Method 8147

IRON (0 to 1.300 mg/L) For water and seawater

FerroZine Method*

1. Enter the stored 2. Press: 37 ENTER 3. Fill a sample cell 4. Insert the blank into
program number for The display will show with 25-mL of sample the cell holder. Tightly
iron (Fe). mg/L, Fe and the (the blank). cover the sample cell
Press: PRGM ZERO icon. Note: Rinse glassware with with the instrument cap.
Note: Total iron a 1:1 Hydrochloric Acid
The display will show: Solution and deionized
determinations need a
PRGM ? prior digestion; use any of water before use to avoid
Note: Adjust the pH of the three procedures given errors due to iron deposits
stored samples before in Digestion (Section 2). on the glass.
analysis.

5. Press: ZERO 6. Fill another sample 7. Add the contents of 8. Press:

The cursor will move to cell with 25 mL of one FerroZine Iron TIMER ENTER
the right, then the sample. Reagent Solution Pillow
A five-minute reaction
display will show: Note: If the sample to the cell (the prepared
period will begin.
contains rust, see sample). Cap and invert
0.000 mg/L Fe Note: A violet color will
Interferences below. to mix.
develop if iron is present.
Note: Do not allow the
clippers to come into
contact with the contents of
the pillow.
Note: If preferred , use
0.5 mL of FerroZine Iron
Reagent Solution in place
of the solution pillow.

* Adapted from Stookey, L.L., Anal. Chem., 42 (7) 779 (1970)

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IRON, continued

9. Place the prepared 10. Press: READ

sample into the cell The cursor will move to
holder. Tightly cover the the right, then the result
sample cell with the in mg/L iron will be
instrument cap. displayed.
Note: Standard Adjust may
be performed using a
prepared standard (see
Section 1).

Sampling and Storage

Collect samples in acid-washed glass or plastic bottles. To
preserve samples, adjust the sample pH to 2 or less with nitric
acid (about 2 mL per liter). Samples preserved in this manner can
be stored up to six months at room temperature. If only dissolved
iron is to be reported, filter sample immediately after collection
and before the addition of nitric acid.

Before testing, adjust the sample pH to 3–5 with ammonium

hydroxide, ACS. Do not exceed pH 5 as iron may precipitate.
Correct test results for volume additions; see Correction for
Volume Additions in Section 1 for more detailed information.

Accuracy Check
Standard Additions Method
a) Snap the neck off an Iron Voluette Ampule Standard, 25
mg/L Fe.
b) Use the TenSette Pipet to add 0.1 mL of standard to the
prepared sample measured in Step 10.
c) Swirl to mix and allow another five-minute reaction
period, then measure the iron concentration as in Step 10.
d) Add two additional 0.1-mL standard increments, taking a

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IRON, continued
concentration reading after allowing the five-minute
reaction period for each increment.
e) Each 0.1 mL of standard added should cause a 0.1 mg/L
increase in the concentration reading.
f) If these increases do not occur, see Standard Additions in
Section 1 for more information.

Standard Solution Method

Prepare a 0.4 mg/L iron working solution as follows:

a) Pipet 1.00 mL of Iron Standard Solution, 100 mg/L Fe,

into a
250-mL volumetric flask.
b) Dilute to volume with deionized water. This solution
should be prepared daily. Analyze the working solution
according to the above procedure.
Method Performance

Precision
In a single laboratory, using a standard solution of 0.80 mg/L iron
and two representative lots of reagent with the instrument, a
single operator obtained a standard deviation of ±0.004 mg/L
iron.

Estimated Detection Limit

The estimated detection limit for program 37 is 0.011 mg/L Fe.
For more information on the estimated detection limit, see
Section 1.

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IRON, continued
Interferences

Interfering
Interference Levels and Treatments
Substance
Strong chelants, Interfere at all levels. Use the FerroVer or TPTZ methods to
EDTA test these samples. Use the TPTZ method for low iron
concentrations.
Cobalt May give slightly high results
Copper May give slightly high results
Hydroxides Boil the sample, with the FerroZine Iron Reagent from Step 7
added to it for 1 minute in a boiling water bath. Cool to 24 °C
(75 °F) before proceeding with Step 8. Return the sample
volume to 25 mL with deionized water.
OR
Use any of the digestions in Section 2.
Magnetite 1. Fill a 25-mL graduated cylinder with 25 mL of sample.
(black iron oxide) 2. Transfer this sample into a 125-mL erlenmeyer flask.
or Ferrites 3. Add the contents of one FerroZine Iron Reagent Solution
Pillow and swirl to mix.
4. Place the flask on a hot plate or over a flame and bring to
a boil.
5. Continue boiling gently for 20 to 30 minutes.
Note: Do not allow to boil dry.
Note: A purple color will develop if iron is present.
6. Return the boiled sample to the 25-mL graduated cylinder.
Rinse the erlenmeyer flask with small amounts of deionized
water and empty into the graduated cylinder.
7. Return the sample volume to the 25-mL mark with
deionized water.
8. Pour this solution into a sample cell. Swirl to mix.
9. Proceed with Step 9.
OR
Use any of the digestions in Section 2.
Rust Boil the sample, with the FerroZine Iron Reagent from Step 7
for 1 minute in a boiling water bath. Cool to 24 °C (75 °F)
before proceeding with Step 8. Return the volume to 25 mL
with deionized water.
OR
Use any of the digestions in Section 2.

Summary of Method
The FerroZine Iron Reagent forms a purple colored complex with
trace amounts of iron in samples that are buffered to a pH of 3.5.
This method is applicable for determining trace levels of iron in
chemical reagents and glycols and can be used to analyze samples
containing magnetite (black iron oxide) or ferrites after treatment
as described in Interferences.

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IRON, continued
REQUIRED REAGENTS AND APPARATUS
Quantity Required
Description Per Test Unit Cat. No.
FerroZine Iron Reagent Solution Pillows................ 1 pillow..................50/pkg ............2301-66
Clippers, for opening pillows ........................................1 ...........................each ..............968-00
Sample Cell, 10-20-25, w/cap .......................................2 .........................6/pkg ..........24019-06

OPTIONAL REAGENTS
Ammonium Hydroxide, ACS................................................................ 500 mL106-49Drinking
Water Standard, Metals, LR (Cu, Fe, Mn) ............................................ 500 mL ..........28337-49
Hydrochloric Acid Solution, 1:1 (6N)................................................... 500 mL ..............884-49
FerroZine Iron Reagent Solution........................................................... 500 mL ............2301-49
Iron Standard Solution, 100 mg/L Fe.................................................... 100 mL ..........14175-42
Iron Standard Solution, Voluette Ampule, 25 mg/L Fe, 10 mL ..............16/pkg ..........14253-10
Nitric Acid, ACS ................................................................................... 500 mL ..............152-49
Nitric Acid Solution, 1:1 ....................................................................... 500 mL ............2540-49
Water, deionized ........................................................................................... 4 L ..............272-56

OPTIONAL APPARATUS
Ampule Breaker Kit ....................................................................................each ..........21968-00
Clippers, shears, 7¼-inch ............................................................................each ..........20658-00
Cylinder, graduated, 25 mL.........................................................................each ..............508-40
Dropper, calibrated, 0.5-mL & 1.0-mL mark............................................6/pkg ..........23185-06
Flask, erlenmeyer, 125 mL..........................................................................each ..............505-43
Flask, volumetric, 250 mL, Class A............................................................each ..........14574-46
Hot plate, 3 ½" diameter, 120 V..................................................................each ..........12067-01
Hot plate, 3 ½" diameter, 240 V..................................................................each ..........12067-02
pH Indicator Paper, 1 to 11 pH..........................................................5 rolls/pkg ..............391-33
Pipet, serological, 2 mL...............................................................................each ..............532-36
pH Meter, sension™1, portable, with electrode...........................................each ..........51700-10
Pipet, TenSette, 0.1 to 1.0 mL .....................................................................each ..........19700-01
Pipet Tips, for 19700-01 TenSette Pipet .................................................50/pkg . 21856-96Pipet
Tips, for 19700-01 TenSette Pipet ......................................................1000/pkg ..........21856-28
Pipet, volumetric, 1.00 mL, Class A ...........................................................each ..........14515-35
Thermometer, –20 to 110 °C, non-mercury ................................................each ..........26357-02
Water Bath, with sample cell rack...............................................................each ............1955-55

For Technical Assistance, Price and Ordering

In the U.S.A.—Call 800-227-4224
Outside the U.S.A.—Contact the Hach office or distributor serving you.

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