Nitrogen, Ammonia, 8038

Nitrogen, Ammonia
USEPA1 Nessler Method2 0.02 to 2.50 mg/L NH3N

DOC316.53.01078 Method 8038

Scope and Application: For water, wastewater and seawater; distillation is required for wastewater and seawater; USEPA accepted for wastewater analysis (distillation required); see Distillation in this procedure.
1 2

USEPA accepted for wastewater analysis (distillation required) Adapted from Standard Methods for the Examination of Water and Wastewater 4500-NH3 B & C.

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 256 Instrument-specific information

Instrument DR 6000 DR 5000 DR 3900 DR 3800, DR 2800, DR 2700 Sample cell 2495402 2495402 2495402 2495402 Cell orientation Fill line faces right Fill line faces user Fill line faces user Fill line faces right

Before starting the test:

Nessler Reagent contains mercuric iodide. Both the sample and the blank will contain mercury (D009) at a concentration regulated as a hazardous waste. Do not pour these solutions down the drain. Refer to a current MSDS for safe disposal and handling instructions. When dispensing reagent from a dropper bottle, hold the bottle vertically. Do not hold the bottle at an angle. If the Flow Cell is used, periodically clean the cells by pouring a few sodium thiosulfate pentahydrate crystals in to the cell funnel. Flush with enough deionized water to dissolve. Rinse the cell thoroughly.

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Collect the following items:
Description Ammonia Nitrogen Reagent set Deionized Water Graduated Mixing Cylinders Sample Cells, 1-inch, 10-mL Serological Pipet, 1-mL See Consumables and replacement items for reorder information. Quantity 1 25 mL 2 2 1

Nessler method

Stored Programs 380 N, Ammonia, Ness Start

1. Select the test. Insert an adapter if required (see Instrumentspecific information). Refer to the user manual for orientation.

2. Prepared Sample: Fill a 25-mL mixing graduated cylinder to the 25-mL mark with sample.

3. Blank Preparation: Fill a 25-mL mixing graduated cylinder to the 25-mL mark with deionized water.

4. Add three drops of Mineral Stabilizer to each cylinder. Stopper and invert several times to mix.

5. Add three drops of Polyvinyl Alcohol Dispersing Agent to each cylinder. Stopper and invert several times to mix.

6. Pipet 1.0 mL of Nessler Reagent into each cylinder. Stopper and invert several times to mix.

7. Start the instrument timer. A one-minute reaction period will begin.

8. Pour 10 mL of each solution into a sample cell.

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Nitrogen, Ammonia Nessler method (continued)

Zero

Read

9. When the timer expires, insert the blank into the cell holder.

10. ZERO the instrument. The display will show: 0.00 mg/L NH3 N

11. Wipe the prepared sample and insert it into the cell holder.

12. READ the results in mg/L NH3 N.

Interferences
Table 257 Interfering substances
Interfering substance Chlorine Interference level Remove residual chlorine from a 250 mL sample by adding 1 drop of sodium thiosulfate for each mg/L chlorine (Cl2). Sodium arsenite can be used instead of sodium thiosulfate. See Sample collection, preservation and storage. A solution containing a mixture of 500 mg/L CaCO3 and 500 mg/L Mg as CaCO3 does not interfere. If the hardness concentration exceeds these concentrations, add extra Mineral Stabilizer. Interferes at all levels by causing turbidity with Nessler Reagent. May be analyzed by adding of 1.0 mL (27 drops) of Mineral Stabilizer to the sample before analysis. This complexes the high magnesium concentrations found in sea water, but the sensitivity of the test is reduced by 30 percent due to the high chloride concentration. For best results, perform a calibration, using standards spiked to the equivalent chloride concentration or distill the sample as described below. Interferes at all levels by causing turbidity with Nessler Reagent. May cause greenish or other off colors or turbidity. Distill the sample if these compounds are present.

Hardness Iron

Seawater

Sulfide Glycine, various aliphatic and aromatic amines, organic chloramines, acetone, aldehydes and alcohols

Sample collection, preservation and storage

Collect samples in clean glass or plastic bottles. If chlorine is present, add one drop of 0.1 N Sodium Thiosulfate* for each 0.3 mg/L Cl2 in a 1-liter sample. Preserve the sample by reducing the pH to 2 or less with sulfuric acid (at least 2 mL/L). Store at 4 C (39 F) or less. Preserved samples may be stored up to 28 days. Warm samples to room temperature and neutralize with 5 N Sodium Hydroxide* before analysis.

* See Optional reagents and apparatus.

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Correct the test result for volume additions.

Accuracy check
Standard additions method (sample spike) Required for accuracy check: Nitrogen Ammonia Voluette Ampule Standard, 50-mg/L NH3N Ampule breaker TenSette Pipet and Pipet Tips 25-mL Mixing cylinders (3)

1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Select standard additions from the instrument menu: OPTIONS>MORE>STANDARD ADDITIONS. 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. Use the TenSette Pipet to prepare spiked samples: add 0.1 mL, 0.2 mL and 0.3 mL of standard to three 25-mL portions of fresh sample in three mixing cylinders. 6. Follow the Nessler method test procedure for each of the spiked samples, 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 solution method
Note: Refer to the instrument user manual for specific software navigation instructions.

Required for accuracy check: Nitrogen Ammonia Standard solution 1-mg/L NH3N

1. Use a 1-mg/L Nitrogen Ammonia Standard solution in place of the sample. Follow the Nessler method test procedure. 2. To adjust the calibration curve using the reading obtained with the standard solution, navigate to Standard Adjust in the software: OPTIONS>MORE>STANDARD ADJUST. 3. 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.

Distillation
1. Measure 250 mL of sample into a 250-mL graduated cylinder and pour into a 400-mL beaker. Destroy chlorine, if necessary, by adding 1 drop of Sodium thiosulfate Solution 0.1 N per mg/L Cl2. 2. Add 25 mL of Borate Buffer Solution and mix. Adjust the pH to about 9.5 with 1 N sodium hydroxide solution. Use a pH meter. 3. Set up the General Purpose Distillation Apparatus as shown in the Distillation Apparatus Manual. Pour the solution into the distillation flask. Add a stir bar.

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4. Use a graduated cylinder to measure 25 mL of deionized water into a 250-mL Erlenmeyer flask. Add the contents of one Boric Acid Powder Pillow. Mix thoroughly. Set the flask under the distillation apparatus drip tube. Elevate the flask so the end of the tube is immersed in the solution. 5. Turn on the heater power switch. Set the stir control to 5 and the heat control to 10. Turn on the water and adjust to maintain a constant flow through the condenser. 6. Turn off the heater after collecting 150 mL of distillate. Immediately remove the collection flask to avoid sucking solution into the still. Measure the distillate to ensure 150 mL was collected (total volume = 175 mL). 7. Adjust the pH of the distillate to about 7 with 1 N sodium hydroxide. Use a pH meter. 8. Pour the distillate into a 250-mL volumetric flask; rinse the Erlenmeyer with deionized water. Add the rinsings to the volumetric flask. Dilute to the mark. Stopper. Mix thoroughly. Analyze as described above.

Method performance
Precision 95% Confidence Limits of Distribution 0.991.01 mg/L NH3 N Sensitivity Concentration change per 0.010 Abs change 0.02 mg/L NH3 N2

Program 380

Instrument DR 5000

Standard 1.00 mg/L NH3N

Summary of method
The Mineral Stabilizer complexes hardness in the sample. The Polyvinyl Alcohol Dispersing Agent aids the color formation in the reaction of Nessler Reagent with ammonia and certain other amines. A yellow color is formed proportional to the ammonia concentration. Test results are measured at 425 nm.

Consumables and replacement items

Required reagents
Description Ammonia Nitrogen Reagent Set, includes: Nessler Reagent Mineral Stabilizer Polyvinyl Alcohol Dispersing Agent Water, deionized Quantity/Test 2 mL 6 drops 6 drops 25 mL Unit 500 mL 50 mL SCDB 50 mL SCDB 4L Catalog number 2458200 2119449 2376626 2376526 27256

Required apparatus
Description Cylinder, graduated, mixing, 25-mL Pipet, serological, 1-mL Pipet Filler, safety bulb Quantity 2 1 1 Unit each each each Catalog number 2088640 919002 1465100

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Recommended standards and apparatus

Description Nitrogen, Ammonia Standard Solution, 1-mg/L NH3N Nitrogen, Ammonia Standard Solution, 10-mL Voluette Ampule, 50-mg/L NH3N Pipet, TenSette 0.1 - 1.0 mL Pipet Tips, for TenSette Pipet 1970001 Pipet Tips, for TenSette Pipet 1970001 Wastewater, Effluent Inorganics, for NH3N, NO3N, PO4, COD, SO4, TOC Unit 500 mL 16/pkg each 50/pkg 1000/pkg 500 mL Catalog number 189149 1479110 1970001 2185696 2185628 2833249

Optional reagents and apparatus

Description Distillation Apparatus, General Heater and Support Apparatus, 115 VAC, 60 Hz Heater and Support Apparatus, 230 VAC, 50 Hz Pour-Thru Cell Kit for DR 2800 Pour-Thru Cell Module for DR 5000 Ampule breaker, Voluette Sodium Thiosulfate, 0.1 N Sodium Hydroxide, 5 N Unit each each each each each each 100 mL 100 mL Catalog number 2265300 2274400 2274402 5940400 LZV479 2196800 32332 245032

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