CT 404jan07 PDF

California Test 404
January 1, 2007
STATE OF CALIFORNIABUSINESS, TRANSPORTATION AND HOUSING AGENCY
DEPARTMENT OF TRANSPORTATION
DIVISION OF ENGINEERING SERVICES
Transportation Laboratory
5900 Folsom Boulevard
Sacramento, California 95819-4612
TEST METHOD FOR THE CHEMICAL ANALYSIS OF PORTLAND CEMENT,

PORTLAND CEMENT CONCRETE, 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 4 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
3. Fusion flux used is a 50 % mixture of

lithium tetraborate and lithium
metaborate.
Lithium
bromide
solution is supplied by the flux device
manufacturer.
This test method is divided into the following

parts:
1. Chemical Analysis of Portland Cement
2. Chemical Analysis of Fly Ash, Pozzolan
and Blended Cement
4. An oscillating hot plate.

5. Simultaneous Carbon and Sulfur
Determinator. Eltra Model CS-800
Induction Furnace has been found
satisfactory.
3. Determination of Chlorides in Hardened

Portland Cement Concrete
4. Safety and Health
6. Muffle
furnace,
maintaining 750C.
PART 1. CHEMICAL ANALYSIS OF

PORTLAND CEMENT
capable
of
7. Various standard cements certified by

the National Institute of Standards
and Technology (NIST).
The procedures used in the chemical analysis

of portland cement are described in this
group of tests. For routine samples, the xray fluorescence method is used. For referee
samples, or samples where there is a
question as to the results, the reference test
methods described in ASTM Designation:
C 114 shall be used.
B. TEST PROCEDURE
1. X-Ray
fluorescence
spectrometer
(XRF) meeting the requirements in
ASTM Designation: D 4326.
Before testing, pass samples through a

U.S. No. 20 sieve in order to mix the
sample, break up lumps and remove
foreign materials.
Discard hardened
lumps that do not break up on sieving or
brushing. Store the cement in airtight
moisture proof containers to prevent
aeration or absorption of moisture prior
to test.
2. Fluxing device with platinum-gold

alloy crucibles as described in ASTM
Designation: D 4326.
1. This portion of the method will

determine the oxides of silica,
aluminum, iron, calcium, magnesium,
A. APPARATUS
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California Test 404

January 1, 2007
b. Weigh 0.50 g of the ashed flyash
sample and 6.5 g of fluxing
material into the crucible. Add
400 L of liquid lithium bromide
to the sample before fusing.
sodium, potassium and sulfur. Test

in
accordance
with
ASTM
Designation: D 4326 except as noted
below.
a. 4Select a series of at least seven
NIST standard cements that will
bracket
the
expected
concentrations of the elements in
the unknown samples. Prepare
standards in the same way as for
samples. It is recommended that
new standard fused disks be made
every 6 months.
2. Determine loss on ignition, available

sodium oxide, available potassium
oxide
and
available
alkali
in
accordance with ASTM Designation:
C 311.
3. Determine sulfur trioxide with the
carbon sulfur determinator. Follow
the manufacturers recommendations
for the testing of cementitious
products.
b. Weigh 1.00 g of cement as

received into the platinum alloy
crucible and 6 g of fluxing
material. Add 3 drops of lithium
bromide solution as recommended
by the manufacturer to prevent
the fused disks from adhering to
the crucibles.
PART 2. DETERMINATION OF CHLORIDES IN

HARDENED CEMENT CONCRETE
This part describes a procedure for determining chlorides in hardened portland
cement concrete. This method includes two
potentiometric titration procedures, one
manual and the other with an automatic
titrator.
c. Fuse the samples following the

manufacturer's recommendations.
Analyze fused disks in the XRF.
2. Determine insoluble residue, carbon
dioxide and loss on ignition in
accordance with ASTM Designation:
C114.
A. APPARATUS
1. Chloride specific ion electrode and a
double junction reference electrode.
3. An alternative test procedure for

sulfur trioxide is to analyze with the
carbon sulfur determinator. Follow
the manufacturers recommendations
for the testing of cement.
2. Standard solutions and reagents:

0.10 N silver nitrate, concentrated
nitric acid, dilute nitric acid (1:99),
0.05 N ammonium thiocyanate. Make
and store solutions in accordance
with ASTM Designation: E 200.
PART 2. CHEMICAL ANALYSIS OF FLY ASH,

POZZOLAN
AND
BLENDED
CEMENT
A.
4. Ferric iron indicator, 5 g of ferric

ammonium sulfate dissolved in 50 mL
of 1 N nitric acid.
TEST PROCEDURE
5. Automatic titrator that will be able to

sense an endpoint with the attached
chloride specific ion electrode and the
reference electrode.
1. Determine the oxides of silica,

aluminum, iron, calcium, magnesium,
total sodium and total potassium in
the same manner as for cement in
Part1 of this test except as indicated
below.
6. 50-mL graduated buret with 0.05 mL

graduations.
a. Heat the sample prior to fusing as

indicated for material previously
ashed in ASTM Designation:
D 4326.
7. An oscillating hot plate.
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California Test 404

January 1, 2007
8. Filtering apparatus consisting of a
Buchner funnel, filter flask and a
vacuum attachment.
13. Titration of Samples:

a. Manual titration using ferric ion
indicator. With concrete that is
low in iron, add a few drops of
ferric iron indicator. Titrate with
0.05 N ammonium thiocyanate
that
has
been
standardized
against the silver nitrate standard
to the first permanent red color.
Use a buret and record all
readings to the nearest 0.01 mL.
B. TEST PROCEDURE
1. Pulverize hardened portland cement
concrete and pass through a U.S.
No. 8 sieve.
2. Weigh 2.0 to 5.0 g of sample, to the
nearest 0.1 g, into a 400-mL breaker.
b. Automatic titration with the

chloride specific ion electrode.
Following
the
manufacturers
instructions, titrate the sample
with
0.05 N
ammonium
thiocyanate
that
has
been
standardized against a silver
nitrate standard solution. Record
the
amount
of
ammonium
thiocyanate needed to titrate the
silver in the sample to the nearest
0.1 mL.
3. Add 100 mL of boiling water and place

on the oscillating hot plate.
4. Add a slight excess of 0.1 N silver
nitrate with a volumetric pipette (5 mL
is an approximate amount of silver
nitrate for concrete that contains no
more than 0.15 % chloride). Record
the amount added.
5. Boil the sample for two minutes,
remove it from the heat and cool
slightly.
14. Calculate chloride by the following

formula:
[( A N ) (B M )] (F )100
Chloride, % =
sample mass, g
6. Slowly add 20 mL of concentrated

nitric acid. Effervescence will often
occur.
7. Heat and break up any lumps of undissolved cement with the flattened
end of a stirring rod, cover the sample
and boil it for 2 min.
Chloride (ppm) = % x 10 000

Where:
8. Filter through a medium speed filter

paper in a Buchner funnel with
suction. The filtrate should be clear.
9. Wash the residue three times with
1:99 nitric acid. Discard the residue
and filter paper.
A
N
B
M
F
=
=
=
=
=
mL of AgNO3
N of AgNO3
mL of NH4SCN
N of NH4SCN
chloride conversion
factor, 0.03546
PART 4. 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.
10. Quantitatively transfer the filtrate to a

400-mL beaker and cool it to room
temperature.
Prior to handling testing or disposing of any

waste materials, testers are required to read
the Caltrans Laboratory Safety Manual.
11. Carry three standards through the

test procedure with the same amount
of acid and silver nitrate but without
cement.
These guidelines pertain to requirements for

general safety principles, standard operating
procedures, protective apparel, disposal of
materials and how to handle spills, accidents,
12. Adjust all standards and samples to

approximately equal volume with deionized water.
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California Test 404

January 1, 2007
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:
ASTM Designations: C 114, C311, D 4326 and
E 200; Caltrans Lab Safety Manual
End of Text
(California Test 404 contains 4 pages)
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California Test 404

STATE OF CALIFORNIABUSINESS, TRANSPORTATION AND HOUSING AGENCY

TEST METHOD FOR THE CHEMICAL ANALYSIS OF PORTLAND CEMENT,

Prior to handling test materials, performing equipment setups, and/or conducting

3. Fusion flux used is a 50 % mixture of

This test method is divided into the following

4. An oscillating hot plate.

3. Determination of Chlorides in Hardened

PART 1. CHEMICAL ANALYSIS OF

7. Various standard cements certified by

The procedures used in the chemical analysis

Before testing, pass samples through a

2. Fluxing device with platinum-gold

1. This portion of the method will

California Test 404

sodium, potassium and sulfur. Test

2. Determine loss on ignition, available

b. Weigh 1.00 g of cement as

PART 2. DETERMINATION OF CHLORIDES IN

c. Fuse the samples following the

3. An alternative test procedure for

2. Standard solutions and reagents:

PART 2. CHEMICAL ANALYSIS OF FLY ASH,

4. Ferric iron indicator, 5 g of ferric

5. Automatic titrator that will be able to

1. Determine the oxides of silica,

6. 50-mL graduated buret with 0.05 mL

a. Heat the sample prior to fusing as

7. An oscillating hot plate.

California Test 404

13. Titration of Samples:

b. Automatic titration with the

3. Add 100 mL of boiling water and place

14. Calculate chloride by the following

6. Slowly add 20 mL of concentrated

Chloride (ppm) = % x 10 000

8. Filter through a medium speed filter

PART 4. SAFETY AND HEALTH

10. Quantitatively transfer the filtrate to a

Prior to handling testing or disposing of any

11. Carry three standards through the

These guidelines pertain to requirements for

12. Adjust all standards and samples to

California Test 404

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