Nitrogen, Total DOC316.53.

01087

Persulfate Digestion Method Method 10208

1 to 16 mg/L N (LR) TNTplus™ 826
Scope and application: For 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 3–12.
The sample temperature must be 15–25 °C (59–77 °F) for accurate results.
The recommended temperature for reagent storage is 15–25 °C (59–77 °F).
Important: Make sure to close each reagent bottle immediately after each use.
The 20-mm reaction tube can be used for 7 tests. After each use, clean the tube thoroughly with a brush and water, then
rinse well with high-quality distilled water and let dry.
Use only high-quality deionized water or organic-free water for standards preparation, sample dilutions or reagent blanks.
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

Nitrogen, Total, LR TNTplus Reagent Set 1

DRB200 reactor with 20-mm wells 1
Pipet, adjustable volume, 1.0–5.0 mL 1

1
Items to collect (continued)
Description Quantity

Pipet, adjustable volume, 0.2–1.0 mL 1

Pipet tips 1
Test tube rack 1

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

Sample collection and storage

• Collect samples in clean glass or plastic bottles.
• Analyze the samples as soon as possible for best results.
• To preserve samples for later analysis, adjust the sample pH to less than 2 with
concentrated sulfuric acid (approximately 2 mL per liter). No acid addition is
necessary if the sample is tested immediately.
• Keep the preserved samples at or below 6 °C (43 °F) for a maximum of 28 days.
• Let the sample temperature increase to room temperature before analysis.
• Before analysis, adjust the pH to 7 with 5 N sodium hydroxide solution.
• Correct the test result for the dilution caused by the volume additions.

Test procedure

1. Set the DRB200 reactor 2. Add 1.3 mL of sample, 3. Insert the reaction tube in 4. Keep the reaction tubes
power to on. Set the 1.3 mL of Solution A and 1 the preheated DRB200 in the reactor for
temperature to 120 °C. Reagent B tablet in quick reactor. Close the lid. 30 minutes.
succession to a dry 20‑mm
reaction tube.
Close the reaction tube
immediately. Do not invert.

2 Nitrogen, Total, Persulfate Digestion TNTplus Method (16 mg/L)

5. When the timer expires, 6. Invert the reaction tube 7. Use a pipet to add 0.5 8. Use a pipet to add 0.2
carefully remove the 2–3 times. mL of the digested sample mL of Solution D to the test
reaction tube from the from the 20‑mm reaction vial.
reactor. Let the temperature tube into a test vial.
of the reaction tube
decrease to room
temperature.

Start

9. Quickly tighten the cap 10. Start the reaction time 11. When the timer expires, 12. DR 1900 only: Select
on the vial and invert until of 15 minutes. clean the vial. program 826. Refer to
completely mixed. Before starting on page 1.

13. Insert the vial into the

cell holder. DR 1900 only:
Push READ.
Results show in mg/L N.

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.

Nitrogen, Total, Persulfate Digestion TNTplus Method (16 mg/L) 3

 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
A light pink color may develop during the reaction. This color does not interfere with the
analysis. Table 2 shows that the ions were individually examined to the given
concentrations and do not cause interference. No cumulative effects or influences of
other ions were found.
Table 2 Interfering substances
Interfering substance Interference level
COD 400 mg/L
Chloride 800 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:
• Nitrogen, Ammonia Standard Solution, 10-mg/L NH3–N

1. Use the test procedure to measure the concentration of the standard solution.
2. 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
Inorganic and organic nitrogen compounds are digested with peroxodisulfate and are
oxidized to nitrate. The nitrate ions react with 2,6-dimethylphenol in a solution of sulfuric
and phosphoric acid to form a nitrophenol. The measurement wavelength is 345 nm.
Consumables and replacement items
Required reagents

Description Quantity/Test Unit Item no.

Nitrogen, Total, LR TNTplus Reagent Set 1 25/pkg TNT826

Required apparatus

Description Quantity/test Unit Item no.

DRB 200 Reactor, 115 VAC option, 9 x 13 mm + 2 x 20 mm, 1 block 1 each DRB200-01
DRB 200 Reactor, 230 VAC option, 9 x 13 mm + 2 x 20 mm, 1 block 1 each DRB200-05
Pipet, adjustable volume, 1.0–5.0 mL 1 each BBP065
Pipet tips, for 1.0–5.0 mL pipet 1 75/pkg BBP068
Pipet, adjustable volume, 0.2–1.0 mL 1 each BBP078
Pipet tips, for 0.2–1.0 mL pipet 2 100/pkg BBP079
Test tube rack for 20-mm vials, 20 holes 1 each 2497912

4 Nitrogen, Total, Persulfate Digestion TNTplus Method (16 mg/L)

Required apparatus (continued)
Description Quantity/test Unit Item no.

Test tube rack for 20-mm vials, 40 holes 1 each 2497902

Light shield, DR 3800, DR 2800, DR 2700 1 each LZV646
Light shield, DR 3900 1 each LZV849

Recommended standards

Description Unit Item no.

Nitrogen Ammonia Standard Solution, 10-mg/L NH3–N 500 mL 15349

Optional reagents and apparatus

Description Unit Item no.

Brush, test tube each 69000

Sampling bottle with cap, low density polyethylene, 500-mL 12/pkg 2087079
Sodium Hydroxide Standard Solution, 5.0 N 100 mL MDB 245032
Sulfuric Acid, concentrated, ACS 500 mL 97949
Water, deionized 4L 27256
Water, organic-free 500 mL 2641549

Nitrogen, Total, Persulfate Digestion TNTplus Method (16 mg/L) 5

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