Iron, TNTplus DOC316.53.

01249

Phenanthroline Method1 Method 10229

0.2 to 6.0 mg/L Fe TNTplus™ 858
Scope and application: For drinking water and wastewater. Digestion can be necessary to determine total iron.
1 Adapted from Standard Methods for the Examination of Water and Wastewater.

Test preparation

Instrument-specific information
Table 1 shows all of the instruments that have the program for this test. The table also
shows the adapter and light shield requirements for the applicable instruments that can
use TNTplus vials.
To use the table, select an instrument, then read across to find the applicable information
for this test.
Table 1 Instrument-specific information for TNTplus vials
Instrument Adapters Light shield
DR 6000, DR 5000 — —
DR 3900 — LZV849
DR 3800, DR 2800 — LZV646
DR 1900 9609900 or 9609800 (A) —

Before starting
DR 3900, DR 3800, DR 2800: Install the light shield in Cell Compartment #2 before this test is started.
Review the safety information and the expiration date on the package.
The recommended sample pH is 3–10.
The recommended temperature for samples and reagents is 15–25 °C (59–77 °F).
The recommended temperature for reagent storage is 2–8 °C (35–46 °F).
To make sure that all forms of the metal are measured, digest the sample with heat and acid. Use the Metals Prep Set
TNTplus 890 to digest the sample.
DR 1900: Go to All Programs>LCK or TNTplus Methods>Options to select the TNTplus number for the test. Other
instruments automatically select the method from the barcode on the vial.
Review the Safety Data Sheets (MSDS/SDS) for the chemicals that are used. Use the recommended personal protective
equipment.
Dispose of reacted solutions according to local, state and federal regulations. Refer to the Safety Data Sheets for disposal
information for unused reagents. Refer to the environmental, health and safety staff for your facility and/or local regulatory
agencies for further disposal information.

Items to collect
Description Quantity

Iron TNTplus Reagent Set 1

Pipet, adjustable volume, 1.0–5.0 mL 1
Pipet tips, for 1.0–5.0 mL pipet 1

Refer to Consumables and replacement items on page 4 for order information.

1
Sample collection and storage
• Collect samples in clean glass or plastic bottles that have been cleaned with 6 N (1:1)
hydrochloric acid and rinsed with deionized water.
• To preserve samples for later analysis, adjust the sample pH to less than 2 with
concentrated nitric acid (approximately 2 mL per liter). No acid addition is necessary if
the sample is tested immediately.
• If only dissolved iron is to be determined, filter the sample before the acid addition.
• Keep the preserved samples at room temperature for a maximum of 6 months.
• Before analysis, adjust the pH to 3–5 with 5 N sodium hydroxide solution.
• Correct the test result for the dilution caused by the volume additions.

Test procedure

1. Use a pipet to add 2.0 2. Tighten the cap on the 3. Start the reaction time of 4. When the timer expires,
mL of sample to the test vial and invert until 15 minutes. clean the vial.
vial. completely mixed.

Start

5. DR 1900 only: Select 6. Insert the vial into the cell

program 858. Refer to holder. DR 1900 only: Push
Before starting on page 1. READ.
Results show in mg/L Fe.

Sample blank
Samples with color or turbidity can cause high test results. Samples without color or
turbidity do not have a sample blank. To adjust for color or turbidity, use the steps that
follow to find the sample blank.

1. Complete the test procedure. Pour the sample into a TNT919 vial. After the
TNT858 results are displayed, place the vial into the cell holder.
2. The instrument automatically calculates the sample blank and displays the corrected
sample concentration by subtracting the sample background color and/or turbidity.
Note: As an alternative, samples with only turbidity can be filtered through a membrane filter,
then analyzed.

2 Iron, Phenanthroline TNTplus Method (6.0 mg/L)

Reagent blank correction
For the best results, measure the reagent blank value for each new lot of reagent.
Replace the sample with deionized water in the test procedure to determine the reagent
blank value. Subtract the reagent blank value from the sample results automatically with
the reagent blank adjust option. Measure the reagent blank value when a new lot of
reagent is used.

1. Use deionized water as the sample in the test procedure to measure the reagent
blank value.
2. Set the reagent blank function to on. The measured reagent blank value is shown.
3. Accept the blank value. The reagent blank value is then subtracted from all results
until the reagent blank function is set to off or a different method is selected.
Note: As an alternative, record or enter the reagent blank value at a different time. Push the
highlighted reagent blank box and use the keypad to enter the value.

Interferences
Ions that do not cause an interference to the maximum tested concentrations are shown
in Table 2. Combinations of ions were not tested.
Table 2 Interfering substances
Interfering substance Interference level
Cd2+ No effect at 70 mg/L.
Ca2+ No effect at 500 mg/L.
CO32– No effect at 50 mg/L.
Cl– No effect at 1000 mg/L.
Cr3+, Cr6+ No effect at 50 mg/L.
Co2+ No effect at 50 mg/L.
Color Can cause high results. To make a correction for the interference, measure a Sample blank.
Cu2+ No effect at 10 mg/L. Higher concentrations cause high results.
Pb2+ No effect at 50 mg/L.
Hg2+ No effect at 50 mg/L.
Ni2+ No effect at 25 mg/L. Higher concentrations cause high results.
NO3 – No effect at 50 mg/L.
Potassium, K+ No effect at 500 mg/L.
Sodium, Na+ No effect at 500 mg/L.

Accuracy check
Standard solution method
Use the standard solution method to validate the test procedure, the reagents and the
instrument.
Items to collect:
• 100-mg/L Iron Standard Solution
• 100-mL volumetric flask, Class A
• Pipet, adjustable volume, 1.0–5.0 mL and pipet tips
• Deionized water

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

a. Use a pipet to add 2.0 mL of a 100-mg/L iron standard solution into the
volumetric flask.

Iron, Phenanthroline TNTplus Method (6.0 mg/L) 3

 b. Dilute to the mark with deionized water. Mix well. Prepare this solution daily.
2. Use the test procedure to measure the concentration of the prepared standard
solution.
3. Compare the expected result to the actual result.
Note: The factory calibration can be adjusted slightly with the standard adjust option so that the
instrument shows the expected value of the standard solution. The adjusted calibration is then
used for all test results. This adjustment can increase the test accuracy when there are small
variations in the reagents or instruments.

Summary of Method
Ferrous iron (Fe2+) forms an orange-red complex with the 1,10-phenanthroline indicator in
the reagent. Any ferric iron (Fe3+) in the water sample is reduced to ferrous iron (Fe2+) by
ascorbic acid before the complex is formed. The measurement wavelength is 515 nm.
Consumables and replacement items
Required reagents

Description Quantity/Test Unit Item no.

Iron TNTplus Reagent Set 1 25/pkg TNT858

Required apparatus

Description Quantity/test Unit Item no.

Pipet, adjustable volume, 1.0–5.0 mL 1 each BBP065

Pipet tips, for 1.0–5.0 mL pipet 1 75/pkg BBP068
Light shield, DR 3800, DR 2800, DR 2700 1 each LZV646
Light shield, DR 3900 1 each LZV849

Recommended standards

Description Unit Item no.

Iron Standard Solution, 100-mg/L Fe 100 mL 1417542

Iron Standard Solution, 1-mg/L Fe 500 mL 13949

Optional reagents and apparatus

Description Unit Item no.

DRB 200 Reactor, 115 VAC option, 9 x 13 mm + 2 x 20 mm, 1 block each DRB20001
DRB 200 Reactor, 230 VAC option, 9 x 13 mm + 2 x 20 mm, 1 block each DRB20005
Flask, volumetric, Class A, 100 mL, glass each 1457442
Metals Prep Set TNTplus 50/pkg TNT890
Nitric Acid, concentrated 500 mL 15249
Sample blank vials for TNTplus methods 5/pkg TNT919
Sampling bottle with cap, low density polyethylene, 500-mL 12/pkg 2087079
Sodium Hydroxide Standard Solution, 5.0 N 100 mL MDB 245032
Water, deionized 4L 27256

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