Nitrite DOC316.53.

01074

USEPA Diazotization Method1 Method 8507

®
0.002 to 0.300 mg/L NO2––N (LR, spectrophotometers) Powder Pillows or AccuVac
0.005 to 0.350 mg/L NO2––N (LR, colorimeters) Ampuls
Scope and application: For water, wastewater and seawater.
1 USEPA approved for wastewater analysis, Federal Register, 44(85), 25505 (May 1, 1979).

Test preparation

Instrument-specific information
The tables in this section show all of the instruments that have the program for this test.
Table 1 shows sample cell and orientation requirements for reagent addition tests, such
as powder pillow or bulk reagent tests. Table 2 shows sample cell and adapter
requirements for AccuVac Ampul tests.
To use either table, select an instrument, then read across to find the corresponding
information for this test.
Table 1 Instrument-specific information for powder pillows
Instrument Sample cell orientation Sample cell
DR 6000 The fill line is to the right. 2495402
DR 3800
DR 2800
DR 2700
DR 5000 The fill line is toward the user.
DR 3900
DR 900 The orientation mark is toward the user. 2401906

Table 2 Instrument-specific information for AccuVac Ampuls

Instrument Adapter Sample cell
DR 6000 — 2427606
DR 5000
DR 900
DR 3900 LZV846 (A)
DR 3800 LZV584 (C) 2122800
DR 2800
DR 2700

1
Before starting
Install the instrument cap on the DR 900 cell holder before ZERO or READ is pushed.
For best results, measure the reagent blank value for each new lot of reagent. Replace the sample with deionized water in
the test procedure to get the reagent blank value. Subtract the reagent blank value from the sample results automatically
with the reagent blank adjust option.
Review the Safety Data Sheets (MSDS/SDS) for the chemicals that are used and use any recommended personal protective
equipment.
Dispose of reacted solutions according to local, state and federal regulations. Use the Safety Data Sheets for disposal
information for unused reagents. Consult the environmental, health and safety staff for your facility and/or local regulatory
agencies for further disposal information.

Items to collect
Powder pillows

Description Quantity
®
NitriVer 3 Reagent Powder Pillows, 10-mL 1
Sample cells. (For information about sample cells, adapters or light shields, refer to Instrument-
2
specific information on page 1.)

Refer to Consumables and replacement items on page 6 for reorder information.

AccuVac Ampuls

Description Quantity
® ®
NitriVer 3 Reagent AccuVac Ampuls 1
Beaker, 50-mL 1
Sample cells (For information about sample cells, adapters or light shields, refer to Instrument-
1
specific information on page 1.)
Stopper for 18-mm tubes and AccuVac Ampuls 1

Refer to Consumables and replacement items on page 6 for reorder information.

Sample collection and storage

• Collect samples in clean glass or plastic bottles.
• To preserve samples for later analysis, keep the samples at or below 6 °C (43 °F) for
up to 48 hours.
• Let the sample temperature increase to room temperature before analysis.

2 Nitrite, Diazotization Method (0.300 mg/L)

Powder pillow procedure

Start

1. Start program 371 N, 2. Prepare the sample: Fill 3. Add the contents of one 4. Swirl to mix.
Nitrite LR PP. For a sample cell with 10 mL of NitriVer 3 Reagent Powder A pink color shows if nitrite
information about sample sample. Pillow. is present in the sample.
cells, adapters or light
shields, refer to Instrument-
specific information
on page 1.
Note: Although the program
name may vary between
instruments, the program
number does not change.

5. Start the instrument 6. Prepare the blank: 7. Clean the blank. 8. Insert the blank into the
timer. A 20-minute reaction When the timer expires, fill a cell holder.
time starts. second sample cell with
10 mL of sample.

Zero Read

9. Push ZERO. The display 10. Clean the prepared 11. Insert the prepared 12. Push READ. Results
shows 0.000 mg/L NO2––N. sample. sample into the cell holder. show in mg/L NO2––N.

Nitrite, Diazotization Method (0.300 mg/L) 3

AccuVac Ampul procedure

Start

1. Start program 375 N, 2. Prepare the sample: 3. Quickly invert the Ampul 4. Start the instrument
Nitrite LR AV. For Collect at least 40 mL of several times to mix. timer. A 20-minute reaction
information about sample sample in a 50-mL beaker. A pink color shows if nitrite time starts.
cells, adapters or light Fill the AccuVac Ampul with is present in the sample.
shields, refer to Instrument- sample. Keep the tip
specific information immersed while the Ampul
on page 1. fills completely.
Note: Although the program
name may vary between
instruments, the program
number does not change.

Zero

5. Prepare the blank: 6. Clean the blank. 7. Insert the blank into the 8. Push ZERO. The display
When the timer expires, fill a cell holder. shows 0.000 mg/L NO2––N.
sample cell with 10 mL of
sample.

Read

9. Clean the AccuVac 10. Insert the prepared 11. Push READ. Results
Ampul. sample AccuVac Ampul into show in mg/L NO2––N.
the cell holder.

Interferences
Interfering substance Interference level
Antimonous ions Interfere by causing precipitation
Auric ions Interfere by causing precipitation

4 Nitrite, Diazotization Method (0.300 mg/L)

Interfering substance Interference level
Bismuth ions Interfere by causing precipitation
Chloroplatinate ions Interfere by causing precipitation
Cupric ions Cause low results
Ferric ions Interfere by causing precipitation
Ferrous ions Cause low results
Lead ions Interfere by causing precipitation
Mercurous ions Interfere by causing precipitation
Metavanadate ions Interfere by causing precipitation
Nitrate Very high levels of nitrate (>100 mg/L nitrate as N) appear to undergo a slight
amount of reduction to nitrite, either spontaneously or during the course of the
test. A small amount of nitrite will be found at these levels.
Silver ions Interfere by causing precipitation
Strong oxidizing and reducing substances Interfere at all levels

Accuracy check
Standard solution method
Use the standard solution method to validate the test procedure, reagents and
instrument.
Items to collect:
• 0.150 mg/L NO2––N standard solution (Nitrite standard solutions are difficult to
prepare. Use the instructions in Standard Methods for the Examination of Water and
Wastewater, Method 4500—NO2-B)

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 slight
variations in the reagents or instruments.

Method performance
The method performance data that follows was derived from laboratory tests that were
measured on a spectrophotometer during ideal test conditions. Users may get different
results under different test conditions.
Program Standard Precision (95% Confidence Interval) Sensitivity
Concentration change per 0.010 Abs change
371 0.150 mg/L NO2––N 0.147–0.153 mg/L NO2––N 0.002 mg/L NO2––N
375 0.150 mg/L NO2––N 0.147–0.153 mg/L NO2––N 0.002 mg/L NO2––N

Summary of method
Nitrite in the sample reacts with sulfanilic acid to form an intermediate diazonium salt.
This couples with chromotropic acid to produce a pink colored complex directly
proportional to the amount of nitrite present. The measurement wavelength is 507 nm for
spectrophotometers or 520 nm for colorimeters.

Nitrite, Diazotization Method (0.300 mg/L) 5

Consumables and replacement items
Required reagents

Description Quantity/test Unit Item no.

®
NitriVer 3 Nitrite Reagent Powder Pillow, 10-mL 1 100/pkg 2107169
OR
® ®
NitriVer 3 Nitrite Reagent AccuVac Ampul 1 25/pkg 2512025

Required apparatus

Description Quantity/test Unit Item no.

Beaker, 50-mL 1 each 50041H

Recommended standards, reagents and apparatus

Description Unit Item no.

Balance, analytical, 80 g x 0.1 mg 100-240 VAC each 2936701

®
AccuVac vials for sample blanks 25/pkg 2677925
®
AccuVac Snapper each 2405200
®
AccuVac Drainer each 4103600
Standard Methods Book, most current edition each 2270800
Sodium Nitrite, ACS 454 g 245201
Water, deionized 4L 27256

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