the original. It also reflects that the distillation effect of the original should be much better than that of B.
3.2 Results and Discussions of Experiments on Distilling Rose Dew
The total ion flow chromatograms (Fig. 11 and Fig. 12) were obtain from the detection of rose dews of A and B. The corresponding compounds were obtained by computer mass spectrometry library and manual analysis. The volatile aroma components are shown in Table.5 and Table.6.
Table.5 Volatile components in flower dew by water distillation with A by GC-MS
No
|
RT
|
SI
|
RSI
|
Prob
|
%Area
|
Compound name
|
1
|
5.94
|
924
|
943
|
77.10
|
2.83
|
furfural
|
2
|
8.23
|
866
|
890
|
58.15
|
0.1
|
Benzene,ethenyl
|
3
|
11.53
|
849
|
893
|
62.19
|
0.12
|
Benzaldehyde
|
4
|
15.93
|
845
|
853
|
41.71
|
1.17
|
Benzyl alcohol
|
5
|
16.44
|
875
|
879
|
53.21
|
1.26
|
Phenylacetaldehyde
|
6
|
19.95
|
716
|
818
|
86.97
|
0.07
|
Ethyl(2E)-2-cyano-2butenoate
|
7
|
20.99
|
715
|
860
|
55.31
|
0.16
|
Penylethanol
|
8
|
24.46
|
824
|
852
|
87.70
|
0.15
|
Silane,cyclohexyldimethoxymethyl-
|
9
|
31.29
|
932
|
932
|
92.21
|
42.37
|
3,5-Dimethoytoluene
|
10
|
32.62
|
820
|
839
|
5.73
|
0.35
|
2,7,10-Trimethyldodecane
|
11
|
40.36
|
852
|
885
|
60.10
|
1.14
|
Benzene,1,3,5-trimethoxy-
|
12
|
41.03
|
790
|
818
|
32.89
|
0.4
|
α-ionol
|
13
|
42.75
|
862
|
889
|
71.87
|
0.48
|
Dihydro-β-ionol
|
14
|
44.09
|
805
|
880
|
11.40
|
0.17
|
2,6,10,-trimethyltridecane
|
15
|
45.15
|
801
|
835
|
37.74
|
0.2
|
β-ionone
|
16
|
46.35
|
868
|
886
|
14.10
|
0.64
|
Pentadecane
|
17
|
46.92
|
888
|
889
|
50.70
|
1.55
|
2,4-Di-tret-buthylphlenol
|
18
|
48.75
|
797
|
850
|
5.84
|
0.46
|
2,6,11,-trimethydodecane
|
19
|
51.42
|
882
|
892
|
42.80
|
0.32
|
Diethyl phthalate
|
20
|
52.13
|
878
|
882
|
12.82
|
0.89
|
Cetane
|
21
|
57.62
|
760
|
844
|
12.53
|
1.42
|
Heptadecane
|
22
|
58.19
|
833
|
848
|
5.86
|
1.74
|
2,6,11,15-tetrmethylhexadecane
|
23
|
65.92
|
866
|
910
|
5.81
|
0.59
|
Phthalic acid,hept-3-yl isobutyly ester
|
24
|
68.34
|
795
|
865
|
91.99
|
0.23
|
1-Oxaspiro[4.5]deca-6,9-diene-2,8dione,7,9-bis(1,1-dimethylethyl)
|
25
|
70.49
|
890
|
921
|
10.46
|
1.02
|
Dibutyl phthalate
|
26
|
77.26
|
853
|
897
|
25.72
|
0.58
|
n-Heneicosane
|
27
|
80.52
|
865
|
871
|
7.72
|
0.93
|
n-Docosane
|
28
|
82.4
|
822
|
832
|
4.42
|
1.65
|
Tricosane
|
29
|
83.82
|
877
|
891
|
20.50
|
2.42
|
Tetracosane
|
30
|
85.96
|
846
|
855
|
5.50
|
4.07
|
Hexacosane
|
31
|
86.95
|
860
|
877
|
9.94
|
3.7
|
Heptacoscane
|
32
|
88.08
|
817
|
852
|
7.95
|
4.02
|
Octacosane
|
Table.6 Volatile components in flower dew by water distillation with B by GC-MS
No
|
RT
|
SI
|
RSI
|
Prob
|
%Area
|
Compound name
|
1
|
4.25
|
882
|
900
|
52.91
|
0.43
|
Toluene
|
2
|
5.96
|
893
|
906
|
72.98
|
1.29
|
Furfural
|
3
|
6.39
|
837
|
895
|
39.58
|
0.09
|
2,4-dimethylhept-1-ene
|
4
|
7.08
|
893
|
917
|
62.13
|
0.12
|
Ethylbenzene
|
5
|
7.38
|
762
|
856
|
22.33
|
0.14
|
m-Xylene
|
6
|
8.25
|
807
|
879
|
37.68
|
0.1
|
Styrene
|
7
|
11.42
|
874
|
895
|
94.27
|
0.52
|
Ethyl cyanoacetate
|
8
|
11.54
|
791
|
976
|
50.81
|
0.19
|
Benzaldehyde
|
9
|
14.19
|
820
|
886
|
23.68
|
0.23
|
Decane
|
10
|
16.44
|
852
|
853
|
39.66
|
0.78
|
Phenylacetaldehyde
|
11
|
19.98
|
734
|
819
|
92.60
|
0.11
|
Ethyl(2E)-2-cyano-2butenoate
|
12
|
24.50
|
800
|
852
|
92.14
|
0.13
|
Silane,cyclohexyldimethoxymethyl
|
13
|
27.28
|
902
|
917
|
23.83
|
0.32
|
Dodecane
|
14
|
30.65
|
838
|
853
|
50.57
|
0.21
|
Benzene,m-di-tert-butyl
|
15
|
31.31
|
921
|
921
|
90.78
|
65.02
|
3,5-Dimethoytoluene
|
16
|
37.15
|
777
|
884
|
55.72
|
0.2
|
Triacetin
|
17
|
40.28
|
854
|
915
|
29.56
|
0.39
|
Tetradecane
|
18
|
40.37
|
888
|
906
|
77.16
|
0.76
|
Benzene,1,3,5-trimethoxy
|
19
|
40.63
|
770
|
909
|
29.00
|
0.13
|
Dodecanal
|
20
|
41.05
|
752
|
789
|
26.39
|
0.23
|
α-ionol
|
21
|
42.75
|
803
|
858
|
53.28
|
0.13
|
Dihydro-β-ionol
|
22
|
46.37
|
825
|
872
|
14.26
|
0.65
|
Pentadecane
|
23
|
46.92
|
900
|
902
|
55.61
|
1.96
|
2,4-Di-tret-buthylphlenol
|
24
|
48.77
|
772
|
850
|
6.66
|
0.44
|
2,6,11,15-tetrmethylhexadecane
|
25
|
52.14
|
884
|
891
|
19.66
|
0.88
|
Cetane
|
26
|
57.65
|
736
|
825
|
9.74
|
1.2
|
Heptadecane
|
27
|
57.99
|
795
|
928
|
5.95
|
0.63
|
2,6,10,-trimethyltretradecane
|
28
|
65.32
|
894
|
907
|
5.58
|
0.21
|
Phthalic acid,hept-3-yl isobutyly ester
|
29
|
68.36
|
781
|
851
|
91.75
|
0.29
|
1-Oxaspiro[4.5]deca-6,9-diene-2,8dione,7,9-bis(1,1-dimethylethyl)-
|
30
|
69.70
|
696
|
750
|
87.38
|
0.28
|
3,5-Bis(1,1dimethylethyl)-4-hydroxybenzenepropanoic acid methyl ester
|
31
|
70.5
|
923
|
937
|
0.59
|
1.6
|
Dibutyl phthalate
|
32
|
87.84
|
792
|
831
|
63.96
|
1.84
|
Erucylamide
|
33
|
88.5
|
716
|
835
|
41.50
|
0.27
|
(E,E,E,E)-squalene
|
There is no report on the analysis of volatile components in the flower dew of this variety Chinese rose used in experiments, so there is no direct component date for comparison. Due to difference the soil, climate, varieties and hybridization, the emergence of new varieties makes the volatile components of roses in different places is inconsistent. Generally speaking, the main aroma components of European roses are phenyl ethanol and monoterpene, while the main volatile components of Rosa chinensis are 3,5-dimethoxytoluene or 1,3,5-trimethoxybenzene [6].
Comparing the detection results of rose dew distilled by two sets of imitations, rose dew of A identified 32 components, 3,5-dimethoxytoluene, accounting for 42.4%. 33 components were identified of rose dew of B, and the highest relative content was 3,5-dimethoxytoluene (65.0%).The volatile components of two dews are almost the same. The highest relative content is 3,5-dimethoxytoluene, which is the main component of rose essential oil. It can be seen that the two sets of imitations can effectively extract rose dew. The components listed above are very volatile components in flower dew, which require high air tightness and cooler. The analysis results of the flower dew obtained in this experiment show that B can completely retain a variety of aroma components of rose petals. The effect of distillation extraction of rose dew is excellent, and the rose aroma components are complete.
Compared with other kinds of rose dew(Table.7). It can be found that phenylethanol and benzyl alcohol are detected in the rose dew with A, but not detected in the rose dew with B, which indicates that the air tightness of A is better that of B. This is due to the lack of imitation.
Table.7 Comparison of main volatile components in rose dew in literature
|
Percentage content(%)
|
Compound name
|
a[7]
|
b[8]
|
c[9]
|
d[10]
|
e[8]
|
f[11]
|
g[11]
|
h(A)
|
h(B)
|
3,5-Dimethoytoluene
|
50.3
|
2.55
|
0.72
|
12.1
|
1.05
|
18.5
|
11.9
|
42.4
|
65.02
|
Benzene,1,3,5-trimethoxy
|
-
|
-
|
-
|
|
-
|
0.84
|
3.22
|
1.14
|
0.76
|
Penylethanol
|
2.76
|
2.17
|
-
|
22.5
|
30.79
|
-
|
-
|
0.16
|
-
|
Benzyl alcohol
|
-
|
3.42
|
-
|
|
1.24
|
-
|
-
|
1.17
|
-
|
Dihydro-β-ionol
|
3.42
|
4.24
|
-
|
|
-
|
4.61
|
-
|
0.48
|
0.13
|
Note: a. hybrid Rosa chinensis; b. large rose; Rosa chinensis Jacq; d. fragrant rose; e. raspberry rose; f. Pink Perfume rose; g. orange yellow perfume rose; h. Chinese rose variety used in experiment (Rosa chinensis) |