Iron Total FerroVer, 8008

Iron, Total DOC316.53.01053

USEPA1 FerroVer® Method2 Method 8008

0.02 to 3.00 mg/L Powder Pillows or AccuVac ® Ampuls
Scope and Application: For water, wastewater and seawater; digestion is required for determining total iron
1 USEPA approved for reporting wastewater analysis, Federal Register, June 27, 1980; 45 (126:43459)
2 Adapted from Standard Methods for the Examination of Water and Wastewater.

Test preparation

How to use instrument-specific information

The Instrument-specific information table displays requirements that may vary between
instruments. To use this table, select an instrument then read across to find the corresponding
information required to perform this test.

Table 198 Instrument-specific information

Powder pillows AccuVac Ampuls

Instrument
Sample cell Cell orientation Sample cell Adapter

DR 6000 2495402 Fill line faces right 2427606 —

DR 5000 2495402 Fill line faces user 2427606 —

DR 3900 2495402 Fill line faces user 2427606 LZV846 (A)

DR 3800, DR 2800, DR 2700 2495402 Fill line faces right 2122800 LZV584 (C)

Before starting the test:

Digestion is required for determining total iron for EPA reporting purposes. Use the mild or vigorous digestion. Refer to the
Water Analysis Guide for more information.

For more accurate results, determine a reagent blank value for each new lot of reagent. Follow the procedure using
deionized water in place of the sample. Subtract the reagent blank value from the final results or perform a reagent blank
adjust. See the user manual for more information.

Adjust pH of stored samples before analysis.

For turbid samples, treat the blank with one 0.1-g scoop of RoVer Rust Remover. Swirl to mix.

Collect the following items:

Description Quantity

Powder Pillow Test:

FerroVer® Iron Reagent Powder Pillow 1

Sample Cells (see Instrument-specific information) 2

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Collect the following items: (continued)

Description Quantity

AccuVac® Ampul test:

FerroVer® Iron Reagent AccuVac® Ampul 1

Beaker, 50-mL 1

Sample Cells (see Instrument-specific information) 1

Stopper of 18 mm tubes 1

See Consumables and replacement items for reorder information.

FerroVer method for powder pillows

Stored Programs

265 Iron, FerroVer

Start

1. Select the test. 2. Prepared sample: Fill 3. Add the contents of 4. Start the instrument
Insert an adapter if a clean sample cell with one FerroVer Iron Reagent timer.
required (see Instrument- 10 mL of sample Powder Pillow to the A three-minute reaction
specific information). sample cell. Swirl to mix. period will begin. An
Refer to the user manual Accuracy is not affected by orange color will form, if
for orientation. undissolved powder. iron is present.
(Allow samples that
contain rust to react for at
least 5 minutes.)

Zero

5. Blank preparation: 6. When the timer 7. ZERO the instrument. 8. Insert the prepared
Fill a second sample cell expires, insert the blank The display will show: sample into the cell holder.
with 10 mL of sample. into the cell holder. READ the results in
0.00 mg/L Fe
mg/L Fe.

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FerroVer method for AccuVac® Ampuls

Stored Programs

267 Iron, FerroVer AV

Start

1. Select the test. 2. Blank Preparation: 3. Prepared Sample: 4. Quickly invert the
Insert an adapter if Fill a round sample cell Collect at least 40 mL of Ampul several times
required (see Instrument- with 10 mL of sample. sample in a 50-mL beaker. to mix.
specific information). Fill a FerroVer Iron Accuracy is not affected by
AccuVac® Ampul with undissolved powder.
Refer to the user manual sample from the beaker.
for orientation. Keep the tip immersed
while the Ampul fills
completely.

Zero

5. Start the instrument 6. Wipe the blank and 7. ZERO the instrument. 8. Wipe the Ampul and
timer. insert it into the cell holder. The display will show: insert it into the cell holder.
A three-minute reaction 0.00 mg/L Fe READ the results in
period will begin. An mg/L Fe.
orange color will develop if
iron is present.

Interferences

Table 199 Interfering substances

Interfering substance Interference level

Calcium, Ca2+ No effect at less than 10,000 mg/L as CaCO3.

Chloride, Cl– No effect at less than 185,000 mg/L.

Copper, Cu2+ No effect. Masking agent is contained in FerroVer Reagent.
High Iron Levels Inhibit color development. Dilute sample and re-test to verify results.
Requires mild, vigorous or Digesdahl digestion. After digestion, adjust sample to pH 3–5 with
Iron Oxide
sodium hydroxide, then analyze.
Magnesium No effect at 100,000 mg/L as calcium carbonate.

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Table 199 Interfering substances (continued)

Interfering substance Interference level
Molybdate Molybdenum No effect at 50 mg/L as Mo.
1. Treat in fume hood or well-ventilated area. Add 5 mL hydrochloric acid1, ACS to 100 mL
sample in a 250 mL Erlenmeyer flask. Boil 20 minutes.
2. Cool. Adjust pH to 3–5 with Sodium Hydroxide1. Readjust volume to 100 mL with
High Sulfide Levels, S2–
deionized water.
3. Analyze using FerroVer method for powder pillows or FerroVer method for AccuVac®
Ampuls.
1. Add 0.1 g scoop of RoVer® Rust Remover to the blank. Swirl to mix.
2. Zero the instrument with this blank.
3. If sample remains turbid, add three 0.2 g scoops of RoVer to a 75 mL sample.
Turbidity
Let stand 5 minutes.
4. Filter through a Glass Membrane Filter and Filter Holder1.
5. Use the filtered sample as the prepared sample and the blank.
Extreme Sample pH Adjust pH to 3–5.
Highly Buffered Samples Adjust pH to 3–5.
1 See Optional reagents and apparatus.

Sample collection, preservation and storage

• Collect samples in acid-cleaned glass or plastic containers. No acid addition is necessary if
analyzing the sample immediately.
• To preserve samples, adjust the pH to 2 or less with concentrated nitric acid (about 2 mL per
liter). Preserved samples may be stored up to six months at room temperature.
• Before analysis, adjust the pH to between 3 and 5 with 5.0 N Sodium Hydroxide Standard
Solution.
• Correct the test result for volume additions.
• If only dissolved iron is to be determined, filter the sample before acid addition.

Accuracy check
Standard additions method (sample spike)
Required for accuracy check:
• Iron Voluette® Ampule Standard, 25 mg/L
• Ampule breaker
• TenSette Pipet and Pipet Tips

1. After reading test results, leave the sample cell (unspiked sample) in the instrument.

2. Select Options>More>Standard Additions from the instrument menu.

3. Accept the default values for standard concentration, sample volume and spike volumes. After
the values are accepted, the unspiked sample reading will appear in the top row. See the user
manual for more information.

4. Open the standard solution ampule.

5. Prepare a 0.1 mL sample spike by adding 0.1 mL of standard to 10 mL of unspiked sample.

Start the instrument timer. After the timer expires, read the result.

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6. Prepare a 0.2 mL sample spike by adding 0.1 mL of standard to the 0.1 mL sample spike. Start
the instrument timer. After the timer expires, read the result.

7. Prepare a 0.3 mL sample spike by adding 0.1 mL of standard to the 0.2 mL sample spike. Start
the instrument timer. After the timer expires, read the result.

8. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard
addition results to the theoretical 100% recovery.

Standard additions method for AccuVac Ampuls (sample spike)

1. Fill three mixing cylinders each with 50 mL of sample and spike with 0.2 mL, 0.4 mL and
0.6 mL of standard. Stopper and invert to mix.

2. Transfer 40 mL from each of the three mixing cylinders to three 50 mL beakers.

3. Analyze each standard addition sample as described in the FerroVer method for AccuVac®
Ampuls.

4. Accept each standard additions reading. Each addition should reflect approximately 100%
recovery.

Standard solution method

Note: Refer to the instrument user manual for specific software navigation instructions.

Required for accuracy check:

• Iron Standard Solution, 100 mg/L
• 100-mL volumetric flask
• Class A volumetric pipet, 2 mL
• Deionized water
• Pipet filler

1. Prepare a 2.00-mg/L Fe standard solution as follows:

a. Pipet 2.00 mL of Iron Standard Solution, 100 mg/L, into a 100 mL volumetric flask.
b. Dilute to the mark with deionized water. Mix well. Prepare this solution daily.

2. Use the 2.00 mg/L Fe standard solution in place of the sample. Follow the FerroVer method for
powder pillows test procedure.

3. To adjust the calibration curve using the reading obtained with the Standard Solution, select
Options>More>Standard Adjust from the instrument menu.

4. Turn on the Standard Adjust feature and accept the displayed concentration. If an alternate
concentration is used, enter the concentration and adjust the curve to that value. Mixed-
parameter standards are also available to simulate various matrices.

Method performance

Precision Sensitivity
Program Standard 95% Confidence Limits of Concentration change
Distribution per 0.010 Abs change
265 2.00 mg/L Fe 1.99–2.01 mg/L Fe 0.021 mg/L Fe
267 2.00 mg/L Fe 1.98–2.02 mg/L Fe 0.023 mg/L Fe

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Summary of method
FerroVer Iron Reagent converts all soluble iron and most insoluble forms of iron in the sample to
soluble ferrous iron. The ferrous iron reacts with the 1-10 phenanthroline indicator in the reagent to
form an orange color in proportion to the iron concentration. Test results are measured at 510 nm.

Consumables and replacement items

Required reagents
Description Quantity/Test Unit Catalog number

FerroVer® Iron Reagent Powder Pillows (for 10-mL sample) 1 100/pkg 2105769
OR
FerroVer® Iron Reagent AccuVac® Ampuls 1 25/pkg 2507025

Required apparatus
Description Quantity Unit Catalog number
Beaker, 50 mL 1 each 50041H
Sample cell, 10 mL round, 25 x 54 mm 1 each 2122800
Sample cell, 10 mL round, 25 x 60 mm 1 6/pkg 2427606
Sample cell, 10 mL square, matched pair 2 2/pkg 2495402
Stopper for 18 mm tube 1 6/pkg 173106

Recommended standards
Description Unit Catalog number
Iron Standard Solution, 100 mg/L 100 mL 1417542
Iron Standard Solution, 10 mL Voluette® Ampule, 25 mg/L as Fe 16/pkg 1425310
Metals Drinking Water Standard, LR for Cu, Fe, Mn 500 mL 2833749
Metals Drinking Water Standard, HR for Cu, Fe, Mn 500 mL 2833649
Water, deionized 4L 27256
Pipet, TenSette, 0.1–1.0 mL each 1970001
Pipet Tips, for TenSette Pipet 1970001 50/pkg 2185696
Pipet Tips, for TenSette Pipet 1970001 1000/pkg 2185628
Flask, volumetric, Class A, 100 mL each 1457442
Pipet, volumetric, Class A, 2.00 mL each 1451536
Pipet Filler, safety bulb each 1465100

Optional reagents and apparatus

Description Unit Catalog number
Beaker, 50 mL each 50041H
Cylinder, mixing, 50 mL each 189641
Hydrochloric Acid, concentrated 500 mL 13449
Nitric Acid, concentrated 500 mL 15249

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Optional reagents and apparatus (continued)

Description Unit Catalog number
Sodium Hydroxide Standard Solution, 5.0 N 100 mL 245032
Glass Membrane Filter, 47 mm 100/pkg 253000
Glass Membrane Filter Holder each 234000
RoVer Rust Remover 454 g 30001
Spoon, measuring, 0.1 g each 51100

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© Hach Company, 2007, 2010, 2012. All rights reserved. Printed in the U.S.A. Edition 7
 Iron Total, 8112

Iron, Total DOC316.53.01051

TPTZ Method1 Method 8112

0.012 to 1.800 mg/L Powder Pillows or AccuVac ® Ampuls
Scope and Application: For water, wastewater and seawater
1 Adapted from G. Frederic Smith Chemical Co., The Iron Reagents, 3rd ed. (1980)

Test preparation

How to use instrument-specific information

The Instrument-specific information table displays requirements that may vary between
instruments. To use this table, select an instrument then read across to find the corresponding
information required to perform this test.

Table 200 Instrument-specific information

Powder pillows AccuVac Ampuls
Instrument
Sample cell Cell orientation Sample cell Adapter

DR 6000 2495402 Fill line faces right 2427606 —

DR 5000 2495402 Fill line faces user 2427606 —

DR 3900 2495402 Fill line faces user 2427606 LZV846 (A)

DR 3800, DR 2800, DR 2700 2495402 Fill line faces right 2122800 LZV584 (C)

Before starting the test:

Digestion is required for determining total iron.

For more accurate results, determine a reagent blank value for each new lot of reagent. Follow the procedure using
deionized water instead of the sample. Subtract the reagent blank value from the final results or perform a reagent blank
adjust.

Rinse all glassware with a 1:1 Hydrochloric Acid Solution1. Rinse again with deionized water. This process will remove iron
deposits that can cause slightly high results.

After adding reagent, a blue color will develop if iron is present.

Adjust the pH of stored samples to 3–4. Do not exceed pH 5 or iron may precipitate.
1 See Optional reagents and apparatus.

Collect the following items:

Description Quantity

Powder Pillow Test:

TPTZ Iron Reagent Powder Pillow 2

Sample Cells (see Instrument-specific information) 2

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Collect the following items:

Description Quantity

AccuVac Test:

TPTZ Low Range Iron Reagent AccuVac® 1

Beaker, 50 mL 1

Stopper for 18 mm tube 1

Sample Cell (see Instrument-specific information) 1

See Consumables and replacement items for reorder information.

TPTZ method for powder pillows

Stored Programs

270 Iron, TPTZ

Start

1. Select the test. 2. Prepared Sample: Fill 3. Start the instrument 4. Blank Preparation:
Insert an adapter if one clean sample cell with timer. Fill a second sample cell
required (see Instrument- 10 mL of sample. A three-minute reaction with 10 mL of deionized
specific information). Add the contents of one period will begin. water.

Refer to the user manual 10-mL TPTZ Iron Reagent Proceed with step 4 and 5
for orientation. Powder Pillow to the while the timer is running.
prepared sample. Swirl at
least 30 seconds to
dissolve.

Zero

5. Add the contents of 6. When the timer 7. ZERO the instrument. 8. Insert the prepared
one 10-mL TPTZ Iron expires, insert the blank The display will show: sample into the cell holder.
Reagent Powder Pillow to into the cell holder. READ the results in
the blank. Swirl at least 30 0.000 mg/L Fe
mg/L Fe.
seconds to dissolve. This
will be the reagent blank.

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TPTZ method for AccuVac® Ampuls

Stored Programs

272 Iron, TPTZ AV

Start

1. Select the test. 2. Blank Preparation: 3. Prepared Sample: 4. Quickly invert the
Insert an adapter if Fill a sample cell with Collect at least 40 mL of Ampul several times
required (see Instrument- 10 mL of sample. sample in a 50-mL beaker. to mix.
specific information). Fill a TPTZ Iron AccuVac
Ampul with sample. Keep
Refer to the user manual the tip immersed while the
for orientation. Ampul fills completely.

Zero

5. Start the instrument 6. Wipe the blank and 7. ZERO the instrument. 8. Wipe the Ampul and
timer. insert it into the cell holder. The display will show: insert it into the cell holder.
A three-minute reaction 0.000 mg/L Fe READ the results in
period will begin. mg/L Fe

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Interferences
Interferences are tested (see the Interfering substances table) with an iron concentration of
0.5 mg/L. The following do not interfere with the method when present up to the levels given.

Table 201 Interfering substances

Interfering substance Interference level
Cadmium 4.0 mg/L
Chromium 3+ 0.25 mg/L
Chromium 6+ 1.2 mg/L
Cobalt 0.05 mg/L
Copper 0.6 mg/L
Cyanide 2.8 mg/L
Manganese 50.0 mg/L
Mercury 0.4 mg/L
Molybdenum 4.0 mg/L
Nickel 1.0 mg/L
Nitrite Ion 0.8 mg/L
In the powder pillow procedure, if the sample, without a TPTZ Iron Reagent Powder Pillow,
Color or turbidity has a color or turbidity greater than the blank (deionized water plus TPTZ Iron Reagent),
then use the sample as the blank.
A sample pH of less than 3 or greater than 4 after the addition of reagent may inhibit color
formation, cause the developed color to fade quickly or to result in turbidity. Adjust the
sample pH in the sample cell before the addition of reagent:
1. Measure the current pH by using a pH meter or pH paper.
pH 2. Adjust the sample pH to between 3 and 4 by adding an appropriate amount of iron-free
acid or base such as 1.0 N Sulfuric Acid Standard Solution1 or 1.0 N Sodium Hydroxide
Standard Solution1.
3. Make a volume correction if significant volumes of acid or base are used. Refer to the
Water Analysis Guide for more information.
1 See Optional reagents and apparatus.

Sample collection, preservation and storage

• Collect samples in acid-washed glass or plastic bottles.
• To preserve samples, adjust the sample pH to 2 or less with about 2 mL/L Nitric Acid, ACS *.
• Store preserved samples up to six months at room temperature.
• If reporting only dissolved iron, filter sample immediately after collection and before adding
nitric acid.
• Before testing, adjust the pH of the stored sample to between 3–4 with 5.0 N Sodium
Hydroxide Standard Solution*. Do not exceed pH 5 as iron may precipitate.
• Correct the test result for volume additions.

* See Optional reagents and apparatus.

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Accuracy check
Standard additions method for powder pillows (sample spike)
Required for accuracy check:
• Iron Standard Solution, 10 mg/L Fe
• Beakers, 50 mL (3)
• Graduated mixing cylinders, 50 mL (3)
• TenSette Pipet

1. After reading test results, leave the sample cell (unspiked sample) in the instrument.

2. Select Options>More>Standard Additions from the instrument menu.

3. Accept the default values for standard concentration, sample volume and spike volumes. After
the values are accepted, the unspiked sample reading will appear in the top row. See the user
manual for more information.

4. Open a fresh bottle of standard solution.

5. Use the TenSette Pipet to prepare spiked samples: add 0.1 mL, 0.2 mL and 0.3 mL of
standard to three 10-mL portions of fresh sample.

6. Follow the TPTZ method for powder pillows test procedure for each of the spiked samples
using the powder pillows or AccuVac ampules, starting with the 0.1 mL sample spike. Measure
each of the spiked samples in the instrument.

7. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard
addition results to the theoretical 100% recovery.

Standard additions method for AccuVac Ampuls (sample spike)

1. Fill three mixing cylinders each with 50 mL of sample and spike with 0.5 mL, 1.0 mL and 1.5
mL of standard. Stopper and invert to mix.

2. Transfer 40 mL from each of the three mixing cylinders to three 50 mL beakers.

3. Analyze each standard addition sample as described in the TPTZ method for AccuVac®
Ampuls.

4. Accept each standard additions reading. Each addition should reflect approximately
100% recovery.

Standard solution method

Note: Refer to the instrument user manual for specific software navigation instructions.

Required for accuracy check:

• Iron Standard Solution, 1 mg/L or
• Iron Standard Solution, 100 mg/L
• 5 mL Class A volumetric pipet and pipet filler
• 500 mL Class A volumetric flask
• Deionized water

1. Use a 1 mg/L Iron Standard Solution or prepare a 1.00 mg/L iron standard solution as follows:

a. Pipet 5.00 mL of Iron Standard Solution, 100 mg/L, into a 500 mL volumetric flask.
b. Dilute to the mark with deionized water. Mix well. Prepare this solution daily.

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2. Use the 1.00 mg/L iron standard solution in place of the sample. Follow the TPTZ method for
powder pillows or Accuvac Ampuls.

3. To adjust the calibration curve using the reading obtained with the 1.00 mg/L Standard
Solution, select Options>More>Standard Adjust from the instrument menu.

4. Turn on the Standard Adjust feature and accept the displayed concentration. If an alternate
concentration is used, enter the concentration and adjust the curve to that value. Mixed-
parameter standards are also available to simulate various matrices.

Method performance

Precision Sensitivity
Program Standard 95% Confidence Limits of Concentration change
Distribution per 0.010 Abs change
270 1.000 mg/L Fe 0.989–1.011 mg/L Fe 0.011 mg/L Fe
272 1.000 mg/L Fe 0.984–1.016 mg/L Fe 0.012 mg/L Fe

Summary of method
The TPTZ Iron Reagent forms a deep blue-purple color with ferrous iron (Fe2+). The indicator is
combined with a reducing agent that converts precipitated or suspended iron, such as rust, to the
ferrous state. The amount of ferric iron (Fe3+) present can be determined as the difference
between the results of a ferrous iron test and the concentration of total iron. Test results are
measured at 590 nm.

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Consumables and replacement items

Required reagents
Description Quantity/Test Unit Catalog number
TPTZ Iron Reagent Powder Pillows (for 10-mL sample) 1 100/pkg 2608799
OR
TPTZ Low Range Iron Reagent AccuVac® Ampuls 1 25/pkg 2510025

Required apparatus
Description Quantity Unit Catalog number
Beaker, 50 mL 1 each 50041H
Sample cell, 10 mL round, 25 x 54 mm 1 each 2122800
Sample cell, 10 mL round, 25 x 60 mm 1 6/pkg 2427606
Sample cell, 10 mL square, matched pair 2 2/pkg 2495402

Recommended standards
Description Unit Catalog number
Iron Standard Solution, 100 mg/L Fe 100 mL 1417542
Iron Standard Solution, 10 mg/L Fe 500 mL 14049
Iron Standard Solution, 1 mg/L Fe 500 mL 13949
Metals Drinking Water Standard, LR for Cu, Fe, Mn 500 mL 2833749
Metals Drinking Water Standard, HR for Cu, Fe, Mn 500 mL 2833649
Water, deionized 4L 27256

Optional reagents and apparatus

Catalog
Description Unit
number
Cylinder, mixing, 50 mL each 189641
Nitric Acid, ACS concentrated 500 mL 15249
Sodium Hydroxide, 5.0 N 50 mL SCDB 245026
Sodium Hydroxide Standard Solution, 1.0 N 100 mL SCDB 127032
Sulfuric Acid, 1.0 N 100 mL MDB 104532
Stopper for 18 mm tube 6/pkg 173106
Tensette Pipet, 0.1–1.0 mL each 1970001
Tips for Tensette Pipet 50/pkg 2185696
Flask, volumetric, 500 mL each 1457449
Pipet, volumetric, 5 mL Class A each 1451537
Pipet Filler, Safety bulb each 1465100

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