U.S. patent number 3,784,358 [Application Number 05/183,697] was granted by the patent office on 1974-01-08 for support for chromogenic glycol test reagent.
This patent grant is currently assigned to Cities Service Oil Company. Invention is credited to Harry N. Drake, Jr..
United States Patent |
3,784,358 |
Drake, Jr. |
January 8, 1974 |
SUPPORT FOR CHROMOGENIC GLYCOL TEST REAGENT
Abstract
An improved supporting medium for a chromogenic reagent for use
in an aldehyde detection test. The chromogenic reagent, preferably
3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate
(MBTH), is absorbed on a porous polymeric material. The preferred
polymeric supporting medium is a film of porous polyethylene. The
chromogenic reagent supported on the porous polymer finds
particular utility in a test for determining the presence of glycol
in engine oil.
Inventors: |
Drake, Jr.; Harry N. (Fairless
Hills, PA) |
Assignee: |
Cities Service Oil Company
(Tulsa, OK)
|
Family
ID: |
22673943 |
Appl.
No.: |
05/183,697 |
Filed: |
September 24, 1971 |
Current U.S.
Class: |
422/420 |
Current CPC
Class: |
G01N
31/22 (20130101) |
Current International
Class: |
G01N
31/22 (20060101); G01n 031/22 () |
Field of
Search: |
;23/253TP |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Reese; Robert M.
Attorney, Agent or Firm: Yates; Edwin T.
Parent Case Text
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is related to U.S. Pat. No. 3,635,677 filed Apr.
30, 1970 and titled "GLYCOL DETECTION KIT"; and U.S. Pat. No.
3,645,696 filed Apr. 30, 1970 and titled "METHOD TO STABILIZE A
CHROMOGENIC TEST REAGENT FOR GLYCOL," both patents being assigned
to the assignee of the present application and having been
co-pending therewith.
Claims
I claim:
1. A stable supported chromogenic reagent comprising a chromogenic
aldehyde reagent selected from the group consisting of
3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate,
salicylalhydrazone, p-nitrobenzalhydrazone,
2-hydrazinobenzothiazole, and
2-hydrazinobenzothiazole-4-nitrobenzenediazonium fluoroborate
wherein said chromogenic reagent is absorbed on a porous polymeric
supporting medium having a pore size within the range of from about
30 to 60 microns.
2. The supported chromogenic reagent of claim 1 wherein the porous
polymeric supporting medium is selected from the group consisting
of polyethylene, polypropylene, polystyrene, and nylon.
3. The supported chromogenic reagent of claim 2 wherein the polymer
is in a physical form selected from the group consisting of
particles and film.
4. The supported chromogenic reagent of claim 3 wherein said
chromogenic reagent is 3-methyl-2-benzothiazolinone hydrazone
hydrochloride monohydrate and the porous polymeric supporting
medium is a polyethylene film having a pore size within the range
of from about 40 to 50 microns.
5. The supported chromogenic reagent of claim 4 which contains
about 2 to 6 weight percent of 3-methyl-2-benzothiazolinone
hydrazone hydrochloride monohydrate.
6. The supported chromogenic reagent of claim 5 wherein said
supported chromogenic reagent is sealed in a plastic beaker.
7. A method for the detection of glycol in oil comprising the
steps:
a. introducing a sample of the oil to be tested into an aqueous
solution of an oxidizer which preferentially oxidizes glycol to an
aldehyde;
b. mixing the oil and aqueous solution containing the oxidizer;
c. separating the aqueous and oil phases; and
d. contacting a sample of said aqueous phase with the supported
chromogenic reagent of claim 1.
8. The method of claim 7 wherein the oxidizer is selected from the
group consisting of sodium periodate, potassium periodate, hydrogen
peroxide, sodium perborate, cerric nitrate, cerric sulfate, and
lead tetraacetate; and the supported chromogenic reagent is
3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate
supported on a porous polyethylene film having a pore size within
the range of from about 40 to 50 microns.
9. The method of claim 8 wherein the oil is acidic.
10. The method of claim 9 wherein the oxidizer is about a 0.001 to
1.0 molar aqueous solution of sodium periodate, and the oil and the
aqueous sodium periodate solution are mixed for about 1 to 2
minutes and allowed thereafter to undergo phase separation for
about 10 to 20 minutes.
11. The method of claim 10 wherein the glycol is ethylene glycol
and the supported chromogenic reagent consists of about 2 to 6
weight percent of 3-methyl-2-benzothiazolinone hydrazone
hydrochloride monohydrate supported on a porous polyethylene film
having a pore size within the range of from about 40 to 50 microns
and wherein said supported chromogenic reagent is sealed in a
plastic beaker.
Description
BACKGROUND OF THE INVENTION
The present invention relates to an improved supporting medium for
a chromogenic reagent for use in an aldehyde detection test. More
particularly, the invention discloses the use of a porous polymeric
material, preferably a film of porous polymeric material, as the
supporting medium for the chromogenic reagent. The chromogenic
reagent supported on the porous polymer finds particular utility in
a test for determining the presence or absence of an aldehyde
derived from glycol in engine oils.
The presence of contaminants in engine oil may have damaging
effects upon the performance of the engine and its internal parts.
The cleanliness of the internal parts of an engine depends upon the
equilibrium between the oil polluting substances and the remaining
effective lubricating oil molecules. Various methods are available
for testing engine oils as to their effective lubrication and
cleansing properties upon engine parts. Both laboratory and field
tests have shown that ethylene glycol is one of the more
particularly hazardous contaminants which may enter engine oil. The
ethylene glycol is derived from the anti-freeze added to the
engine's cooling system. Through abusive wear of the engine and
failure of sealing members within the engine glycol may enter the
crankcase and lubricating system of the engine and cause pasty
emulsions which may plug oil filters, pump screens, oil feed lines
and passages within the engine. The presence of ethylene glycol
also presents a problem in the engine combustion chamber where
temperatures are high enough to convert the glycol into a
varnish-like substance which causes valves to stay open, valve
lifters to bend in their guards, and piston rings to stick in their
grooves. Consequences of the above-mentioned malfunctions of the
engine may result in extreme engine abuse, engine lifetime
diminishment and eventual engine failure. The elimination of
ethylene glycol in the crankcase oil is a matter of extreme
importance in maintenance of the engine in that no engine oil
additives appear to be available on the market to combat the
incompatibility properties of glycol.
The most common method used to combat ethylene glycol contamination
in engine oil and subsequent seizure of engine parts is to change
the engine oil periodically so that the concentration of ethylene
glycol never exceeds a maximum tolerable concentration which would
damage the engine's moving members. More than about 50 p.p.m.
ethylene glycol is usually considered to be excessive. What is
required is an ethylene glycol testing method which will indicate
the concentration of ethylene glycol after certain periodic
intervals of engine-hour usage, such that the engine may be
serviced and the oil changed. This ethylene glycol test method must
include a procedure by which servicing personnel may periodically
check engine oil for glycol concentration without a rigorous
analytical technique being required. The test must, therefore, be
simple enough for layman's usage and also provide positive
identification of the presence of ethylene glycol. To date, no
suitable ethylene glycol test method is available for service
station or industrial usage. It has been suggested that the
presence of glycol in engine oil may be detected by treating a
sample of oil with an oxidizer to oxidize any glycol present to
aldehyde and then utilizing a chromogenic reagent adsorbed on a
particulate support to detect the presence of the aldehyde. A
problem with chromogenic reagent adsorbed on the surface of a
particulate supporting medium is poor bonding between the reagent
and the supporting medium with subsequent separation.
SUMMARY OF THE INVENTION
It is an object of this invention to provide an improved supporting
medium for a chromogenic reagent for use in an aldehyde detection
test.
It is another object of this invention to provide a kit for the
detection of ethylene glycol in crankcase oil which utilizes a
stabilized chromogenic reagent which is tightly bound within the
pores of a porous polymeric material.
It is still another object of this invention to provide an improved
process for the detection of glycol in oil.
Yet other objects will be apparent to those skilled in the art from
this disclosure.
The foregoing objects are achieved in accordance with this
invention. Broadly, this invention consists of a stable supported
chromogenic reagent comprising a chromogenic aldehyde reagent
selected from the group consisting of 3-methyl-2-benzothiazolinone
hydrazone hydrochloride monohydrate, salicylalhydrazone,
p-nitrobenzalhydrazone, 2-hydrazinobenzothiazole, and
2-hydrazinobenzothiazole-4-nitrobenzenediazonium fluoroborate
wherein said chromogenic reagent is adsorbed on a porous polymeric
supporting medium; and a method for the detection of glycol in oil
comprising the steps:
a. introducing a sample of the oil to be tested into an aqueous
solution of an oxidizer which preferentially oxidizes glycol to an
aldehyde;
b. mixing the oil and aqueous solution containing the oxidizer;
c. separating the aqueous and oil phases; and
d. contacting a sample of said aqueous phase with the above
chromogenic reagent adsorbed on a porous polymeric supporting
medium.
Thus by the practice of this invention, an improved supporting
medium for a chromogenic aldehyde reagent is provided. Moreover, an
improved process for the detection of ethylene glycol in engine oil
and an improved kit for use in said detection process are provided
by the instant invention.
DETAILED DESCRIPTION OF THE INVENTION
The objects of this invention are therefor accomplished by an
improved supporting medium for a chromogenic aldehyde reagent and a
method wherein the supported chromogenic reagent of the invention
is used to detect the presence or absence of glycol in oil. The
improved supporting medium for the chromogenic reagent is a porous
polymeric material, the use of which results in a stabilized
chromogenic reagent tightly bound within the pores of the porous
polymeric supporting medium. Use of the supported chromogenic
reagent of the invention in a test to detect the presence or
absence of a glycol, especially ethylene glycol, in oil involves
introducing a sample of the oil to be tested into an aqueous
solution of an oxidizer which preferentially oxidizes the glycol to
an aldehyde. The oil and the aqueous solution of oxidizer are
thoroughly mixed, and the mixture is thereafter allowed to separate
into the oil phase and the aqueous phase. A portion of the aqueous
phase is then brought into contact with a chromogenic aldehyde
reagent absorbed on a porous polymeric supporting medium. Whether
or not the chromogenic reagent developes the appropriate color
indicates the presence or absence of glycol in the oil; the
intensity of the color indicates the amount of glycol present.
Most oxidizers which will transform glycols into aldehydes may be
used in the present invention. However, the oxidizer must have the
characteristic of not tinting the aqueous solution such that the
colorimetric determination may not be used. Accordingly, standard
oxidizers such as potassium permanganate and ferric sulfate would
not be suitable for the present invention as they would leave a
distinct color in the aqueous phase which would conceal the color
change of the chromogenic aldehyde reagent. Suitable oxidizers for
use in practicing the instant invention include sodium periodate,
potassium periodate, hydrogen peroxide, sodium perborate, ceric
nitrate, ceric sulfate, and lead tetraacetate. In particular, the
sodium and potassium periodates are preferred oxidizers which
selectively oxidize ethylene glycol to formaldehyde without side
reactions which form other oxidized compounds. In most cases, the
oxidizer, in particular the periodate solution, will be about 0.001
to 1.0 molar, and preferably about 0.01 to 0.5 molar, in
concentration. By use of concentrations within this range, an
economic quantity of the oxidizer is utilized and strong oxidation
does not take place. In most instances, between about 0.5 and about
10 milliliters, and preferably about 1 to 3 milliliters, of
oxidizing solution per milliliter of oil sample will be sufficient
to fully oxidize the ethylene glycol contained in an oil sample
withdrawn from an engine crankcase.
In the field application of a preferred embodiment of the present
invention, generally 5 to 10 milliliter oil samples are withdrawn
from the engine crankcase by means of a piece of tubing or by a
syringe-type instrument introduced into the crankcase through the
oil dip tube. The engine oil is withdrawn and dropped into the
solution of oxidizer held in a container. The container is then
sealed and vigorously shaken. After thorough mixing has occurred,
the solution is allowed to separate into a lower aqueous phase and
an upper oil phase. The aqueous phase, containing formaldehyde
resulting from the oxidation of any ethylene glycol present in the
oil phase, may be used to determine whether or not formaldehyde is
present and, if present, its semiquantitative concentration.
Many chromogenic aldehyde reagents exist, but the reagent used must
be highly specific for formaldehyde or other aldehyde and not be
influenced by other substances which may be oxidized or may be
contained as additives or original components of the engine oil.
Examples of chromogenic aldehyde reagents which are specific to
aldehydes and may be utilized in accordance with the present
invention are 3-methyl-2-benzothiazolinone hydrazone hydrochloride
monohydrate, salicylalhydrazone, p-nitrobenzalhydrazone,
2-hydrazinobenzothiazole, and
2-hydrazinobenzothiazole-4-nitrobenzenediazonium fluoroborate. It
is pointed out that oil samples tested in accordance with the
present invention, especially crankcase oils, are often acidic by
nature. The chromogenic aldehyde reagent used must therefore
preferably be able to respond to the presence of an aldehyde in an
acidic medium when testing such acidic oils. This criterion
eliminates a number of excellent chromogenic aldehyde reagents
which will not perform under acidic conditions. For example,
reagents such as 2-hydrazinobenzothiazole and
2-hydrazinobenzothiazole-4-nitrobenzenediazonium fluoroborate are
excellent for the detection of aliphatic, aromatic, and
heterocyclic aldehydes. However, these reagents require an alkaline
medium and are therefore not suitable for practicing the preferred
embodiment of this invention when the oil sample tested is an
acidic crankcase oil.
Another criterion for preferred aldehyde reagents is the
stabilization of the color after introduction of the aldehyde into
the presence of the chromogenic aldehyde reagent. The color should
remain stable for several minutes so that the operator may observe
the reagent color against predetermined charts or a blank for a
quantitative determination of the amount of glycol present in the
oil sample. A study made by Sawicki, et al., Analytical Chemistry,
33, No. 1, 93 (1961) has indicated that
3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate
(MBTH) is an excellent reagent for the determination of
formaldehyde and thus is a preferred reagent in practicing the
preferred embodiment of the instant invention which involves
detection of ethylene glycol in engine oil.
As with the oxidizing agents, the porous polymeric supporting media
used to absorb the chromogenic aldehyde reagent should be
translucent or opaque such that any color imparted from the support
will not interfere with the chromogenic test. Therefore, it is a
necessary criterion of the porous polymeric supporting medium that
it not have an interferring background color which will interfere
with the color test.
Examples of suitable porous polymeric supporting media are porous
polyethylene, polypropylene, nylon, and polystyrene. The porous
polymer may be particulate, i.e., powder or chips, or it may be a
film such as a disk or small rectangular or square sheet. The
preferred porous polymeric support is a porous polyethylene film,
e.g., a disk or small rectangular or square sheet.
Means for preparing porous polymeric materials are well known, and
the method of preparing a porous polymeric material is not critical
to the practice of this invention. For example, polyethylene or
polypropylene may be rendered porous by means of unreacted monomer
contained therein. In this procedure, unreacted gaseous monomer is
dissolved in the polymer which is prepared in a closed system under
high pressure. Release of the pressure causes the unreacted gaseous
monomer to come out of solution in the polymer with the resultant
formation of open pores by the expanding gas. Porous polystyrene,
for example, is commonly prepared by the impregnation of the
polymer with a volatile hydrocarbon such as pentane followed by
heating, whereupon the vaporized pentane forms open pores in the
polymer. Another common method of forming pores in polymers is to
use carbon dioxide as a blowing, or pore-forming, agent. For
example, a metal carbonate may be physically incorporated in the
polymer followed by contacting the polymer-metal carbonate mixture
with an acid at a temperature above the softening point of the
polymer whereby the liberated carbon dioxide forms pores in the
polymer. Alternatively, the carbon dioxide may be injected under
high pressure into fluid polymer, for example in the barrel of a
plastics extruder, and on release of the pressure the escaping
carbon dioxide forms a porous polymer. Polymers may also be
rendered porous by well known chemical blowing agents which, on
heating, decompose to gaseous products. Also, soluble salts such as
sodium chloride may be physically incorporated in the polymer and
subsequently leached out by a solvent for the salt to thereby leave
pores in the polymer. The foregoing merely serves to illustrate how
porous polymers may be prepared, but it will be understood that the
method of preparing the porous polymer is not critical to the
practice of my invention.
It will be apparent to those skilled in the art that the pore size
in the porous polymeric supporting medium should broadly be large
enough to accommodate the chromogenic aldehyde reagent molecule and
that the optimum pore size will vary depending on the size of the
chromogenic reagent molecule. Generally, a pore size within the
range of about 30 to 60 microns is desirable and, when the
chromogenic reagent is the preferred MBTH, the preferred pore size
has been found to be from about 40 to 50 microns.
In the preparation of a supported chromogenic reagent, which is
generally unstable on exposure to air and thereby rendered
unsuitable for the determination of aldehydes, the chromogenic
reagent generally is dissolved in a solvent. In most applications,
the solvent used for making the solution is deionized or distilled
water. After the solution is formed it is brought into contact with
a suitable porous polymeric supporting medium which will absorb the
chromogenic reagent. An inert atmosphere may be maintained above
the supporting medium during the absorption process so that no
oxidation of the chromogenic reagent will occur during the
absorption step. The absorption step may be enhanced by
simultaneously drying the chromogenic reagent on the supporting
medium to thereby strip off the solvent. This drying process may
take from five minutes to an hour depending on the amount of
solution brought into contact with the supporting medium. As
mentioned above, the preferred chromogenic aldehyde reagent is
3-methyl-2benzothiazolinone hydrazone hydrochloride monohydrate
(MBTH). The MBTH solution in deionized or distilled water generally
has a concentration of about 0.5 to 5 percent by weight.
The inert atmosphere during the absorption step is maintained by
means of an inert gas such as nitrogen or argon. When, for example,
the porous polymeric supporting medium is particulate, a column of
the supporting medium and the chromogenic reagent solution may have
the inert gas passed therethrough so that the inert gas is
constantly in contact with the chromogenic reagent and the
supporting medium. When the porous polymeric supporting medium is
in the form of a film, the film may be immersed in the solution of
chromogenic reagent and an inert gas, advantageously with stirring,
may be bubbled into the solution. The drying procedure for removal
of the solvent from the solution of chromogenic reagent, which may
be simultaneous with the absorption step, is carried out at
temperatures below about 100.degree. C so that no thermal
degradation of the chromogenic reagent will occur. The drying step
may be carried out in an inert atmosphere or it may be carried out
under reduced pressure which, in effect, lowers the oxygen
concentration. The chromogenic aldehyde reagent in effect forms a
complex with the porous polymeric supporting medium so that after
it is absorbed on the supporting medium it will remain stable and
will not be subject to attack by atmospheric oxygen.
It has been found that when the chromogenic reagent supported on a
porous polymeric supporting medium comprises about 2 to 6 weight
percent of chromogenic reagent, sufficient reagent is provided to
achieve the desired results, namely the detection of glycol in oil.
It is preferred that the supported chromogenic reagent comprise
about 3 to 5 weight percent of chromogenic reagent. The preferred
reagent is MBTH.
In testing a sample of oil for the presence of glycol, a mixture of
the oil and the aqueous solution of oxidizer in the proportions
described above are shaken vigorously for at least 1 minute and
preferably for at least 2 minutes to allow intimate contact of the
two phases. The oil-aqueous oxidizer mixture is allowed to stand
for at least about 10 minutes and preferably for about 15 to 20
minutes to allow the phases to separate and the oxidation of glycol
to be essentially completed. The aqueous phase, containing the
aldehyde resulting from oxidation of the glycol, is then brought
into contact with the chromogenic reagent supported on the porous
polymeric supporting medium. The time for color development,
depending on the concentration of the aldehyde, will be anywhere
from instantaneous to about 5 to 10 minutes.
In one embodiment of this invention, chromogenic reagent absorbed
on a particulate porous polymeric supporting medium is introduced
into a container such as a hypodermic syringe. It has been found
that about 2 cubic centimeters of the treated polymer particles in
a 5 ml. syringe is an appropriate quantity. A sample of the aqueous
phase is withdrawn from the container holding the oil and aqueous
phases and brought into contact with the supported chromogenic
reagent in the syringe by means of the syringe plunger. Generally,
from about 0.5 to about 2.0 ml. of aqueous phase are used per cubic
centimeter of supported chromogenic reagent. The reagent will turn
color within about 10 minutes if a glycol is present in the
oil.
In another embodiment of the present invention, chromogenic reagent
absorbed on a porous polymeric film is sealed in a receptacle such
as a plastic pillow pack or a small plastic beaker. The receptacle
serves not only to protect the chromogenic reagent absorbed on the
film from air and, to at least some extent, light, but it serves
also as a container for carrying out the test. A piece of film
about 1/16 inch thick by about 1/2 inch in diameter or 1/2 inch
square has been found to be an appropriate size. A sample of the
aqueous phase is withdrawn from the container holding the oil and
aqueous phases and is placed in the receptacle containing the
chemically treated film. The amount of aqueous phase is not
critical provided there is sufficient to thoroughly contact the
treated film. As noted above, the reagent will turn color within
about 10 minutes if a glycol is present in the oil.
In practicing the invention using sodium periodate as the oxidizer
and MBTH as the chromogenic aldehyde reagent, the reactions
occurring may be summerized as follows. Sodium periodate oxidizes
the ethylene glycol to formaldehyde. The formaldehyde then
contained in the aqueous phase is withdrawn and contacted with the
supported MBTH chromogenic reagent. The formaldehyde reacts with
the MBTH to form the azine. In addition, some MBTH is oxidized to a
reactive cation which combines with the azine to form a blue dye.
Therefore, the normally translucent chromogenic formaldehyde
reagent absorbed on a porous polymeric support will turn a dark
blue if ethylene glycol is present in the oil. A blank may be run
by taking an uncontaminated sample of the oil, mixing it with the
aqueous periodate solution, and then contacting the separated
aqueous phase with the supported chromogenic formaldehyde reagent.
The reagent turns purple to indicate that no ethylene glycol is
present in the blank. Shades of color between blue and the purple
color of the blank indicate the concentration of ethylene glycol. A
color chart may be prepared to show the colors corresponding to
various amounts of ethylene glycol in parts per million which are
contained in the engine oil. With this method, the operator knows
at any time what the ethylene glycol concentration is and when the
oil must be changed. Each time the oil is checked, the reading is
recorded until a maximum allowable concentration of ethylene glycol
in the engine oil is detected. The oil is then changed and the
process repeated. The equations are formulated below for the
reaction of formaldehyde with 3-methyl-2-benzothiazolinone
hydrazone hydrochloride (A) to form the azine (B), oxidation of (A)
to a reactive cation (C), and formation of the blue cation (D).
##SPC1##
In a preferred embodiment of the instant invention, MBTH is
absorbed in the desired concentration on a film of porous
polyethylene and the chemically treated film is sealed in a small
plastic, disposable beaker until such time as it is used in a test
for the presence of ethylene glycol in engine oil.
In the test for the presence of ethylene glycol in engine oil, an
oil sample is withdrawn from the crankcase by means of a plastic
syringe of about 10 ml. capacity and equipped with a suitable
length of small bore plastic tubing. The oil sample is discharged
into a container, for example a one ounce vial, containing
approximately an equal volume of an aqueous sodium periodate
solution. The mixture in the closed vial is vigorously shaken by
hand for at least about 1 minute and is then allowed to stand for
at least about 10 minutes to allow separation of the phases and
oxidation of ethylene glycol to formaldehyde. The beaker containing
the porous polyethylene film having MBTH absorbed thereon is
unsealed and by means of, for example, a hypodermic syringe, about
2 to 5 ml. of the aqueous solution are added thereto. The presence
or absence of ethylene glycol, and its concentration if present,
can be determined by observing whether the chemically treated
polyethylene film is purple, dark blue, or an intermediate
color.
The present invention will be further illustrated by the following
examples .
EXAMPLE I
A number of porous polyethylene squares about one-half inch on a
side by about 1/16 inch thick and having an average pore size of
about 45 microns are weighed and placed in a 4 weight percent
aqueous solution of MBTH contained in an evaporation flask. Using
an infrared lamp for heat, the water is evaporated under reduced
pressure, leaving a coating of MBTH absorbed on the polyethylene
squares. The chemically treated polyethylene squares are reweighed
and are found to contain 3.2 weight percent absorbed MBTH.
The chemically treated polyethylene squares are individually placed
in 5 ml. plastic beakers and sealed therein by welding a film of
polyvinyl chloride over the mouth of each beaker. The sealed
beakers may then be stored in a light proof container until ready
for use.
EXAMPLE II
Motor oil compositions containing measured amounts of ethylene
glycol are prepared. The motor oil compositions, respectively
containing 1,000 p.p.m., 100 p.p.m. and 25 p.p.m., as well as a
blank motor oil containing no ethylene glycol, are each shaken for
two minutes in a 1:1 volume ratio with aqueous sodium periodate
solutions of various concentrations. The oil-aqueous sodium
periodate solutions are then allowed to stand for 10 or 20 minutes
to allow for phase separation and oxidation of ethylene glycol to
formaldehyde. A portion of the aqueous phase in every case is then
placed in a beaker containing a MBTH treated polyethylene square
described in Example I. Development of a blue color indicates the
presence of ethylene glycol in the motor oil while a purple color
indicates a negative test for the presence of ethylene glycol. In
every case, color development is detected within one minute. The
results of the tests are set forth in the table.
______________________________________ Ethylene Color of MBTH
Treated Polyethylene ______________________________________ Glycol
Phase Separation Time ______________________________________
NaIO.sub.4 p.p.m. 10 min. 20 min.
______________________________________ 0.10M 1000 Blue -- 100
Purple -- 25 Purple -- -- Purple --
______________________________________ 0.05M 1000 Blue -- 100 Light
Blue -- 25 Light Blue -- -- Purple --
______________________________________ 0.025M 1000 Blue -- 100 Blue
-- 25 Purple Blue -- Purple --
______________________________________ 0.010M 1000 Blue -- 100 Blue
-- 25 Purple Blue -- Purple --
______________________________________
From the Table, it is seen that, by the practice of this invention,
ethylene glycol concentrations in oil that are as low as 25 p.p.m.
may be detected. Thus by use of the present invention, the ethylene
glycol content in motor oil may be specifically determined by means
of an improved supported chromogenic reagent. The invention
provides the ability to warn of ethylene glycol leakage into the
engine crankcase and to avoid severe damage therefrom.
While the present invention has been described above with respect
to certain embodiments thereof, it will be understood by those
skilled in the art that various changes and modifications may be
made without departing from the spirit and scope of the invention
as set forth herein.
* * * * *