Nitrate Method 8192 Cadmium Reduction Method Powder Pillows LR (0.01 to 0.50 mg/L NO37-N) ‘Scope and Application: For water, wastewater, and seawater HF] 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. ‘A deposit of unoxidized metal will remain after the NitraVer® 6 dissolves. The deposit will not affect results ‘Shaking time and technique influence color development. Analyze a standard solution several times and adjust the shaking time to obtain the correct result. Use this time for analyzing samples. Rinse the sample cell and mixing cylinder immediately after use to remove all cadmium particles Properly dispose of the used sample, Prepared samples contain cadmium and must be disposed of according to Federal, State, and local hazardous waste regulations, Refer to the current MSDS for safe handling and disposal information. Collect the following ems: ‘Quantity NitraVer®6 Nitrate Reagent powder plow NitraVer® 3 Nitrite Reagent powder pillow Cylinder, graduated, mixing, 25-ml. Sample Cells, t-inch square, 10-mL ‘Note: Reorder information for consumables and replacement items is on page 5. 351 N, Nitrate LR Stored Programs a < 1. Press 2. Select he test 3. Fila25mi gaduated 4 Add the contents of STORED PROGRAMS, ming evindorwith 18m one NiraVer6 Reagent creampie Poder Plow othe cylinder. Stopper. Nitrate Nivate 6192_PP_LR 26004m Page 1 of 6Nitrate LR (0.01 to 0.50 mg/L NO3--N) ox | 03:00 5. Press TIMER>OK, 6. Shake the cylinder vigorously during the A3-minute reaction time three-minute timer. will begin. % ox 00:30 9. Prepared Sample: 10. Press TIMER>OK. Add the contents of one NitriVer 3 Nitrite Reagent Powder Pillow to the sample cell Os Ug 14, Insert the blank into the cell holder with the fil line facing right. A 30-second reaction time will begin. 13, Blank Preparation: When the timer expires, fill a second square sample cell with 10 mL of original sample. a 02:00 7. When the timer expires, press TIMER>OK again. A 2-minute reaction period will begin, 44. Cap and shake the sample cell gently during the 30-second timer. A pink color will develop if nitrate is present. zero 15. Press ZERO, The display will show: 0.00 mg/l. NO3--N 8. When the timer expires, carefully pour 10 mL of the sample into a clean square sample cell Do not transfer any cadmium particles to the sample cell Ea 15:00 12, Press TIMER>OK, ‘A 15-minute reaction period will begin ig Read 16. Insert the prepared sample into the cell holder with the fil line facing right. Press READ. Results are in mg/L NO3--N. Nitrate Page 2 of 6Nitrate LR (0.01 to 0.50 mg/L NOz Interferences Table 1 Interfering Substances and Levels Interfering Substance Interference Levols and Treatments Calcium 100 mat ‘Chloride concentrations above 100 mall will cause low results. The test may be used at igh Chloride chloride concentrations (seawater) but a calibration must be done using standards spiked to the same chloride concentration, Ferric ron Alllevels ‘Al levels: This method measures both the nitrate and nitite in the sample. If niite is present, the nitrite nitrogen test (Program #371) should be done on the sample, Pretreat the nitrate nitrogen sample with the folowing pretreatment, Then subtract the amount of nitrite found | from the results of the LR nitrate nitrogen test. Nivite ‘Add 30-il. Bromine Water" dropwise to the sample in step 4 until a yellow color remains. Mix after each drop. ‘Add one drop of 30-g/L Phenol Solution to destroy the color. Proceed withthe LR Nitrate procedure. Highly buffered samples or extreme sample pH may exceed the buffering capacity ofthe pH reagents and require sample pretreatment. Sirong oxidizing and reducing | itenereg at all ievels Strong oxic Interfores at al ove 11See Optional Reagents and Apparatus on page 5 Sample Collection, Storage, and Preservation More reliable results are obtained when samples are analyzed as soon as possible after collection. If prompt analysis is impossible, store samples in clean plastic or glass bottles for up to 48 hours at 4 °C. To preserve samples for longer periods, add 2 mL of Concentrated Sulfuric Acid® per liter and store at 4 °C. Before analysis, warm the sample to room temperature and adjust the pH to 7 with 6.0 N ‘Sodium Hydroxide Standard Solution’, Do not use mercury compounds as preservatives, Correct the test result for volume additions by dividing the total volume (acid + base + sample) by the original sample volume and multiplying the test result by this factor. Accuracy Check Standard Additions Method (Sample Spike) 1. Afler reading test results, leave the sample cell (unspiked sample) in the instrument, Verify the chemical form. 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, 4, Snap the neck off a Nitrate Nitrogen Voluette® Ampule Standard, 12.0-mg/L NOs--N*. Nitrate Nivate 6192_PP_LR 26004m Page 3 of 6Nitrate LR (0.01 to 0.50 mg/L NO3--N) 5. Prepare three sample spikes, Fill three mixing cylinders* with 15 mL of sample. Use the ‘TenSette® Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively, to each sample and mix thoroughly. 6. Analyze each sample spike as described in the procedure above, starting with the 0.1 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 1. To test accuracy, use a 0.40-mg/l. NO3--N standard in place of the sample and perform the procedure as described, Prepare this standard by diluting 4.00 mL of a 10-mg/L Nitrate Nitrogen Standard Solution to 100.0 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. Summary of Method Cadmium metal reduces nitrates in the sample to nitrite, The nitrite ion reacts in an acidic ‘medium with sulfanilic acid to form an intermediate diazonium salt. The salt couples with chromotropic acid to form a pink-colored product. Test results are measured at 507 nm. See Optional Reagents and Apparalus on page 6. Nitrate Page 4 of 6