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Old 22-02-2005, 09:22 AM
farzadmokh
 
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Default Please guide me about lab methods of stearoptene

Dear All friends

I'm glad to join your group.
I want to know how I can determine stearoptene in rose oil in my lab
and how can I remove it in an industrial projects

If it's possible please guide me kindly.

Yours faithfully

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Old 28-02-2005, 09:14 AM
Malar Maalai
 
Posts: n/a
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farzadmokh wrote:
Dear All friends

I'm glad to join your group.
I want to know how I can determine stearoptene in rose oil in my lab
and how can I remove it in an industrial projects



It sounds like the separation of stearoptene from the oil is
accomplished by cooling the rose oil to 12.5° C. This references may be
of some use to you:
http://www.ibiblio.org/herbmed/eclec...rosa_oleu.html
The relevant passage says:
"Tedermann (Zeit. An. Chem; 1895, 5) reached the conclusion, after much
experimenting, that there is no reliable chemical or physical test for
the adulteration of oil of rose with geranium oil. The sense of smell,
according to Conroy, furnishes the best means of determining the
quality; he recommends the dissolving of one drop of oil of rose in
twenty drops of alcohol, pouring the solution in one fluid ounce of warm
water, shaking, and comparing the odor with that of a standard sample
treated in the same way. (P. J., 1896, 474; see also C. D., 1897, 53.)
O. Helm (A. Pharm., 1885) states that the test with a mixture of five
parts of chloroform and twenty parts of alcohol cannot be relied upon,
as no separation of crystalline scales took place in four different rose
oils which were doubtless genuine. But Flückiger, on the other hand,
stated that in an experience of many years it had never failed.
According to Bauer, the best tests of the purity of the oil are found in
its congealing, in five minutes, at a temperature of 12.5° C. (54.5°
F.), and its crystallizing, as a solid mass, in light, shiny plates,
present everywhere throughout the liquid. These crystals are truncated
semi-sided prisms, the angles of which are unequal, and which must be
classed in the rhombic system. This stearoptene melted and allowed to
cool, crystallizes in a manner so complete that the microscope can
readily reveal the presence of foreign substances, such as spermaceti,
fatty bodies, wax, and other analogous amorphous substances."

Here is another reference from the nineteenth century:
http://www.swsbm.com/AJP/AJP_1889_No_7.pdf
The relevant passage says:
"(1) Isolation and determination of the stearoptene. Fifty grams of oil
are heated with 500 grams of 75 per cent. spirit to a temperature of 70
to 80. Upon cooling the stearoptene separates nearly entirely. It is
removed from the liquid and treated similarly with 200 grams more of 75
per cent. spirit, and this operation is repeated until the stearoptene
is obtained perfectly odorless, a second treatment of the crude
stearoptene being usually sufficient. In this way the following results
were obtained with different samples of German and Turkish oil.
(2) Determination of an Admixture of Spermaceti.—3-5 grams of the
stearoptene are boiled for five or six hours in a return condenser with
20 to 25 grams of 5 per cent. alcoholic potash solution; the alcohol is
then driven off and the residue treated with hot water. Upon cooling the
greater part of the stearoptene separates on the surface as a
crystalline mass. The alkaline liquor is then poured off, the
stearoptene washed with some cold water, then again melted down with hot
water, allowed to cool and the water poured off, and this is repeated
until the wash-water is neutral. The united aqueous liquor is shaken
twice with ether, to remove suspended stearoptene, and after separation
of the ether is acidulated with dilute sulphuric acid and again
extracted with ether, which upon evaporation should leave no residue
(fat acid). As a check the stearoptene, including that withdrawn from
the alkaline liquid, is dried at 90 and weighed. There will, however, be
a small loss due to the volatilization of some stearoptene. In a control
experiment in which equal to 1.7 per cent. of spermaceti was added to a
sample of Turkish oil 1.5 per cent. was recovered.

The melting-points of stearoptene from samples of German rose oil ranged
from 35 to 36.5; those of stearoptene from Turkish oil from 33.5 to 35;
that of the stearoptene from the oil to which 1.7 per cent. of
spermaceti had been added was 31.5—32.

Rose oil, from which stearoptene has been removed in the above-described
manner, is perfectly liquid at 0; but when placed in a cooling mixture
it solidifies to a gelatinous mass, so that it is not quite free from
stearoptene. This liquid oil is described as having an extraordinarily
fine powerful odor, and as presenting the advantage that when used
dissolved in spirit it does not give rise to any crystalline separation."

Hope that helped. Wish you luck in preparing your report - sounds like
it would be quite a prohibitively experiment to actually perform, so, I
hope that what is required of you is to simply report the method to be
used, not actually conduct the experiment in the laboratory!


--
Radika
California
USDA 9 / Sunset 15











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Old 28-02-2005, 09:19 AM
Radika Kesavan
 
Posts: n/a
Default

Radika wrote:

It sounds like the separation of stearoptene from the oil is
accomplished by cooling the rose oil to 12.5° C. This references may
be of some use to you:
http://www.ibiblio.org/herbmed/eclec...rosa_oleu.html SNIP

Here is another reference from the nineteenth century:
http://www.swsbm.com/AJP/AJP_1889_No_7.pdf ... Hope that helped. Wish
you luck in preparing your report - sounds like it would be quite a
prohibitively experiment to actually perform, ...


Oops. I meant to say "- sounds like it would be quite a prohibitively
EXPENSIVE experiment to actually perform,..." - sorry about the typo.


--
Radika
California
USDA 9 / Sunset 15











  #4   Report Post  
Old 28-02-2005, 08:14 PM
Radika Kesavan
 
Posts: n/a
Default

farzadmokh wrote:
Dear All friends

I'm glad to join your group.
I want to know how I can determine stearoptene in rose oil in my lab
and how can I remove it in an industrial projects



It sounds like the separation of stearoptene from the oil is
accomplished by cooling the rose oil to 12.5° C. This references may be
of some use to you:
http://www.ibiblio.org/herbmed/eclec...rosa_oleu.html
The relevant passage says:
"Tedermann (Zeit. An. Chem; 1895, 5) reached the conclusion, after much
experimenting, that there is no reliable chemical or physical test for
the adulteration of oil of rose with geranium oil. The sense of smell,
according to Conroy, furnishes the best means of determining the
quality; he recommends the dissolving of one drop of oil of rose in
twenty drops of alcohol, pouring the solution in one fluid ounce of warm
water, shaking, and comparing the odor with that of a standard sample
treated in the same way. (P. J., 1896, 474; see also C. D., 1897, 53.)
O. Helm (A. Pharm., 1885) states that the test with a mixture of five
parts of chloroform and twenty parts of alcohol cannot be relied upon,
as no separation of crystalline scales took place in four different rose
oils which were doubtless genuine. But Flückiger, on the other hand,
stated that in an experience of many years it had never failed.
According to Bauer, the best tests of the purity of the oil are found in
its congealing, in five minutes, at a temperature of 12.5° C. (54.5°
F.), and its crystallizing, as a solid mass, in light, shiny plates,
present everywhere throughout the liquid. These crystals are truncated
semi-sided prisms, the angles of which are unequal, and which must be
classed in the rhombic system. This stearoptene melted and allowed to
cool, crystallizes in a manner so complete that the microscope can
readily reveal the presence of foreign substances, such as spermaceti,
fatty bodies, wax, and other analogous amorphous substances."

Here is another reference from the nineteenth century:
http://www.swsbm.com/AJP/AJP_1889_No_7.pdf
The relevant passage says:
"(1) Isolation and determination of the stearoptene. Fifty grams of oil
are heated with 500 grams of 75 per cent. spirit to a temperature of 70
to 80. Upon cooling the stearoptene separates nearly entirely. It is
removed from the liquid and treated similarly with 200 grams more of 75
per cent. spirit, and this operation is repeated until the stearoptene
is obtained perfectly odorless, a second treatment of the crude
stearoptene being usually sufficient. In this way the following results
were obtained with different samples of German and Turkish oil.
(2) Determination of an Admixture of Spermaceti.—3-5 grams of the
stearoptene are boiled for five or six hours in a return condenser with
20 to 25 grams of 5 per cent. alcoholic potash solution; the alcohol is
then driven off and the residue treated with hot water. Upon cooling the
greater part of the stearoptene separates on the surface as a
crystalline mass. The alkaline liquor is then poured off, the
stearoptene washed with some cold water, then again melted down with hot
water, allowed to cool and the water poured off, and this is repeated
until the wash-water is neutral. The united aqueous liquor is shaken
twice with ether, to remove suspended stearoptene, and after separation
of the ether is acidulated with dilute sulphuric acid and again
extracted with ether, which upon evaporation should leave no residue
(fat acid). As a check the stearoptene, including that withdrawn from
the alkaline liquid, is dried at 90 and weighed. There will, however, be
a small loss due to the volatilization of some stearoptene. In a control
experiment in which equal to 1.7 per cent. of spermaceti was added to a
sample of Turkish oil 1.5 per cent. was recovered.

The melting-points of stearoptene from samples of German rose oil ranged
from 35 to 36.5; those of stearoptene from Turkish oil from 33.5 to 35;
that of the stearoptene from the oil to which 1.7 per cent. of
spermaceti had been added was 31.5—32.

Rose oil, from which stearoptene has been removed in the above-described
manner, is perfectly liquid at 0; but when placed in a cooling mixture
it solidifies to a gelatinous mass, so that it is not quite free from
stearoptene. This liquid oil is described as having an extraordinarily
fine powerful odor, and as presenting the advantage that when used
dissolved in spirit it does not give rise to any crystalline separation."

Hope that helped. Wish you luck in preparing your report - sounds like
it would be quite a prohibitively expensive experiment to actually
perform, so, I
hope that what is required of you is to simply report the method to be
used, not actually conduct the experiment in the laboratory!


--
Radika
California
USDA 9 / Sunset 15










  #5   Report Post  
Old 28-02-2005, 08:14 PM
Radika Kesavan
 
Posts: n/a
Default

farzadmokh wrote:
Dear All friends

I'm glad to join your group.
I want to know how I can determine stearoptene in rose oil in my lab
and how can I remove it in an industrial projects



It sounds like the separation of stearoptene from the oil is
accomplished by cooling the rose oil to 12.5° C. This references may be
of some use to you:
http://www.ibiblio.org/herbmed/eclec...rosa_oleu.html
The relevant passage says:
"Tedermann (Zeit. An. Chem; 1895, 5) reached the conclusion, after much
experimenting, that there is no reliable chemical or physical test for
the adulteration of oil of rose with geranium oil. The sense of smell,
according to Conroy, furnishes the best means of determining the
quality; he recommends the dissolving of one drop of oil of rose in
twenty drops of alcohol, pouring the solution in one fluid ounce of warm
water, shaking, and comparing the odor with that of a standard sample
treated in the same way. (P. J., 1896, 474; see also C. D., 1897, 53.)
O. Helm (A. Pharm., 1885) states that the test with a mixture of five
parts of chloroform and twenty parts of alcohol cannot be relied upon,
as no separation of crystalline scales took place in four different rose
oils which were doubtless genuine. But Flückiger, on the other hand,
stated that in an experience of many years it had never failed.
According to Bauer, the best tests of the purity of the oil are found in
its congealing, in five minutes, at a temperature of 12.5° C. (54.5°
F.), and its crystallizing, as a solid mass, in light, shiny plates,
present everywhere throughout the liquid. These crystals are truncated
semi-sided prisms, the angles of which are unequal, and which must be
classed in the rhombic system. This stearoptene melted and allowed to
cool, crystallizes in a manner so complete that the microscope can
readily reveal the presence of foreign substances, such as spermaceti,
fatty bodies, wax, and other analogous amorphous substances."

Here is another reference from the nineteenth century:
http://www.swsbm.com/AJP/AJP_1889_No_7.pdf
The relevant passage says:
"(1) Isolation and determination of the stearoptene. Fifty grams of oil
are heated with 500 grams of 75 per cent. spirit to a temperature of 70
to 80. Upon cooling the stearoptene separates nearly entirely. It is
removed from the liquid and treated similarly with 200 grams more of 75
per cent. spirit, and this operation is repeated until the stearoptene
is obtained perfectly odorless, a second treatment of the crude
stearoptene being usually sufficient. In this way the following results
were obtained with different samples of German and Turkish oil.
(2) Determination of an Admixture of Spermaceti.—3-5 grams of the
stearoptene are boiled for five or six hours in a return condenser with
20 to 25 grams of 5 per cent. alcoholic potash solution; the alcohol is
then driven off and the residue treated with hot water. Upon cooling the
greater part of the stearoptene separates on the surface as a
crystalline mass. The alkaline liquor is then poured off, the
stearoptene washed with some cold water, then again melted down with hot
water, allowed to cool and the water poured off, and this is repeated
until the wash-water is neutral. The united aqueous liquor is shaken
twice with ether, to remove suspended stearoptene, and after separation
of the ether is acidulated with dilute sulphuric acid and again
extracted with ether, which upon evaporation should leave no residue
(fat acid). As a check the stearoptene, including that withdrawn from
the alkaline liquid, is dried at 90 and weighed. There will, however, be
a small loss due to the volatilization of some stearoptene. In a control
experiment in which equal to 1.7 per cent. of spermaceti was added to a
sample of Turkish oil 1.5 per cent. was recovered.

The melting-points of stearoptene from samples of German rose oil ranged
from 35 to 36.5; those of stearoptene from Turkish oil from 33.5 to 35;
that of the stearoptene from the oil to which 1.7 per cent. of
spermaceti had been added was 31.5—32.

Rose oil, from which stearoptene has been removed in the above-described
manner, is perfectly liquid at 0; but when placed in a cooling mixture
it solidifies to a gelatinous mass, so that it is not quite free from
stearoptene. This liquid oil is described as having an extraordinarily
fine powerful odor, and as presenting the advantage that when used
dissolved in spirit it does not give rise to any crystalline separation."

Hope that helped. Wish you luck in preparing your report - sounds like
it would be quite a prohibitively expensive experiment to actually
perform, so, I
hope that what is required of you is to simply report the method to be
used, not actually conduct the experiment in the laboratory!


--
Radika
California
USDA 9 / Sunset 15










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