Nitrogen, Ammonia

Method 8155 Salicylate Method1

Powder Pillows (0.01 to 0.50 mg/L NH3–N)
Scope and Application: For water, wastewater, and seawater
1 Adapted from Clin. Chim. Acta., 14, 403 (1966)

Test Preparation

Collect the following items: Quantity

Ammonia Cyanurate Reagent pillows 2
Ammonia Salicylate Reagent pillows 2
Sample Cells, 1-inch square, 10-mL 2
Note: Reorder information for consumables and replacement items is on page 5.
Note: A green color will develop if ammonia nitrogen is present.

Powder Pillows Method 8155

IF
LL
IL
EN

1. Select the test. 2. Insert the Multi-cell 3. Prepared Sample: 4. Blank Preparation:
Adapter with the 1-inch Fill a square sample cell to Fill a second square
square cell holder facing the 10-mL mark with sample cell to the 10-mL
the user. sample. mark with deionized water.

(0.01 to 0.50 mg/L NH3–N)

Nitrogen, Ammonia (0.01 to 0.50 mg/L NH3–N)

5. Add the contents of 6. Press TIMER>OK. A 7. When the timer 8. Press TIMER>OK. A
one Ammonia Salicylate three-minute reaction expires, add the contents 15-minute reaction period
Powder Pillow to each cell. period will begin. of one Ammonia Cyanurate will begin.
Reagent Powder Pillow to
Stopper and shake to A green color will develop if
each cell.
dissolve. ammonia-nitrogen
Stopper and shake to is present.
dissolve.

9. When the timer 10. Press ZERO. The 11. Wipe the sample and
expires, insert the blank display will show: insert it into the cell holder
into the cell holder with the 0.00 mg/L NH3–N with the fill line facing the
fill line facing the user. user. Results are in mg/L
NH3–N.

Nitrogen, Ammonia
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 Nitrogen, Ammonia (0.01 to 0.50 mg/L NH3–N)

Interferences
Table 1 Interfering Substances and Levels
Interfering Substance Interference Levels and Treatments
Calcium Greater than 1000 mg/L as CaCO3
All levels. Correct for iron interference as follows:
1. Determine the amount of iron present in the sample by following one of the Iron, Total,
Iron procedures.
2. Add the same iron concentration to the ammonia-free water in step 4. The interference will
be successfully blanked out.
Magnesium Greater than 6000 mg/L as CaCO3
Monochloramine present in chloraminated drinking water interferes directly at all levels, giving
Monochloramine high results. Use Method 10200, Free Ammonia and Monochloramine, to determine free
ammonia in these sample matrices.
Nitrate Greater than 100 mg/L as NO3––N
Nitrite Greater than 12 mg/L as NO2––N
Phosphate Greater than 100 mg/L as PO43––P
Sulfate Greater than 300 mg/L as SO42–
Sulfide will intensify the color. Eliminate sulfide interference as follows:
1. Measure about 350 mL of sample in a 500-mL Erlenmeyer flask1.
Sulfide 2. Add the contents of one Sulfide Inhibitor Reagent1 Powder Pillow. Swirl to mix.
3. Filter the sample through a Folded Filter Paper1 and Filter Funnel1.
4. Use the filtered solution in step 3.
Less common interferences such as hydrazine and glycine will cause intensified colors in the
prepared sample. Turbidity and color will give erroneous high values. Samples with severe
Other Substances
interferences require distillation. Use the distillation procedure with the General Purpose
Distillation Set.

1 See Optional Reagents and Apparatus on page 5.

Sample Collection, Storage, and Preservation

Collect samples in clean plastic or glass bottles. Most reliable results are obtained when
samples are analyzed as soon as possible after collection.

Adjust the pH to 2 or less with concentrated (about 2 mL per liter) Sulfuric Acid. Store samples
at 4 °C or less. Samples preserved in this manner can be stored up to 28 days. Just before
testing the stored sample, warm to room temperature and neutralize with 5.0 N Sodium
Hydroxide Standard Solution. Correct the test result for volume additions.

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

2. Press OPTIONS>MORE. Press STANDARD ADDITIONS. A summary of the standard

additions procedure will appear.

3. Press OK to accept the default values for standard concentration, sample volume, and
spike volumes. Press EDIT to change these values. After values are accepted, the
unspiked sample reading will appear in the top row. See the user manual for more
information.

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Nitrogen, Ammonia (0.01 to 0.50 mg/L NH3–N)

4. Open an Ammonia Nitrogen Standard Solution, 10-mg/L as NH3–N.

5. Prepare three sample spikes. Fill three mixing cylinders with 25 mL of sample.Use the
TenSette® Pipet to add 0.2 mL, 0.4 mL, and 0.6 mL of standard, respectively to the
cylinders and mix each thoroughly.

6. Analyze each sample spike as described in the procedure above, starting with the 0.2 mL
sample spike. Accept each standard additions reading by pressing READ. Each addition
should reflect approximately 100% recovery.

7. After completing the sequence, press GRAPH to view the best-fit line through the standard
additions data points, accounting for matrix interferences. Press IDEAL LINE to view
relationships between the sample spikes and the “Ideal Line” of 100% recovery.

Standard Solution Method

Prepare a 0.40 mg/L ammonia nitrogen standard as follows:

1. Diluting 4.00 mL of the Ammonia Nitrogen Standard Solution, 10-mg/L, to 100 mL with
deionized water. Or, use the TenSette® Pipet to prepare a 0.40 mg/L ammonia nitrogen
standard by diluting 0.8 mL of an Ammonia Nitrogen Voluette® Standard Solution, 50-mg/L
as NH3–N, to 100 mL with deionized water.

2. To adjust the calibration curve using the reading obtained with the standard solution, press
OPTIONS>MORE on the current program menu. Press STANDARD ADJUST.

3. Press ON. Press ADJUST to accept the displayed concentration. If an alternate

concentration is used, press the number in the box to enter the actual concentration, then
press OK. Press ADJUST.

Method Performance
Precision
Standard: 0.40 mg/L NH3–N

Program 95% Confidence Limits of Distribution

385 0.38–0.42 mg/L NH3–N

Sensitivity

Portion of Curve ∆Abs ∆Concentration

Entire range 0.010 0.004 mg/L NH3–N

Summary of Method
Ammonia compounds combine with chlorine to form monochloramine. Monochloramine reacts
with salicylate to form 5-aminosalicylate. The 5-aminosalicylate is oxidized in the presence of a
sodium nitroprusside catalyst to form a blue-colored compound. The blue color is masked by
the yellow color from the excess reagent present to give a final green-colored solution. Test
results are measured at 655 nm.

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 Nitrogen, Ammonia (0.01 to 0.50 mg/L NH3–N)

Consumables and Replacement Items

Required Reagents
Description Quantity/Test Unit Cat. No.
Ammonia Nitrogen Reagent Set for 10-mL samples (100 tests), includes: — — 26680-00
Includes:
(2) Ammonia Cyanurate Reagent Powder Pillows 2 100/pkg 26531-99
(2) Ammonia Salicylate Reagent Powder Pillows 2 100/pkg 26532-99

Required Apparatus
Description Quantity/Test Unit Cat. No.
Sample Cells, 1-inch square, 10-mL, matched pair 2 2/pkg 24954-02

Recommended Standards and Apparatus

Description Unit Cat. No.
Nitrogen, Ammonia Standard Solution, 10-mg/L NH3–N 500 mL 153-49
Nitrogen, Ammonia Standard Solution, 2-mL PourRite® Ampule, 50-mg/L NH3–N 20/pkg 14791-20
Wastewater, Effluent Inorganics, for NH3–N, NO3–N, PO4, COD, SO4, TOC 500 mL 28332-49
Pipet, TenSette® 0.1 - 1.0 mL each 19700-01
Pipet Tips, for TenSette Pipet 19700-01 50/pkg 21856-96
Pipet Tips, for TenSette Pipet 19700-01 1000/pkg 21856-28
Flask, volumetric, Class A, 100 mL each 14574-42
Pipet, volumetric, Class A, 4.00 mL each 14515-04
Pipet Filler, safety bulb each 14651-00
Water, deionized 4L 272-56

Optional Reagents and Apparatus

Description Cat. No.
Cylinder, mixing 20886-40
Distillation Set 22653-00
Erlenmeyer Flask 505-49
Filter Funnel 1083-67
Filter Paper 1894-57
Sodium Hydroxide Standard Solution, 5.0 N 2450-26
Sulfide Inhibitor Reagent Powder Pillow 2418-99
Sulfuric Acid 979-49

Nitrogen, Ammonia
NitrogenAmm_8155_PP_SAL.fm Page 5 of 6
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© Hach Company, 2005. All rights reserved. Printed in Germany. Updated April 05 Edition 1