Nitrogen, Free Ammonia, 10201

Nitrogen, Free Ammonia

Indophenol Method1 (0.01 to 0.50 mg/L NH3N)

DOC316.53.01084 Method 10201 Powder Pillows

Scope and Application: For controlling free ammonia levels during the production of chloramines, at booster stations and for monitoring free ammonia levels in potable distribution system waters.
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U.S. Patent 6,315,950

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 270 Instrument-specific information

Instrument DR 6000 DR 5000 DR 3900 DR 3800, DR 2800, DR 2700 Sample Cell 4864302 4864302 4864302 5940506 Cell Orientation Orientation key faces right Orientation key toward user Orientation key inserted in adapter slot 1-cm (flat) path aligned with the arrow on the adapter Adapter A23618 LZV846 (A) LZV585 (B)

Before starting the test:

Use Method 10200, Nitrogen, Free Ammonia and Chloramine (Mono) to determine free ammonia and monochloramine simultaneously on the same sample. In bright light conditions (e.g. direct sunlight) it may be necessary to close the cell compartment with the protective cover during measurements. Dispose of reacted solutions according to local, state and federal regulations. Use the guidance given on the Material Safety Data Sheets to dispose of unreacted reagents. Consult local regulatory agencies for further disposal information.

Description Free Ammonia Reagent Set Free Ammonia Reagent Solution Monochlor F Reagent Pillows Sample Cell (see Instrument-specific information) See Consumables and replacement items for reorder information.

Quantity 1 drop 2 2

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Nitrogen, Free Ammonia Indophenol method for powder pillows

Stored Programs 388 N, Ammonia Free Start

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

2. Fill two cells to the 10-mL line with sample. Label one cell sample and one cell blank.

3. Prepared Sample: Add one drop of Free Ammonia Reagent Solution to the sample.

4. Cap the reagent bottle to maintain reagent performance and stability.

5. Cap and invert the sample to mix. If the sample becomes cloudy by the end of the reaction period, pretreat the sample and retest. See Interferences.

6. Start the instrument timer. A 5-minute reaction period will begin. Color development time depends on sample temperature. For accurate results allow the full reaction period to occur. See Color development based on sample temperature.

7. When the timer expires, add the contents of one MonoChlor F powder pillow to each cell.

8. Cap and shake both cells about 20 seconds to dissolve the reagent. A green color will develop if monochloramine is present.

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Nitrogen, Free Ammonia Indophenol method for powder pillows (continued)

Zero

9. Start the instrument timer. A 5-minute reaction period will begin. Color development time depends on sample temperature. For accurate results allow the full reaction period to occur. See Color development based on sample temperature.

10. When the timer expires, insert the blank vial into the cell

11. ZERO the instrument. The display will show: 0.00 mg/L NH3N f Remove the blank.

12. Insert the sample into the cell

Read

13. READ the results in mg/L NH3N f.

Interferences
This method is intended for finished, chloraminated drinking water samples that have a measurable combined (total) chlorine disinfectant residual. Samples where the disinfectant residual has disappeared and samples which exhibit a chlorine demand may produce low ammonia test results. Blanks and ammonia standards analyzed without a disinfectant residual must be prepared using high quality, reagent grade water. The following do not interfere in the free ammonia determination at or below the stated concentration.

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Nitrogen, Free Ammonia

Table 271 Interfering substances

Interfering substance Aluminum Chloride Copper Iron Manganese Nitrate Nitrite Phosphate Silica Sulfate Zinc Interference level 0.2 mg/L 1200 mg/L Cl1 mg/L Cu 0.3 mg/L Fe 0.05 mg/L Mn 10 mg/L NO3N 1 mg/L NO2N 2 mg/L oPO4 100 mg/L SiO2 1600 ppm as CaCO3 5 ppm Zn

Samples containing high levels of both Total Hardness and Alkalinity may become cloudy after the addition of the Free Ammonia Reagent Solution. If this occurs by the end of the first reaction period, the sample for Free Ammonia measurement must be pretreated as follows:
Note: The blank does not need pretreatment.

1. Measure 10 mL of sample into the cell labeled for the sample. 2. Add the contents of one Hardness Treatment Reagent Powder Pillow to the sample. 3. Cap the cell and invert until the reagent is dissolved. 4. Remove the cap. 5. Continue with the analysis at step 2 using the pretreated sample as the sample.

Color development time

Test results are strongly influenced by sample temperature. Both reaction periods in the procedure are the same and depend on the temperature of the sample. The reaction periods indicated in the procedure are for a sample temperature of 1820 C (6468 F). Adjust both reaction periods (see Color development based on sample temperature). The samples can be read up to 15 minutes after the development times listed in Table 272 as the developed color is stable for an extended period of time.

Table 272 Color development based on sample temperature

Sample Temperature Development Time (minutes) C 5 7 9 10 12 14 16 18 F 41 45 47 50 54 57 61 64 10 9 8 8 7 7 6 5

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Nitrogen, Free Ammonia Table 272 Color development based on sample temperature
Sample Temperature Development Time (minutes) C 20 23 25 greater than 25 F 68 73 77 greater than 77 5 2.5 2 2

Sample collection, preservation and storage

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

Accuracy check
Dilution water is required when testing a diluted sample and preparing standard solutions. Dilution water must be free of ammonia, chlorine and chlorine demand. A convenient source is a recirculating, deionizer system with carbon filtration which produces 18 megohm-cm water. Standard additions method (sample spike) Required for accuracy check: Ammonia Nitrogen Standard, 10 mg/L as NH3-N Ampule breaker TenSette Pipet and Pipet Tips Mixing cylinders, 50 mL (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. 5. Use the TenSette Pipet to prepare spiked samples: add 0.3 mL, 0.6 mL and 1.0 mL of standard to three 50-mL portions of fresh sample. 6. Follow the Indophenol method for powder pillows test procedure for each of the spiked samples, starting with the 0.3 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.

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Nitrogen, Free Ammonia

Standard solution method
Note: Refer to the instrument user manual for specific software navigation instructions.

Required for accuracy check: Ammonia Nitrogen Standard Solution, 10 mg/L NH3N Deionized water Volumetric Pipet, 2 mL or Tensette Pipet and Pipet tips Volumetric flask, 100 mL

1. Prepare a 0.20 mg/L ammonia nitrogen standard solution as follows: Dilute 2.00 mL of Ammonia Nitrogen Standard Solution, 10 mg/L to 100 mL with deionized water. Or, use the TenSette Pipet to dilute 0.4 mL of a Ammonia Nitrogen Voluette Standard Solution, 50 mg/L as NH3N, to 100 mL with dilution water.

2. Use this solution in place of the sample. Follow the Indophenol method for powder pillows test procedure. 3. To adjust the calibration curve using the reading obtained with the standard solution, navigate to Standard Adjust in the software: OPTIONS>MORE>STANDARD ADJUST. 4. 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.

Method performance
Precision95% Confidence Limits of Distribution 0.190.21 mg/L NH3N Sensitivity Concentration per 0.010 Abs 0.01 NH3N

Program 388

Standard 0.20mg/L NH3N

Summary of method
Monochloramine (NH2Cl) and free ammonia (NH3 and NH4+) can exist in the same water sample. Added hypochlorite combines with free ammonia to form more monochloramine. In the presence of a cyanoferrate catalyst, monochloramine in the sample reacts with a substituted phenol to form an intermediate monoimine compound. The intermediate couples with excess substituted phenol to form a green-colored indophenol, which is proportional to the amount of monochloramine present in the sample. Free ammonia is determined by comparing the color intensities, with and without added hypochlorite. Test results are measured at 655 nm.

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Nitrogen, Free Ammonia

Consumables and replacement items

Required reagents
Description Free Ammonia Reagent Set (50 tests), includes: (1) 2802299, (1) 2877336 Free Ammonia Reagent Solution Monochlor F Reagent Pillows 1 drop 2 4 mL SCDB 100/pkg 2877336 2802299 Quantity/Test Unit Catalog number 2879700

Recommended standards
Description Hardness Treatment Reagent Pillows (1 per test) Nitrogen Ammonia Standard Solution, 10 mg/L as NH3N Nitrogen Ammonia Standard Ampule, 50 mg/L as NH3N, 10 mL Water, organic-free water Unit 50/pkg 500 mL 16/pkg 500-mL Catalog number 2882346 15349 1479110 2641549

Optional reagents and apparatus

Description Ampule Breaker Kit Flask, volumetric, Class A, 100 mL Pipet Filler, Safety Bulb Pipet, TenSette, 0.1 to 1.0 mL Pipet Tips, for TenSette Pipet 1970001 Thermometer, 10 to 110 C Wipers, Disposable, 30 x 30 cm, 280/box Pipet, volumetric, Class A, 2.0 mL Cylinder, graduated mixing, 50 mL Unit each each each each 50/pkg each box each each Catalog number 2196800 1457442 1465100 1970001 2185696 187701 2097000 1451536 189641

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