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Wax usually refers to a substance that is a solid
at ambient temperature and that, on being subjected to slightly higher temperatures, becomes a low viscosity liquid.
The chemical composition
of waxes is complex; all of the products have relatively wide molecular weight
profiles, with the functionality ranging from products, which contain mainly
normal alkanes to those, which are mixtures of hydrocarbons and reactive
functional species.
For centuries, the honeycomb of bees, i.e., beeswax, was the material commonly
referred to as wax. Substances having typical wax characteristics have
traditionally come from insects, e.g., beeswax; from vegetables, e.g., carnauba.
And from animal, e.g., spermaceti, origins (1). Waxes from mineral and synthetic
Supplies have been developed both as substitutes for waxes from traditional
Supplies and for new applications. Waxes from minerals and synthetic Supplies
now surpass waxes from traditional Supplies in tonnage and commercial
importance.
Waxes obtained from natural Supplies such as vegetables or insects are subject
to weather conditions, which may severely affect the stability of supply and
price and, to a lesser extent, the consistency of the products. Waxes from
minerals and synthetic Supplies are less susceptible to weather conditions, and
thus have a more stable supply and price.
Insect and Animal Waxes
Beeswax.
White [8012-89-3J and yellow [8006-40-4J beeswax has been known for over 2000
years, especially through its use in the fine arts (2). References to wax prior
to the nineteenth century are probably to beeswax. Beeswax is secreted by bees
and is used to construct the combs in which bees store their honey. Removing the
honey and melting the comb in boiling water harvest the wax; the melted product
is then filtered and cast into cakes. The yellow beeswax cakes can be bleached
with oxidizing agents to white beeswax, a product much favored in the cosmetic
industry.
The composition of beeswax varies, depending on its
geographic origin. The major components are esters of C30 and C32 alcohols with
C16 acids, free C25 to C31 carboxylic acids, and C25 to C31 hydrocarbons (4).
Beeswax typically has a melting point of 640C, a penetration (hardness) of 20
dmm at 250C and 76 dmm at 43.30C (ASTM D1321), a viscosity of 1470 mm2/s at
98.90C, an acid number of 20, and a saponification number of 84.
The major use of beeswax is in the
cosmetic industry, with smaller amounts used in pharmaceuticals and candle
production.
Spermaceti.
Spermaceti [8002-23-il is derived from the head oil of the perm whale. Owing to
the present status of the sperm whale as an endangered species, however, the
material is no longer an item of commerce and has been replaced by other natural
and synthetic waxes.
Vegetable Waxes
Carnauba.
The source of carnauba wax [8015-86-9] is the palm tree, whose wax-producing
stands grow almost exclusively in the semiarid northeast section of Brazil. Carnauba
wax forms on the fronds of the palm, and is removed by cutting the
fronds, drying, and mechanically removing the wax. Impurities are removed from
the wax by melting and filtering or centrifuging. Wide fluctuations in price and
availability have caused markets served by carnauba wax to seek replacements.
Whereas there is no other single wax, which combines all the properties of
carnauba, suitable substitutes are available for most applications.
The major components of carnauba wax are aliphatic and aromatic esters of
long-chain alcohols and acids, with smaller amounts of free fatty acids and
alcohols, and resins. Carnauba wax is very hard, with a penetration of 2 dmm at
250C and only 3 dmm at 43.30C. Carnauba also has one of the higher melting
points for the natural waxes at 840C, with a viscosity of 3960 mm2/s at 98.90C,
an acid number of 8, and a saponification number of 80.
The hardness and high melting point, when combined with its ability to disperse
pigments such as carbon black, allows Carnauba wax increasing use in the thermal
printing inks. Carnauba is also widely used to gel organic solvents and oils,
making the wax a valuable component of solvent and oil paste formulations.
Carnauba polishes to a high gloss and thus is widely used as a polishing agent
for items such as leather, candies, and pills. Other uses include cosmetics and
investment casting applications (see COPPER ALLOYS, CAST COPPER ALLOYS).
Candelilla.
Candelilla wax [8006-44-8j is harvested from shrubs in the Mexican states of
Coahuila and Chihuahua and, to a very small degree, in the Big Bend region of
Texas in the United States (6). The entire mature plant is uprooted and immersed
in boiling water acidified with sulfuric acid. The wax floats to the surface and
is filtered .The major components of Candelilla wax are hydrocarbons, esters of
long-chain alcohols and acids, long-chain alcohols, sterols, and neutral resins,
and long-chain acids. Typically, Candelilla wax has a melting point of 700C, a
penetration of 3 dmm at 250C, an acid number of 14, and a saponification number
of 55. Principal markets for Candelilla include cosmetics, foods, and
pharmaceuticals
Japan Wax.
Japan wax [8001-39-6] is a fat and is derived from the berries of a small tree
native to Japan and China cultivated for its wax. Japan wax is composed of
triglycerides, primarily tripalmitin. Japan wax typically has a melting point of
530C, an acid number of 18, and a saponification number of 217. Principal
markets include the formulation of candles, polishes, lubricants, and as an
additive to thermoplastic resins. The product has some food-related
applications.
Ouricury Wax.
Ouricury wax [68917-70-4] is a brown wax obtained from the fronds of a palm
tree, which grows in Brazil. Ouricury is difficult to harvest, as it does not
flake off the frond as does carnauba wax; rather, it must be scraped free.
Ouricury is sometimes used as a replacement for carnauba in applications that do
not require a light-colored wax.
Rice-Bran Wax.
Rice-bran wax [8016-60-2] is extracted from crude rice-bran oil. It can be
degummed, the fatty acid content reduced by solvent extraction, and bleached.
The wax is primarily composed of esters of lignoceric acid ~43 wt %), behenic
acid (16 wt %), and C22-C36 alcohols (28 wt %).
Jojoba.
Jojoba oil [61789-91-1] is obtained from the seeds of the jojoba plant grown in
semiarid regions of Costa Rica, Israel, Mexico, and the United States. The oil
is made up of ca 80 wt % of esters of eicos- 1 1-enoic and docos- 13-enoic
acids, and eicos-11-en-1-ol, and docos-13-en-1-ol, ca 17 wt % of other liquid
esters, with the balance being free alcohols, free acids, and steroids. Jojoba
oil is used primarily in the formulation of cosmetics. Hydrogenated jojoba oil
is a wax used in candles and other low volume specialty applications.
Castor Wax. Castor wax [8001-78-31 is catalytically hydrogenated castor
bean oil. The wax has a melting point of 860C, acid number of 2, saponification
number of 179, and an iodine number of 4. Castor wax is used primarily in the
formulation of cosmetics. Derivatives of castor wax are used as surfactants and
plastics additives.
Bayberry Wax.
Bayberry wax [8038-77-5] is removed from the surface of the berry of the
bayberry (myrtle) shrub by boiling the berries in water and skimming the wax
from the surface of the water. The wax is green and made up primarily of lauric,
myristic, and palmitic acid esters. The wax has a melting point of 45~C, an acid
number of 15, a saponification number of 220, and an iodine number of 6. The wax
has an aromatic odor and is used primarily in the manufacture of candles and
other products where the distinctive odor is desirable.
Mineral Waxes
Montan Wax.
Montan wax [8002-53-7] is derived by solvent extraction of lignite (qv). The
earliest production on a commercial scale was in Germany during the latter half
of the nineteenth century, and Germany continues to supply the majority of the
world’s production of Montan wax. Montan wax production at Amsdorf is part of
a massive coal-mining operation from a continuous vein and raw material is
expected to last for decades.
The composition of Montan wax depends on the material from which it is
extracted, but all contain varying amounts of wax, resin, and asphalt. Black
Montan wax may be further processed to remove the resins and asphalt, ~ is known
as refined Montan wax. White Montan wax has been reacted with alcohols to form
esters. The wax component of Montan is a mixture of long. chain (C24-C30) esters
(62-68 wt %), long-chain acids (22-26 wt %), and long. chain alcohols, ketones,
and hydrocarbons (7-15 wt %). Crude Montan wax fro~ Germany typically has a
melting point of 800C, an acid number of 32, and a saponification number of 92.
The largest traditional use for Montan waxes was as a component in on~ time
hot-melt carbon-paper inks. With the decrease in the use of carbon-paper inks,
uses for the refined grades have become predominant, mainly in the formulation
of polishes and as plastics lubricants.
Peat Waxes.
Peat waxes are much like Montan waxes in that they contain three main
components: a wax fraction, a resin fraction, and an asphalt fraction. The
amount of asphalt in the total yield is influenced strongly by the solvent used
in the extraction. Montan waxes contain ca 50 wt % more of the wax fraction than
peat waxes, and correspondingly lower percentages of the resin and asphalt
fractions. The wax fraction in peat wax is chemically similar to that of the wax
fraction in Montan wax.
Ozokerite and
Ceresin
Waxes.
Ozokerite wax [OO1-75-O] was a product of Poland, Austria, and in the former
USSR where it was mined. True ozokerite no longer seems to be an article of
commerce, and has been replaced with blends of petroleum-derived paraffin and
microcrystalline waxes. These blends are designed to meet the specific physical
properties required by the application involved.
Ceresin wax [8001-75-0] originally was a refined and bleached ozokerite wax, but
now is a paraffin wax of very narrow molecular weight distribution or blend of
petroleum waxes.
Petroleum Waxes.
Waxes derived from petroleum are hydrocarbons of three types: paraffin
[64742-43-4] (clay-treated); semi microcrystalline or intermediate; and
microcrystalline [64742-42-31 (clay-treated). Semi microcrystalline waxes are
not generally marketed as such (7). Others include acid-treated, chemically
neutralized, and hydro treated; and paraffin and hydrocarbon waxes, untreated.
The quality and quantity of the wax separated from the crude oil depends on the
source of the crude oil and the degree of refining to which it has been
subjected prior to wax separation. Petroleum waxes are produced in massive
quantities throughout the world. Subject to the wax content in the crude,
paraffin and, to a substantially lesser degree, microcrystalline waxes are
produced in almost all countries of the world that refine crude oil.
A paraffin wax
is a petroleum wax consisting
principally of normal alkanes. Microcrystalline wax is a petroleum wax
containing substantial proportions of branched and cyclic saturated
hydrocarbons, in addition to normal alkanes. Semi microcrystalline wax contains
more branched and cyclic compounds than paraffin wax, but less than
microcrystalline. A classification system based on the refractive index of the
wax and its congealing point as determined by ASTM D938 was developed (9).
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Table 3. Typical
Properties of Petroleum Waxes
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Wax
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Property
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Paraffin
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Microcrystalline
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Flash point, closed cup, C
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204’
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260’
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Viscosity at 98.90C,
mm-9/s
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4.2-7.4
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10.2-25
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Melting range, ~C
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46-68
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60-93
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Refractive index at 98.9~C
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1.430-1.433
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1.435-1.445
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Number average molecular
weight
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350-420
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600-800
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Carbon atoms per molecule
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20-36
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30-75
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Ductility crystallinity of
solid wax
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Friable to crystalline
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Ductile-plastic to
tough-brittle
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Value is minimum.
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Paraffin wax is macro crystalline, brittle, and is composed of 40-90 wt % normal
alkanes, with the remainder C18-C36 isoalkanes and cycloalkanes. Paraffin wax
has little affinity for oil content: fully refined paraffin has less than 1 wt
%; crude scale, 1-2 wt %, and slack [64742-61-61, above 2 wt %. Within these
classes, the melting point of the wax determines the actual grade, with a range
of about 46-71”C. Typical properties of petroleum waxes are listed in
Table‘3.
The separation of paraffin wax from crude oil occurs during distillation, as
shown in Figure 1. The distillate is processed to remove oil to the degree
desired through solvent extraction. It is then decolorized, usually by
hydrogenation, but percolation through bauxite is also used. Microcrystalline
wax is produced either from the residual fraction of crude oil distillation or
from crude oil tank bottoms 10). After deasphalting of the residual fraction,
heavy lubricating oil is removed by solvent extraction. The degree of solvent
extraction is dictated by the economics of the lubrication oil market. The
filtrate is crude petrolatum, a dark-colored, unctuous material containing oil
and microcrystalline wax. Percentages of each may vary, but are usually about 40
wt % wax and 60 wt % oil. This material is then solvent-extracted for the wax.
Because microcrystalline wax has great affinity for oil, the oil content of the
wax is 1-4 wt %, depending on the grade of the wax. Unlike paraffin wax, oil is
held tightly in the crystal lattice of the microcrystalline wax, and does not
migrate to the surface. The microcrystalline waxes obtained from petrolatums are
generally known as plastic grades, with penetrations greater than 11 dmm at
25’C.
Crude oil contains high molecular weight fractions, which are soluble at the
high temperatures found in underground formations, but not very soluble at
ambient conditions once the crude oil is produced. These high molecular weight
fractions precipitate onto the walls and floors of storage tanks, and are known
as crude oil tank bottoms. Crude oil tank bottoms are essentially crude Oil with
very high wax contents and are processed as indicated in Figure 1. The
microcrystalline waxes obtained from crude oil tank bottoms are generally known
as hard grades, with penetrations less than 11 dmm at 250C.
The Bundesges undheitsamt (BGA) of Germany also has
specifications for refined petroleum waxes used in food applications. Many other
countries reference either the FDA or BGA specifications for their food
regulations. Petroleum wax is widely used in chewing gum to modify the
properties of the chewing gum base. The wide range of properties available help
chewing gum base manufacturers formulate a broad variety of chewing gum, ranging
from the traditional hard stick gum to the softer bubble gum. Petroleum wax can
also be used as protective coatings for fruits, vegetables, and cheeses.
Petroleum wax is outstanding as a cost-effective moisture and gas barrier, and
food-packaging applications are a major market for refined food-grade petroleum
wax. Blends of paraffin and microcrystalline wax are used by themselves or in
combination with other additives such as high molecular weight polyethylene and
ethylene vinyl acetate copolymers to improve the performance of paper packaging
such as paperboard boxes, paper containers, and flexible packaging.
Petroleum waxes are also widely used in other industrial applications. Paraffin
waxes are added to rubber during compounding, and exude to the surface during
curing, which helps protect the rubber from degradation resulting from ozone.
Paraffin and other waxes can be added to plastics, especially poly (vinyl
chloride) (PVC) as lubricants. Both paraffin and microcrystalline waxes are
widely used to help control the properties of hot-melt adhesives. Dispersions of
microcrystalline are added to ink to improve slip and rub properties. Petroleum
waxes are used in many consumer applications such is cosmetics, polishes, and
candles. Unrefined petroleum waxes are often used n fireplace logs.
Synthetic Waxes
Polyethylene Waxes.
Low molecular weight (less than ca 10,000 Mn) polyethylenes [9002-88-41 having
wax like properties are made either by high-pressure polymerization or
low-pressure (Zeigler-type catalysts) polymerization. All the products have the
same basic structure, but the processes yield products h distinctly different
properties. Some polyethylenes have fairly low density owing to branching that
occurs during the polymerization. Molecular weight distributions, expressed as
the weight average molecular weight divided by the number average molecular
weight, or polydispersity, also varies widely among the different processes, as
does the range of molecular weights available.
Differences among the processes have a major impact on the use of the products.
Products from a particular process or manufacturer may dominate one market,
while products from a different process may be preferred in a different
application. Major uses include hot-melt adhesives for applications requiring
high temperature performance, additives to improve the processing of plastics,
slip and rub additives for inks and paints, and cosmetic applications.
Products used in food applications require regulatory approvals. This regulation
includes a maximum amount of hexane-soluble material with other requirements.
The amount of material extracted by hexane is a function of molecular weight and
branching. The FDA under the synthetic petroleum wax regulation, 21 CFR 172.888,
regulates polyethylenes in the 500-1200-molecular weight range. In addition to
molecular weight requirements, this regulation includes an absorbance test to
verify the suitability of the product for food applications.
Some by-product polyethylene waxes have been recently introduced. The feedstock
for these materials is mixtures of low molecular weight polyethylene fractions
and solvent, generally hexane, produced in making polyethylene plastic resin.
The solvent is stripped from the mixture, and the residual material offered as
polyethylene wax. The products generally have a wider molecular weight
distribution than the polyethylene waxes synthesized directly, and are offered
to markets able to tolerate that characteristic. Some of the by-product
polyethylene waxes are distilled under vacuum to obtain a narrower molecular
weight distribution.
Several of the polymerization processes allow different functionality to be
added to the backbone of the polymer, including copolymers of ethene, propene,
hexene, vinyl acetate, and acrylic acid, with warlike properties. Copolymers of
ethene with other olefins provide a method of extending the range of properties
available. The addition of other olefins creates a branched polymer, which
decreases the melting point and hardness, while increasing viscosity as compared
to a linear polyethylene of the same molecular weight distribution. Longer
branches created through the addition of hexene show a larger effect than those
from propene. Copolymers with vinyl acetate and acrylic acid provide a method of
introducing oxygen functionality. These products may be further reacted with
metal salts to form ionomers.
In addition to co polymerization, polyethylene's terminated as ketones. Alcohols,
and carboxylic acids with molecular weights as high as 700 Daltons are now
available. The products offer the same chemical functionality as common fatty
alcohols and acids, but are higher melting and harder. Similar to the fatty
alcohols and acids, derivatives such as ethoxylates, esters, and amides also are
available as higher melting versions of the fatty derivatives.
Functional polyethylene waxes provide both the physical properties obtained by
the high molecular weight polyethylene wax and the chemical properties of an
oxidized product, and one derived from a fatty alcohol or acid. The functional
groups improve adhesion to polar substrates, compatibility with polar materials,
and dispersibility into water. Uses include additives for inks and coatings,
pigment dispersions, plastics, cosmetics, toners, and adhesives.
Fischer-Tropsch Waxes.
Polyethylene wax [8OO2-74-2] production is based on the Fischer-Tropsch
synthesis, which is basically the polymerization of carbon monoxide under high
pressure and over special catalysts to produce hydrocarbons (see FUELS,
SYNTHETIC-LIQUID FUELS). Distillation is then used to separate the hydrocarbons
into different products, including liquid fuels and waxes with melting points
ranging from about 45-1060C. Currently the waxes are produced in large volumes
in South Africa and Malaysia, with an estimated 12,000-14,000 t consumed in the
United States in 1994. Uses are similar to those for polyethylene waxes,
including hot-melt adhesives and additives for inks and coatings.
Chemically Modified
Waxes.
Hydrocarbon waxes of the microcrystalline, polyethylene, and polyethylene
classes are chemically modified to meet specific market needs. In the vast
majority of cases, the first step is air oxidation of the wax with or without
catalysts (11). The product has an acid number usually no higher than 30 and a
saponification number usually no lower than 25. An alternative step is the
reaction of the wax with a polycarboxylic acid, e.g., maleic, at high
temperature (12). Through its carboxyl groups, the oxidized wax can be further
modified in such reactions as saponification or esterification. Oxidized wax is
easily emulsified in water through the use of surfactants or simple soaps, and
is widely used in many coating and polish applications.
Substituted Amide
Waxes.
The product of fatty acid amidation has unique wax like properties (13). Probably
the most widely produced material is N,N’distearylethylenediamine [110-30-5],
which has a melting point of ca 140’C, an acid number of ca 7, and a low melt
viscosity. Because of its unusually high melting point and unique functionality,
it is used in additive quantities to raise the apparent melting point of
thermoplastic resins and asphalts, as an internal-external lubricant in the
compounding of a variety of thermoplastic resins, and as a processing aid for
elastomers.
Polymerized a-Olefins. Some polymers of higher a-olefins, e.g., C>20,
have wax like properties and are sold as synthetic waxes. The polymerization
process yields highly branched materials, with broad molecular weight
distributions. Properties of the individual products are highly dependent on the
a-olefin monomers and polymerization conditions. Melting points for the products
range from 540C to 740C, with number average molecular weights ca 2600-2800, and
penetrations at 250C of 5-12 dmm. The unique structure makes these products very
effective when used in additive amounts to modify the properties of paraffin
wax, primarily for use in candles. The products can increase the hardness and
opacity of the paraffin, without increasing the cloud point or viscosity. Other
uses include mold release for polyurethane foams, additives for casting wax, and
additives for leather treating.
Analytical Techniques
Most waxes are complex mixtures of molecules with different carbon lengths,
structures, and functionality. Attempts to measure the exact chemical
composition are extremely difficult, even for the vegetable waxes, which are
based on a relatively few number of basic molecules. Products such as oxidized
microcrystalline wax not only have a mixture of hydrocarbon lengths and types as
starting materials, but also add complexity through the introduction of various
types of carboxylic functionality onto those hydrocarbons during the oxidation
process.
Because of the difficulty in analysis of chemical composition, most of the
routine test procedures on waxes are for the measurement of the physical
proper-ties of the waxes and are used to compare the properties of waxes within
a class. Some properties, such as acid number or saponification number, give
insight into the chemical functionality of the product, and are widely used for
products, which contain carboxyl groups such as vegetable, Montan, and oxidized
waxes. Increasingly, instrumental methods such as gas chromatography (GC), gel
permeation (also known as size exclusion) chromatography (GPC), refractive index
(RI), differential scanning calorimetry (DSC), infrared spectroscopy (IR), and
nuclear magnetic resonance (NMR) are being used to further characterize the
products. Properties such as molecular weight distribution, degree of branching,
degree of crystallinity, and functionality can be readily measured with these
techniques.
Melting and Congealing Points.
Selection of the proper melting point method depends upon the characteristics of
the wax. Drop melting point (ASTM D127) is suitable for amorphous waxes, e.g.,
microcrystallines, but is not reliable for higher viscosity synthetic waxes, for
which ring-and-ball softening point (ASTM D36) should be used. ASTM D87 may
evaluate waxes whose time-temperature cooling curves exhibit plateaus, e.g.,
paraffin wax. Open or closed capillary tubes are used to measure the melting
point of many of the natural waxes. The congealing point (ASTM D938) is the
temperature at which a melted wax ceases to flow, and is more consistent than
melting points for some waxes.
Hardness
(Penetration). The standard test for the hardness of waxes in industry is the
penetration test (ASTM D1321). This test measures the depth in tenths of a
millimeter that a needle of a certain configuration under a given weight
penetrates the surface of a wax at a given temperature. A series of penetrations
measured at different temperatures, rather than at a single temperature, is
preferred.
Color.
On solidification of a wax and depending on factors such as the rate of cooling,
the amount of occluded air, and surface finish, the color of solidified samples
of the same wax may be different. For this reason, the color of most waxes is
judged only while molten, although some commercial standards for certain waxes,
e.g., carnauba, are based on the color of the solid wax. The accurate
measurement of color in light-colored, i.e., amber to off-white to white, waxes
is difficult but very important because of the additional processing costs
required to achieve the light color. The two most widely used color standards
providing numerical measurement are ASTM D1500, which is used to measure
dark-brown to off-white color, and ASTM D156, which is used to measure off-white
to pure white.
Oil content.
The production of petroleum waxes involves the removal of oil; therefore, the
oil content (actually the percentage of oil and low molecular weight fractions)
is one indication of the quality of the wax. Oil content is determined (ASTM
D721) as that percentage of the wax soluble in methyl ethyl ketone at -31.7
degrees C.
Viscosity.
Although traditionally of little importance in the evaluation of vegetable and
insect waxes, viscosity is an important test for mineral and synthetic waxes.
One of the most frequently used tests, ASTM D88, is used to measure the time in
seconds required for a specified quantity of wax at a specified temperature to
flow by gravity through an orifice of specified dimensions. This viscosity is
expressed in Saybolt Universal Seconds (SUS) at the temperature of the test. The
SI unit for kinematic viscosity is mm2/s (=cSt).
Acid Number.
The acid number (ASTM D1386) is the milligrams of potassium hydroxide necessary
to neutralize one gram of wax, and indicates the amount of free carboxylic acid
present. The test is widely used for vegetable and insect waxes, and synthetic
waxes containing carboxylic acid groups.
Saponification
Number.
The saponification number (ASTM D1387) is the milligrams of potassium hydroxide,
which react with one gram of wax under elevated temperatures, and indicates the
amount of free carboxylic acid plus any ester materials, which may be saponified.
Both the acid number and saponification numbers are generally provided to give
an indication of the free carboxylic acid and ester content of vegetable and
insect waxes, and synthetic waxes containing carboxylic acids and or esters.
Differential Scanning
Calorimetry (DSC).
The dsc has become widely used to characterize waxes. Under controlled heating
and cooling rates, the amount of energy consumed or released is measured. Curves
of heat flow v/s temperature provide insight into the thermal characteristics of
a wax, including crystalline transitions such as solid-to-solid,
solid-to-liquid, and liquid-to-solid. Common values obtained from the curves
include the initial and ending temperatures for heat flow, and heat of fusion,
expressed as joules per gram.
Gas Chromatography
(GC).
Gas chromatography has been used for many years, especially on the relatively
simple structures of vegetable and insect waxes. Use of the GC for petroleum and
synthetic waxes was limited by the maximum carbon number which could be eluted,
and the number of isomers for each carbon number. Improvements in technology
have allowed wider use of this technique, with columns and equipment available,
which can resolve carbon numbers up to C100. Good resolution can be obtained on
products with generally only one type of structure, e.g., paraffins with a high
preponderance of primary alkanes. Products such as microcrystalline wax, which
contain several different branched isomers for each carbon number, plus some
cyclic compounds, cannot be completely resolved, although useful information can
still be obtained.
Gel Permeation
Chromatography (GPC).
The gpc (also known as size exclusion chromatography) is widely used to measure
the molecular weight distribution for synthetic polyethylene waxes. Whereas gpc
cannot match the resolution available in GC techniques, useful information
regarding the molecular weight, and molecular weight distribution can be
obtained for products with molecular weights too high for gas chromatography.
The molecular weight is normally reported using the number average, Mn, or the
weight average, Mw The ratio of the weight average to the number average is
known as the
polydispersity.Pd.
Infrared
Spectroscopy
(Ir).
Infrared curves are used to identify the chemical functionality of waxes.
Petroleum waxes with only hydrocarbon functionality show slight differences
based on crystallinity, while vegetable and insect waxes contain hydrocarbons,
carboxylic acids, alcohols, and esters. The ir curves are typically used in
combination with other analytical methods such as DSC or gc/gpc to characterize
waxes.
Nuclear
Magnetic Resonance
(NMR).
The NMR analysis has been used in the polymer industry to measure
properties such as amount and type of branching, polymerized ethylene oxide
content, and hydroxyl content. The same techniques are applicable to waxes, and
are used for both characterization and quality control.
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