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the first phase. The variable parameters in the second phase are
presented in Table 2.
Results of the second phase confirmed the initial findings:
The type of grinder is the most important factor that affects the
yield of volatile oils. A 20 mesh product has marginally better
yield than a 40 mesh product and significantly higher yield than
a 60 mesh product. Problems with repeatability were corrected
by the new cleaning procedure. No significant difference was
found between crank and clevenger traps, 5 versus 8 or 12 h
distillation periods, and between low and high temperature settings.
962.17, Volatile Oil in Spices
First Action 1962
Final Action 1965
Revised First Action 1996
(Applicable to determination of steam-volatile oil in spices.)
Caution: See Appendix B, safety notes on safe handling of
alkaliespotassium hydroxideand on safe handling of acidschromic and sulfuric acids. Chromium(VI) is extremely
toxic and a suspected carcinogen. Do not discharge into sewers
or waterways. See material safety data sheets or equivalent for
all reagents. Dispose of waste solvents in an appropriate manner compatible with applicable environmental rules and regulations.
A. Principle
Ground spice sample is boiled in H2O or NaCl solution. Released volatile oil (vapor form) is condensed and collected in
trap and then measured through trap calibration.
B. Apparatus
(a) Volatile oil trap.5 mL, without stopcock, clevenger
receivers crankcase oil, ASTM 5.0 0.1 mL subdivisions (Figure 962.17). Available from Lurex (clevenger trap, Part No.
720-1075, and crankcase trap, Part No. LX 4448-1002), Rt 40
& Oak Rd, Buena, NJ 08310-0688, USA. Once a year, calibrate
trap for xylene retention by running 3 blanks. Use average volume.
(b) West condenser.400 mm long with drip tip and
Ts 24/40 ground joints.
C. Reagents
(a) Xylene.Reagent grade.
(b) Sodium chloride (NaCl) solution.10%.
(c) Antifoam B.Silicone emulsion containing 1% hydrogenated tallow glycerides (Dow Corning or equivalent).
(d) Chromic acidsulfuric acid solution.For cleaning
volatile oil trap. Mixture of 97.8% sulfuric acid, 0.5% chromium trioxide, and 1.7% H2O. Store at room temperature.
Chromic acidsulfuric acid solution is stable up to 2 years.
(e) Potassium hydroxide (KOH) solution.0.05%. For
rinsing volatile oil trap.
(f) Dishwashing liquid.
D. Determination
Blend all samples from a given lot in mixer and weigh 200 g
representative test sample. Ginger and turmeric samples must
be cracked before grinding. Set grinder with 0.75 mm mill
screen. Grind test sample. More than 99% sample must pass
through 0.85 mm sieve during the first run. Regrind oversize
until sample passes sieve.
Mix ground sample thoroughly and store in refrigerator (2
6C) in tightly sealed container until analysis.
Clean volatile oil trap by soaking overnight in chromic
acidsulfuric acid solution, C(d). Rinse with tap H2O followed
by rinsing with KOH solution, C(e). Rinse again with tap H2O.
Check cleanliness of trap by adding small volume of distilled
H2O. Water should flow down the wall of trap smoothly. Otherwise, repeat cleaning procedure. Immediately before use,
clean trap again with dishwashing liquid and test for cleanliness
as above.
Before removing aliquot for analysis, mix sample in container by rotating, to avoid stratification. Allow sample to
equilibrate to ambient temperature.
Weigh test sample as specified in Table 962.17. Quantitatively transfer sample to 2 L Erlenmeyer flask. Add ca 1200 mL
H2O or NaCl solution, C(b). (See Table 962.17 for distillation
solvent.) Add 23 drops of antifoam. Insert stirring bar.
E. Calculations
Calculate concentration of volatile oil in test sample as follows:
Volatile oil, % (v/w) =
Vo
100
Ws
Vo Vx
100
Ws
w+x+y+z
4
0.500 + 0.536 + 1.000 + 0.929
=
4
= 0.74
t+u+w+z
4
3.375 + 2.875 + 3.000 + 2.875
=
4
= 3.031
The percent volatile oil collected in phases I and II determined by using the same type of calculations as above are presented in Table 5.
There has been an error in phase I concerning distillation
temperature. High temperature was applied to s, u, v, w and z
instead of just s, v, w, z. Therefore, the calculation for this factor
has been modified as follows:
Temperature, option I =
s+u+v+w+z
5
Temperature, option II =
t+x+y
3
Distillation
solvent
Allspice
40
10% NaCl
Xylene, 2.0 mL
Anise
Basil
Bay leaf
Caraway
Cardamon
Celery seed
50
50
60
50
50
50
10% NaCl
H2O
H2O
H2O
H2O
H2O
Xylene, 2.0 mL
Cloves
Coriander
Cumin
Dill seed
Fennel
Fenugreek
10
70
50
50
50
50
10% NaCl
H2O
H2O
H2O
H2O
H2O
Xylene, 2.0 mL
Ginger
Marjoram
Nutmeg
Mace
Oregano
Black pepper
White pepper
Rosemary
Sage
Savory
Tarragon
Thyme
Turmeric
50
40
30
20
40
50
40
50
50
40
40
50
50
10% NaCl
H2O
H2O
H2O
H2O
H2O
H2O
H2O
H2O
H2O
H2O
H2O
H2O
Spice
Trap additive
Option I
Option II
Particle size
Repeatability measurement within laboratory
Trap type
Grinder type
Distillation time
Option I
Option II
Black pepper
Coriander
Allspice
Cloves
Oregano
1.885
2.012
0.50
0.741
3.90
4.032
18.95
19.275
3.375
3.288
(6.3)
(32.5)
(3.3)
(1.7)
(2.6)
1.848
2.05
(9.9)
0.536
0.706
(24.1)
3.928
4.005
(1.9)
19.025
19.2
(0.9)
3.125
3.538
(11.7)
2.0
1.898
0.616
0.625
3.962
3.97
19.225
19.0
3.35
3.312
(5.1)
(1.4)
(0.2)
(1.2)
(1.1)
2.035
1.862
(8.5)
0.759
0.482
(36.5)
3.99
3.942
(1.2)
19.15
19.075
(0.4)
3.538
3.125
(11.7)
1.912
1.985
(3.7)
0.608
0.634
(4.1)
3.90
4.032
(3.3)
18.95
19.275
(1.7)
3.312
3.35
(1.1)
1.94
1.963
(1.2)
0.572
0.702
(18.5)
3.958
3.975
(0.4)
19.025
19.20
(0.9)
3.325
3.342
(0.5)
1.962
1.935
(1.4)
0.634
0.607
(4.3)
3.99
3.942
(1.2)
19.15
19.075
(0.4)
3.35
3.312
(5.6)
Black pepper
Oregano
Coriander
Allspice
Cloves
1.612
1.762
3.094
3.031
0.75
0.759
3.796
3.816
18.594
18.609
(8.5)
(2.0)
(1.2)
(0.5)
(0.1)
1.825
1.55
3.25
2.875
0.866
0.643
3.792
3.821
18.984
18.219
(15.1)
(11.5)
(25.8)
(0.8)
(4.0)
1.688
1.688
3.0
3.125
0.75
0.759
3.796
3.816
18.672
18.531
(0)
(4.0)
(1.2)
(0.5)
(0.8)
1.762
1.612
(8.5)
3.094
3.031
(2.0)
0.804
0.705
(12.3)
3.816
3.796
(0.5)
18.688
18.516
(0.9)
1.75
1.625
3.094
0.031
0.776
0.732
3.696
3.916
18.688
18.516
(7.1)
(2.0)
(5.7)
(5.6)
(0.9)
1.688
1.688
3.00
3.125
0.768
0.741
3.733
3.879
18.766
18.438
(0)
(4.0)
(3.5)
(3.8)
(1.7)
1.65
1.725
3.094
3.031
0.777
0.732
3.792
3.821
18.594
18.609
(4.3)
(2.0)
(5.8)
(0.8)
(0.1)
Cleaning procedure
a
New method
ASTA
1.900
0.500
4.000
19.300
2.875
1.750
0.536
3.940
19.000
2.875
2.300
1.000
4.190
19.800
3.775
2.100
0.929
4.000
19.000
3.625
1.800
0.786
3.833
19.062
3.000
1.850
0.857
3.750
18.750
3.375
1.600
0.679
4.000
18.125
2.875
1.800
0.714
3.683
18.500
2.875
Phase I
Black pepper
Coriander
Allspice
Cloves
Oregano
1.900
0.536
3.830
18.800
3.375
1.840
0.572
3.940
19.000
3.375
1.900
0.429
3.830
19.000
3.375
1.900
0.464
4.000
19.000
3.375
Phase II
Black pepper
Coriander
Allspice
Cloves
Oregano
1.850
0.964
3.583
19.375
3.250
1.800
0.857
4.000
18.750
3.375
1.500
0.571
3.767
18.125
2.875
1.300
0.607
3.833
18.125
2.875