Research and Development Laboratories

of the
Portland Cement Association

RESEARCH DEPARTMENT
Bulletin 194

Use of Infrared Spectrophotometry

for the Detection and Identification
of Organic Additions in Cement
and Admixtures in Hardened Concrete

By
W. G. Hime, W. F. Mivelaz and J. D. Connolly

Authorized Reprint from the Copyrighted

ANALYTICAL
TECHNIQUES
FORHYDRAULIC
CEMENT
ANDCONCRETE
STP No. 395, 18-29 (1966)
Published by
American Society for Testing and Materials
 USE OF INFRARED SPECTROPHOTOMETRY
FOR THE DETECTION AND IDENTIFICATION
OF ORGANIC ADDITIONS IN CEMENT
AND ADMIXTURES IN HARDENED CONCRETE

By

W. G. Hime, W. F. Mivelaz and J. D. Connolly

PORTLAND CEMENT ASSOCIATION

RESEARCH AND DEVELOPMENT LABORATORIES
5420 Old Orchard Road
Skokie, Illinois 60076
W. G. Hime,l W. F. Mivelaz,’ and J. D. Connolly’

We of Infrared Spectrophotometry for the

Detection and Identification of Organic
Additions in Cement and Admixtures
in Hardened Concrete

KEY WORDS: chemical analysis, concretes, cements, quali-

tative analysis, infrared spectroscopy, cement additions, ad-
mixtures (concrete), organic compounds, extraction, ligno-
sulfonates

ABSTRACT: Procedures of solvent extraction and infrared

analysis for identification of organic additions in cement and
admixtures in hardened concrete were developed. Three ex-
traction procedures — chloroform, acid-chloroform, and
sodium carbonate anion-exchange are detailed in the ap-
pendixes. Using these procedures a number of organic com-
pounds have been identified. The sodium carbonate anion-
exchange procedure is almost entirely restricted to
lignosulfonates. Once a compound is identified, quantitative
analysis by other methods can be performed, if it can be ex-
tracted completely and is the only one present.
REFERENCE: W, G. Hime, W. F. Mivelaz, and J. D. Con-
nolly, ‘TJse of Infrared Spectrophotometry for the Detection
and Identification of Organic Additions in Cement and Ad-
mixtures in Hardened Concrete, ” Analytical Techniques for
Hydraulic Cements and Concrete, ASTM STP 395, Am. Sot.
Testing Mats,, 1965, p. 18.

In recent years, increasing quantities of organic materials have been

sold for use in portland cement and portland-cement concrete. For ex-
ample, lignosulfonates (as the metallic salts of lignosulfonic acid) are
sometimes added as grinding aids during the manufacture of cement,
They are also added to concrete as water-reducing agents, as set-retarding
agents, or both. The use of these organic materials has created a number of
problems for the chemist analyzing cement, who may be called upon to
detect, identify, and determine such materials, Since the number and

1Supervisor, associate research chemist, and laboratory assistant, respectively,

Analytical Chemistry Research Laboratories, Portland Cement Assn., Skokie, Ill,
W. G. Hime is a Personal Member ASTM.
18
 HIME ET AL ON USE OF INFRARED SPECTROPHOTOMETRY 19

variety of marketed organic additions and admixtures is quite large, it

is important to have methods of analysis that are specific and rapid.
No general methods are available for detecting and identifying such
organic compounds in cement or concrete. The number of pubiished
papers in this field [1-6]Z is small, and each is limited to a specific type
of compound. Two procedures deal with extraction methods for fatty
anhydrides [1] and Vinsol resin3 in portland cement. Other organic ma-
terials that may be extracted under the conditions of the test cannot be
differentiated from these materials. For the Vinsol resin determination a
more specific procedure has been developed,4 but this procedure, which
involves a gas evolution step, also has qualitative limitations. For ex-
ample, methyl cellulose would interfere. Bean and Peppier [2] compared
the “evolution” procedure to the “extraction” method.
A Russian paper [3] describes a method for the determination of
plasticizing agents that involves the reaction of an extract of the cement
with a known excess of an oxidizing agent. This method is not specific.
Two papers [4,5] report that lignosulfonates can be determined in
cements and pastes by ultraviolet spectrophotometry. These methods do
not provide positive proof that the determined material is a lignosulfonate,
nor can they be used for the identification or determination of other
additions,
A Japanese paper [6] describes a calorimetric method for sugar in
hydrated cement, It is based upon the color developed by the action of
phenol and concentrated sulfuric acid on any sugar present in an aqueous
extract of the hydrated cement. The method is limited to sugar-like
materials.
A procedure for a specific air-entraining material, Darex AEA, was
part of ASTM specifications from 1946 through 1,955.5 This method
determines nitrogenous material and cannot differentiate between Darex
AEA and other materials that yield ammonia under the test conditions.

Problems Involved in the Detection of Organic Materials in Cement and

Concrete
The lack of a significant number of published analytical methods for
the identification of organic materials in cement and, especially, in con-
crete is doubtless due to the complicated problems involved. Four of
these are discussed:
1. The organic material is present in only small concentrations, generally
from 0.0015 to 0.30 per cent. Thus an analytical specimen of convenient
size, 40 g, may contain less than 0.001 g of the organic component.
z The italic numbers in brackets refer to the list of references appended to the end of
this paper.
3 ASTM Tentative Methods of Chemical Analysis of Portland Cement (C 114 – 61 T).
4ASTM Standard Methods of Chemical Analysis of Portland Cement (C 114 – 63).
c ASTM Methods of Chemical Analysis of Portland Cement (C 114 – 51 T).
20 ANALYTICAL TECHNIQUES FOR HYDRAUUC CEMENTS AND CONCRETE

2. It is almost always necessary to extract the organic component

from the cement or concrete. This extraction is the initial step in most
methods of analysis. In the eme of concrete, the admixture may be so
strongly held by cement gel or other concrete components that extraction
is impossible unless the concrete or paste structure is destroyed. Such a
process may lead to loss or decomposition of the organic material.
3. The organic material may be converted into other substances by
interaction with the concrete components, and identification of these sub-
stances does not necessarily permit us to predict what materials were added
to the cement or concrete. In such cases successful analysis requires that
results be related back to the original compound by “chemical intuition”
or by comparison to previously investigated specimens containing known
amounts of the addition,
4. Some proprietary materials contain two or more constituents, thus
making identification and quantitative determination even more difficult.
In spite of these problems, our studies have indicated that many organic
compounds may be detected and identified in cement or hardened con-
crete by combining certain extraction methods with infrared spectro-
photometry. This paper describes the basis for these procedures and
gives detailed directions for the identification of a number of materials.

Use of Infrared Spectrophotometry

Conventional wet-chemical methods for detecting and identifying

organic materials cannot be easily applied to cement and concrete systems.
Infrared spectrophotometry, however, appears to be a promising means
for rapid and specific identification of small amounts of such organic
materials, and may be defined as the determination of the infrared-ab-
sorption spectrum of a material, Infrared-radiation wavelengths from
2 to 15 P are generally used for analytical purposes. It has been found
that the infrared spectrum of an organic compound is a characteristic
of the particular molecule and is therefore useful for qualitative analysis.
Thus, if a file of known spectra is available, the spectra of unknown
materials can be compared and identified. The infrared spectra of several
water-reducing retarders [7] and silicone admixtures [8], in their com-
mercial form, have been published.
In order to obtain the infrared spectrum of a material present in a
cement or concrete specimen, it is first necessary to concentrate the nlate-
rial by extraction, A spectrum of the extract is then obtained using an
infrared spectrophotometer. This instrument consists of a source of
infrared radiation, a compartment where this radiation is passed through
the specimen, a monochromator to disperse the radiation into its com-
ponent wavelengths, and a detector to measure the infrared radiation
transmitted through the specimen. A recorder is used for readout of the
 HIME ET AL ON USE OF INFRARED SPECTROPHOTOMETRY 21

per cent transmission of incident radiation through the specimen versus

either the wavelength or the frequency of the radiation,
The infrared instrument used in our studies was a Perkin-Elmer Model
421 spectrophotometer. It is a double-beam automatic-recording instru-
ment, employing a grating monochromator.

Extraction
An extract of a cement or concrete specimen containing organic matter
will ideally have an infrared spectrum identical to that of the original
addition or admixture, or to the active component of such material.
Unfortunately, extracted organic substances are not always identical with
the substances originally added. The authors have often found that addi-
tions or admixtures have undergone hydrolysis or salt formation upon

FIG. I—Acid-chloroform extract of cement containing 0.01 per cent calcium stearate
addition (infrared spectrum).

contact with the cement, cement paste, or solvent. Figure 1 illustrates such
a change. The extracted material shown here, stearic acid, was identified by
comparison with known spectra, Calcium stearate was the added com-
ponent.
To date three procedures, described in Appendixes I, II, and III, have
been developed for the extraction of many types of commercial organic
materials likely to be encountered, The first procedure involves simply an
extraction with chloroform and an evaporation to recover the extracted
organic matter. This “chloroform procedure” has proved useful for the
detection of paraffins and waxes, unreacted amines, and certain free organic
acids.
A second procedure, called the “acid-chloroform” method, involves
reaction of the celment or concrete with hydrochloric acid, followed by
extraction of the mixture with chloroform. The chloroform solution is
evaporated to recover extracted materials for infrared analysis. This pro-
cedure permits the identification of many types of organic material.
Neither chloroform procedure extracts small quantities of lignosulfo-
22 ANALYTICAL TECHNIQUES FOR HYDRAULIC CEMENTS AND CONCRETE

nates, For this type of material another procedure was developed. It

utilizes an extraction with sodium carbonate solution, followed by con-
centration and purification of the extracted lignosulfonate. As a result of
a great many experiments an anion-exchange column was found to ac-
complish these latter steps. The lignosulfonate is eluted from the column
in very pure form, suitable, after evaporation, for infrared analysis. Figure
2 illustrates the spectrum of an extracted lignosulfonate and contrasts it to
that of the original material. In general, absorption maxima are in identical
positions in both patterns.
If the extraction process is complete, and only a single extracted sub-

WAVELENGTH (MICRONS)
2,5 3 4 5 6 7 69101215

w
v
z
a
t-
~
z
(n
z
u I
a
+*
w
>
1=
<
-1
k’

FIG. 2—Lignosulfonate spectra.

stance is indicated by infrared analysis, a quantitative analysis is possible.

A separate extraction is made on a portion of the original specimen,
and the weight of the dried extract is determined in order to calculate
the concentration of the organic component.

Applicability of Methods
Detailed procedures are given in Appendixes I, II, and 111for identifica-
tion of many organic additions and admixtures. The substances listed in
Table 1 are examples.
The substances shown in Table 2 are among those that have been identi-
fied in concrete (or in hardened cement paste),
The sodium carbonate anion-exchange method has successfully detected
lignosulfonate in cement and concrete specimens that contained about
 HIME ET AL ON USE OF INFRARED SPECTROPHOTOMETRY 23

0,01 per cent of the lignosulfonate (as the sodium, calcium, or ammonium
salt).

Discussion
A large part of the present work was developed by using field specimens
of concrete. Often the ages and compositions of the specimens were un-

TABLE I—Materials Detected in Portland Cement by Acid-Chloroform

Extraction Method.”

Substance Concentrationin
Cement,per centb

Alkyl aryl polyether alcohols (for example, ethoxylated nonyl-

phenol) .,............,,,.....,,,,.. . . . unknown
Fatty acids and salts of fatty acids (for example, stearic acid
andcalcium stearate) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.001
Rosins and rosin esters (for example, sodium abietate and
gycerol ester ofabietic acid), ,, . . . . . . . . . . . . . . . . . . . . . . . . . 0.01
Saponified tall oils . ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.17

a See Appendixes.
* A concentration, if given, was a known value. It does not necessarily repre-
sent detection limits.

TABLE 2—Materials Identified by Acid- Cldoroform Extraction Method and

by Comparison with Spectra of Pure and Commercial Materials.
Concentrationin
Substance Concrete,percent

A1kyl aryl polyether alcohols (for example, ethoxylated nonyl-

phenol) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . unknown”
Alkyl aryl sulfonates (for example, dodecyl benzene sodium
sulfonate), . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.05
Esters (for example, diglycol stearate and phthalic acid esters). 0.05
Poly(vinyl acetate) and copolymers . unknown”
Rosins and rosin esters (for example, sodium abietate and
glycerol ester ofabietic acid).,,,. ....... .. ............... 0.02
Salts of organic acids (for example, sodium benzoate). . . . . . . 0.05
Sulfonamides (for example, o- and p-toluene ethyl sulfon-
amide) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . unknown”

a Field specimens.

known. Although the compounds listed above were detected in particular

concrete specimens, they would not be detectable in the same specimens
at a later date if they had deteriorated with age or had leached from the
concrete.
Detection limits vary with compound, instrument, specimen, and
technique, Our studies indicate that, using the procedures described in
the Appendixes, materials of resinous or polymeric nature can be detected
in amounts of about 0.01 per cent, while substances of simpler structure
may often be detected at the 0.001 per cent level. The reason for these
24 ANALYTICAL TECHNIQUES FOR HYDRAULIC CEMENTS AND CONCRETE

differences lies partly in the infrared spectra of these types of materials.

The absorption peaks of the simpler substances are sharp and easily
identified (Fig, 2), while the peaks of many resinous materials are broad
(Fig. 3) and more difficult to interpret. Larger specimens and special
infrared equipment and techniques designed for micronized specimens
could increase detection limits 10 or more times.
A systematic study has yet to be made of all components that might
be identified in cement and concrete by the methods described in the
present paper. In addition to the compounds listed above, there are

WAVELENGTH (MICRONS)
2
100

g 80
hi
:60
<
1-
~ 40
=
z 20
a
:0

FIG. 3—Poly(vinyl acetate) (infraredspectrum),

WAVELENGTH (MICRONS)

I
#
w-
Ll
z
a
E
5
z
a
a
1-

FIG. 4—Extraction “blank” (infrared spectrum).

undoubtedly many more compounds that could be identified by the use

of the acid-chloroform extraction method. However, the sodium carbon-
ate anion-exchange method is probably limited to Iignosulfonates and
other large anionics that have a strong affinity for the exchange resin,
For several reasons, test results must be interpreted with caution.
First, as previously stated, the material extracted from the cement or con-
crete may not be the material originally added. Second, it is usually im-
possible to determine an inorganic constituent of the compound or ad-
mixture. For example, it is very difficult or impossible to determine whether
a lignosulfonate was added to the cement or concrete as the sodium,
calcium, or ammonium salt. Third, if a commercial admixture contains
 HIME ET AL ON USE OF INFRARED SPECTROPHOTOMETRY 25

more than one compound, it may be difficult to identify all the com-
ponents.
On two occasions we have. obtained the spectrum of a polyvinyl ace-
tate) (PVA) from the acid-chloroform extract of concretes supposedly
containing commercial lignosulfonate admixtures. Subsequent work has
not indicated the source of the PVA, that is, whether the PVA was used
instead of the lignosulfonate, was a component of the lignosulfonate
admixture, or was created by a chemical breakdown of the Iignosulfonate
molecule. Figure 3 illustrates the spectrum of PVA as extracted from
concrete by acid-chloroform.
Figure 4 is a typical “blank” spectrum resulting from an extraction
of a concrete known to not contain organic substances. Such spectra should
generally be considered as due to the extraction solvent. However, the
“blank” spectrum is similar to the spectrum of a hydrocarbon oil, and
large quantities of residue having such a spectrum may indicate the pres-
ence of an oil. In such cases the experienced analyst will rely upon the
appearance and amount of the extraction residue to aid in interpreting
the data.
When a cement or concrete is analyzed for a particular commercial
addition, it is best to compare the infrared spectrum of the unknown
extracted material with that of a similar extract of a cement or concrete
known to contain the addition. Since the spectrum of a commercial
material is usually a characteristic of its particular composition, identifica-
tion may only require comparisons to “known” spectra, and not a knowl-
edge of the actual composition of the material. Such comparisons assume
that the proprietary material has a constant composition.

Quantitative Analyses

Although the magnitude of absorption by a specimen of infrared ra-

diation at a particular wavelength is proportional to the concentration of
the specimen component absorbing the radiation, quantitative infrared
analyses are extremely difficult. Infrared information may enable quanti-
tative analyses by other methods, however. Thus, if an infrared spectrum
of an acid-chloroform extraction indicates only tallow, a second extrac-
tion can be made, and the weight of the extract used to determine the
tallow concentration. Combination of the ASTM Chloroform-Soluble
Organic Substances Method with infrared spectroscopy may give ac-
curate quantitative and qualitative information.
Quantitative determinations are indicated when a complete extraction
can be made of the substance and infrared analysis indicates onIy one
substance is present in the extract. Quantitative extraction procedures
are being developed by the authors for a number of materials of interest
to the cement industry,
26 ANALYTICAL TECHNIQUES FOR HYDRAULIC CEMENTS AND CONCRETE

Conclusion
Difficulties involved in developing methods for qualitative and quanti-
tative analyses of admixtures in concrete have been discussed above. Many
of these difficulties were noted previously by Mielenz [9]. It is interesting
that he stated, “Considering the various difllculties touched on above,
dependable quantitative methods for detection of organic admixtures in
hardened concrete are not likely to be developed in the near future.”
We feel that infrared spectroscopy offers the best approach to such
analyses. We have presented procedures that enable a number of organic
materials in cement or concrete to be identified. When such procedures
indicate that only one organic compound or admixture is present, quanti-
tative analyses are possible.

APPENDIX I

ChloroformMethod
Procedure
Place 40 g of cement or pulverized concreteG (passing No. 50 sieve) in a 400-
ml beaker, Add 100 ml of reagent-grade chloroform and heat on a steam-bath,
stirring occasionally, to boiling.
Filter through a Buchner funnel fitted with Whatman No. 40 paper or equiv-
alent. Place the filtrate in a 250-ml beaker and evaporate to dryness at a tem-
perature not over 53 C. Reserve the residue for infrared analysis, using the
procedure given for the acid-chloroform extraction method.

APPENDIX II

Acid-Chloroform-ExtractionMethod
Procedure
Use cement samples as received. Crush concrete samples8in a large porcelain
mortar. Remove by hand as much as possible of the aggregate in order to con-
centrate the hydrated-cement-paste fraction of the concrete. Reduce size of the
paste fraction by grinding until it passes through a No. 50 sieve.
Add 40 g of the sample to a 1-liter beaker containing approximately 250 ml of
distilled water, Stir the mixture vigorously to effect complete dispersion of the
sample. Add an additional 250 ml of water and stir again. Without delay, care-
fully and slowly add 185 ml of concentrated hydrochloric acid to the mixture
while stirring, Place the beaker in cold water, and cool to room temperature

0Concrete samples should be selected with care. ASTM Method of Test for Cement
Content of Hardened Portland Cement Concrete (C 85), provides a general sampling
procedure that may be used for this purpose.
 HIME ET AL ON USE OF INFRARED SPECTROPHOTOMETRY 27

with periodic stirring. Quantitatively transfer the contents of the beaker to a

1-liter separator funnel (the stopcock should not be greased). Use a fine stream
of water from a wash bottle and a rubber policeman to aid the transfer. Add 75
ml of reagent-grade chloroform to the separator funnel, stopper, and shake
vigorously for 5 min. During the shaking period occasionally release the pressure
built up by inverting the funnel and opening and closing the stopcock, A11ow
the separator funnel to stand undisturbed until two layers are formed (about
15 rein),
Draw off the lower chloroform layer, including the scum and undissolved
concrete, into a 125-mlseparator funnel. Shake the funnel vigorously to ensure
complete extraction of the scum. Filter the contents of the separator funnel
through a Buchner funnel fitted with Whatman No. 40 paper or equivalent.
Place the filtrate in a clean, dry, 125-ml separator funnel and draw off the
chloroform layer, leaving the small aqueous layer in the funnel. Evaporate the
chloroform to dryness at a low temperature (not over 53 C). Reserve the residue
in the beaker for infrared analysis.
Infrared Analysis
If the residue in the beaker is solid and can be scraped from the bottom of
the beaker with a spatula, grind to a powder in a small mortar. This powder
may be further dried at a low temperature in an oven. Mix all or part of the
residue with infrared-grade potassium bromide so that the mixture obtained
contains about 0.5 to 1 per cent of the residue. Grind this mixture in a small
mortar or, more appropriately, a mechanical mixing device to ensure complete
mixing of the residue and the potassium bromide. Transfer the mixture into an
evacuable potassium bromide pellet die, and evacuate the assembly to an ab-
solute pressure of 1 cm of mercury or less. Retain the vacuum for about 2 min
and then pelletize, while continuing evacuation, by placing the die in a press and
slowly applying a 50,000-psi load. Hold for about 1 rein, then slowly increase
the load to 125,000 psi and maintain for 1 min. Release the pressure, remove the
potassium bromide pellet or disc from the die, and place it in the infrared spec-
trophotometer. Obtain the spectrum of the pellet over the 2.5- to 15-P region.
If the residue from the extraction is not of a quantity necessary to permit the
above preparation, add the potassium bromide directly to the beaker containing
the residue. Add a few milliliters of chloroform and mix well before the chloro-
form evaporates, Allow all the chloroform to evaporate (preferably under
vacuum) and then press into a pellet as described above.
If the residue is an oil, it may be pressed between two rock-salt plates and
analyzed directly.

APPENDIX Ill

Sodium-Carbonate Anion-Exchange Method

The following procedure was developed for Iignosulfonate.
Extraction (Cement)
Shake 50 g of cement and 50 ml of 10 per cent sodium carbonate solution for
2 min in a separator funnel. Filter the slurry through Whatman No, 41 paper
(or equivalent) using a Buchner funnel and suction flask. Discard the filter cake
in the funnel and keep the filtrate.
28 ANALYTICAL TECHNIQUES FOR HYDRAULIC CEMENTS AND CONCRETE

Extraction (Concrete)
Shake 100 g of the concrete” (passing No. 50 sieve) and 100 ml of 10 per cent
sodium carbonate solution for 5 min in a separator funnel. (For cement pastes,
use about one milliliter of the carbonate solution per gram of cement in the
specimen.) Filter the slurry through Whatman No. 41 paper (or equivalent)
using a Buchner funnel and suction flask. Remove the filter cake from the
Buchner funnel and transfer back to the separator funnel. Shake with 50 ml of
10 per cent sodium carbonate solution for 5 rein, and then filter the slurry as
described above. Use a new filter paper if necessary. Again remove the filter
cake from the funnel, extract, and filter, as described above. Combine the fil-
trates from the three extractions.
Neutralize the filtrate from the cement or concrete specimen with concentrated
hydrochloric acid (dispensed from a buret), using litmus or pH paper, Do not
add the test paper to the beaker containing the filtrate, but test the acidity of the
solution by removing a drop of it by means of a glass stirring rod and touching
it to the test paper, Add about 0.5 ml excess of the acid. Allow the solution to
cool to room temperature.

Anion Exchange
Prepare an ion-exchange column containing about 10 ml of anion-exchange
resin (hydrated) of the strongly basic type, in the chloride form. A 50- or 100-ml
buret maybe used for the column. A small piece of glass wool at the bottom of
the buret will hold the resin. The resin should be of analytical grade and should
be washed with acid and base to remove all soluble material. The manufacturer’s
literature generally gives a detailed procedure for purifying the particular resin
used.
Pass the acidified filtrate through the column, Since the affinity of the anion-
exchange resin for the Iignosulfonate is very great, a fairly fast flow-rate from
the column may be used, The filtrate can thus be added in large aliquots, or all
at once if the column is sufficiently large. After all the filtrate has been passed
through the column, introduce hydrochloric acid (about 0.5 M) to the column
until the effluent is free of sulfate (as indicated by a lack of precipitate after the
addition of a barium chloride solution to a portion of the effluent). Then add an
additional 20 ml of the acid. Discard the effluent from the 0,5-J4 acid treatment.
Elute the column with 15 to 20 ml of dilute (1:1) hydrochloric acid (which may
be added to the column all at once). Use a flow-rate such that the acid does not
remain in contact with the resin for more than about 5 min. This rapid flow
reduces to a minimum the amount of resin that might dissolve and produce an
interfering infrared spectrum. Collect the effluent in a small clean beaker, and
evaporate to near-dryness on a steam bath. Remove the last traces of acid by
evaporating at room temperature (preferably under vacuum).

Infrared Analysis
Add several drops of water to the residue in the beaker, then enough potassium
bromide to yield a pellet containing about one per cent residue. Mix the con-
tents of the beaker thoroughly, and dry in an oven at 100 C. Scrape the dried
residue from the bottom of the beaker with a small spatula. Transfer the con-
tents of the beaker (not necessarily quantitatively) to a small mortar or appro-
priate mixing device and mix for a few minutes until the residue is well dispersed
in the potassium bromide. Dry the mixture in an oven at 110 C until all traces
of moisture have been removed. Without delay, press a pellet from the mixture
according to the procedure given previously.
 HIME ET AL ON USE OF INFRARED SPECTROPHOTOMETRY 29

Obtain the infrared spectrum of the pellet between about 2.5 and 15 ~. Identify
the pattern by comparison to the infrared spectrum of a pure lignosulfonate.

References
[1] J. L. Heitzman and G. Coventry, “Determination of Fatty Anhydrides in Cement,”
Rock Products, Vol. 35, June, 1932, p. 36.
[2] L. Bean and R. B. Peppier, “Determination of Vinsol Resin in Portland Cement,”
Rock Products, Vol. 49, July, 1946, pp. 71-73 and 108-110.
[3] N. M. Nashchadimova and I. V. Bogdanova, “Determination of Plasticizing Addi-
tion in Cement and Slurry,” Tsement, Vol. 21, 1955, PP. 25-26,
[4] E. G. Swenson and T. Thorvaldson, “Detection of Lignosulfonate Retarder in
Cement Suspensions and Pastes,” Symposium on Effect of Water-Reducing Ad-
mixtures and Set Retarding Admixtures on Properties of Concrete, ASTM STP 266,
Am. Sot. Testing Mats., 1960, PP. 159-169.
[5] A. S. Wexler and F. D. Brake, “Use of Ultraviolet Spectrophotometry in Determin-
ing Lignosulfonate Additions in Cement,” Materials Research & Standards, Vol. 3,
1963, pp. 364-368.
[6] Ikup Shims and Teiji Nishi, “Determination of Saccharose in Hydrated Cement,”
Semento Gijutsu Nempo, Vol. 17, JuIY, 1964, pp. 106-109.
[7] Woodrow J. Halstead and Bernard Chaiken, “Water-Reducing Retarders for Con-
crete—Chemical and Spectral Analyses,” Public Roads, Vol. 31, No. 6, February,
1961, pp. 126-135.
[8] William E. Grieb, ‘(Silicones as Admixtures for Concrete,” Public Roads, Vol. 32,
No. 9, August, 1963, pp. 214-219.
[9] Richard C. Mielenz, “Diagnosing Concrete Failuresj” Cement, Lime aud Grave/,
Vol. 40. No. 4, April, 1965, pp. 135-142.

PCA.R&D,Ser.1169.2
 Bulletins Published by the
Research Department
Research and Development Laboratories
of the
Portland Cement Association

100. “List of Published Bulletins and Papers of the Research Department,”

May, 1959 (Also lists earlier research papers of the Portland Cement
Association).
101. “Determination of the Apparent Density of Hydraulic Cement in Water
Using a Vacuum Pycnometer,” by C. L. FORD.
Reprinted from ASTM BuUetin, No. 231, 81-84 (July, 1958).

102. “Long-Time Study of Cement Performance in Concrete—Chapter 11.

Report on Condition of Three Test Pavements After 15 Years of Serv-
ice,” by FRANK H. JACKSON.
Reprinted from .Toumalof the American Concrete Institute (June, 1958): Pro-
ceedings, 54, 1017-1032 (1957-1958).

103. “Effect of Mixing and Curing Temperature on Concrete Strength,” by

PAUL KLIEGER.
Reprinted from Journat of the American Concrete Institute (June, 1958); Pro-
ceedings, 54, 1063-1081 (1957-1958).
104. “The Successive Determination of Manganese, Sodium and Potassium
Oxide in Cement by Flame Photometry,” by C. L. FORD.
Reprinted from ASTM BuItetin, No. 233, 57-63 (October, 1958).
105. “The Surface Energy of Tobermorite,” by STEPHEN BRUNAUER, D. L.
KANTRO and C. H. WEISE.
Reprintedfrom Canadian Journal of Chemistrv, 37, 714-724 (April, 1959).
106. “The F1OW of Water in Hardened Portland Cement Paste,” by T. C.
POWERS, H. M. MANN and L. E. COPELAND.
Reprinted from HighWav Resea@z Board Special Report 40, 308-323 (1$358).
107. “The Ball-Mill Hydration of Tricalcium Silicate at Room Temperature,”
by D. L. KANTRO, STEPHEN BRUNAUICti and C. H. WEISE.
Reprinted from Jou?ma~ of CoUaidScience, 14, 383-378 (1959).

108. “Quantitative Determination of the Four Major Phases of Portland

Cement by Combined X-Ray and Chemical Analysis,” by L. E. CoPE-
LAND,STEPHENBRUNAUER,D. L, KANTRO,EDITH G. SCHULZand C. H’. WEISE.
Reprinted from Anatyticat Che?nistw, 31, 1521-1530 (September, 1959).
109. “Function of New PCA Fire Research Laboratory,” by C. C. CARLSON.
Reprinted from the Journat of the PCA Research and Development Labora-
tories, 1, No. 2, 2-13 (May, 1959).

110, “Capillary Continuity or Discontinuity in Cement Pastes,” by T. C.

POWERS, L. E. COPELAND and H. M. MANN.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 1, No. 2, 3848 (May, 1959).

111. “Petrography of Cement and Concrete,” by L. S. BROWN.

Reprinted from the Journal of the PCA Research and Development Labora-
tories, 1, No. 3, 23-34 (S@emb,er, 1959).
112. “The Gravimetric Determination of Strontium Oxide in Portland
Cement,” by C. L, FORD.
Reprinted from ASTM 13tdletin, No. 245, 71-75 (April, 1960).
113. “Quantitative Determination of the Four Major Phases in Portland
Cement by X-Ray Analysis,” by STEPHEN BRUNAUER, L. E, COPELAND,
D. L. KANTRO, C. H. WEISE and EDITH G. SCHULZ.
Reprinted from Proceedings of the American Societv for Testing Materials, 59,
1091-1100 (1959).
114. “Long-Time Study of Cement Performance in Concrete—Chapter 12.
Concrete Exposed to Sea Water and Fresh Water,” by I. L. TYLm.
Reprinted from Joumat of the American Concrete Institute (March, 1960);
Proceedings, 56, 826-836 (1960).
115. “A Gravimetric Method for the Determination of Barium Oxide in Port-
land Cement,” by C. L. FORD.
Reprinted from ASTM 13uUetin, No. 247, 77-60 (July, 1960).
116. “The Thermodynamic Functions for the Solution of Calcium Hydroxide
in Water, ” by S. A. GREENBERG and L. E, COPELAND.
Reprinted from Journal of l%vsical Chemistrv, 64, 1057-1059(August, 19~).
117. “Investigation of Colloidal Hydrated Silicates. I. Volubility Products,”
by S. A. GREENBERG, T. N, CHANG and ELAINE ANDERSON.
Reprinted from Journal of Phwsical Chemistw, 64, 1151-1156 (September, 1960).
118. “Some Aspects of Durability and Volume Change of Concrete for Pre-
stressing,” by PAUL KLIEGER.
Reprinted from the Jorwnat of the PCA Research and Devetoprnent Labora-
tories, 2, No, 3, 2-12 (September, 1960).
119. “Concrete Mix Water—How Impure Can It Be?” by HAROLD H. STEINouR.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 2, No. 3, 32-50 (September, 1960).
120. “Corrosion of Prestressed Wire in Concrete,” by G. E. MONFORE and
G. J. VERBECK.
Reprinted from Jou?wd of the American Concrete Institute (November, 1960):
P~oceedings, 57, 491-515 (1960).
121. “Freezing and Thawing Tests of Lightweight Aggregate Concrete,” by
PAUL KLIEGER and J. A. HANSON.
Reprinted from Jowmat of the American Concrete Institute (January, 1961):
P~oceedings, 57, 779-796 (1961).
122. “A Cement-Aggregate Reaction That OccurS With Certain Sand-Gravel
Aggregates,” by WILLIAM LERCH,
Reprinted from the Journal of the PCA liesea~cit and Development Laborato-
ries, 1, No. 3, 42-50 (September, 1959).
123, “Volume Changes of Concrete Affected by Aggregate Type,” by
HAROLD ROPER,
Reprinted from the Journal of the PCA Research and Development Labora-
to~ies, 2, No, 3, 13-19 (September, 1960).

124. “A Short Method for the Flame Photometric Determination of Magne-

sium, Manganic, Sodium, and Potassium Oxides in Portland Cement, ”
by C, L. FORD,
Reprinted from ASTM BuUetirz, No. 250, 25-29, (December, 1960).

125. “Some Physical Aspects of the Hydration of Portland Cement,” by

T. C. POWERS.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 3, No. 1, 47-56 (January, 1961).
126. “Influence of Physical Characteristics of Aggregates on Frost Re-
sistance of Concrete,” by GEORGE VERBECK ana ROBERT LANDGREN.
Reprintedfrom Proceedings of the American SocietU for Testing Materials, 60,
1063-1079(1960).
127. “Determination of the Free Calcium Hydroxide Contents of Hydrated
Portland Cements and Calcium Silicates,” by E. E. PRESSLER,STEPHEN
BRUNAUER,D. L. KANTRO, and C. H. WEISE.
Reprinted from Analytical Chemist?y, 33, No, 7, 877-682 (June, 1961).
128. “An X-ray Diffraction Investigation of Hydrated Portland Cement
Pastes,” by D. L. KANTRO, L. E. COPELAND, and ELAINE R., ANDERSON.
Reprinted from Proceedings of the American Society for Testing Materials, 60,
1020-1035 (1960).
129. “Dimensional Changes of Hardened Portland Cement Pastes Caused
by Temperature Changes,” by R. A. HELMUTH.
Reprinted from Highwag Research Board Proceedings, 40, 315-336 (1961).
130. “Progress in the Chemistry of Portland Cement, 1887-1960,” by HAROLD H.
STEINOUR,
Reprinted from the Jou?vsa! of the PCA Research and Development Labora-
tories, 3, No. 2, 2-11 (Mey, 1901),
131. “Research on Fire Resistance of Prestressed Concrete,” by HUBERT
WOODS,including discussion by V. PASCHKIS, and author’s closure.
Reprinted from Journal of the Structural Division, Proceedings of the Ameri-
can Society of CWU Engineers, Proc. Paper 2640, 86, ST 11, 53-64 (November,
1960); Discussion, 87, ST 2, 59-60 (February, 1961); Closure, 87, ST 5, 81 (June,
1961).
132. “Centralized Control of Test Furnaces in the PCA Fire Research Labo-
ratory,” by PHIL J. TATMAN.
Reprinted from the Journal of the PCA Research and Deve~op?nent Labo~a-
tories, 3, No. 2, 22-26 (May, 1981).
133. “A Proposed Simple Test Method for Determining the Permeability of
Concrete,” by 1. L. TYLER and BERNARD ERLIN.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 3, No. 3, 2-7 (September, 1901).

134. “The Behavior at High Temperature of Steel Strand for Prestressed

Concrete, ” by M. S. ABRAMS and C. R. CRUZ.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 3, No. 3, 8-19 (September, 1961).
135. “Electron Optical Investigation of the Hydration Products of Calcium
Silicates and Portland Cement,” by L. E. COPELAND and EDITH G. SCHULZ.
Reprinted from the JournaC of the PCA Research and Development Labora-
tories, 4, No, 1, 2-12 (January, 1962).

136. “Soil-Cement Technology—A Resume,” by MILES D. CATTON.

Reprinted from tbe Journal of the PCA Research and Deoetopment Labora-
tories 4, No. 1, 13-21 (.7enuary, 1962).

137. “Surface Temperature Measurements With Felted Asbestos Pads,” by

M. S. A~RAMS.
Reprinted from the Journal of the PCA Resewch and Development Labora-
tories, 4, No. 1, 22-30 (January, 1962).

138. “Tobermorite Gel—The Heart of Concrete,” by STEPHEN BRUNAUER.

Reprinted from the American Scientist, 50, No. 1, 210-229 (March, 1962).

139, “Alkali Reactivity of Carbonate Rocks—Expansion and Dedolomitiza-

tion,” by DAVID W. HADLEY.
Reprinted from Highwav Research Board Proceedings, 40, 462-474 (1981).
140, “Development of Surface in the Hydration of Calcium Silicates,” by
D. L. KANTRO, STEPHEN BRUNAUER, and C. H. WEISE,
Reprfnted from Solid Surfaces and the Gas.SoUd Interface, Advances in
Chemistry Series 33, 199-219 (1961).

141. “Thermodynamic Theory of Adsorption,” by L. E. COPELAND and T. F.

YOUNG.
Reprinted from Solid Surfaces and the Gas-Solid Interface, Advances in
Chemistry Series 33, 34S.356 (1961),
and
“Thermodynamics of Adsorption. Barium Sulphate—Water System,” by
Y. C. Wu and L. E. COPELAND.
Reprinted from Solid Surfaces and the Gas.SoUd Interface, Advances in
Chemistry Series 33, 357-366 (1961).

142. “The New Beam Furnace at PCA and Some Experience Gained from
Its Use,” by C. C. CARLSON and PHIL J. TATMAN,
Reprinted from Symposium on Fire Test Methods. ASTM Special Tecimicut
Publication No. 301, 41-59 (1961) .

143. “New Techniques for Temperature and Humidity Control in X-Ray Dif-
fractometry,” by PAUL SELIGMANN and N. R. GREENING.
Reprinted from the Journal of the PCA Research and Development Labora.
tories, 4, No. 2, 2-9 (May, 1962),

144. “An Optical Method for Determining the Elastic Constants of Concrete,”
by C. R. CRUZ.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 4, No. 2, 24-32 (May, 1962).
145. “Physical Properties of Concrete at Very Low Temperatures,” by G. E.
MONFORE and A. E. LENTZ.
Reprinted from the Journal of the PCA Research and Deoetopment Labora-
tories, 4, No. 2, 33-39 (May, 1962).
146. “A Hypothesis on Carbonation Shrinkage, ” by T. C, POWERS.
Reprinted from the Jou?Wl of the PCA Research and Development Labora-
tories, 4, No. 2, 40-50 (May, 1962).
147. “Fire Resistance of Prestressed Concrete Beams. Study A — Influence
of Thickness of Concrete Covering Over Prestressing Steel Strand, ” by
C, C. CARLSON.
Published by Portland Cement Association, Reeearch and Development Labora-
tories, Skokie, Illinois, (July, 1962).
148. “Prevention of Frost Damage to Green Concrete, ” by T. C. POWERS.
Reprinted from R&snion Mernationale des Labo?wtotres d’Essais et de Fte-
cherches SUT les Matd?’iaum et tes Constructions, RILEM Bulletin 14, 120-124
(March, 1962),
149. “Air Content of Hardened Concrete by a High-Pressure Method,” by
BERNARD ERLIN.
Reprinted from the Journal of the PCA Research and Development Labor&
tories, 4, No. 3, 24-29 (September, 1962),
150. “A Direct Current Strain Bridge, ” and “A Biaxial Strain Apparatus for
Small Cylinders,” by G. E. MONFORE.
Reprinted from the Journal of the P(2A Research and Development Labora-
tories, 4, No. 3, 2-9 (September, 1962).
151. “Development of Surface in the Hydration of Calcium Silicates. II. Ex.
tension of Investigations to Earlier and Later Stages of Hydration,”
by D, L. KANTRO, STEPHEN BRUNAUER, and C. H. WEISE,
~9:~inted from The Journal of Ph@cal, Che?nk?trw, 66, No. 10, 1604-9 (October,
152. “The Hydration of Tricalcium Silicate and &Dilcalcium Silicate at
Room Temperature,” by STEPHEN BRUNAUER and S. A. GREENBERG.
Reprinted from Chemistry of Cement, Proceedings of the Fourth International
Symposium, Washington, D. C., 1960, held at the National Bureau of Standards
(U.S. Department of Commerce), Monograph 43, Vol. I, Session III, Paper
III-1 , 135-165.
153, “Chemistry of Hydration of Portland Cement,” by L. E. COPELAND, D. L.
KANTRO, and GEORGE VERBECK,
Reprinted from Chemistry of Cement, Proceedings of the Fourth International
,$ymposium, Washington, D. C,, 1960, held at the National Bureau of Standards
(U.S. Department of Commerce), Monograph 43, Vol. 1, Session IV, Paper
IV-3, 429-465.
154. “Physical Properties of Cement Paste, ” by T. C. POWERS.
Reprinted from Chemistry of Cement, Proceedings of the Fourth International
Sumposium, Washington, D. C., 1960, held at the National Bureau of Standards
(U.S. Department of Commerce), Monograph 43, Vol. II, Session V, Paper
V-1, 577-609.
i55. “The Rheology of Fresh Portland Cement Pastes, ” by MOSHE ISH-SHALOM
and S. A. GREENBERG.
Reprinted from Chemistry of Cement. Proceedings of the Fourth International
Sumposium, Washington, D. C,, 1960, held at the National Bureau of Standards
(U.S. Department of Commerce), NIonOgraph 43, Vol. II, Session V, PaPer
V-S4, 731-744.
156. “Capillary Size Restrictions on Ice Formation in Hardened Portland
Cement Pastes,” by R. A. HELMUTH.
Reprinted from Chemistry of Cement, Proceedings of the Fourth Internatio?tat
Sumposium, Washington, D. C,, 1960, held at the National Bureau of Standards
(U.S. Department of Commerce), Monograph 43, Vol. II, Session VI, Paper
vI-s2, 855-869.
157. “Extensions to the Long-Time Study of Cement Performance in Con-
crete, ” by PAUL KLIECER.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 5, No. 1, 2-14 (January, 1963).
158. “Durability Studies of Exposed Aggregate Panels, ” by A. W. ISBERNER.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 5, No. 2, 14-22 (May, 1963).
159. “Corrodibility of Prestressing Wire in Concretes Made With Type I and
Type IS Cements,” by BORJE OST and G, E. MONFORE.
Reprinted from the Journal of the PCA Research and Development .Ld)OT@
tories, 5, No, 2, 23-26 (May, 1963).
160. “A Small Probe-Type Gage for Measuring Relative Humidity, ” by G. E.
MONFORE.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 5, No. 2, 41-47 (May, 1963).
161. “Abnormal Cracking in Highway Structures in Georgia and Alabama,”
by CALVXN C. OLESON.
Reprinted from Journal of the American COncTete Instttute (March, 1963):
P~oceedings, 60, 329-353 (1963).
162. “Rheology of Fresh Portland Cement Pastes: Influence of Calcium Sul-
fates,” by S, A. GREENBERG and L. M, MEYER.
Reprinted from ~igh~av Research Record, Number 3, 9-29 (1963).
163. “A Sonic Method to Determine Pavement Thickness,” by RICHARD
MUENOW.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 5, No. 3, 6-21 (September, 1963).
164. “Effect of Restraint on Fire Resistance of Prestressed Concrete, ” by
S. L. SELVAGGIO and C. C. CARLSON,
Reprinted from Symposium on Fire Test Methods, ASTM Special Technical
Publication iVO. 344, 1-25 (1962).
165. “Effect of Surface Grinding and Joint Sawing on the Durability of Pav-
ing Concrete,” by WILLIAM PERENCHIO.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 6, No. 1, 16-19 (January, 1964).
166. “Quantitative Determination of the Major Phases in Portland Cements
by X.Ray Diffraction Me6hods,” by D. L. KANTRO, L. E. COPELAND, C. H.
WEISE, and STEPHEN BRUNAUER.
Reprinted from the Journat of the PCA Research and Development Labora-
tories, 6, No. 1, 20-40 (January, 1964).
167. “Pore Structures and Surface Areas of Hardened Portland Cement
Pastes by Nitrogen Adsorption,” by R. SH. MIKHAIL, L. E, COPELAND,
and STEPHEN BRUNAUER.
~g::~nted from Canadian Journal of Chemistr~, 42, No. 2, 426-438 (February,

168. “Influence of the Cement on the Corrosion Behavior of Steel in Con.

crete, ” by HAROLD H. STEINOUR.
Published by Portland Cement Association, Research and Development Labora-
tories, Skokie, Illinois, May, 1964,
169. “Silicone Influence on Concrete Resistance to Freeze-Thaw and De-
icer Damage, ” by PAUL KLIEG~R and WILLIAM PERENCHIO.
Reprinted from Ifightoa~ Research Reco~d, Number 18, 33-47 (1963).
170. “Properties of Expansive Cement Made With Portland Cement, Gypsum,
and Calcium Aluminate Cement, ” by G. E. MONFORE.
Reprinted from the Joumat of the PCA Research and Development Labo~a-
torir?s, 6, No. 2, 2-9 (May, 1864).
171. “Fire Resistance of Prestressed Concrete Beams. Study B. Influence of
Aggregate and Load Intensity,” by S. L. SELVAGGIO and C. C. CARLSON.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 6, No. 1, 41-64 (January, 1964), and 6, No. 2, 10-25 (May, 1964).
172. “Petrographic Studies on Concrete Containing Shrinking Aggregate,” by
HAROLD ROPER, J. E, Cox and BERNARD ERLIN.
Reprinted from the Journal of the PCA Research and Development Labora-
to~ies, 6, No, 3, 2-18 (September, 1964).
173. “Corrosion of Aluminum Conduit in Concrete,” by G. E. MONFORE and
BORJE OST.
Reprinted from the Journal of the PCA Res earth and Development Labora-
tories, 7, No. 1, 10-22 (January, 1965),
174. “Topics in Concrete Technology — 1. Geometric Properties of Particles
and Aggregates, 2. Analysis of Plastic Concrete Mixtures, 3. Mixtures
Containing Intentionally Entrained Air, and 4. Characteristics of Air-
Void Systems, ” by T. C. POWERS.
Reprinted from the Journal of the PCA Research and Development Labora-
tories, 6, No. 1, 2-15 (January, 1964), 6, No. 2, 48-64 (May, 1964), 6, No. 3, 19-42
(September, 1964), and 7, No. 1, 23-41 (January, 1965).
175, “Twenty-Year Report on the Long-Time Study of Cement Performance
in Concrete, ” by Advisory Committee, Long-Time Study of Cement Per-
formance in Concrete, W. C. HANSEN, Chairman.
Published by Portland Cement Association, Research and Development Labora-
tories, Skokie, Illinois, May, 1965.
176. “Alkali Reactivity of Dolomitic Carbonate Rocks,” by DAVID W. HADLEY.
Reprinted from Highwau Resea~ch Record, Number 45, 1-19 (1964).
177. “Alkali-Reactive Carbonate Rocks in Indiana—A Pilot Regional Investi-
gation, ” by DAVID W. HADLEY.
Reprinted from ~ighwag Research Reco~d, Number 45, 196-221 (1964).
178, “Water-Vapor Adsorption-Desorption Characteristics of Selected Light-
weight Concrete Aggregates,” by ROBERT LANDGREN.
Reprinted from Proceedings of the American Society for Testing and Materials,
64, 830-845 ( 1984).

179. “Determining the Water Absorption of Coarse Lightweight Aggregates

for Concrete,” by ROBERT LANDGREN.
Reprinted from Proceedings of the American Societv for Testing and lllateTials,
64, 646-865(1984).
180. “Investigation of Colloidal Hydrated Calcium Silicates. II. Volubility
Relationships in the Calcium Oxide-Silica-Water System at 25° ,“ by
S. A. GREENBERG and T. N, CHANG,
Reprinted from Journal oj Plwsicat Ci?emistrw, 69, No. 1, 182-188(January, 1965).

181. “Concrete Drying Methods and Their Effect on Fire Resistance,” by

M. S. ABRAMS and D. L. ORALS.
Reprinted from Moisture of Materials in Relation to Fire Tests, ASTM Special
Technicat Publication No. 385, 52-73 (1965).
182. ‘(Thermal Conductivity of Concrete at Very Low Temperatures,” by
A. E. LENTZ and G, E. MONFORE,
Reprinted from the Journal of the PCA Research and Development Labor-
atories, 7, No. 2, 39-46 (May 1965).

183. “An Improved Procedure for Proportioning Mixes of Structural Light-

weight Concrete,” by R. LANDGR~N, J, A. HANSON, and D. W. PFEIFER.
Reprinted from the Journat of the PCA Research and Development Labor-
atories, 7, No. 2, 47-65 (May 1965).
184. “Particle Size Distribution of Portland Cement from Wagner Turbidi-
meter Data,” by W. G. HIME and E. G. LABONDE.
Reprinted from the Jownat of the PCA Research and Development Labor-
atories, 7, No. 2, 66-75 (May 1985).

185. “Studies of Early Hydration Reactions of Portland Cement by X-Ray

Diffraction,” by PAUL SELIGMANN and NATHAN R. GREENING.
Reprinted from Ffighway Research Record, Number 62, 80-105 (1964).
186. “Application of a Small Probe-Type Relative Humidity Gage to Re-
search on Fire Resistance of Concrete,” by M. S. ABRAMS and G. E.
MONFORE,
Reprinted from the JoUT7td of the PCA ReseaTch and Devetop?nent Labora-
tories, 7, No. 3, 2-12 (September 1965).

187. “A Rapid Method for Studying Corrosion Inhibition of Steel in Con-

crete, ” by VENICE K. GOUDA and G. E. MONFORE.
Reprinted from the Journal of the PCA ReSeaTCh and Development Labora-
tories, 7, No. 3, 24-31 (September 1965).

188, “Oxygen Enrichment of Combustion Air in Rotary Kilns,” by ROBERT A.

GAYDOS.
Reprinted from the JouT?2al of the PCA Research and Development LabOTa-
toTies, 7, No. 3, 49-56 (September 1965).

189, “Cement Hydration Reactions at Early Ages,” by GEORGE VERBECK.

Reprinted from the Jou?mal of the PCA Research and Development Labora-
tories, 7, No. 3, 57-63 (September 1965).

190. “Expansive Concrete—Laboratory Tests of Freeze-Thaw and Surface

Scaling Resistance,” by A. H. GUSTAFERRO, N. GREENING, and P. KLIEGER.
Reprinted from the Journat of the PCA Research. and Development Labora-
tories, 8, No. 1, 10.36 (January 1966).
191, “Elastic Properties of Concrete at High Temperatures,” by CARLOSR.
CRUZ.
Reprinted from the .JOUT?2UL of the PCA Research and Development Labora.
tories, 8, No. 1, 37-45 (January 1966).
192, “Penetration of Chloride into Concrete,” by BORJE OST and G. E. MON-
FORE.
Reprinted from the Journat of the PCA Research and Development Labora-
tories, 8, No. 1, 46-52 (January 1966).

193, “Methods Used in Petrographic Studies of Concrete,” by BERNARD ERLIN,.

Reprintedfrom Analytical Techniques for Hydraulic Cement and Concrete,
ASTM Specia~ Technical Publication No. 395, 3-17 (1966).
194. “Use of Infrared Spectrophotometry for the Detection and Identification
of Organic Additions in Cement and Admixtures in Hardened Concrete, ”
by W’. G. HIME, W. F. MIVELAZ, and J. D. CONNOLLY.
Reprinted from Analytical Techniques for Hydraulic Cement and Concrete,
ASTM Special Tecimicat Publication No. 395, 18.29 (1966).

Printed in U.S.A.