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Product Information

METHOCEL K15M
Cellulose Ether

General METHOCEL* K15M is a cellulose ether suitable for various applications.


Description

Industrial METHOCEL K15M can successfully be used in mortars and plasters which are
Applications manually applied. The product imparts good workability to mortars and plasters
and enhances water retention.

Typical Properties

Viscosity Ubbelohde [mPa·s] 15000


2% in water @ 20ºC
Moisture Content [%] < 5.0
Sodium Chloride [%] < 2.0
Particle Size [%] > 95
< 70 U.S. Standard Sieve, 212 μm

Safety and Handling For specific safe use and handling information, or to obtain a Materials Safety Data Sheet,
contact your local Dow representative.

Contact us:
NOTICE: No freedom from any patent owned by Seller or others is to be inferred. Because use conditions and applicable laws
North America: 1-800-447-4369
Europe: +800 3 694 6367 may differ from one location to another and may change with time, Customer is responsible for determining whether products
+32 3 450 2240 and the information in this document are appropriate for Customer’s use and for ensuring that Customer’s workplace and
disposal practices are in compliance with applicable laws and other governmental enactments. Seller assumes no obligation or
www.methocel.com liability for the information in this document. NO WARRANTIES ARE GIVEN; ALLIMPLIED WARRANTIES OF
MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY EXCLUDED.

Page 1 of 1 * Trademark of The Dow Chemical Company Form No. 192-01316-1003 KP


Technical Handbook
METHOCEL Cellulose Ethers
Technical Handbook
Contents
An Introduction to METHOCEL Cellulose Ethers . . . . . . . . . . . . . . . . . . . . 1

General Properties of METHOCEL Cellulose Ethers . . . . . . . . . . . . . . . . . 3

Applications for METHOCEL Cellulose Ethers . . . . . . . . . . . . . . . . . . . . . . 7

Regulated Uses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
Table of Contents

How to Prepare Aqueous Solutions of METHOCEL Cellulose Ethers. . . . 11

How to Prepare Solutions of METHOCEL Cellulose Ethers


in Nonaqueous Solvents and Nonsolvent Media. . . . . . . . . . . . . . . . . . . 14

Properties of METHOCEL Cellulose Ethers in Powder Form . . . . . . . . . . . 15

Properties of Solutions of METHOCEL Cellulose Ethers . . . . . . . . . . . . . . 16

Thermal Gelation in Aqueous Media. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

Properties of Films of METHOCEL Cellulose Ethers. . . . . . . . . . . . . . . . . . 26

Analytical Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

Handling Considerations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
An Introduction to METHOCEL Cellulose Ethers
METHOCEL* cellulose ethers are to obtain the optimum degree of Available as Powders,
water-soluble polymers derived thickening, binding, moisture Surface-treated Powders, and
from cellulose, the most abundant retention, and other properties in Granular Form
polymer in nature. For over 50 desired in a given formulation.
years these versatile products For further formulating versatility,
have played an important role in Premium and Food Grades for METHOCEL products are available
foods, cosmetics, pharmaceuticals, Food and Drug Applications in three different forms: powder,
latex paints, construction surface-treated powder, and granular.
METHOCEL Premium and Food The form influences the techniques
products, ceramics, and a host products have long been used by
of other applications. used in making solutions. Untreated
the food and drug industries. Both powders are soluble in cold water,
METHOCEL products are used as methylcellulose and hydroxypropyl but must be thoroughly dispersed
thickeners, binders, film formers, methylcellulose are recognized as before they begin to dissolve.
and water-retention agents. They acceptable food additives by the Surface-treated powders and granular
also function as suspension aids, U.S. Food and Drug Administration products can be added directly to
surfactants, lubricants, protective (FDA) and are listed in the Food aqueous systems. The dissolution of
colloids, and emulsifiers. In addition, Chemicals Codex and the these products can be controlled by
solutions of METHOCEL thermally International Codex Alimentarius. a shift in pH.
gel, a unique property that plays a Both are included in the United
key role in a surprising variety of States Pharmacopoeia (USP XXI). Techniques commonly used in
applications. You won’t find this Methylcellulose is considered preparing solutions with different
valuable combination of properties Generally Recognized As Safe physical forms of METHOCEL
in any other water-soluble polymer. (GRAS) by the FDA. products are summarized on
pages 11–14 of this handbook.
Multifunctionality and Efficiency Standard Grades for Other
Improve Formulation Economy Applications Key to Product Nomenclature for
METHOCEL Products
The fact that so many useful Standard grade METHOCEL
properties are simultaneously products have the same performance METHOCEL is a trademark of
present and often act in properties as Premium grades. The Dow Chemical Company for a
combination can be a significant The major difference is that line of cellulose ether products. An
economic advantage. In many Standard grades can have slightly initial letter identifies the type of
applications, two, three, or more higher levels of impurities. Standard cellulose ether. “A” identifies
ingredients would be required to grades are not approved for use in methylcellulose products. “E”, “F”,
do the same job performed by a foods, although some Standard “J”, and “K” identify different
single METHOCEL product. In grade products may be used as hydroxypropyl methylcellulose
addition, METHOCEL cellulose components of containers coming products.
ethers are highly efficient, often in contact with food (indirect
food additive). The number that follows identifies
yielding optimum performance the viscosity in millipascal-seconds
at a lower concentration than Viscosity Grades (mPa·s) of that product measured at
that required with other water- from 3 to 100,000 mPa· s 2% concentration in water at 20°C.
soluble polymers. In designating viscosity, the letter
METHOCEL cellulose ether “C” is frequently used to represent
Range of Products Offers products are available in various
Formulating Versatility 100 and the letter “M” is used to
viscosity grades, ranging from 3 to represent 1,000.
The broad range of METHOCEL over 200,000 mPa·s.† Because the
products available is certainly one viscosity of a solution depends on Several different suffixes are also
reason they’ve been used successfully the concentration of METHOCEL, used to identify special products.
in so many different applications. this wide range of product viscosity “P” is sometimes used to identify
There are two different chemical allows you to obtain the viscosity METHOCEL Premium grade
types and each is available in you want in a formulation, while products. “LV” refers to special
different grades, physical forms, and using a concentration that gives “low viscosity” products. “G”
viscosities. By choosing a specific the desired level of other identifies “granular” products.
METHOCEL product, it’s possible performance properties. The letter “S” identifies

* Trademark of The Dow Chemical Company


† Note: mPa.s (millipascal-seconds) is equivalent to centipoise. All solution viscosities are measured
with Ubbelohde viscometers at 2% concentration in water at 20˚C (68˚F).
1
“surface-treated” products, “CR” Free Samples and Literature Contact Us Today!
denotes a controlled-release grade, Available
and “FG” identifies food grade. Again, if you would like samples,
Developmental grades are denoted Sample quantities of METHOCEL additional literature, or technical
by the letter X plus a second products are available free of assistance, don’t hesitate to call.
letter (usually U or Y) plus a five- charge for your developmental Our numbers are listed on the
digit code. work. You can obtain samples by back cover of this brochure. Call
calling one of the numbers listed today. The sooner you get started
There are also a number of special- on the back cover of this brochure. formulating with METHOCEL,
purpose METHOCEL products Literature covering the use of the sooner you’ll start seeing
developed for cosmetics, METHOCEL products in many of improved performance and
pharmaceuticals, ceramics, and the applications listed on pages 7–9 economy in your products.
other applications which have of this handbook is also available Our website also contains
different systems of nomenclature. on request. Just tell us what types valuable information to assist
For example, METHOCEL 40- of formulations or products you you in learning more about
Series products make up a family are evaluating, and we’ll send METHOCEL.
of special surface-treated products you all the current literature that
for cosmetic formulations. applies. Or visit our website at
www.methocel.com for a complete
Example A: METHOCEL A4C selection of downloadable literature.
Premium is the designation for a
Premium grade methylcellulose Our Technical Service and
product having a viscosity of Development Staff Can Help
400 mPa·s.
Talking with someone on our
Example B: METHOCEL J5MS Technical Service and Development
is a Standard grade hydroxypropyl (TS&D) staff can save you a great
methylcellulose product with a deal of formulation time. In certain
viscosity of 5,000 mPa·s, which applications, a blend of METHOCEL
has been surface-treated for products may give the best results,
easy dispersion. and the details may have already
been worked out by someone in
How to Get Started Formulating our lab. We have technical personnel
with METHOCEL who specialize in foods, ceramics,
To completely evaluate how paints, cosmetics, pharmaceuticals,
METHOCEL cellulose ethers can construction products, and other
improve quality, performance, and specific uses for METHOCEL
economy in your formulations, products. By taking advantage of
you’ll want to try them in your their experience with METHOCEL,
own lab. Whether you are you’ll get a head start with your
developing an entirely new product formulation and be certain of
or working to improve an existing getting the most out of these
one, chances are you’ll find a versatile products.
METHOCEL product that’s
ideally suited to your needs.

2
General Properties of METHOCEL Cellulose Ethers
General properties common to the Surface activity. METHOCEL used to retain moisture and prevent
whole family of METHOCEL products act as surfactants in oil absorption during cooking.
cellulose ether products are listed aqueous solutions to provide
below. Individual METHOCEL emulsification, protective colloid Binding. METHOCEL cellulose
products exhibit these properties action, and phase stabilization. ethers are used as high-performance
to varying degrees and may have Surface tensions range from 42 to binders for pigments, paper, tobacco
additional properties that are 64 mN/m. The surface tension of products, structured foods,
desirable for specific applications. water is 72 mN/m; a typical pharmaceutical products,
Detailed information on the surfactant has a surface tension and ceramics.
performance properties of of 30 mN/m.
METHOCEL products can be
Lubrication. METHOCEL products
found on pages 15–21. Metabolic inertness. Used as food are used to reduce friction in rubber,
and drug additives, METHOCEL cement, and ceramic extrusions.
Water solubility. METHOCEL products do not add calories to They are also used to improve
cellulose ethers dissolve in water the diet. pumpability of concrete and spray
with no sharp solubility limit. plasters, such as stucco, and in
Surface-treated and granular Enzyme resistance. Enzyme- food applications as lubricity aids
METHOCEL products can be resistant METHOCEL products in extrusion and other
added directly to aqueous systems. provide excellent viscosity stability forming processes.
This feature provides exceptional during long-term storage.
handling flexibility and control of
Suspending. METHOCEL products
solubilization rate. Although
Low taste and odor. METHOCEL are used to control settling of solid
untreated METHOCEL powders are
cellulose ethers have excellent (low) particles, for example, herbs and
soluble in cold water, they must first
flavor and aroma properties, spices in salad dressings, solids
be thoroughly dispersed in the water
which is important in food and in ceramic slips, and antacid
to prevent lumping. Dispersion
pharmaceutical applications. suspensions.
techniques are described on pages
11–13. The maximum concentration
is limited only by solution viscosity. pH stability. METHOCEL cellulose Protective colloidal action.
ethers are stable over a pH range of METHOCEL products are used to
2.0 to 13.0. prevent droplets and particles from
Organic solubility. Certain types and
coalescing or agglomerating.
grades of METHOCEL cellulose
ethers are also soluble in binary Water retention. METHOCEL
organic and organic solvent/water cellulose ethers are highly efficient Emulsification. METHOCEL
systems, providing a unique water-retention agents. This is cellulose ethers stabilize emulsions
combination of organic solubility valuable in food products, ceramics, by reducing surface and interfacial
and water solubility. coatings on adsorbent construction tensions and by thickening the
substrates, and many other aqueous phase.
applications.
No ionic charge. METHOCEL
cellulose ethers are nonionic and
will not complex with metallic salts Thickening. METHOCEL cellulose
or other ionic species to form ethers thicken both aqueous and
insoluble precipitates. nonaqueous systems. The viscosity
is related to the molecular weight,
chemical type, and concentration of
Thermal gelation. Aqueous solutions
the specific METHOCEL product.
of METHOCEL products gel
when heated above a particular
temperature, providing controllable Film formation. METHOCEL
quick-set properties. Unlike gels products form clear, tough, flexible
formed by protein thickeners, films that are excellent barriers to
the gels go back into solution oils and greases. In food
upon cooling. applications, this property is often

3
Nonaqueous Solvent Solubility Table 1: Typical Nonaqueous Solvents Used Solvent Solubility at Elevated
with METHOCEL Cellulose Ethers Temperatures
In general, binary solvent systems
• Furfuryl alcohol METHOCEL E and METHOCEL J
function more effectively with
• Dimethyl formamide cellulose ether products possess
METHOCEL products than single • Dimethyl sulfoxide
solvents. Where alcohols comprise structures that provide unusual
• Methyl salicylate
part of the binary solvent, solubility solubility properties. They are
• Propylene carbonate
improves as the molecular weight • Formic acid
soluble in certain nonaqueous media
of the alcohol decreases. Table 1 • Glacial acetic acid at elevated temperatures, permitting
lists several compounds which are • Pyridine the formulation of mixes which can
typical of the types of solvents • Mixtures of methylene chloride and be fabricated by techniques of
that can be used with certain ethyl, methyl, or isopropyl alcohols extrusion, hot-melt casting, and
METHOCEL cellulose • Mixtures of chloroform and methanol injection and compression molding.
ether products. or ethanol Examples of suitable “hot solvents”
• N-Methyl pyrrolidone are found in Table 2.

METHOCEL 310 Series Products


Table 2: Representative Solvents for METHOCEL E and METHOCEL J Cellulose Ether Products METHOCEL 310 Series products
at Elevated Temperatures are granular, high-viscosity materials
(Table 3) that are sold only in
Boiling Point Solubility Point Degree of
Solvent °C °C Solubilitya Europe at this time. Controlled
granulometry provides good dry-
Glycols flow properties, low dust formation,
Ethylene glycol 197.3 158 C and lump-free dispersibility in
Diethylene glycol 244.8 135 C
Propylene glycol 188.2 140 C
water as well as organic solvents.
1,3-Propanediol 214 120 C Their carefully balanced level of
Glycerine 290 260 P substitution renders them soluble
DOWANOL* EE ethylene 134.7 120 C in both water and certain organic
glycol, ethyl ether solvents or blends of solvents
DOWANOL TPM 242.4 160 P
tripropylene glycol,
(Table 4). METHOCEL 310
methyl ether cellulose ether products can be
Esters added directly to any solvent or
Ethyl glycolate 160 110 C blend of solvents under normal
Glyceryl monoacetate (Acetin) 127 100 C agitation. When using solvent blends
at 4 mbar
Glyceryl diacetate (Diacetin) 123–133 100 C
there is no need to pre-disperse the
at 5 mbar product in a non-solvent or low-
Amines solvent component.
Monoethanolamine 170–172 120 C
Diethanolamine 268–269 180 C

* Trademark of The Dow Chemical Company


a
C= completely soluble; P= partially soluble

4
Table 3: Typical Properties for METHOCEL 310 Cellulose Ether

Physical Form Slightly off-white granules

Solvent Type after 1 hour after 24 hours


Nominal viscosity in methanol (MeOH) 500 mPa.s 650 mPa.s
1% Brookfield RVT, in ethanol (EtOH) 600 mPa.s 900 mPa.s
RT, 20 rpm in methylene chloride (MeCl2) 7,500 mPa.s 10,000 mPa.s

Moisture (as packaged) max. 8%

Sodium chloride max. 1.5%

Particle size ca. 100-500 micron

Table 4: Some Typical Solvents and Solvent Blends for METHOCEL 310 Cellulose Ether

Solution Appearance

Solvents Clear, Hazy,


Smooth Structured Swellable Insoluble
Ethanol (EtOH) •
Methanol (MeOH) •
Ethanol/H2O 40/60 •
Methanol/H2O 40/60 •
Methylene chloride (MeCl2) •
MeCl2/EtOH 84/16 •
MeCl2/MeOH 84/16 •
Tetrahydrofuran (THF) •
THF/H2O 90/10-80/20 •
Isopropanol •
Isopropanol/H2O 90/10-60/40 •
Isopropanol/MeCl2 •
1,1,1-Trichloroethane •
Polypropylene glycol •
Polypropylene glycol/H2O 70/30 •
delayed thickening

Butylglycol •
Butylglycol/H2O 50/50 •
Dioxane • •
Acetone •
CELLOSOLVE™ •
Dimethylformamide •
DOWANOL PM • •

5
Chemistry of METHOCEL Figure 1: Typical Chemical Structures of METHOCEL Products
Cellulose Ethers
CH3
METHOCEL cellulose ether CH3 H H O H3C H
H H
products are available in two basic O O O OH
HO H CH2 O HO H
types: methylcellulose and
H H H
hydroxypropyl methylcellulose. O
H
HO O
Both types of METHOCEL have the HO CH2 O O CH2
polymeric backbone of cellulose, a H H
O CH3 H H O
natural carbohydrate that contains CH3 CH3
a basic repeating structure of n-2
anhydroglucose units (Figure 1). Methylcellulose
METHOCEL A brand products
During the manufacture of cellulose
ethers, cellulose fibers are heated CH3
with a caustic solution which in turn CH3 H O H
H H
is treated with methyl chloride, O O CH2 HO OH
HO H O HO H
yielding the methyl ether of cellulose. H
H H
The fibrous reaction product is H
O O
purified and ground to a fine, HO CH2 HO O
O CH2
H
uniform powder. H O CH3CHCH2 H O
Methylcellulose is made using CH2CHCH3 O CH3
n-2
only methyl chloride. These are OH CH3
METHOCEL A brand products. Hydroxypropyl Methylcellulose
For hydroxypropyl methylcellulose METHOCEL E, METHOCEL F, METHOCEL J, and METHOCEL K brand products
products (METHOCEL E, F, J, and
K brand products), propylene
oxide is used in addition to methyl If all three available positions on Higher degrees of substitution
chloride to obtain hydroxypropyl each unit are substituted, the D.S. is produce methylcellulose products
substitution on the anhydroglucose designated as 3; if an average of two that are soluble only in
units. This substituent group, on each ring are reacted, the D.S. is organic solvents.
–OCH2CH(OH)CH3–, contains designated as 2, etc.
a secondary hydroxyl on the In the METHOCEL E,
number two carbon and may also The number of substituent groups METHOCEL F, and METHOCEL
be considered to form a propylene on the ring determines the K cellulose ether products, the
glycol ether of cellulose. These properties of the various products. methoxyl substitution is still the
products possess varying ratios METHOCEL A cellulose ether major constituent (Table 5). The
of hydroxypropyl and methyl contains 27.5 to 31.5% methoxyl, molar substitution (MS) reports the
substitution, a factor which or a methoxyl D.S. of 1.64 to 1.92, number of moles of hydroxypropyl
influences organic solubility and the a range that yields maximum water groups per mole of anhydroglucose.
thermal gelation temperature of solubility. A lower degree of In the METHOCEL J and 310-
aqueous solutions. substitution gives products having Series products, the hydroxypropyl
lower water solubility, leading to substitution is about 50% of the
There are also special-grade products that are only soluble in total substitution.
METHOCEL products available caustic solutions.
that have been formulated to
meet the requirements of specific Table 5: Degree of Substitution for METHOCEL Products
industries.
Methoxyl Degree Methoxyl Hydroxypropyl Hydroxypropyl
Product of Substitution % Molar Substitution %
Degree of Substitution METHOCEL A 1.8 30 — —
The amount of substituent groups METHOCEL E 1.9 29 0.23 8.5
METHOCEL F 1.8 28 0.13 5.0
on the anhydroglucose units of
METHOCEL J 1.3 18 0.82 27
cellulose can be designated by weight METHOCEL K 1.4 22 0.21 8.1
percent or by the average number METHOCEL 2.0 25 0.8 25
of substituent groups attached to 310 Series
the ring, a concept known to
cellulose chemists as “degree of
substitution” (D.S.).
6
Applications for METHOCEL Cellulose Ethers
The diverse products and processes Wallpaper pastes. Used as the Extrusion forming. Used as a
listed here all have one thing in primary adhesive in dry mixes, temporary binder and processing
common: All benefit significantly METHOCEL cellulose ether aid, METHOCEL cellulose ethers
from remarkably small concentrations provides the wet tack required to allow precise control of rheology in
of METHOCEL cellulose ethers. hold a variety of paper types on the ceramic mixes, permitting broader
In most cases, the major benefits wall, yet has excellent slip properties operating ranges. Lubricity reduces
are improved physical properties, so patterns can easily be matched. energy consumption and die wear,
but in many applications there are In premixed pastes, METHOCEL and promotes smoother surfaces.
improvements in processing efficiency is used to control viscosity and Thermal gelation permits extrusion
and overall economy as well. improve wet tack. Pastes made with of extremely delicate, thin-walled
METHOCEL cellulose ethers are shapes without sag or deformation.
For more detailed information on
easily cleaned up with water and
any of these applications, contact Dry and isostatic pressing.
don’t provide a source of
one of the numbers listed on the METHOCEL products provide
nourishment for insects.
back cover of this brochure or visit optimum grain lubrication for
our website at www.methocel.com. Latex adhesives. METHOCEL tighter, more uniform packing.
products are used as thickeners in The results are more predictable
Adhesives a variety of latex adhesives, such as green densities, less shrinkage during
adhesives used in shoe manufacturing. firing, and higher fired strengths.
Carpet backsizing compounds. Fast drying speeds and high
METHOCEL products impart Glazes/porcelain enamel.
wet-tack strength due to thermal
excellent foaming characteristics METHOCEL cellulose ethers
gelation are key benefits in many
or “pan froth” to backsizing improve control of viscosity and
of these applications.
compounds. This helps keep the rheology and fire out completely in
adhesive in the glue line instead of the kiln.
Agricultural Chemicals
soaking into the backing materials. Injection molding. Use of
Also, due to thermal gelation, Dispersing agents. METHOCEL METHOCEL cellulose ethers
adhesives set quickly and dry faster cellulose ethers are used as suspending provides higher green densities
at elevated temperatures. and dispersing aids for wettable and better green strength. In high-
pesticide and fertilizer powders. temperature coatings/refractory
Leather processing adhesives.
They provide high wet tack and mixes and mortars, METHOCEL
METHOCEL cellulose ethers are
adhesion to waxy plant surfaces. improves workability and
used to paste hides to smooth
Chemically inert and nonionic, application properties. Because
porcelain or glass surfaces in leather
METHOCEL cellulose ether is METHOCEL products have low
drying processes. Because of its
compatible with a wide range of ionic salt residues, they won’t lower
water retention efficiency and
active ingredients. melting points. In fact, they can
thermal gelation, METHOCEL is
much more effective than starch- Spray adherents. Spray adherents permit a reduction in use of
based pastes. or “seed stickers” made with plasticizers with low melting points.
METHOCEL products effectively
Plywood laminating adhesives.
bind pesticides, inoculants, and Chemical Specialties
METHOCEL products are used
nutrients to seeds. METHOCEL
in plywood laminating adhesives Resins. METHOCEL cellulose
products feature low plant toxicity
to control viscosity in glues for ethers are used to control rheology
and won’t harm germinating plants.
plywood manufacture. Thermal and as a colloidal stabilizer in a
gelation and thickening properties variety of epoxy, fiberglass, and
of METHOCEL products keep Ceramics Processing urea-formaldehyde resins.
the adhesive from soaking into Tape casting. Use of METHOCEL METHOCEL provides ideal flow
the wood. products provides better flow and and leveling characteristics, plus
leveling and more uniform quick-set properties due to
Cigar and cigarette adhesives.
thickness. Low sodium residues thermal gelation.
Safe and efficient, METHOCEL
products have long been used as provide the purity necessary for
binders for reconstituted tobacco electronic items. Thermal gelation
sheets and as adhesives for cigar and reduces binder migration and
cigarette manufacture. surface faults.

7
Rubber. METHOCEL products Cement plaster and stucco. Structured vegetable products.
are used as mold-release agents, METHOCEL cellulose ethers METHOCEL products offer
stabilizers, and thickeners in rubber provide water retention for proper excellent film formation and high
latexes. METHOCEL cellulose curing, improved workability, and binding performance for foods that
ethers contribute to more uniform pumpability. need to keep their components
drying and less pinholing. together. Products like vegetarian
Foods burgers, onion rings, and formed
PVC suspension polymerization.
Bakery products. Thermal gelation potato products are all improved
METHOCEL products are used in
aids in gas retention during baking, by the binding strength and
PVC polymerization as primary and
increasing baked volumes and film formation qualities of
secondary suspension agents. They
improving texture. METHOCEL METHOCEL products.
provide excellent particle size control,
good porosity for improved plasticizer also provides a more moist texture, Structured and extruded foods. Low
absorption, low reactor scaling, and increased shelf life, improved concentrations of METHOCEL
high bulk densities. emulsification of batters, and better give optimum binding strength in
freeze/thaw stability. matrix systems. Due to moisture
Construction Products Confections. In glazes, icings, and retention and oil insolubility
Drywall tape-joint compounds. coatings, METHOCEL food gums properties, fried foods are more
METHOCEL products impart add lubricity for easier application, moist, less greasy. Thermal gelation
workability, shrink and crack provide creamier texture, improved gives increased control over texture
resistance, slip, and adhesion in spreadability, and clean flavor and “bite.” Increased lubricity aids
tape-joint compounds. Water release. In addition, METHOCEL in processing.
retention properties increase open gums thermally gel during heating, Frying batters. In addition to
times and help maintain a wet edge. keeping icings and glazes intact, and forming an oil-insoluble barrier to
during cooling revert to the original block oil absorption and moisture
Cement-based tile mortars.
consistency of the product. loss during frying, METHOCEL
METHOCEL cellulose ethers provide
water retention and workability Pie and pastry fillings. Thermal products improve adhesion of
to Portland cement-based ceramic gelation reduces boil-over during batters to meat and vegetable
tile mortars and grouts. They also baking and inhibits moisture substrates. As a result, blow-off of
improve adhesion, reduce skinning, migration from fillings to crusts batters is reduced and the life of
and increase open time. during freezing. METHOCEL also frying oil is extended.
improves freeze/thaw stability. Salad dressings and sauces. Better
Masonry mortars. Used as
performance additives in masonry Frozen desserts. METHOCEL stability for oil-in-water emulsions
mortars, METHOCEL products products modify ice-crystal size to extends the shelf life of products
extend board life and improve give smoother textures and improve containing METHOCEL. Solids stay
workability. METHOCEL also emulsion stability. Increased air in suspension longer and body and
contributes to air entrainment, often entrainment improves overrun. pouring characteristics are controlled.
reducing the need for other additives
Whipped toppings. METHOCEL Gelled Fuels
for this purpose.
products improve whipping
Fuel thickeners. METHOCEL
Gypsum adhesives and gypsum and properties for better body and
cellulose ethers are used as thickeners
cement hand and spray plasters. appearance. Improved emulsion
for gelled alcohol used in charcoal
METHOCEL cellulose ethers stability prevents syneresis and
lighters, restaurant candles, and
impart workability, pumpability, extends open times. METHOCEL
canned-fuel products.
and consistency to adhesives and inhibits phase separation in frozen
hand and spray plasters. They also toppings, even through repeated
provide water retention and anti- freeze/thaw cycles. Household Products
sag properties. Cleaners and detergents. Use
of METHOCEL provides viscosity
Wall and ceiling textures. control, cling, foaming, soil
METHOCEL products impart anti-redeposition, and emulsion
pumpability, adhesion, workability, stabilization to household
and water retention in wall and cleaners and detergents.
ceiling texturizing products.

8
Paints level, it’s the thickener of choice ETHOCEL* ethylcellulose resins.
Latex paints. METHOCEL for shampoos designed for dry and The water-soluble METHOCEL
cellulose ethers are used as normal hair. METHOCEL also dissolves out of the film, leaving
thickeners, protective colloids, and helps stabilize foams, so shampoos the water-insoluble ETHOCEL
pigment-suspension aids in latex have better lather characteristics. ethylcellulose. Drug diffusion and
paints. They provide high enzyme film porosity are controlled by the
Body Gels. The natural lubricity of
resistance which helps stabilize amount of METHOCEL used.
METHOCEL products can improve
viscosity. Film-forming properties product flow, aid in dispensing and Water-soluble thermoplastics.
contribute to better paint film enhance sensory characteristics. Just METHOCEL cellulose ethers can
quality with fewer pinholes. The as in shampoos, METHOCEL be heated and mixed with a
product uniformity offered by cellulose ethers add texture and plasticizer for extrusion or molding
METHOCEL cellulose ethers can provide a superior volume of into a wide range of physical forms.
mean lower quality control costs lubricious, stable lather especially This process is used to produce
and more predictable performance important in the formation of single-unit matrix tablets; multi-
for paints. Their use also improves bubble baths and shower gels. particle delivery, such as extruded
wet-edge retention. They offer beads or chips; transdermal patches;
flexibility and ease of incorporation. Creams and lotions. METHOCEL
suppositories; or liquid-filled
can contribute film-forming and
hard-shell capsules.
Paint Removers secondary-thickening properties
which improve after-feel and other Liquid preparations. METHOCEL
Scrape-off and flush-off paint
sensory characteristics in creams products are used in oral and
removers. The unique combination
and lotions. topical liquid pharmaceuticals
of organic and water solubility
because they are excellent thickeners,
offered by METHOCEL products
Pharmaceuticals improve emulsion stability, suspend
makes them ideal thickeners for
Tablet coatings. METHOCEL solids, lubricate, and retain moisture.
scrape-off and flush-off paint
cellulose ethers form strong films The protective colloid action
removers (both methylene chloride
with good adhesion. They provide and emulsifying properties of
and alternative paint strippers).
taste-masking films and act as METHOCEL also benefit many
They provide the thickening and
excellent barriers for water-sensitive liquid formulations.
cling needed to retain the paint
remover on vertical or inclined drugs or components. Coatings
surfaces, yet permit the softened of METHOCEL also increase Printing
paint to be rinsed off easily compressive strength and Printing inks. METHOCEL
with water. reduce friability. cellulose ethers are used as
thickeners and suspending agents
Granulation. Used at low
Paper Products for water-based inks.
concentrations as binders in the
Grease-proof coatings, adhesives, granulation process, METHOCEL
release coatings, and surface products produce hard tablets Textiles
sizings. Grease and oil barrier with low friability, yet don’t Textile printing pastes. Used as
properties, in conjunction with negatively affect tablet disintegration. emulsion stabilizers in textile
film-forming capabilities, make METHOCEL allows the reduction printing pastes, METHOCEL
METHOCEL valuable in a variety of compression force, an important cellulose ethers help keep inks from
of paper coatings and sizings. The factor in extending the life of wicking into fabrics.
excellent film properties (high tensile tooling and equipment. Fabric sizings. METHOCEL
strength and good elongation) helps hold fibers together, which
Controlled release. METHOCEL
offered by METHOCEL play key strengthens fabrics during
cellulose ether can be used for
roles in these applications. manufacturing processes. The
controlled-release pharmaceuticals
using two different methods. It is lubricity of METHOCEL helps cut
Personal Care Products used in hydrophilic-matrix tablets or friction, permitting faster
Shampoos. METHOCEL cellulose capsules as described in a separate equipment speeds.
ether is widely used as a thickener bulletin on sustained release. In Temporary adhesives. Excellent
in shampoos. Because the thickening addition, METHOCEL is used in wet-tack and quick-set properties
performance of METHOCEL diffusion control films comprised of make METHOCEL an ideal
doesn’t depend on a high surfactant METHOCEL cellulose ethers and temporary fabric adhesive.

* Trademark of The Dow Chemical Company 9


Regulated Uses
Chemical Inventory To support new drug applications in METHOCEL E, F, or K products,
the United States, masters files for one could use “hydroxypropyl
METHOCEL products,
these products are on file at the methylcellulose” or “carbohydrate
methylcellulose and hydroxypropyl
Bureau of Drugs of the U.S. Food gum.” METHOCEL products are
methylcellulose, comply with all
and Drug Administration. also certified as kosher for year-
applicable rules and orders under
round and Passover use by the
Toxic Substances Control Act
Union of Orthodox Jewish
PL94-469. The Chemical Abstracts Foods
Congregations of America.
Services Registry No. (CAS) is
METHOCEL food gums have
9004-67-5 for methylcellulose and
long been used in the food industry. Pesticide Use
9904-65-3 for hydroxypropyl
METHOCEL food gums are Under 40CFR 180.1001, certain
methylcellulose.
approved within the Food inert ingredients used in pesticide
METHOCEL products have Chemicals Codex and are listed as formulations are exempt from the
also been reported for the methylcellulose and hydroxypropyl requirements of a tolerance.
following inventories: methylcellulose. Methylcellulose and hydroxypropyl
European Inventory of Existing In the U.S., methylcellulose is methylcellulose may be used in
Chemical Substances (EINECS) approved as a multiple purpose formulations applied to growing
GRAS food substance according to crops or raw agricultural
Australia Inventory of Chemical commodities after harvest. Both
21CFR 182.1480. It is also allowed
Substances (AICS) Standard and Premium grade
for use in meat products according
Ministry of International Trade and to 9CFR 318.7 and 9CFR 381.147. METHOCEL cellulose ether
Industry Inventory (MITI, the Hydroxypropyl methylcellulose is products are appropriate.
Japanese inventory) approved for direct food use by the
FDA under 21CFR 172.874. It is
Canadian Domestics Substances
also approved by the USDA as an
List (DSL)
emulsifying agent, binder, thickener,
Many countries are in the midst of and stabilizer and is listed in the
creating new chemical inventories. Standards and Labeling Policy Book
published by the USDA. Because
Pharmaceuticals they are approved for direct food
use, METHOCEL products can also
Premium grades of METHOCEL A, be used as packaging components
METHOCEL E, METHOCEL F, and in indirect food applications.
and METHOCEL K products are
used for pharmaceutical and topical In the European Union,
applications. Premium grades of METHOCEL food gums are
METHOCEL products meet the approved for use within the
specifications of the United States European Directive 95/2/EC.
Pharmacopoeia (USP XXIII), Hydroxypropyl methylcellulose and
European Pharmacopoeia (EP) and methylcellulose are included in
Japanese Pharmacopoeia (JP) and Annex I of this Directive.
are listed as methylcellulose and When labeling these food
hypromellose1. In addition, ingredients, one can use either their
methylcellulose (METHOCEL A proper chemical names or their
products) is Generally Recognized common names. Therefore, one
As Safe (GRAS) by the U.S. Food could use “methylcellulose” or
and Drug Administration. “modified vegetable gum” for
METHOCEL A products. For

1 Theformer official monograph name of hypromellose


was “hydroxypropyl methylcellulose” or “HPMC.” 10
How To Prepare Aqueous Solutions of
METHOCEL Cellulose Ethers
METHOCEL cellulose ether the METHOCEL product to be systems. A trigger can conveniently
products are carbohydrate added to a formulation and be used by adding a small amount
polymers which dissolve in cold dispersed at relatively low shear of a base, such as ammonium
water (and in some instances in without any significant viscosity hydroxide, sodium bicarbonate,
certain organic solvents) by increase initially. etc. If METHOCEL is dispersed in
swelling and subsequent hydration. neutral water (pH approximately 7),
The “time delay” of the hydration
There is no sharp solubility limit there is adequate time for thorough
or viscosity build is a function of
such as occurs in the dissolution of dispersion. Addition of base to
the level of surface treatment as
ionizing salts. The concentration of raise the pH to approximately 9
well as temperature, pH of the
METHOCEL in solution is usually causes the hydration to be
system, and concentration of the
limited by the viscosity that a completed in just a few minutes.
METHOCEL product. Normally,
manufacturer is equipped to handle.
the concentration of METHOCEL For best results and to achieve
It also depends on the viscosity
in the system does not become a maximum hydration, surface-treated
and chemical type of METHOCEL
factor until the concentration powders should be added with
product used. Solutions of low-
exceeds 5% by weight (relative good agitation to a neutral pH
viscosity products can be made at
to water in the system). At higher system. The system should be
10% to 15% concentration. High-
concentrations, the time of agitated thoroughly for a few
viscosity products find a normal
hydration (referred to as delay minutes, followed by an adjustment
limit at 2% to 3% concentration.
time) is reduced. The delay time is of pH to 8.5 to 9.0 with continued
The form of METHOCEL generally reduced as temperature agitation, until full viscosity is
cellulose ether product chosen is raised. Figure 2 shows a typical reached (usually 10 to 30 minutes).
(powder or surface-treated powder, delay time as a function of pH, Once the pH has been shifted to
or granules) influences the techniques evaluated at room temperature. the alkaline side (pH 8.5 to 9.0),
used to make solutions. Surface- allowing full and rapid
In many cases it is desirable to
treated and granular products can solubilization of the surface-treated
“trigger” viscosity build immediately
be added directly to aqueous product, solutions are stable over
following dispersion. Aqueous
systems. They disperse readily with the pH range of 3 to 11.
slurries can be held for 45 minutes
mild agitation and dissolve (build
and still remain usable in neutral
viscosity) gradually under neutral
conditions. The dissolution rate
of surface-treated products can Figure 2: Typical Hydration Delay Time of Surface-treated METHOCEL
be increased by adjusting to an Products as a Function of pH
alkaline pH after dispersing the 1000.0
powder in water. Although
untreated METHOCEL powders
are soluble in cold water, they
must first be thoroughly dispersed 100.0
Hydration Time, min

in the water to prevent lumping.

Working with Surface-treated 10.0


Dispersible Powders
In many applications, the
combination of easy dispersion in 1.0
cold water and rapid hydration
(viscosity build) is desirable.
Surface-treated METHOCEL
powders are chemically treated so 0.1
that they become temporarily 0 2 4 pH 6 8 10
insoluble in cold water. This allows

11
The addition of a slurry to an Working with Untreated Powders Dispersion in Hot Water
alkaline pigment grind or filler
dispersion, or the addition of a Although METHOCEL powders Often called the “hot/cold” technique,
slurry to a basic pigment-latex are soluble in cold water, they must this method takes advantage of the
formulation, provides rapid first be thoroughly dispersed in the insolubility of METHOCEL cellulose
solubilization and uniform viscosity water to prevent lumping. In some ethers in hot water. The powder is
development. The addition of dry, applications, dispersion can be first dispersed by mixing thoroughly
alkaline pigments or fillers to a accomplished at ambient with 1/5 to 1/3 of the total required
slurry on high-speed or low-speed temperatures or in cold water by volume of water that has been
mixing equipment also results in using an eductor funnel or high- heated to above 90°C (194°F).
rapid solubilization and viscosity shear mixer. However, if untreated Mixing continues until all particles
development. powders are added directly to cold are thoroughly wetted.
water without sufficient agitation, a
For complete solubilization, the
CAUTION: Attempts to adjust the pH of lumpy solution may result. Lumping
high-concentration slurries may lead to remainder of the water is then
results from incomplete wetting of
excessively high viscosity so that they cannot added as cold water or ice to lower
the individual powder particles.
be pumped or poured. The pH adjustment the temperature of the dispersion.
Only part of the powder dissolves,
should be made only after a slurry is diluted to Once the dispersion reaches the
a gelatinous membrane which
the concentration at which it will be used. temperature at which that particular
shields the remaining powder from
METHOCEL product becomes
complete hydration. Several
Dispersion Technique water soluble, the powder begins to
dispersion techniques are commonly
hydrate and viscosity increases.
1. Add the surface- used and are described below. Each
treated METHOCEL has advantages in certain
powder to the water. applications.
Begin agitation. Figure 3: Viscosity Development of METHOCEL A and
2. Continue agitation METHOCEL K Products Slurried at 2% in Hot Water
and add sufficient
ammonium hydroxide,
sodium bicarbonate, 10,000
or other alkaline
material (e.g., pigment
grind) to the dispersion
to obtain a pH of 8.5 to 9.0. Viscosity on Initial
This will result in rapid viscosity Cooling of
development. Continue agitation METHOCEL A Premium
until sufficient hydration has 1,000
Viscosity, mPa.s

been achieved.

Viscosity on Initial
Cooling of
METHOCEL K Premium
100

10
100 80 60 40 20 0
Temperature, °C

12
In some applications, it may be Dispersion Technique Dispersion Technique
desirable to heat the entire volume 1. Heat approximately 1. Combine
of water, disperse the METHOCEL 1/3 the required METHOCEL powder
powder, then cool the mixture while volume of water to at with other dry-powder
agitating until hydration is complete. least 194°F (90°C). ingredients. The
It is very important, however, to
suggested ratio of other
have adequate cooling after wetting
dry-powder ingredients
with hot water to ensure complete 2. Add the METHOCEL
to METHOCEL is 7:1; however, the
hydration and viscosity development. powder to the heated
water with agitation. ratio may vary from 7:1 to 3:1.
For improved clarity and reproducible
control of viscosity, solutions of
METHOCEL A cellulose ether 3. Agitate the mixture 2. Thoroughly blend
products (methylcellulose) should be until the particles are the dry components.
cooled to 0° to 5°C (32° to 41°F) thoroughly wetted
for 20 to 40 minutes. In general, and evenly dispersed.
solutions of METHOCEL E, 3. Add the dry mix
METHOCEL F, METHOCEL J, to the water with
and METHOCEL K brand 4. For complete agitation. The rate of
cellulose ethers (hydroxypropyl solubilization, add hydration will depend
methylcellulose) require cooling to the remainder of the upon both the relative
20° to 25°C (68° to 77°F) or below. water as cold water particle sizes and the rate of
or ice to lower the agitation during and after addition
Because complete hydration depends
temperature of the dispersion. of the mixture to the water.
on adequate cooling, METHOCEL
Once the dispersion reaches the
E, F, J, and K brand products are 4. Agitate until the
temperature at which that particular
frequently used in applications METHOCEL powder
METHOCEL product becomes
where cold water is not available. has completely
water soluble, the powder begins to
Figure 3 illustrates the effects of hydrated and the
hydrate and viscosity increases.
cooling hot slurries of METHOCEL solution is consistently
See pages 12 and 13 for cooling
A and METHOCEL K products. smooth. Your solution
times and temperatures for specific
This figure shows that a slurry of of METHOCEL
METHOCEL products.
METHOCEL K brand cellulose cellulose ether is now ready for
ether requires much less cooling 5. Continue agitation further processing.
for hydration than a slurry of for at least 30 minutes
METHOCEL A cellulose ether. after the proper Dispersion in Concentrated Salt
Slurries of METHOCEL E, F, and J temperature is Solutions
brand products also require less reached. Your
cooling than METHOCEL A solution of Both untreated and surface-treated
brand products. METHOCEL cellulose METHOCEL cellulose ethers can
ether is now ready to use. be dispersed in concentrated salt
solutions. Dissolution occurs when
Dispersion by Dry-Blending the brine is diluted with cold water.

Dry-blending involves mixing


METHOCEL powder with other
dry ingredients before adding the
water component. Dry-blending
separates the particles of METHOCEL
cellulose ethers to allow thorough
wet-out and complete hydration
when water is added. The minimum
ratio of other dry, powdered
ingredients to METHOCEL powder
varies from 7:1 to 3:1.

13
How To Prepare Solutions of METHOCEL Cellulose
Ethers in Nonaqueous Solvents and Nonsolvent Media
Solubility in Nonaqueous Dispersion Technique
Solvents
The solubility of METHOCEL 1. Add the METHOCEL
cellulose ethers in nonaqueous media cellulose ether to the
varies according to the nature and non-solvent. A ratio of
quantity of substituent groups on the 5–8 parts non-solvent to
anhydroglucose chain. When using a 1 part METHOCEL is
water-miscible, organic solvent, such recommended to obtain
as an alcohol or glycol, use a ratio a liquid slurry.
of at least 5 to 8 parts of solvent to
1 part METHOCEL.
2. Agitate the mixture
Dispersion in Non-solvent Media and METHOCEL
powder until the particles
Untreated METHOCEL cellulose of METHOCEL cellulose
ethers may also be dispersed in ether are evenly dispersed.
non-solvent media such as vegetable
oil, propylene glycol, polyethylene
glycol, glycerine, corn syrup, and 3. The dispersion of
high-fructose corn syrup. A ratio of METHOCEL in a non-
5 to 8 parts non-solvent to 1 part solvent medium may be
METHOCEL is recommended to added to cold water, or
obtain a fluid slurry. The dispersion the cold water may be
of METHOCEL in a non-solvent added to the dispersion.
medium may then be added to cold
water, or the cold water may be
added to the dispersion. 4. Continue mixing until
the METHOCEL powder
is completely hydrated
and the solution is
smooth. You can now add
the remaining ingredients
in your formulation.

14
Properties of METHOCEL Cellulose Ethers in
Powder Form
METHOCEL cellulose ether Resistance to Microorganisms As the cellulose is modified by
products are white to slightly off- substitution with various radicals,
An important property of
white powders which are essentially such as alkyl and hydroxyalkyl
METHOCEL cellulose ether
odorless and tasteless. The apparent groups, resistance to microbial
products is their high resistance
density of the powders ranges from attack increases. Several researchers
to attack by microorganisms.
0.25 to 0.70 g/cm3 (250–700 kg/m3). have reported that the degree of
METHOCEL products with higher
substitution (D.S.) of water-soluble
degrees of substitution are especially
Moisture Sorption cellulose derivatives was a primary
resistant to enzymes. The fact that
factor, with a threshold D.S. value
METHOCEL products sealed in virtually all METHOCEL
of 1.0 required for protection.†
their original shipping containers methylcellulose and METHOCEL
absorb little to no atmospheric hydroxypropyl methylcellulose Because METHOCEL cellulose
moisture. Once a container is ethers pass through the intestinal ether products have excellent
opened, however, there is pickup tract essentially unchanged attests to uniformity of substitution, with a
of moisture from the air. When the stability of these products to a D.S. much higher than 1.0, they
“exposed” METHOCEL cellulose wide range of biochemical and possess excellent resistance to
ether is weighed, a portion of the enzymatic systems. Shelf-life in microbial attack.
total weight, therefore, may be paints and other latex-based
water. Such weight must be corrected coatings, and stability of
for moisture content to ensure that solutions and other products
the proper weight of METHOCEL containing METHOCEL cellulose
is used to give the desired viscosity. ether, can be greatly increased by
this resistance to microorganisms.
To minimize moisture pickup,
opened bags should be tightly
Figure 4: Equilibrium Moisture Content
resealed. The moisture-sorption vs. Percent Relative Humidity, 25°C
rate of METHOCEL K brand
80
products is somewhat greater than
for METHOCEL A brand products. 70
However, the moisture-sorption
rates are about the same within a 60
single chemical type. Typical
%H2O, 25°C

50
moisture sorption is shown in
Figure 4. 40

30

20

10

0
0 10 20 30 40 50 60 70 80 90 100
% Relative Humidity, Mean Average Value,
+95% Probability

†H.S. Levinson and E.T. Reese, J. Gen. Physiol. 33, No. 601 (1950).
E.T. Reese, R.G.H. Siu, and H.G. Levinson, J. Bacteriology 59, No. 485 (1950).
E.T. Reese, Ind. Eng. Chem. 49, No. 104 (1957).

15
Properties of Solutions of METHOCEL Cellulose Ethers
Some of the general solution Rheology of an aqueous solution
properties of METHOCEL cellulose of METHOCEL is affected by its
ether products are listed in Table 6. molecular weight, concentration,
temperature, and by the presence of
Rheology of Solutions of other solutes. In general, aqueous
METHOCEL Cellulose Ether solutions of METHOCEL exhibit
pseudoplastic flow behavior.
The rheology of solutions of Pseudoplasticity increases with
METHOCEL plays an important increasing molecular weight or
role in many practical applications concentration. However, at very
where the modification of flow low shear rates, all solutions of
behavior is essential (for example, METHOCEL cellulose ether appear
paints, cosmetics, food products, to be Newtonian and the shear rate
building products). A Newtonian below which the solution becomes
fluid is one whose viscosity is Newtonian increases with decreasing
independent of shear rate (or molecular weight or concentration.
velocity gradient of flow). In actual Figures 5 and 6 illustrate this
practice many systems exhibit non- behavior (the numbers on curves
Newtonian flow behavior where indicate viscosity types).
apparent viscosity may decrease
(pseudoplastic) or increase (dilatant)
with increasing rate of shear.

Table 6: General Solution Properties

Specific gravity, 4°C, all types


1% solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.0012
5% solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.0117
10% solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.0245
Refractive index, 2% solutions, all types
1.336
Partial specific volume
4,000 mPa·s METHOCEL A . . . . . . . . . . . . . . . . . . . . . . . 0.725 cm3/g (0.087 gal/lb)
4,000 mPa·s METHOCEL E . . . . . . . . . . . . . . . . . . . . . . . 0.767 cm3/g (0.092 gal/lb)
4,000 mPa·s METHOCEL F . . . . . . . . . . . . . . . . . . . . . . . 0.734 cm3/g (0.087 gal/lb)
5,000 mPa·s METHOCEL J . . . . . . . . . . . . . . . . . . . . . . . 0.725 cm3/g (0.087 gal/lb)
4,000 mPa·s METHOCEL K . . . . . . . . . . . . . . . . . . . . . . . 0.717 cm3/g (0.086 gal/lb)
15,000 mPa·s METHOCEL K . . . . . . . . . . . . . . . . . . . . . . 0.724 cm3/g (0.087 gal/lb)

Freezing point, 2% solutions, all types


0.0°C at 2% concentration
Surface tension, 25°C, 0.05% concentration
Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72–74 x 10-3 Newton/meter (72–74 dynes/cm)
Methylcellulose. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53–59 x 10-3 Newton/meter (53–59 dynes/cm)
Hydroxypropyl methylcellulose . . . . . . . . . . . . . . . . . . . 43–55 x 10-3 Newton/meter (43–55 dynes/cm)

16
Figure 5: Apparent Viscosity vs. Shear Rate, 2% Aqueous Solutions, 20°C
10,000

4,000
Apparent Viscosity, mPa.s

1,500
1,000
400

100
100

25

10
0.1 1 10 100 1,000
Shear Rate, s-1

Figure 6: Apparent Viscosity vs. Shear Rate, for Aqueous Solutions of 4,000
mPa.s METHOCEL Cellulose Ethers at Various Concentrations
10,000

2%
Apparent Viscosity, mPa.s @ 20°C

1.5%

1,000

1%

100

0.5%

10
0.1 1 10 100 1,000
Shear Rate, s-1

17
Molecular Weight/Viscosity Figure 7: Molecular Weight/Viscosity Correlation, 20°C
Relationships
The apparent viscosity of an
aqueous solution of a METHOCEL
cellulose ether is proportional to the 100,000
molecular weight or chain length of
the specific METHOCEL product Mn
used. Commercial designations of
METHOCEL products are based
on viscosity values determined in
water at 20°C, with a concentration 10,000
of 2% METHOCEL. The
measurement methods used are
Viscosity of an Aqueous Solution, mPa.s @ 20°C
described in the current ASTM
monographs D1347 and D2363.
The correlation between the number
average molecular weight (Mn) and
1,000
the commercial viscosity designation
for METHOCEL A cellulose ethers
is shown in Figure 7.
Mw
Table 7 provides further information
regarding the correlation of number
average molecular weight with the 100
commercial viscosity designation.
Intrinsic viscosity is the limiting
quotient of the specific viscosity
divided by the concentration as
infinite dilution is approached (as
the concentration approaches zero).
10
The number average molecular
weight (Mn) is calculated from the
limiting osmotic pressure of the
solvent as the concentration of
the solute approaches zero. The
average molecular weight (Mw)
will be 3 to 10 times the Mn. 0
1,000 10,000 100,000
Molecular Weight
Effect of Concentration on
Viscosity
Most formulations require a Table 7: Viscosity of Methylcellulose of Various Molecular Weights
predetermined product viscosity of
Intrinsic Number Average Number Average
METHOCEL cellulose ether. Figure Viscosity Grade Viscosity Degree of Molecular
8 shows how the concentration of 2%, 20°C, mPa·s (h), dL/g Polymerization Weight (Mn)
METHOCEL products of varying
5 1.2 53 10,000
viscosity affects the aqueous solution 10 1.4 70 13,000
viscosity at 20°C. The measurements 40 2.0 110 20,000
were made using an Ubbelohde 100 2.6 140 26,000
viscometer (ASTM D2363). Data 400 3.9 220 41,000
1,500 5.7 340 63,000
for both low and high molecular
4,000 7.5 460 86,000
weight METHOCEL products are 8,000 9.3 580 110,000
shown and represent the average 15,000 11.0 650 120,000
material found within a viscosity 19,000 12.0 750 140,000
specification. 40,000 15.0 950 180,000
75,000 18.4 1,160 220,000

18
This graph is plotted on an 8th Blending for Intermediate starting materials are 400 mPa·s
root scale, not a logarithmic scale. Viscosity on the left and 15,000 mPa·s on
The 8th root of the viscosity is the right.
METHOCEL products of the same
a roughly linear function of
substitution type, but of different Now find the desired final
the concentration.
viscosity grades, can be blended to viscosity on either axis and draw a
The equation which expresses obtain an intermediate viscosity horizontal line that intersects with
the illustrated approximate grade. Figure 9 is a blending chart the first line. From this intersection
relationship between solution that can be used for this purpose. point, draw a vertical line down to
viscosity and polymer the bottom scale. The number of
To use the chart, mark the
concentration is 1/8 = (C·) + 1, that scale shows the percentage of
viscosity of one material along the
where  is the solution viscosity Scale B Material needed in the
left axis (Scale A) and the viscosity
in millipascal-seconds, C is the blend. In this example 4,000 mPa·s
of the other material along the
polymer concentration in solution is the desired final viscosity. So the
right axis (Scale B). Connect the
(expressed in percent), and  is a required blend is 60% of the
two points in a straight line that
constant specific to the molecular 15,000 mPa·s (Scale B) material
crosses the graph. In the example
weight. The value of  may be and 40% of the 400 mPa·s
shown, the viscosities of the
calculated by substitution and may (Scale A) material.
then be used to calculate the
approximate viscosity at the
Figure 8: Viscosity/Concentration Relationships
desired concentration.
100,000
For example, for a 4,000 mPa·s 75,000
product, (4,000)1/8 = (C·) + 1. 100,000
Solving for  yields a value of 50,000
40,000 1,500
0.910. For a 1,500 mPa·s product,
(1,500)1/8 = (C·) + 1. Solving for 15,000
 yields a value of 0.747. Having
calculated  for a particular 15,000
400
METHOCEL product, this value 10,000
Viscosity, mPa.s @ 20°C

can be used to calculate viscosity


at other concentrations.
4,000
4,000
To find the line for any intermediate
grade, locate the desired 2% 50

viscosity above 2% on the abscissa 1,500


and draw a straight line to the 1,000
point of origin.
100 15
400
250

100
50
5
25
15
10

1
0 1 2 3 4 5 6 7
% METHOCEL Cellulose Ether

19
The relationship may be expressed Figure 9: Blending Chart
mathematically as: B1/8 = x111/8 + 100,000 100,000
x221/8 , where x1 and x2 are the
weight fractions of components
one and two, respectively.
The example on the chart shows
that 60% of 15,000 mPa·s material 15,000
and 40% of the 400 mPa·s material
are needed to make a blend having
a viscosity of 4,000 mPa·s. 10,000 10,000

Viscosity, mPa.s @ 20°C


4,000

Viscosity, mPa.s @ 20°C


Effect of pH on Viscosity
Because METHOCEL products
are nonionic, the viscosities of
their solutions are generally stable
1,000 1,000
over a wider pH range than are
the viscosities of gums that are

Scale B
Scale A

ionic in nature. Outside the range


400
of pH 3 to 11, however, there may
be a gradual loss of viscosity at 100 100
higher temperatures or after long
periods of standing, especially with
high-viscosity solutions. Solutions
of METHOCEL cellulose ethers in 10 10
acids or in strong caustic solutions
will decrease in viscosity. This
factor should be considered
0 20 40 60 80 100
when determining the shelf life
of products. % of Scale B Material in Blend

Effect of Additives on Viscosity


In systems having lower precipitates or haze. This lack of
In the preparation of formulations, concentrations of additives (~1%), phase separation on freezing is
viscosities may occasionally result METHOCEL A or METHOCEL F particularly important in frozen
which are considerably higher than products are frequently suitable. In food items. As solutions of
expected. This phenomenon can systems where the concentration of METHOCEL cellulose ether
be caused by the interaction of additives is rather high (~10%), products are cooled, solubilization
METHOCEL with one or more the more highly substituted increases, as evidenced by
of the formula ingredients. As a products such as METHOCEL E, increasing viscosity and improved
result, it may be possible to use J, or K products may be more clarity of solutions. When the
less thickener and still have compatible. solutions freeze, part of the water
adequate viscosity. is held in the latent super-cooled
Effect of Freezing on Solutions state and does not freeze. The heat
This effect usually passes through
normally released on freezing (heat
a maximum that is dependent on Solutions of METHOCEL cellulose of fusion) is decreased by the
the concentration of the interacting ether products do not undergo amount of the super cooling.
materials and on the presence of separation into phases upon
other ingredients such as pigments, freezing. There is no separation
latex particles, or preservatives. of fluid layers (syneresis) or
formation of insoluble

20
Defoamers for Aqueous Solutions Compatibility of Aqueous
Solutions
The foaming of solutions of
METHOCEL cellulose ethers is The methylcellulose molecule is
easily controlled by using foam nonionic and is not precipitated as
stabilizers and defoamers. an insoluble salt by multivalent
metal ions. However, METHOCEL
Defoamer concentrations should
cellulose ethers can be salted out
be kept to the minimum required
of solution when the concentration
because these materials are generally
of electrolytes or other dissolved
low in water solubility. The choice
materials exceeds certain limits.
of a defoamer depends on the type
This is caused by competition
of surfactant, latex, and other
of the electrolytes for water and
ingredients in the system. For
results in reduced hydration of the
defoaming complex systems,
cellulose ether.
consultation with the supplier of
defoamers is suggested. Because of the difference in the
amounts of organic substitution,
Antifoam agents are extremely
METHOCEL E, F, J, K, and
efficient surface-active compositions
310-Series brand hydroxypropyl
which displace other surface-active
methylcellulose products generally
substances at the air/water interface.
exhibit a higher tolerance for salts in
Their use, therefore, might interfere
solution than METHOCEL A brand
with the performance of METHOCEL
methylcellulose products. There is
products in applications where the
only a slight variation in electrolyte
mechanical properties of solution-
tolerance among the various
surface films is critical.
METHOCEL hydroxypropyl
methylcellulose products.
Preservatives for Aqueous
Solutions Water-insoluble materials such as
pigments, fillers, etc. will not
METHOCEL cellulose ethers adversely affect METHOCEL
normally do not require cellulose ethers. Actually, solutions of
preservatives. They are not, METHOCEL often serve as excellent
however, antimicrobial agents. dispersing media for such materials.
If contamination occurs, Other water-soluble substances, such
microorganism growth will not as starches, glues, and resins, may or
be inhibited. may not be compatible with
To preserve solutions of METHOCEL. Tests should be run
METHOCEL, addition of 0.05% on these materials to determine
to 0.15% of DOWICIDE* A compatibility. Because METHOCEL
antimicrobial or DOWICIL* 75 cellulose ether products are not
preservative is suggested. More soluble in concentrated salt solutions,
information on these products is these media can be used as
available upon request. For regulated non-solvent dispersing media for
uses, you should use the appropriate non-surface-treated METHOCEL
permitted preservative. products. Subsequent dilution
reduces the salt concentration to a
level that allows dissolution of the
METHOCEL product.

* Trademark of The Dow Chemical Company

21
Thermal Gelation in Aqueous Media
METHOCEL cellulose ethers Gel strength continues to build as
possess unique solubility properties the temperature is held above the
in aqueous media. These products gel point.
are insoluble in water that has
When the solution is cooled, the gel
been heated above a particular
effect begins to reverse and viscosity
temperature. Below those
drops rapidly. Finally, the viscosity
temperatures, the solution and
of the cooling solution merges
solubility of the METHOCEL
with the original heating curve
cellulose ether products increase as
and increases as the temperature
the temperature is lowered. Aqueous
decreases. Once the solution has
solutions of METHOCEL cellulose
cooled, the viscosity is the same as it
ethers will gel when heated to
was originally. Thus, the thermal
temperatures that are specific for
gelation process is reversible and
each type. The gels are completely
can be repeated if desired.
reversible and the solutions liquefy
upon cooling. This unique bulk
thermal-gelation property proves Figure 10: Gelation of 2.0% Aqueous Solution
valuable, compared to that of other of METHOCEL A100 Methylcellulose, Heating
natural and synthetic gums, in a 0.25 Rate
C/min 0.25°C/min
wide variety of applications. 200

Bulk thermal gelation of aqueous

Continued Heating
Gelled
solutions of METHOCEL is thought
to be primarily caused by the 160
hydrophobic interaction between Co
oli
molecules containing methoxyl ng
groups. In a solution state at lower
Viscosity, mPa.s

temperatures, molecules are hydrated 120


and there is little polymer-to-polymer
interaction other than simple
entanglement. Figure 10 shows the
viscosity of a typical solution as it is 80
He
a

heated to its gel temperature, then


tin
g

cooled to the original temperature.


As the temperature of the solution 40
is increased, the cellulosic polymers
Incipient Gelation
gradually lose their water of Temperature
hydration, and viscosity decreases.
When the gel point is reached, 0
sufficient dehydration of the 0 10 20 30 40 50 60 70
Temperature, °C
polymer occurs to cause a
polymer-to-polymer association,
and the solution begins to gel.

22
Controlling Gel Temperature METHOCEL used. In applications Figure 11: Gelation Temperature as
where a strong, elastic gel is desired a Function of Concentration
The specific temperature at which
at slight elevations in temperature, 60
bulk thermal gelation occurs (the
METHOCEL A products are 55 METHOCEL E
incipient gelation temperature or

Gelation Temperature,°C
recommended. For softer, non- Slope = -1.0
IGT) and the firmness of the gel are 50
rubbery gels, METHOCEL F or
governed by the nature and quantity
E products should be used. For 45
of the substituent groups attached to
an even softer gel texture, 40
the anhydroglucose ring and, thus, METHOCEL F
METHOCEL K or METHOCEL J Slope = -1.77
vary with each type of cellulose 35
products are suggested. METHOCEL A
ether. The molecular weight of the 30 Slope = -2.33
particular METHOCEL product In general, the strength of the gel
25
selected has little effect on the gel increases sharply as molecular 1 2 3 4 5 6 7 8 9 10 11 12
temperature. However, increasing weight increases and gradually Concentration, Wt. %

the concentration of the solution becomes constant at or above a


lowers the gel temperature as shown viscosity of 400 mPa·s. Gel
in Figure 11. strength also increases with applications where a protective
increasing concentration. colloid, emulsification, or surfactant
Within the range of viscosity
function is desirable. Examples
available in the “A” type, the low-
Effect of Concentration on Thermal include: suspension polymerization
viscosity products will have gel
Gelation of vinyl chloride; aqueous foam
points substantially higher than
stabilization in shampoos, bubble
those of the high-viscosity As the temperature of a solution of baths; and the stabilization of
products. The spread between high METHOCEL cellulose ether is non-dairy whipped toppings and
and low viscosity for the other raised, hazing of the solution occurs salad dressings.
METHOCEL cellulose ether types immediately prior to gelation, and
is relatively narrow. the viscosity may start to rise. At To achieve bulk thermal gelation,
this point, if the concentration is concentrations of 1.5 wt % are
The Effects of Heating Rate and high enough, the solution will generally necessary. However, even
Agitation on Gelation change to a soft or firm gel. If the at concentrations as low as 0.001
concentration is below 0.5%, a fluid wt %, many METHOCEL products
Accurate measurement of gelation exhibit surface thermal gelation
mixture of individual gel particles
temperature requires care because due to the migration of polymer
and water is formed, rather than a
it is a function of the rate of heating molecules to the air/water interface.
firm gel.
and the rate of shear. Both a high Maximum gelation properties are
rate of shear and a fast heating In general, as the concentration achieved with METHOCEL A, E,
rate result in an apparently high of METHOCEL cellulose ether is and F.
gel temperature. increased, the gelation temperature
will be lowered. An increase of 2% The equilibrium concentration of
Agitation also affects the strength of METHOCEL products at any given
in concentration can cause a 10°C
the gel. Continued rapid agitation interface depends upon the nature
drop in the gelation temperature
during gelation may break down of the interface, presence of other
for METHOCEL A cellulose ether
the gel structure and alter both the solvents, temperature, and potential
products. A 2% increase in
texture and strength of the gel. For for formation of associative
concentration of a solution of
maximum development of gel structures with other surfactants.
METHOCEL F cellulose ether
strength, heat the solution well However, the concentration of
product lowers the gelation
above the gelation temperature METHOCEL at an interface can be
temperature by only 4°C.
under quiescent conditions. orders of magnitude greater than
Interfacial Gelation that presumed to be present in the
Gel Strength and Texture bulk phase. As a result, surface film
In addition to bulk-phase gelation, formation (surface gelation) occurs.
The texture and strength of gels
METHOCEL cellulose ethers also
produced by heating solutions of
exhibit interfacial or surface gelation
METHOCEL cellulose ethers varies
phenomena as a result of their
with the product type, viscosity
surfactant nature. Interfacial gelation
grade, and concentration of
plays an important role in many

23
Table 8: Effect of Additives on Gelation Temperature for 2% Solutions of METHOCEL Cellulose Ether This is due to the solubilizing effect
which they impart. Additives such
% METHOCEL METHOCEL METHOCEL METHOCEL as glycerin, sorbitol, and salts lower
Additive Additive A15C, °C F4M, °C K4M, °C J5M, °C
gel points by lowering the solvency of
None 0 50 63 85 62
the aqueous system, resulting in a
NaCl 5 33 41 59 42
MgCl2 5 42 52 67 50
more rapid dehydration of the
FeCl3 3 42 53 76 53 METHOCEL product (Table 8).
Na2SO4 5 salted out salted out salted out salted out If a manufacturer requires a high
Al2(SO4)3 2,5 salted out 45 48 41
thermal gelation temperature and
Na2CO3 5 salted out salted out salted out salted out
plans to use additives known to
Na3PO4 2 32 42 52 43
Sucrosea 5 51 66 84 60
reduce the gel temperature, a
Sucrose 20 44 59 61 53 METHOCEL product with a gel
Sorbitol 20 30 46 48 — point higher than the temperature
Glycerine 20 34 60 65-70 55 required should be used. As the
Ethanola 20 >75 >75 >75 >78 concentration of the gel-causing
Polyethylene additive increases, the thermal gel
Glycol 400a 20 52 >80 >80 >78 temperature decreases. Although the
Propylene behavior of a particular solute must
glycola 20 59 >80 >80 >78
be determined empirically, the
a
Note: This material raises the gelation temperature. following general guidelines apply.
As a specific example, a 0.01 wt % Generally speaking, increasing the
solution of METHOCEL A15 LV molecular weight, concentration,
cellulose ether exhibits surface or temperature of a solution of
gelation at 20°C, whereas bulk METHOCEL will promote the
gelation with the same product onset of surface gelation just as
would require a concentration in bulk thermal gelation.
exceeding 12 wt % at such a low
temperature. A 0.01 wt % solution Effect of Additives on Thermal
of METHOCEL A15 LV cannot be Gelation
made to undergo bulk gelation at
any temperature. Additives may either increase
or decrease thermal-gelation
Surface gelation (filming) occurs temperature, depending on whether
very rapidly in many solutions of the additive exhibits a coagulant
METHOCEL products whether or a solubilizing effect on the
dilute or concentrated. This effect METHOCEL product. For example,
is most evident (and troublesome) solutes such as ethanol, PEG 400,
when one employs du Nouy and propylene glycol all raise the gel
tensiometry to determine points of METHOCEL products.
surface tension.

24
Additives Which Lower Gel Points
Figure 12: Effect of Ethanol on Gel
Most electrolytes, as well as Temperature, 2% Solutions
sucrose, glycerine, etc., lower the 25
gel point because they have a

Change in Thermal Gel Temp.,°C


greater affinity for water and 20
dehydrate the cellulosic polymer.
Decreases in gel temperature are
a function of the ions present in 15
METHOCEL A4M
the additive. (4,000 mPa.s)
10
Additives Which Raise Gel Points
The effect of an additive that raises 5
METHOCEL F4M
gel point varies with different (4,000 mPa.s)
METHOCEL products. For 0
example, the amount of propylene 0 5 10 15 20
glycol required to increase the Ethanol, % by Volume
thermal gel point of a solution of
METHOCEL A cellulose ether by
4˚C will increase the gel point of Figure 13: Effect of Propylene Glycol on Gel
Temperature, 2% Solutions
a solution of METHOCEL F by
10˚C and METHOCEL K 25
by 20˚C.
Change in Thermal Gel Temp.,°C

20
The increase in the thermal gel
point is directly proportional to
the increase in concentration of 15
METHOCEL F4M
(4,000 mPa.s)
the additive. Figures 12 and 13
illustrate the relationship between 10
concentrations of ethanol and METHOCEL A4M
propylene glycol and the thermal (4,000 mPa.s)
gel point of representative 5
METHOCEL products.
0
0 5 10 15 20
Propylene Glycol, % by Volume

25
Properties of Films of METHOCEL Cellulose Ethers
Table 9: Properties of Unplasticized Films of METHOCEL Cellulose Ethers cross-linking compounds and resins.
The degree of insolubility can be
Propertiesa METHOCEL A15 LV METHOCEL E15 LV controlled by the choice and quantity
Specific gravity 1.39 1.29 of a cross-linking reagent. All urea
Area factor 24,000 in2/lb/mil 25,860 in2/lb/mil formaldehyde, melamine
Moisture vapor formaldehyde, and resorcinol
transmission rate, formaldehyde resins can be used.
100°F (38°C), 50% RH 67.5 g/100 in2/24 h/mil 65 g/100 in2/24 h/mil Dialdehydes such as glyoxal are also
Oxygen transmission effective. Supplier literature should
rate, 75°F (24°C) 25 cm3/100 in2/24 h/mil 70 cm3/100 in2/24 h/mil
be consulted for selection of
Tensile strength,
75°F (24°C), 50% RH 9,000 Ib/in2 (62 MPa)±10% 10,000 Ib/in2 (69 MPa)
catalysts and curing compounds.
±10%
Elongation, Resistance of Films to Solvents
75°F (24°C), 50% RH 5-15% 5-15%
Stability to ultraviolet Films and coatings of METHOCEL
light, 500 h, are unaffected by animal and
Fadeometer exposure Excellent Excellent
vegetable oils, greases, and petroleum
Resistance to oils
and most solvents Excellent Excellent hydrocarbons. Of the different
Ultraviolet transmission (2 mil film) types of products, METHOCEL A,
400 nm 55% 82% METHOCEL F, and METHOCEL
290 nm 49% 34% K brand products are most resistant.
210 nm 26% 6%
a
Typical properties, not to be construed as sales specifications. Data based on a 1 mil dry film. Thermoplastic Forming
Procedures for preparing a dry-mix
High-strength, water-soluble films,
formulation of METHOCEL E or
supported or unsupported, may
J cellulose ether products with
be rolled, cast, or extruded from
propylene glycol and other
formulations of METHOCEL
plasticizers are available for extruded
cellulose ether products. These
sheeting and injection or compression
clear, smooth films or coatings
molding. Such mixes may be
are impervious to oils, greases,
compounded in a ribbon-type
and most solvents. They are also
blender at room temperature and
effective binders, even when loaded
satisfactorily handled by a feeder
with inert materials.
designed for powders. Most feeders
Tensile and elongation properties perform better if the dry mix is first
of typical films of METHOCEL densified by being passed through
cellulose ethers cast from water are a set of press rolls or through a
shown in Table 9. The need for a pellet mill.
plasticizer may be more pertinent
Flakes of METHOCEL E or J
when using low viscosity 5 mPa·s
cellulose ether products with
METHOCEL cellulose ethers
propylene glycol and other
because of lower film elongation
plasticizers may be extruded or
properties. This can be more acute if
molded directly into a finished,
drying temperatures are too high.
water-soluble product at
temperatures ranging from 80 to
Effect of Additives on Film 160°C (176 to 320°F). Properly
Solubility plasticized sheet and tubing of
The water solubility of films and METHOCEL cellulose ether can be
coatings of METHOCEL cellulose heat-sealed at about 130°C (266°F).
ethers can be altered by the use of

26
Analytical Methods
Measuring Viscosity Viscosity may also be determined
using a rotational viscometer such
Certain precautions must be
as the Brookfield model LVF†
observed for the accurate
viscometer. When the viscosity of a
measurement of the viscosity of
solution is less than 500 mPa·s, the
solutions of METHOCEL
viscosity is less dependent on shear,
cellulose ethers because they
and the solution may be regarded
exhibit a nonlinear shear
as near-Newtonian. The apparent
stress/shear rate relationship,
viscosity of a solution of higher
which results in pseudoplastic
viscosity will be highly dependent
viscosity behavior at most
on the rate of shear, decreasing as
shear rates.
the rate of shear is increased.
Dow employs the ASTM reference
The rotational instrument should
method (D1347 and D2363) as its
be calibrated against standard oils.
standard procedure. This method
It’s important to note, however,
involves the use of Ubbelohde
that there is no direct correlation
viscometers, one type for low
between Ubbelohde and Brookfield
viscosities and another for high
measurements for non-Newtonian
viscosities. The Ubbelohde
liquids. For details regarding
viscometer is a precision device
analysis methods, please contact
which requires only a small
your local salesperson for
test sample.
METHOCEL cellulose ethers.
For measuring low viscosity, the
appropriate capillary tube size is
Table 10: Capillary Tubes for Measuring
chosen to obtain a flow time of 50 Viscosity
to 150 seconds (see Table 10). The
viscometer is placed in a 20°C Viscosity, Size of Heavy Wall Tubing,
bath, and the length of time mPa.s Inside Diameter
required to deliver a given volume Low viscosity
through the capillary tube is 15 1.5 mm
measured. The time in seconds is 25 1.8 mm
100 2.4 mm
then converted to millipascal-
400 3.2 mm
seconds (mPa·s). Detailed
procedures are given in current High viscosity
ASTM standards D1347 and 1,500 5.0 mm
D2363. The most reproducible 4,000 6.0 mm
viscosities are obtained by cooling 8,000 7.5 mm
15,000 10.0 mm
to 4°C and holding for at least
50,000 15.0 mm
one-half hour before testing
75,000 15.0 mm
at 20°C.

†Brookfield
Synchrolectric viscometer, Brookfield
Engineering Co., Stoughton, MA. 27
Published Analytical Methods Application of Anthrone Test to
Determination of Cellulose
Procedures for the analysis of
Derivatives in Nonaqueous Media
METHOCEL cellulose ether
– Aldrich, J.C., Samsel, E.P., Anal.
products have been standardized
Chem. 29, 574-76 (1957).
under ASTM D1372 and ASTM
D2372. These and other Hydroxypropyl Methylcellulose –
information on analysis are listed The National Formulary, American
in the following references. Pharmaceutical Association,
Washington, D.C., Current
Methods for Testing
Edition.
Methylcellulose – Current ASTM
D1372, American Society for Colorimetric Determination of
Testing and Materials, 1916 Race Methylcellulose with
Street, Philadelphia, PA 19103. Diphenylamine – Danzaki, Grace,
Berger, Eugene Y., Anal. Chem. 31,
Methods for Testing
1383-5 (1959).
Hydroxypropyl Methylcellulose –
Current ASTM D2372, American Colorimetric Method for
Society for Testing and Materials, Determination of Sugars and
1916 Race Street, Philadelphia, PA Related Substances – Dubois, M.,
19103. Gilles, K.A., Hamilton, J.K.,
Repers, P.A., Smith, F., Anal.
Methoxyl and HydroxypropyI
Chem. 28, 350-356 (1956).
Substitution in Cellulose Ether
Products by Gas Chromatography Methylcellulose – U.S.
– Current ASTM D3876, Pharmacopoeia, Bethesda, MD,
American Society for Testing and The United States Pharmacopoeial
Materials, 1916 Race Street, Convention, Inc., Current Edition.
Philadelphia, PA 19103.
Determination of Alkoxyl
Methylcellulose – Food Substitution in Cellulose Ethers by
Chemicals Codex, Washington, Zeisel-Gas Chromatography –
D.C., National Academy of Hodges, K., Kester, W.,
Sciences and National Research Wiederrich, D., Grover, J., Anal.
Council, Current Edition. Chem. 51, 2172-2176 (1979).
Hydroxypropyl Methylcellulose –
Food Chemicals Codex,
Washington, D.C., National
Academy of Sciences and National
Research Council, Current Edition.
The Determination of Particle Size
Distribution of METHOCEL
Cellulose Ethers – Dow Method
No. Mc-l IA (1973).

28
Handling Considerations
Material Safety Data Sheets/Safety means, avoiding any raising of with cold water before disposal.
Data Sheets for METHOCEL dust by strong water jets. Dow Likewise, accumulation of dust
products are available from The recommends the use of water should be avoided to control
Dow Chemical Company to help spray, carbon dioxide, or powder this hazard.
you further satisfy your own handling, extinguishers.
disposal, and safety needs and those Disposal
that may be required by government Storage
regulations. Such information should Despite the very slow rate of
be requested prior to handling or Caution: A fine dust of this material biodegradation, cellulose ether
use. The following comments are is capable of forming an explosive products should not present any
general and are not a substitute for mixture with air. Powder samples hazard in the waste/soil compartment.
the detailed safety information should not be exposed to Their behavior is similar to wheat
found in the Material Safety Data temperatures above 135° to 145°C. flour or sawdust. Although Dow
Sheet/Safety Data Sheet. Samples may decompose and lead to studies using standard procedures
a possible dust explosion. As in showed no 5-day, 10-day, or 20-day
storage of any dusts or fine powders, BOD values, activated sludge studies
Health
good housekeeping is required to with (14C) methylcellulose showed
METHOCEL cellulose ether prevent dusts in air from reaching that methylcellulose was 96%
products resemble the naturally possibly explosive levels. When degraded or otherwise removed
occurring plant and seaweed gums handling in large quantities or in from solution in 20 days. Thus,
in many of their chemical, physical, bulk, the general precautions METHOCEL cellulose ethers should
and functional properties. All of outlined in NFPA 63, “Prevention present no ecological hazard to
these materials possess a basic of Dust Explosions in Industrial aquatic life.
carbohydrate structure. Plants,” and in NFPA bulletins 68,
Because METHOCEL cellulose
69, and 654 are recommended.
METHOCEL products have had ether products and their aqueous
extensive evaluation and testing in With METHOCEL cellulose ether solutions present no significant
both acute and long-term feeding products with particle sizes of 74 ecological problems, they can be
studies in a number of species, µm or less (finer than 200 mesh), disposed of by industrial incineration
including humans. Their many years critical levels are reached at or in an approved landfill, providing
of use in a wide variety of food concentrations of 28 g/m3 (0.03 regulations are observed.
items attests to the safety of oz/ft3). The minimum ignition Incineration should be done under
METHOCEL Premium products. energy required to cause a dust carefully controlled conditions to
explosion is 28mJ. Static from a avoid the possibility of a dust
Although dust from METHOCEL
human body has about 25mJ. This explosion. Customers are advised to
cellulose ether products could
is normally not enough energy to review their local, state, provincial
conceivably cause temporary
ignite the powder. or national regulations governing
mechanical irritation to the skin
the disposal of waste materials to
and eyes under extreme conditions As with any organic chemical
determine appropriate means of
and may be considered a nuisance material, METHOCEL cellulose
disposal in their area.
dust if inhaled, the products are ethers should not be stored next to
considered to present no significant peroxides or other oxidizing agents.
health hazard in handling. Please Customer Notice
review the handling precautions Accidental Spills and Dow encourages its customers to
within the Material Safety Data Housekeeping review their applications of Dow
Sheet/Safety Data Sheet for products from the standpoint of
more information. Solutions of METHOCEL cellulose
human health and environmental
ethers are slippery. To prevent
quality. To help ensure that Dow
Flammability employee falls and injury, floor spills
products are not used in ways for
of dry powder should be thoroughly
which they are not intended or
Cellulose ether products are vacuumed or swept up. Any slight tested, Dow personnel will assist
organic polymers that will burn residual product on the walls or customers in dealing with ecological
when exposed to heat and a floor can then be flushed with water and product safety considerations.
sufficient oxygen supply. Fires can into a sewer. If the spill is a viscous Please contact us at the numbers
be extinguished by conventional solution, it should be further diluted listed on the back cover.

29
For more information, complete literature, and product samples, you can
reach a Dow representative at the following numbers:

From the United States and Canada:


call 1-800-447-4369
fax 1-989-832-1465

In Europe:
toll-free +800 3 694 6367†
call +32 3 450 2240
fax +32 3 450 2815

From Latin America and Other Global Areas:


call 1-989-832-1560
fax 1-989-832-1465

www.methocel.com


Toll free from Austria (00), Belgium (00), Denmark (00), Finland (990),
France (00), Germany (00), Hungary (00), Ireland (00), Italy (00),
The Netherlands (00), Norway (00), Portugal (00), Spain (00), Sweden (00),
Switzerland (00) and the United Kingdom (00).

NOTICE: No freedom from any patent owned by Seller or others is to be inferred. Because use conditions and applicable laws may differ from one
location to another and may change with time, Customer is responsible for determining whether products and the information in this document are
appropriate for Customer’s use and for ensuring that Customer’s workplace and disposal practices are in compliance with applicable laws and other
governmental enactments. Seller assumes no obligation or liability for the information in this document. NO WARRANTIES ARE GIVEN; ALL
IMPLIED WARRANTIES OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY EXCLUDED.

Printed in U.S.A. *Trademark of The Dow Chemical Company Form No. 192-01062-0902 AMS
Published September 2002

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