Nitrogen, Total Kjeldahl, 8075

Nitrogen, Total Kjeldahl

Nessler Method1 (Digestion Required) 1 to 150 mg/L
Scope and Application: For water, wastewater and sludge; digestion is required.
1

DOC316.53.01091 Method 8075

Adapted from Hach, et. al., Journal of Association of Official Analytical Chemists, 70(5) 783-787 (1987); Hach, et. al., Journal of Agricultural and Food Chemistry, 33(6) 1117-1123 (1985); Standard Methods for the Examination of Water and Wastewater

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 1 Instrument-specific information

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

Before starting the test:

For more accurate results, determine a reagent blank value for each new lot of reagent. Follow the procedure using deionized water in place of the sample. Subtract the reagent blank value from the final results or perform a reagent blank adjust. If using a Pour-Thru system, periodically clean the cell by pouring a few sodium thiosulfate pentahydrate crystals into the cell funnel or rinse with a solution of sodium thiosulfate. Flush it through the funnel and cell with enough deionized water to dissolve. Rinse out the crystals. Hold droppers and dropper bottles vertically, not at an angle, when dispensing reagent. Nessler reagent contains mercuric iodide. Both the sample and blank will contain mercury (D009) at concentrations regulated as a hazardous waste by the Federal RCRA. Do not pour these solutions down the drain. Refer to the current MSDS for safe handling and disposal instructions. Because of the methods sensitivity, it is recommended to use the Standards and Calibration Adjust feature..

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Nitrogen, Total Kjeldahl

Collect the following items:

Description Boiling Chips, silicon carbide Cots, finger Cylinder, graduated mixing, 25 mL Digesdahl Digestion Apparatus Hydrogen Peroxide, 50% Mineral Stabilizer Nessler Reagent Polyvinyl Alcohol Dispersing Agent Potassium Hydroxide (KOH) Standard Solution, 1.0 N Potassium Hydroxide (KOH) Standard Solution, 8.0 N Sulfuric Acid, ACS, concentrated TKN Indicator Solution Pipet, TenSette, 0.11.0 mL, plus tips Safety Shield Sample Cell (see Instrument-specific information) See Consumables and replacement items for reorder information. Quantity 23 2 2 1 20 mL 6 drops 2 mL 6 drops varies varies 6 mL 2 drops 1 1 2

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Nitrogen, Total Kjeldahl Nessler method

Stored Programs 399 Nitrogen, TKN Start

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

2. Prepared Sample: Digest the sample amount as described in the Digesdahl Digestion Apparatus Instruction Manual.

3. Blank Preparation: Digest an equal amount of deionized water as the blank.

4. Select the appropriate analysis volume of the digested sample given in the Aqueous samples (solutions or suspensions in waterless than 1% solids), Dry samples or Oils and fats tables depending on the sample. Pipet the analysis volume from the sample and the blank into separate 25-mL mixing graduated cylinders.

5. Add one drop of TKN Indicator to each cylinder.

6. If the aliquot is less than 1 mL, proceed to step 7. If it is greater than 1 mL, add drops of 8.0 N KOH to each cylinder until the first flash of blue color appears. Stopper and invert the cylinder after each addition. Proceed to the next step.

7. Add 1.0 N KOH to each cylinder, one drop at a time, mixing after each addition. Continue until the first permanent blue color appears.

8. Fill both cylinders to the 20-mL mark with deionized water.

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Nitrogen, Total Kjeldahl Nessler method (continued)

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

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

11. Fill both cylinders to the 25-mL mark with deionized water. Stopper and invert several times to mix.

12. Pipet 1.00 mL of Nessler Reagent to each cylinder. Stopper and invert repeatedly. The solution should not be hazy. Any haze (turbidity) will cause incorrect results.

Zero

13. Start the instrument timer. A two-minute reaction period will begin.

14. When the timer expires, pour the contents of the cylinders into separate square sample cells.

15. Wipe the blank and insert it into the cell holder.

16. ZERO the instrument. The display will show: 0 mg/L TKN

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Nitrogen, Total Kjeldahl Nessler method (continued)

Read

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

18. READ the results in mg/L TKN.

19. Calculate sample TKN as follows: Where:

75 A ppm TKN = ---------------B C

A = mg/L read from the display B = g (or mL of water) sample taken for digest C = mL analysis volume of digested sample

Interferences
Table 2 Aqueous samples (solutions or suspensions in waterless than 1% solids)
Expected nitrogen concentration (mg/L) 0.528 2112 11560 452250 42522500 Analysis volume (mL) 10.0 5.0 2.00 1.00 0.50

Table 3 Dry samples

Expected nitrogen concentration (mg/L) 422200 1065600 35018,000 100056,000 4200220,000 Analysis volume (mL) 10.0 5.00 2.00 1.00 0.50

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Nitrogen, Total Kjeldahl Table 4 Oils and fats

Expected nitrogen concentration (mg/L) 854500 21011,000 2100110,000 Analysis volume (mL) 10.0 5.00 1.00

Sample collection, preservation and storage

Collect samples in clean glass or plastic containers. Adjust sample pH to 2 or less with Sulfuric Acid (about 2 mL per liter) and cool to 4 C (39 F). Preserved samples can be stored up to 28 days.

Accuracy check
Kjeldahl Nitrogen standard method This procedure checks digestion efficiency and indicates the amount of bound nitrogen that is released during digestion. The methods and standards available to check digestion technique are found in the Accuracy Check section following the procedure in the Digesdahl Digestion Apparatus Instruction Manual. Using the digested Kjeldahl standard, perform the Nessler method on a colorimeter. The TKN value should come within 3% of the value of the prepared Kjeldahl standard. Standard solution method (to check calibration accuracy only)
Note: Refer to the instrument user manual for specific software navigation instructions.

Required for accuracy check: 1.0-mg/L NH3N solution TKN indicator Dropper Graduated cylinders (2) Deionized water Mineral Stabilizer Polyvinyl Alcohol Dispersing agent

1. Add one drop of TKN Indicator to each 25-mL graduated mixing cylinder. 2. Fill one cylinder to the 20-mL mark with deionized water. Fill the other cylinder to the 20-mL mark with a 1.0-mg/L NH3N solution. 3. Add 3 drops of Mineral Stabilizer to each cylinder. Invert several times to mix. 4. Add 3 drops of Polyvinyl Alcohol Dispersing agent to each cylinder. Invert several times to mix. 5. Perform the TKN procedure as described in step 11 to step 18. Accurate calibrations will show 2627 mg/L TKN.

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Nitrogen, Total Kjeldahl

Method performance
Precision95% Confidence Limits of Distribution 7082 mg/L NH3N Sensitivity DConcentration per 0.010 DAbs 1 mg/L NH3N

Program 399

Standard 76 mg/L NH3N

Summary of method
The term Total Kjeldahl Nitrogen refers to the combination of ammonia and organic nitrogen. However, only the organic nitrogen compounds appearing as organically bound nitrogen in the trinegative state are determined in this test. Nitrogen in this form is converted into ammonium salts by the action of sulfuric acid and hydrogen peroxide. The ammonia is then analyzed by a modified Nessler method test. Test results are measured at 460 nm.

Consumables and replacement items

Required reagents
Description Nitrogen Reagent Set, 0150 mg/L, Nessler Method, includes: Hydrogen Peroxide, 50% Mineral Stabilizer Nessler Reagent Polyvinyl Alcohol Dispersing Agent Potassium Hydroxide Standard Solution, 1.0 N Potassium Hydroxide Standard Solution, 8.0 N Sulfuric Acid, ACS, concentrated TKN Indicator Solution Quantity/Test 20 mL 6 drops 2 mL 6 drops varies varies 6 mL 2 drops Unit 250 tests 490 mL 50 mL SCDB 500 mL 50 mL SCDB 50 mL SCDB 100 mL MDB 500 mL 50 mL SCDB Catalog number 2495300 2119649 2376626 2119449 2376526 2314426 28232H 97949 2251926

Required apparatus
Description Boiling Chips, silicon carbide Cots, finger Cylinder, graduated mixing, 25-mL Digesdahl Digestion Apparatus, 115 VAC OR Digesdahl Digestion Apparatus, 220 VAC Pipet, TenSette, 0.11.0 mL Pipet Tips, for TenSette Pipet 1970001 Safety Shield 1 1 2 1 each each 50/pkg each 2313021 1970001 2185696 5003000 Quantity 23 2 2 1 Unit 500 g 2/pkg each each Catalog number 2055734 1464702 2636240 2313020

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Nitrogen, Total Kjeldahl

Recommended standards
Description Nitrogen, Primary Standard Set for TKN Nitrogen Standard Solution, 1-mg/L NH3N Nitrogen Standard Solution, Voluette Ampule, 150-mg/L NH3N, 10-mL Wastewater Influent Inorganics Standard for NH3N, NO3N, PO4, COD, SO4, TOC Unit each 500 mL 16/pkg 500 mL Catalog number 2277800 189149 2128410 2833149

Optional reagents and apparatus

Description Sodium Thiosulfate, Pentahydrate Pour-Thru Cell Kit (DR 2700, DR 2800) Pour-Thru Cell Kit (DR 5000) PourRite Ampule breaker 2-mL Voluette Ampule breaker 10 mL Pipet, TenSette, 1.010.0 mL Pipet Tips, for TenSette Pipet 1970010 Pipet Tips, for TenSette Pipet 1970010 Pipet Tips, for TenSette Pipet 1970010 Ammonia Nitrogen Standard Solution, 10-mg/L NH3N Ammonia Nitrogen Standard Solution, 100-mg/L NH3N Ammonia Nitrogen Standard Solution, 1000-mg/L NH3N Ammonia Nitrogen Standard Solution, 10-mL Voluette Ampules, 50 mg/L Balance, analytical, 80 g capacity Weighing Paper, 76 x 76 mm Ammonia Nitrogen Standard Solution, 2-mL PourRite Ampule, 50 mg/L Unit 454 g each each each each each 50/pkg 250/pkg 1000/pkg 500 mL 500 mL 1L 16/pkg 115 VAC 500/pkg 20/pkg Catalog number 46001 5940400 LZV479 2484600 2196800 1970010 2199796 2199725 2185628 15349 2406549 2354153 1479110 2936701 1473800 1479120

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