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California Test 404

STATE OF CALIFORNIA—BUSINESS, TRANSPORTATION AND HOUSING AGENCY August 1998

DEPARTMENT OF TRANSPORTATION
ENGINEERING SERVICE CENTER
Transportation Laboratory
5900 Folsom Boulevard
Sacramento, California 95819-4612

METHODS OF TEST FOR THE CHEMICAL


ANALYSIS OF PORTLAND CEMENT,
FLY ASH, POZZOLAN, AND BLENDED CEMENT

CAUTION: Prior to handling test materials, performing equipment setups, and/or conducting this
method, testers are required to read “SAFETY AND HEALTH” in Part 3 of this
method. It is the responsibility of the user of this method to consult and use
departmental safety and health practices and determine the applicability of regulatory
limitations before any testing is performed.

SCOPE
2. Atomic Absorption Spectrophotometer -
This test method is divided into the (AAS) - The Perkin-Elmer AAnalyst 100
following parts: has been found to be satisfactory.

1. Determination of Major Constituents of 3. Carbon and Sulfur Analyzer - The LECO


Portland Cement Corp. Model CS-225 induction furnace
has been found satisfactory.
2. Determination of Chlorides
B. P R O C E D U R E
3. Safety and Health
Before testing, pass samples through a
PART 1. DETERMINATION OF MAJOR 850-µm sieve in order to mix the sample,
CONSTITUENTS OF
break up lumps and remove foreign materials.
PORTLAND CEMENT
Discard foreign materials and hardened
lumps that do not break up on sieving or
The procedures used in the chemical analysis
brushing. Store the cement in airtight
of portland cement are described in this group
moisture proof containers to prevent aeration
of tests. For routine samples, the atomic
or absorption of moisture prior to test.
absorption method is used. For referee
samples, or samples where there is a question
as to the results, the official methods 1. Rapid Chemical Analysis Method:
described in ASTM Designation: C 114 are
used. The determination of oxides of silica,
aluminum, iron, calcium, magnesium,
A. APPARATUS sodium and potassium using an atomic
absorption spectrophotometer and that of
1. Unless otherwise indicated, all reagents sulfur trioxide using the LECO induction
shall conform to the specifications of the furnace are described in the method.
Committee on Analytical Reagents of the
American Chemical Society (where such
specifications are available).

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California Test 404
August, 1998

a. Selection of National Institute of and c are diluted to 1 to 10 with the


Standards and Technology (NIST) final dilution containing 0.5 % of
Standards: lanthanum, which is found to be
effective for the suppression of
Select a series of at least four chemical interferences. Standards
standard cement samples that will are diluted similarly.
bracket the expected concentrations of
the elements in the unknown samples. d. Preparation of Fly Ash, Pozzolan,
and Blended Cement Samples:
b. Preparation of Standards:
Follow the procedures as described in
ASTM Designations: C 311 and C 595,
Weigh 0.250 g of NIST standard
except modify the fusion procedure as
cement into a 100-mL beaker.
follows. A quantity of the ignited
Disperse with 20 mL of distilled
sample, equivalent to 0.250 g of the
water and 4 mL of concentrated
moisture free sample, is mixed with
hydrochloric acid. Break up lumps of
1.5 g of an equal mixture of Li 2B 4O7
cement with a rubber policeman or
glass stirring rod, rinse and remove and LiBO2. The fusion procedure
the policeman or rod from the beaker. is described in ASTM Designation:
Cover the sample with a watch glass E 886. The fused mixture is then
and digest the sample on a low hot dissolved in 80 mL of 1:8 hot
plate for 15 min at approximately hydrochloric acid. The resulting
75˚C. During digestion, continuously solution is filtered and finally
stir the sample. An oscillating hot diluted to 200 mL. NIST standards
plate is preferred for this process. for calibration are prepared in the
Filter through a medium-texture same way.
filter paper into a 200-mL volumetric
flask, scrubbing the beaker with a e. Sulfur Trioxide Determination Using
rubber policeman. Wash the sample an Induction Furnace:
thoroughly with hot hydrochloric Follow the manufacturer's recom-
acid (1:99), then with several rinses mendations. The following has been
of hot distilled water. Cool the found to be a satisfactory method
sample to room temperature, then using a LECO induction furnace.
dilute to a volume of 200 mL. It is
recommended that new standards be Weigh a 0.15 g sample into a
made up each month. combustion crucible. Add one scoop of
Lecocel and one scoop of iron chip
c. Preparation of Samples: accelerator. Follow the instrument
manufacturer’s directions for this
Weigh 0.125 g of cement into a 100-mL analysis. Standardize the instrument
beaker. Disperse it with 10 mL of with NIST cement standards using
distilled water and 2 mL of the same procedure as described
concentrated hydrochloric acid. above.
Digest and prepare the sample
exactly as described in Section b, 2. Reference Analysis
“Preparation of Standards.” The
final filtrate is diluted to a volume of
For silica, ammonium hydroxide group,
100 mL.
aluminum oxide, ferric oxide, calcium
oxide, magnesium oxide, sulfur trioxide,
For the determinations of calcium
ignition loss, insoluble residue, sodium
oxide and magnesium oxide, a portion
oxide and potassium oxide, follow
of the solutions prepared in Sections b
ASTM Designation: C 114.

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California Test 404
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9. Quantitatively transfer the filtrate to a


PART 2. DETERMINATION OF CHLORIDES 400-mL beaker and cool it to room
temperature.
This part describes a procedure for deter-
mining chlorides in portland cement and 10. Carry three standards through the test
portland cement concrete. procedures with the same amount of acid
and silver nitrate but without cement.
A. APPARATUS
11. Adjust all standards and samples to
1. Chloride specific ion electrode approximately equal volume with
distilled water to eliminate blank
2. Double junction reference electrode determination.

3. Millivoltmeter compatible with the 12. Titration of Samples:


electrodes
a. Titration using a ferric ion indicator.
B. P R O C E D U R E With cements that are low in iron,
add a few drops of ferric iron
1. Weigh 2.0 to 5.0 g of portland cement into indicator (5 g of ferric ammon-
a 400-mL breaker. ium sulfate dissolved in 50 mL
of 1 Normal nitric acid). Titrate
with 0.05 Normal ammonium
2. Add 100 mL of boiling water.
thiocyanate that has been stand-
ardized against the silver nitrate
3. Add a slight excess of 0.1 Normal silver standards to the first permanent red
nitrate from a buret (5 mL is an color. Use burets with 0.05-mL
approximate amount of silver nitrate for graduations and make all readings
cement that contains no more than 0.15 % carefully to the nearest 0.01 mL.
chloride). Record the amount added.
b. Titration with a specific ion
4. Boil the sample for two minutes, remove electrode. Following the manu-
it from the heat, then cool it slightly. facturer's recommendation for the use
of specific ion electrode, titrate the
5. Slowly add 20 mL of concentrated nitric samples with the 0.05 Normal
acid, efflorescence will often occur. ammonium thiocyanate that has been
standardized against the silver
6. Heat and break up any lumps of nitrate standards prepared in
undissolved cement with the flattened Step 10. Plot a curve of the change in
end of a stirring rod, cover the sample and potential against volume of
boil it for 2 min. thiocyanate to find the end point.

7. Filter through a medium speed (90-mm 13. Calculate chlorides by the following
“OK” is satisfactory) paper in a Buchner formula:
funnel with suction. The filtrate should
be clear. Add approximately 1 g of
% chlorides = [(A x N) - (B x M)] x F x
diatomaceous earth to aid filtering if
100/mass of the sample, to the
desired.
nearest 1g
8. Wash the residue three times with 1:99
nitric acid. Discard the residue. Chlorine (ppm) = % x 10 000

Where A = mL of AgNO3
N = Normality of the AgNO3

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California Test 404
August, 1998

B = mL of NH4 SCN
M = Normality of the NH4 SCN
F = conversion factor to Cl,
or 0.03546

PART 3. SAFETY AND HEALTH

This method may involve hazardous


materials, operations and equipment. This
method does not purport to address all the
safety problems associated with its use. It is
the responsibility of the user of this method
to consult and establish appropriate safety
and health practices and determine the
applicability of regulatory limitations prior
to use. This method involves the handling of
hazardous chemicals and samples,
compressed and flammable gases, and
sophisticated instruments which can be
dangerous.

Prior to handling testing or disposing of any


waste materials, testers are required to read
the Caltrans Laboratory Safety Manual

These guidelines pertain to requirements for


general safety principles, standard operating
procedures, protective apparel, disposal of
materials and how to handle spills,
accidents, emergencies, etc. Testers are
mandated to always observe good hygiene
practices. Wash hands after handling
samples and before eating, drinking or
smoking. Users of this method do so at their
own risk.

REFERENCES:
Caltrans Lab Safety Manual
ASTM Designation: C 114
AASHTO Designation: T 105
Portland Cement Association, Research
Department Bulletin 214, “Analysis of Portland
Cement by Atomic Absorption.”

End of Test (California Test 404 contains 4 pages)

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