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User`s Manual C

1. Fluoride At all leves Iron reater than 20 mg L Phosphate _ Greater than 50 mg L Polyphosphate At all levels by causing negative errors Must be converted to orthophosphate Sampling Collect samples in a clean glass or plastic container Preserved the sample by adjusting the pH to 2 Storage or less with nitric acid about 1 5mL per liter Can be 6 months at room temperature amp Preservation Before analysis adjust the pH to 3 5 4 5 with 5 0 N NaOH solution Tips Digestion is required for determining total aluminum Clean glassware with 6 0 N HCI and Deionized water amp before analysis The sample temperature must be between 20 25 C for accurate results Techniques Clean glassware with soap and a brush immediately following analysis Aluminum 1 Aluminum E Procedures Aluminon Method 5 Pour the 25mL of solution from the cylinder into a second 25mL sample cell A 15 minute reaction period will begin This is the blank 1 Fill the cylinder to the 50 mL and Add the contents of one Ascorbic Acid Pillow Stopper Invert several times to dissolve powder 2 Add the contents of one Aluminum Reagent Powder Pillow Stopper Invert for lminute to dissolve the powder completely Red Orange color will develop if Aluminum is present 6 After choosing C MAC mode in the program choose Prog 1 HACH DR 890 1 DR 2010 2500 10 DR 4000 1000 7 Within 3 minutes after the timer beep wipe the blank
2. Bromine 4 Chlorine Free A Chlorine Free 0 02 2 00 mg L Cle DPD Method mac Required DPD Free Chlorine Reagent Pillow Cat NO 11210 00 Reagents Greater an 150 mg L 57 aC Os Neutralize wane OO iaa SNL O O t No effect at less than 1 000 mg L as CaCO OOO yg aaa Chloramines organic e Hardness After adjusting sample pH to 6 7 add 3 drops KI 30g L to a 25mL sample Mix and wait 1 minute Add 3 drops sodium arsenite 5g L and mix Analyze 10mL of the treated sample Substract the result from this test from the original analysis to obtain the correct bromine concentration Interferences Mi Mear Cro When read within 1 minutes after reagent addition 3mg L monochloramine Monochloramine E i e causes less than a 0 1 mg L increase in the reading Ozone At all levels Peroxides _ May interfere Extreme sample pH or Neutralize to pH 6 7 with 1N H gt S0O4 or 1N NaOH highly buffered samples S ES Avoid plastic containers Pretreat glass sample containers to remove any chlorine demand by soaking in a dilute bleach solution Bleach 1mL per liter for at least 1hour Rinse thoroughly with deionized or distilled water If sampling from a tap allow the water to flow at least 5minutes to ensure a representative sample Allow several volumes of water to overflow the container and cap the container so there is no headspace above the sample Analyze samples immediately Do not preserve S
3. Ji Digestion is required for determining total manganese ips amp Techniques For more accurate results detemine 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 of perform a reagent blank adjust Manganese HR 41 Manganese HR E Procedures Periodate Oxidation Method 5 After choosing C MAC mode in the program choose Prog 41 HACH DR 890 41 DR 2010 amp 2500 295 DR 4000 2250 1 Fill a sample cell with 10 mL of sample the prepared sample 6 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 2 Add the contents of one Buffer Pillow to each cell Cap and mix gently 3 Add the contents of one Sodium Periodate Pillow to each cell Cap and mix gently A violet color will develop if manganese is present A 2 minute reaction period will begin 7 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Mn 4 Fill another sample cell with 10 mL of sample the blank Manganese HR 42 C mac Required Reagents Interferences Sampling Storage amp Preservation Tips amp Techniques Nitrate HR Nitrate HR Nitrate HR 0 2 30 0 mg L NO3 N Chromotropic Acid Method Nitrate HR Vial Nitrate Reagent 1 Pillow
4. Nitrate MR Reagent Pillow Cadmium Reduction Method Cat NO 10423 11 Calcium 100 mg L Concentrations Above 100 mg L will cause low results The test may be used at seawater but Chloride e E f f _ a calibration must be done using standards spiked to the same chloride concentration Ferric ion At all levels At all levels This method measures both the nitrate and nitrite in the sample If nitrite is present NO2 N LR Test Prog 60 should be done on the sample Pretreat the nitrate nitrogen sample with the following Nitrite pretreatment Then subtract the amount of nitrite found from the results of the NO2 N LR Test E Add 30 g L Bromine Water dropwise to the sample in step 2 until a yellow color remains Mix after each drop Add one drop of 30 g L Phenol Solution to destroy the color Le E ee require sample pretreatment 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 2mL of sulfuric acid per liter and store at 4 C Before analysis wam the sample to room temperature and adjust the pH to 7 with 5N NaOH solution Do not use mercury compounds as preservatives 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 s
5. 371 DR 4000 2610 Nitrite LR Nitrite LR Diazotization Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 6 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L NO N 392 Nitrite LR TEST KIT AA Mac Nitrite LR 0 003 0 500 mg L NOz2 N Diazotization Method TEST KIT Required Reagents Nitrite LR Vial Cat NO 10512 01 Aluminous ions Auric ions L a ae Ge Sa S e SES A S S Sg e E Mercurous ions Metavanadate ions Interferences Silver ions Cupric ions Ferrous ions 0 Cause low results E ea on oa Fee a a T i At all levels highly buffered samples Sampling Collect samples in clean plastic or glass bottles Store at 4 C 30 F or lower if the Storage sample is to be analyzed within 24 to 48 hours Warm to room temperature before running amp Preservation the test Do not use acid preservatives Tips For more accurate results determine a reagent blank value for each new lot of reagent amp Follow the procedure using deionized water in place of the sample Subtract the reagent Techniques blank value from the final results of perform a reagent blank adjust Nitrite LR 53 D Procedures Nitrite LR 1 Fill a vial with 5 mL of sample the prepared sample 2 Cap and shake to dissolve the powder A pink color wil
6. Interferences the test results by 1 02 to correct for sample dilution by the formaldehyde Hardness Substitute a copper reagent powder A for Copper Reagent Pillow Iron Fei Substitute a copper reagent powder A for Copper Reagent Pillow If a turbidity remains and turns black silver interference is likely Add l 10 drops of saturated KCI solution to 75 mL of sample followed by filtering through a fine or highly retentive filter Use the filtered sample in the procedure Silver Ag Collect samples in acid washed glass or plastic containers To preserve samples adjust Sampling Storage the pH to 2 or less with nitric acid about 2mL per liter amp Preservation Store preserved samples at room temperature up to six months Before analysis adjust the pH to 4 6 with 8 N KOH Do not exceed pH 6 as copper may precipitate Tips Digestion is required for determining total copper Techniques Accuracy is not affected by undissolved powder Copper 17 Copper E Procedures Bicinchoninate Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 1 Fill a sample cell with 10 mL of sample 6 Within 30 minutes after the timer beeps wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Cu 2 Add the contents of one Copper Reagent Pillow to the sample cell Cap and invert gently
7. Orthophosphate LR Phosphorus Reactive LR Ascorbic Acid Method SCH 0 06 5 00 mg L PO 0 02 1 60 mg L P i Required Phosphorus Vial Cat NO 10712 00 Reagents PO P LR Reagent Pillow Aluminum Greater than 200 mg L Arsenate At all levels Chromium 0 Greater than 100 mg L Copper Silicate Greater than 10 mg L Iron Greater than 100 mg L Nickel Greater than 300 mg L Interferences Highly buffered May exceed the buffering capacity of the reagents and require sample amples OF ENE Pl priremi SE Ss SEN EE Silica eer eee SES gt a ee Ee Sulfide drop wise until a permanent yellow color appears Add phenol solution drop wise until the yellow color disappears A eee a eC Collect samples in plastic or glass bottles that have been acid cleaned with 1 1 HCI and rinsed with Samplin ae e Ane deionized water Do not use commercial detergents containing phosphate for cleaning glassware used in Storage amp Preservation this test Analyze samples immediately after collection for best results If prompt analysis is impossible preserve samples up to 48 hours by filtering immediately and storing at 4 C Warm samples to room temperature before analysis Tips amp d Store the PO4 P LR reagent pillows in a cool dry environment Techniques Phosphorus Reactive Orthophosphate LR 77 Phosphorus Reactive Orthophosphate LR E Procedures Ascorbic Acid Method 5 Add th
8. Required Cyanuric Acid Reagent Pillow Cat NO 11910 00 Reagents Sampling Storage Collect samples in clean plastic or glass bottles Samples must be analyzed Preservation within 24 hours Filter highly turbid samples with filter paper and a funnel Tips S After adding the reagent a white turbidity will form if cyanuric acid is present j Clean sample cells with soap water and a brush soon after each test to avoid Techniques a build up of film on the sample cell Cyanuric Acid 25 Cyanuric Acid E Procedures Turbidimetric Method 5 Wipe the blank and place it into the cell holder 1 Fill a sample cell with 25 mL of sample Place the cover on the sample cell Press Zero 6 Within 7 minutes after the timer beeps wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter 2 Add the contents Cyanuric Acid Reagent Pillow Cap and swir to mix the prepared sample A 3 minute reation period will begin Results will appear in mg L Cyan Acid 3 Fill another round sample cell with 25 mL of sample the blank 4 After choosing C MAC mode in the 1 C MAC Mode program choose Prog 24 HACH DR 890 24 DR 2010 amp 2500 170 Cyanuric Acid 26 Fluoride e Fluoride 0 02 2 00 mg L F SPADNS Method mac Required Reagents Interferences Sampling Storage amp Preservation Tips amp Techniques Fluoride SPADNS re
9. Retum the boiled sample to the 25 mL graduated cylinder Return the _ sample volume to the 25 mL mark with deionized water Pour this solution into a sample cell and swirl to mix Proceed with sten Collect samples in acid washed glass or plastic bottles To preserve samples adjust the sample Samplin Gola pH to 2 or less with concentrated Nitric Acid about 2 mL per liter Samples preserved in this manner Storage amp Preservation can be stored up to six months at room temperature If you are only reporting dissolved iron filter the sample immediately after collection and before adding nitric acid Before testing adjust the sample pH to 3 5 with Ammonium Hydroxide Do not exceed pH 5 or iron may precipitate Ji Digestion is required for total iron determination Rinse glassware with a 1 1 HCI and rinse again with ips amp Techniques deionized water 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 of perform a reagent blank adjust iron 33 D Procedures iron 1 Fill a sample cell with 25 mL of sample the prepared sample 2 Add the contents of one Iron Reagent Solution Pillow to the sample cell Cap and mix A 5 minute reacition period will begin A violet color will develop if iron is present 3 Fill another sample cell with 25 mL of sample
10. Sampling Collect samples in acid washed plastic bottles Adjust the sample pH to 2 or less with Nitric Acid Storage about 5 mL per liter Cool samples to 4 C Preserved samples can be stored up to six months amp Preservation Before analysis adjust the sample pH to between 3 and 8 with 5 0 N NaOH Solution For the most accurate magnesium test results keep the sample temperature between 21 29 C The test will detect any calcium or magnesium contamination in the mixing cylinder measuring Tips i droppers or sample cells To test cleanliness repeat the test until result are consistent Total hardness in mg L equals mg L Ca as CaCO plus mg L Mg as CaCOs Techniques Remaining traces of EDTA or EGTA from previous tests will give erroneous results Rinse sample cells thoroughly before using Hardness 29 Hardness E Procedures Calmagite Colorimetric Method 1 Pour 100 mL of sample into a 100 mL graduated mixing cylinder 5 Add one drop of EDTA Solution to the first cell the blank Swirl to mix 2 Add 1 mL of Calcium and Magnesium Indicator Solution Stopper the cylinder and invert it several times 6 Add one drop of EGTA Solution to the second cell Swirl to mix 7 After choosing C MAC mode in the 3 Add 1 mL of Alkali Solution for Calcium program choose Prog 30 and Magnesium Test Stopper the cylinder 1 C MAC Model HACH DR 890 30 and invert it several times DR 2010 2500 225 DR 4000 2020
11. Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell 1 Pipet 10 mL of sample into a dry round sample cell the prepared sample Pipet 10 mL of deionized water into a second dry round sample cell the blank Ab Press Enter Results will appear in mg L F 2 Carefully pipet 2 mL of SPADNS Solution into each cell Swin to mix A 1 minute reaction period will begin 3 After choosing C MAC mode in the program choose Prog 27 C MAC Model HACH DR 890 27 DR 2010 2500 190 DR 4000 1900 4 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero Fluoride 28 Hardness e Hardness 0 07 4 00 mg L Ca and Mg as CaCOs Calmagite Colorimetric Method mac Alkali Solution for Ca and Mg Test Required Ca and Mg Indicator Solution Reagents EDTA Solution 1M EGTA Solution Cat NO 12010 00 crt Above 0 25 mg L EDTA or EGTA Traces remaining in sample cells from previous tests will give erroneous results _ Rinse cells thoroughly before using Fei Above 1 4 mg L Interferences a E Fe Above 2 0 mg L Mn Above 0 2 mg L Zn Above 0 05 mg L Ca gt 1 0 mg L For the most accurate calcium test result rerun the test on a diluted sample if the calcium is over 1 0 and the magnesium is over 0 25 mg L as CaCO Mg gt 0 25 mg L No retesting is needed if either is below those respective concentrations
12. 1 C MAC Mode 6 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks 7 Place the blank into the cell holder Place the cover on the vial Press Zero 8 Place prepared sample into the cell holder Place the cover on the vial Press Enter Results will appear in mg L COD 70 Oxygen Demand Chemical CODcr SC LR 10 150 mg L COD Chemical Oxygen Demand CODcr LR Reactor Digestion Method Required Reagents Interference Sampling Storage amp Preservation Tips amp Techniques COD LR Vial Cat NO 10112 00 Chloride is the primary interference when determining COD concentration Samples with higher chloride concentrations should be diluted If sample dilution will cause the COD concentration to be too low for accurate determination add 0 5 g oft mercuric sulfate to each COD vial before the sample is added Maximum cal ne l Suggested cr of 8 When 0 59 HgSO4 added a mg L _ diluted samples mg L Maximum CI mg L ULR 2000 1000 NA LR HR 2000 1000 E _8000 PRE 20007 Eo gt 000 SE e 000 EE E E bt Collect samples in glass bottles Use plastic bottles only if they are known to be free of organic contamination Test biologically active samples as soon as possible Homogenize samples containing solids to assure representative samples Samples treated with sulfuric acid to a pH of less than 2 about 2 mL per liter and refrigerat
13. 8 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 4 Pour 25 mL of the solution into each of three round sample cells Hardness 30 Hardness E Procedures Calmagite Colorimetric Method 9 Wipe the second cell and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Mg as CaCO 10 Do not remove the cell from the instrument Record the results Press ESC In program choose Prog 29 HACH DR 890 29 DR 2010 2500 220 DR 4000 2010 Zero No PageDown 11 Press Zero 12 Wipe the third cell and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Mg as CaCO x Total hardness Ca as CaCO Mg as CaCO3 Hardness 31 Iron e Iron 0 009 1 300 mg L Fe Iron Method Smac Required Iron Reagent Solution Cat NO 12210 00 Reagents Strong chelants EDTA At all levels Cobalt May give slightly high results _ After Adding Iron Reagent Heat in a boiling water bath for 1 minute Hydroxides Rust Cool to 24 C before proceeding next step Retum the sample volume to O Pour 25mL of sample in 125mL flask Add the contents of Iron Reagent Solution and swir to mix Boil gently for 20 30 minutes Magnetite black iron Do not allow to boil dry A purple color will develop if iron is present oxide or Ferrites
14. Chromotropic Acid Method Cat NO 10413 00 Barium A negative interference at concentrations greater thanl mg L Chloride 0 Does not interfere below 1000 mg L A positive interference at concentrations greater than 12 mg L Nitrite Remove nitrite interference up to 100 mg L by adding 400mg of urea to 1OmL of sample swirl to dissolve Copper Positive at all levels Collect samples in clean plastic or glass bottles Store at 4 C 39 F or lower if the sample is to be analyzed within 24 to 48 hours Warm to room temperature before running the test For longer storage periods up to 14 days adjust sample pH to 2 or less with Concentrated Sulfuric Acid about 2 mL per liter Sample refrigeration is still required Before testing the stored sample warm to room temperature and neutralize with 5N NaOH solution Do not use mercury compounds as preservatives This test is technique sensitive Invert the vials as described here to avoid low results Hold the vial in a vertical position with the cap pointing up Tum the vial upside down Wait for all of the solution to flow down to the cap Pause Retum the vial to an upright position Wait for all the solution to flow to the bottom of the vial This process equals one inversion 43 Nitrate HR E Procedures Chromotropic Acid Method 1 Add 1 mL of sample to one Nitrate HR Chromotropic Acid Method Vial the prepared sample Add 1 mL of deionized water to another vial th
15. Enter 2 Add 1 mL of Sulfide Solution 1 reagent to each cell Swirl to mix Results will appear in mg L Ss 3 Add 1 mL of Sulfide Solution 2 reagent to each cell Cap and immediately inver to mix A 5 minute reaction period will begin 4 After choosing C MAC mode in the program choose Prog 93 1 C MAC Model HACH DR 890 93 DR 2010 2500 690 DR 4000 3500 Sulfide 94 Zinc ES Zinc 0 01 3 00 mg L Zn Zincon Method Smac Required Zinc reagent pillow Gem 13610 00 Reagents Cyclohexanone solution Aluminum _ Above 6 mg L Cadmium Above 0 5 mg L Copper _ Above 5 mg L Iron Ferric _ Above 7 mg L Interferences Manganese Above 5 mg L Nickel Above 5 mg L Organic material Large amounts may interfere Pretreat the sample with a mild digestion Highly buffer amp May exceed the buffering capacity of the reagents and require sample pretreatment Extreme e SS Sampling Collect samples in acid cleaned plastic or glass bottles If prompt analysis is impossible preserve the Storage sample by adjusting to pH 2 or less with nitric acid about 2 mL per liter amp Preserved samples may be stored up to six months at room temperature Before analysis adjust the pH Preservation to 4 5 with 5 0 N NaOH Do not exceed pH 5 as zinc may precipitate Digestion is required for determining total zinc Zinc Reagent contains cyanide and is very poisonous if taken intemally or if fumes are inhaled Do not add to an ac
16. L PO a negative 2 interference occurs Phosphate 3 e gt 75 mg L PO a negative 11 interference occurs Sulfides At all levels Collect samples in clean plastic bottles Analyze samples as soon as possible after collection If prompt analysis is not possible store samples at 4 C 39 F for up to 28 days Warm samples to room temperature before analyzing Occasionally a sample contains silica which reacts very slowly with molybdate The nature of these molybdate unreactive forms is not known A pretreatment with Sodium Bicarbonate then Sulfuric Acid will make these forms reactive to molybdate The pretreatment is given in Standard Methods for the Examination of Water and Wastewater under Silica Digestion with Sodium Bicarbonate A longer reaction time with the sample and the molybdate and acid reagents before adding citric acid may help instead of the bicarbonate treatment Sample temperature should be 15 25 C 59 77 F Silica 89 D Procedures Silica 1 Fill a sample cell with 10 mL of sample the prepared sample 2 Add the contents of one Molybdate Reagent Pillow to the sample cell Swirl until completely dissolved 3 Add the contents of one Acid Reagent Pillow for Silica to the sample cell Swirl to mix A yellow color will develop if silica or phosphorus is present A 10 minute reaction period will begin 4 Add the contents of one Citric Acid Pillow for Silica to the samp
17. Lead gt 260 IL Tin gt 6 mg L Collect samples in clean plastic or glass bottles Best results are obtained with immediate analysis Adjust sample pH to 2 or less with Concentrated Sulfuric Acid about 2 mL per liter Store at 4 C 39 F or less Preserved samples may be stored up to 28 days Warm the samples to room temperature and neutralize with 5N NaOH solution before analysis This test is technique sensitive Invert the vials as described here to avoid low results Hold the vial in a vertical position with the cap pointing up Turn the vial upside down Wait for all of the solution to flow down to the cap Pause Retum the vial to an upright position Wait for all the solution to flow to the bottom of the vial This process equals one inversion 65 Total Nitrogen TN HR E Procedures Chromotropic Acid Method 1 Add the contents of Total Nitrogen Persulfate Reagent Pillow to each Total Nitrogen Hydroxide Vial Wipe off any reagent that may get on the lid or the vial threads 5 Remove the caps from the digested vials and add the contents of one Total Nitrogen Reagent 1 Pillow to each vials 2 Add 0 5 mL of sample to one Ammonia Nitrogen LR Vial the prepared sample Add 0 5 mL of deionized water to another vial the blank 6 Cap the vials and shake for 15 seconds A 3 minute reaction period will begin 3 Cap vials and shake to dissolve vigorously for at least 30 seconds to mix The reagent may not dissol
18. TP HR oF ighiy EE en a SC E x ae E Se SS rr erentrs samples or extreme DH sample pretreatment Temperature Less than 18 C Greater than 25 C Fluoride thorium bismuth thiosulfate or thiocyanate Pyrophosphate tetraborate selenate benzoate citrate oxalate Other lactate tartrate salicylate Al Fe Mg Ca Baier Li Nat Kt NHa Ca Mn NO3z NO7 SO4 SO3 Pb Hg Hg sn Cu Ni Ag U Zu ASOs Br COs CIO4 CN Je SON Above 1000 mg L Collect samples in plastic or glass bottles that have been acid cleaned with 1 1 HCI and rinsed with deionized water Do not use commercial detergents containing phosphate for cleaning glassware used in this test Analyze samples immediately after collection for best results If prompt analysis is impossible samples may be preserved up to 28 days by adjusting the pH to 2 or less with sulfuric acid about 2 mL per liter and storing at 4 C Warm samples to room temperature and neutralize with 5N NaOH before analysis 85 D Procedures 1 Add 5 mL of sample to one Ammonia Nitrogen HR Vial the prepared sample Add 5 mL of deionized water to another vial the blank 2 Add the contents of TP Persulfate Reagent Pillow to each vial 3 Cap and mix to dissolve 4 Place the vials in the reactor preheated to 120 C Heat for exactly 30 minutes Place the hot vials into a rack from the reactor Cool the vials to room temperature Pho
19. a sample cell with 10 mL of deionized water the blank 6 After choosing C MAC mode in the program choose Prog 43 HACH DR 890 43 DR 2010 amp 2500 290 DR 4000 2260 2 Fill another sample cell with 10 mL of sample the prepared sample 7 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 3 Add the contents of one Ascorbic Acid Powder Pillow to each cell Cap and mix gently 8 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Mn 4 Add 15 drops of 0 6 mL akaline cyanide Reagent Solution to each cell Cap and mix gently A cloudy solution may form The turbidity should dissipate after step 5 Manganese LR 40 Manganese HR Manganese HR 0 2 20 0 mg L Mn Periodate Oxidation Method amac Required Buffer Pillow l Cat NO 12510 00 Reagents Sodium Periodate Pillow Calcium 700 mg L Chloride 70 000 mg L Iron 5 mg L Interferences _ ens Ki a Magnesium 100 000 mg L H Highly buffered samples or extreme sample pH may exceed the buffering capacity of the reagents and require sample pretreatment Sampling Collect samples in acid washed glass or plastic bottles Do not glass bottle Storage If samples are acidified adjust the pH 4 5 with 5N NaOH before analysis amp Preservation Do not exceed pH 5 as manganese may precipitate
20. 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 of perform a reagent blank adjust Rinse the sample cell and mixing cylinder immediately after use to remove all cadmium particles A deposit of unoxidized metal will remain after the Nitrate HR Reagent Pillow 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 49 D Procedures 1 C MAC Mode Nitrate HR 1 Fill a sample cell with 10 mL of sample the prepared sample 2 Add the contents of one Nitrate HR Reagent Pillow to the cylinder Stopper Shake the sample cell vigorously for 1 minutes A 5 minute reaction period will begin An amber color will develop if nitrate is present 3 Fill another sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 51 HACH DR 890 51 DR 2010 2500 355 DR 4000 2530 Nitrate HR Cadmium Reduction Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 6 Within 1 minutes after the timer beeps Wipe the prepared sample and place it into the cell holder Place the cover on th
21. and place it into the cell holder Place the cover on the sample cell Press Zero 3 Pour 25 mL of the mixture into a 25 mL sample cell This is the prepared sample 8 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L A 4 Add the contents of one Bleaching Reagent Pillow to the remaining 25mL in the cylinder Stopper Shake for 30 seconds vigorously Aluminum 2 C mac Bromine Bromine Bromine 0 05 4 50 mg L Bro DPD a Required Reagents Interferences Sampling Storage 8 Preservation Tips 8 Techniques lodine At all levels DPD Free Chlorine Reagent Pillow Cat NO 11010 00 Acidity l Greater than 150 mg L as CaCO Neutralize with 1N NaOH Alkalinity Greater than 250 mg L as CaCO Neutralize with 1N H504 Chlorine Chlorine Dioxide At all levels chloramine organie May mtema EA After adjusting sample pH to 6 7 add 3 drops KI 30g L to a 25mL sample Mix and wait 1 minute Add 3 drops sodium arsenite 5g L and mix Analyze 10mL of the treated sample Substract the result from this test from the original analysis to obtain the correct bromine concentration 1112 Mn Mn or Cre Monochloramine Ozone At all levels TOD a A A Extreme sample pH or highly buffered samples Neutralize to pH 6 7 Collect samples in clean dry glass containers If sampling from a tap allow
22. be diluted If sample dilution will cause the COD concentration to be too low for accurate determination add 0 5 g Ont mercuric sulfate to each COD Vial before the sample is added Maximum cr Suggested cr of When 0 59 HgSO4 added mg L diluted samples mg L Maximum CT mg L ULR 2000 1000 NA LR HR E 2000 1000 LR 8000 HR 2000 Collect samples in glass bottles Use plastic bottles only if they are known to be free of organic contamination Test biologically active samples as soon as possible Homogenize samples containing solids to assure representative samples Samples treated with sulfuric acid to a pH of less than 2 about 2 mL per liter and refrigerated at 4 C can be stored up to 28 days Some of the chemicals and apparatus used in this procedure may be hazardous to the health and safety of the user if inappropriately handled or accidentally misused Wear appropriate eye protection and clothing for adequate user protection If contact occurs flush the affected area with running water Place a safety shield in front of the COD reactor to prevent injury if splattering occurs The reagent mixture is light sensitive Keep unused vials in the opaque shipping container Refrigerate if possible Spilled reagent will affect test accuracy and is hazardous to skin and other materials Wash spills with running water Run one blank with each set of samples Run all tests the samples and the blank with the same lot of vials For greater a
23. reagent addition 3mg L monochloramine Monochloramine E i e causes less than a 0 1 mg L increase in the reading Ozone At all levels Peroxides _ May interfere Extreme sample pH or Neutralize to pH 6 7 with 1N H gt S0O4 or 1N NaOH highly buffered samples S ES Avoid plastic containers Pretreat glass sample containers to remove any chlorine demand by soaking in a dilute bleach solution Bleach 1mL per liter for at least 1hour Rinse thoroughly with deionized or distilled water If sampling from a tap allow the water to flow at least 5minutes to ensure a representative sample Allow several volumes of water to overflow the container and cap the container so there is no headspace above the sample Analyze samples immediately Do not preserve Sampling Storage amp Preservation Chlorine Total 7 Chlorine Total E Procedures DPD Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 1 Fill a sample cell with 10 mL of sample the prepared sample 6 Within 3 minutes after the timer beep wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Ch 2 Add the contents of one DPD Total Chlorine Reagent Pillow to the sample cell Swirl the sample cell for 20 seconds to mix A 3 minute reaction period will begin Perform next steps during this period 3 Fill a secon
24. tele KEIER 65 Oxygen Demand Chemical CODcr ULR Reactor Digest 69 Oxygen Demand Chemical CODcr LR Recto Ee ee EE 71 Oxygen Demand Chemical CODcr HR Reactor Jee Eege EE 73 Oxygen Demand Chemical CODcr UHR REACO DIGESUONS EE 75 Phosphorus Reactive Orthophosphate LR Le Te WEE ET 77 Phosphorus Reactive Orthophosphate HR Gel uge Tat 79 Phosphorus Total TP LR tie WE ELE ii A a e 81 Phosphorus Total TP HR MOIM ONENE ate capo ets rane e ne Sac eees Seana eee 85 Silica SiC OMOly Date sires cascevss ues a plemented o s 89 Sulfate SS LN Feet re o NI eC yD ED TED ec A EE 91 Sulfide Methylene Blin eege 93 Zinc GEELEN 95 Procedures Aluminum e Aluminum 0 008 0 800 mg L AUT Aluminon Method Mac Aluminum Reagent Pillow Ascrobic Acid Pillow Cat NO 10810 00 Bleaching Reagent Pillow Required Reagents l If greater than 300 mg L acidity as CaCO3 Add one drop of m Nitrophenol Indicator Solution and 5N NaOH Solution to the sample Invert to mix Repeat as often as necessary until the color changes from colorless to yellow Add one drop of 5 25 N Sulfuric Acid Standard Solution to change the solution from yellow back to colorless Acidity 1000 mg L as CaCO Add one drop of m Nitrophenol Indicator Solution to the sample Alkalinity l A yellow color indicates excessive alkalinity Add one drop of 5 25 N Sulfuric Acid Standard Interferences Solution to change the solution from yellow back to colorless
25. the blank 4 After choosing C MAC mode in the program choose Prog 37 HACH DR 890 37 DR 2010 amp 2500 260 DR 4000 2175 Iron Iron Method Zerolo i it i L 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell 6 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Fe 34 Iron Ferrous Iron Ferrous 0 02 3 00 mg L Fe 1 10 Phenanthroline Method Mac Required Ferrous Iron Reagent Pillow Cat NO 12310 00 Reagents Sampling Storage Collect samples in plastic or glass bottles Analyze samples as soon as amp Preservation possible after collection For more accurate results determine a reagent blank value for each new lot Tips of reagent Follow the procedure using deionized water in place of the sample Subtract the reagent blank value from the final results of perform Techniques a reagent blank adjust Iron Ferrous 35 D Procedures 1 C MAC Mode iron Ferrous 1 Fill a sample cell with 25 mL of sample the prepared sample 2 Add the contents of one Ferrous Iron Reagent Pillow to the sample cell Cap and mix A 3 minute reacition period will begin An orange color will develop if Ferrous Iron is present 3 Fill another sample cell with 25 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog
26. the water to flow at least 5minutes to ensure a representative sample Avoid excessive agitation and exposure to sunlight Allow several volumes of water to overflow the container and cap the container so there is no headspace above the sample Analyze samples immediately Do not preserve If the samples temporarily turns yellow after reagent addition dilute a fresh sample and repeat 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 of perform a reagent blank adjust Bromine E Procedures DPD Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 1 Fill a sample cell with 10 mL of sample 2 Add the contents of one DPD Free Chlorine Reagent Pillow to the sample cell the prepared sample Stopper Invert to dissolve the powder A 3 minute reaction period will begin A pink color will develop if Bromine is present 6 Within 3 minutes after the timer beep wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Br 3 Fill a second sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 4 1 C MAC Mode HACH DR 890 4 DR 2010 amp 2500 50 DR 4000 1300
27. velocity 2 3 mL min Collecting the distillate at 100 mL mass cylinder filled with 2 NaOH 20mL until volume is 90 mL Seperate the condenser and rinse the inside of condeser with deionized water Dillute to 100 mL 22 Cyanide E Procedures Pyridine Pyrazalone Method 1 Using a graduated cylinder fill a round sample cell with a 10 mL of sample the prepared sample 5 Fill another round sample cell with 10 mL of sample The blank 6 After choosing C MAC mode in the program choose Prog 23 HACH DR 890 23 DR 2010 2500 160 DR 4000 1750 2 Add the contents Cyanide 1 Reagent Pillow Cap and shake for 30 seconds Leave the sample cell undisturbed for an additional 30 seconds 3 Add the contents Cyanide 2 Reagent Pillow Cap and shake for 10 seconds Immediately proceed to next step Delaying the addition of the Cyanide 2 reagent will produce low test results 7 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 4 Add the contents Cyanide 3 Reagent Pillow Cap and shake vigorously A 30 minute reation period will begin If cyanide is present the solution will tum from pink to blue 8 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L CN Cyanide 23 Cyanuric Acid Cyanuric Acid 5 50 mg L Cyan Acid Turbidimetric Method mac
28. 0 should be done on the sample Pretreat the nitrate nitrogen sample with the following Nitrite pretreatment Then subtract the amount of nitrite found from the results of the NO2 N LR Test Add 30 g L Bromine Water dropwise to the sample in step 2 until a yellow color remains Mix after each drop Add one drop of 30 g L Phenol Solution to destroy the color oH Highly buffered samples or extreme sample pH may exceed the buffering capacity of the reagents and require sample pretreatment 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 2mL of sulfuric acid per liter and store at 4 C Before analysis warm the sample to room temperature and adjust the pH to 7 with 5N NaOH solution Do not use mercury compounds as preservatives 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 of perform a reagent blank adjust Rinse the sample cell and mixing cylinder immediately after use to remove all cadmium particles A deposit of unoxidized metal will remain after the Nitrate LR Reagent Pillow dissolves The deposit will not affect results Shaking time and technique influence color development Anal
29. 00 Collect samples in glass bottles Use plastic bottles only if they are known to be free of organic contamination Test biologically active samples as soon as possible Homogenize samples containing solids to assure representative samples Samples treated with sulfuric acid to a pH of less than 2 about 2 mL per liter and refrigerated at 4 C can be stored up to 28 days Some of the chemicals and apparatus used in this procedure may be hazardous to the health and safety of the user if inappropriately handled or accidentally misused Wear appropriate eye protection and clothing for adequate user protection If contact occurs flush the affected area with running water Place a safety shield in front of the COD reactor to prevent injury if splattering occurs The reagent mixture is light sensitive Keep unused vials in the opaque shipping container Refrigerate if possible Spilled reagent will affect test accuracy and is hazardous to skin and other materials Wash spills with running water Run one blank with each set of samples Run all tests the samples and the blank with the same lot of vials For greater accuracy analyze a minimum of three replicates and average the results Oxygen Demand Chemical CODc HR 73 D Procedures 1 Hold one vial at a 45 degree angle Add 2 mL of sample to vial the prepared sample Hold one vial at a 45 degree angle Add 2 mL of deionized water to vial the blank 2 Cap the vials tightl
30. 0mL of sample 2 Add the contents of one Zinc Reagent Pillow to the cylinder Stopper Invert several times to dissolve the powder completely Inconsistently readings may result for low zinc concentrations if all the particles are not dissolved 3 Pour 10 mL of the solution into a sample cell the blank 4 Add 0 5 mL of Cyclohexanone solution to the remaining solution in the cylinder A 30 second reaction period will begin During the reaction period stopper the cylinder and shake vigorously Zinc Zincon Method 5 A 30 second reaction period will begin Pour the solution from cylinder into a sample cell the prepared sample 6 After choosing C MAC mode in the program choose Prog 97 HACH DR 890 97 DR 2010 2500 780 DR 4000 3850 7 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 8 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Zn 97
31. 33 HACH DR 890 33 DR 2010 2500 255 DR 4000 2150 Iron Ferrous 1 10 Phenanthroline Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 6 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Fe 36 Iron Total A Iron Total 0 02 3 00 mg L Fe Total Iron GH amac Required Total Iron Reagent Pillow Cat NO 12410 00 Reagents Ca No effect at less than 10 000 mg L as CaCO3 cr No effect at less than 185 000 mg L High Iron Levels Inhibit color development Dilute sample and re test to verify results Iron Oxides _ After mild vigorous digestion adjust sample to pH 3 5 with NaOH Solution Magnesium _No effect at 10 000 mg L as CaCO3 Molybdate Molybdenum No effect at 50 mg L as Mo Interferences Treat in fume hood or well ventilated area Add 5 mL HCI to 100mL sample ina High Sulfide Levels 250mL Erlenmeyer flask Boil 20 minutes and cool Adjust pH to 3 5 with NaOH Solution Readjust volume to 100mL with deionized water Add 0 1 g scoop of Rust Remover to the blank Swirl to mix Zero the instrument Turbidity with this blank If sample remains turbid add three 0 2 g scoops of Rust Remover to a 75 mL sample Let stand 5 minutes Filter through a glass membrane filter Extreme sample pH or f a i Adjust pH to 3 5 highly buffered samples Se Collect samples i
32. C MAC Test kit User s Manual WwWw c mac net a C MAC Co Procedures A Procedures mac ITEM METHOD PAGE Aluminum AUMIA 23 tats se Eden a same 1 Bromine DD sara aa ate oes ace ae ee aera hens ee ators Ua acters ct Tee dao ace ect Baul Rare Ace ce a 3 Chlorine Free DPD recta te teccc ct EE EE EE cae ake 5 Chlorine Total Big Base apa EE UNG Ary EH 7 Chlorine Dioxide DPD tic ti ide as cs ica 9 Chrome Hexavalent NN ele e eM eee ee eee 11 Chrome Total Alkaline Hypobromite Oxidation ci ete a RRE Eeer es aoe ae 13 Copper BICING MONIMALG He ca giscet el ce aelece EE es aos 17 Copper ROTA SL A VI 19 Cyanide EMO EE EE EEN 21 Cyanuric Acid RU eeng une 25 Fluoride O A eee E ES EEA P AE EEEE 27 Hardness Calmagite Colorimetric senian A EE 29 Iron et EE EE Ee 33 Iron Ferrous 1 10 Phenanthroline 2brt nan nan nro nanna nana na nnanannananaananaanananass 35 Iron Total A len EE 37 Manganese LR PAN ico 39 Manganese HR HEET EE R 41 Nitrate HR Chromotropic ACI as ios Ee Ze lad bide aaah 43 Procedures Procedures ITEM METHOD PAGE CA Nitrate LR Cadmium REQUCHON cin etsinnes 45 Nitrate MR SAMURAI 47 Nitrate HR Cadmium REGUCHONE 2275d cos4 s0006anets ensaneeaneed opero rr tt 49 Nitrite LR BIER le eoosal 51 Nitrite LR Diazotization Test Kit 53 Nitrite HR PAKNE A EE 55 Nitrogen Ammonia LR SMN a al du ed 57 Nitrogen Ammonia HR A EE eee es 59 Nitrogen Total TN LR Acid Perl lA TEE 61 Nitrogen Total TN HR
33. For turbid samples prepare a sulide free blank as follows Use it in place of the deionized water blank in the procedure 1 Measure 25 mL of sample into a 50 mL Erlenmeyer flask Turbidity 2 Add Bromine Water dropwise with constant swirling until a permanent yellow color just appears 3 Add Phenol Solution dropwise until the yellow color just disappears Use this solution to replace the deionized water Collect samples in clean plastic or glass bottles Fill completely and cap tightly Avoid excessive agitation or prolonged exposure to air Analyze samples immediately Analyze samples immediately Do not preserve for later analysis Avoid excessive agitation of samples to minimize sulfide loss Some sulfide loss may occur if dilution is necessary Determine soluble sulfides by centrifuging the sample in completely filled capped tubes and analyzing the supematant Insoluble sulfides are then estimated by subtracting the soluble sulfide concentration from the total sulfide result 93 Sulfide E Procedures Methylene Blue Method 1 Avoid excessive agitation of the sample use a pipet add 25 mL of sample to a sample cell the prepared sample use a pipet add 25 mL of deionized water to a second sample cell the blank 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell a Press Zero 6 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press
34. N Pyridine Pyrazalone Method Mac Cyanide 1 Reagent Pillow Required es Ge Cyanide 2 Reagent Pillow Cat NO 11810 00 S Cyanide 3 Reagent Pillow Large amounts of chlorine in the sample will cause a milky white precipitate after the addition of the Cyanide 3 Chlorine reagent If chlorine or other oxidizing agents are known to be present pretreat the sample before testing using the l procedure in this table for oxidizing agents Ni or Co up to i mg L do not interfere Eliminate the interference from up to 20 mg L Cu and ZS mg L ir iron a by adding _ Metals the contents of one Chelating Reagent Powder Pillow to the sample and then mixing before adding Cyanide 1 Reagent g Powder Pillow Prepare a reagent blank of deionized water and reagents to zero the instrument D Adjust a 25 mL portion of the alkaline sample to pH 7 9 with 2 5 N HCI Standard Solution Count the number of drops of acid added Add 2 drops of KI Solution and 2 drops of Starch Indicator Solution to the sample Oxidizing Swirl to mix The sample will turn blue if oxidizing agents are present Add Sodium Arsenite Solution drop wise until the sample tums colorless Agents p Swirl the sample thoroughly after each drop Count the number of drops g Take another 25 mL sample and add the total number of drops of HCI Standard Solution counted in step Interferences Subtract one drop from the amount of Sodium Arsenite Solution added in step Add this amount to the s
35. SE S a EES EE aan SE NN E drop wise until a permanent yellow color appears Add phenol solution drop wise until the yellow color disappears Sulfide Collect samples in plastic or glass bottles that have been acid cleaned with 1 1 HCI and rinsed with deionized water Do not use commercial detergents containing phosphate for cleaning glassware used in this test Analyze samples immediately after collection for best results If prompt analysis is impossible samples may be preserved up to 28 days by adjusting the pH to 2 or less with sulfuric acid about 2 mL per liter and storing at 4 C Warm samples to room temperature and neutralize with 5N NaOH before analysis Store the PO P LR reagent pillows in a cool dry environment Place a safety shield in front of the COD reactor to prevent injury if splattering occurs Final samples will contain molybdenum and have a pH less than 2 and are considered corrosive 81 Total Phosphorus TP LR E Procedures Acid Persulfate Method 5 Add 2 mL of TP Solution 1 to the 1 Add 5 mL of sample to a vial vial 2 Add the contents of one TP Persulfate 6 Cap and invert to mix Reagent Pillow to the vial P 7 After choosing C MAC mode in the program choose Prog 82 HACH DR 890 82 DR 2010 535 DR 2500 536 DR 4000 3036 3 Cap tightly and shake to dissolve 4 Place the vials in the reactor preheated to 120 C Heat for exactly 30 minutes Place the hot vials i
36. agent solution Cat NO 13310 00 Alkalinity as CaCO 0 At 5000 mg L it causes a 0 1 mg L F error At 0 1 mg L it causes a 0 1 mg L F error To check for interferences from aluminum read the concentration one minute after reagent addition then again Aluminum after 15 minutes An appreciable increase in concentration suggests aluminum interference Waiting 2 hours before making the final reading will eliminate the effect of up to 3 0 mg L aluminum Chloride At 7000 mg L it causes a 0 1 mg L F error SPADNS Reagent contains enough arsenite to eliminate interference up Chlorine to 5 mg L chlorine For higher chlorine levels add one drop of Sodium Arsenite Solution to 25 mL of sample for each 2 mg L of Chlorine Iron Ferric At 10 mg L it causes a 0 1 mg L F error Phosphate ortho At 16 mg L it causes a 0 1 mg L F error Sodium Hexameta Ar 1 0 mg L it causes a 0 1 mg L F error phosphate Sulfate AE 200 mg L it causes a 0 1 mg L F eror Samples may be stored in glass or plastic bottles for at least seven days when cooled to 4 C 39 F or lower Warm samples to room temperature before analysis Distillation is required Interference is eliminated mostly in this procedure The sample and deionized water should be at the same temperature 1 C Temperature adjustments may be made before or after reagent addition Fluoride reagent solution is toxic and corrosive 27 Fluoride E Procedures SPADNS Method 5
37. ample Subtract the reagent blank value from the final results of perform a reagent blank adjust Rinse the sample cell and mixing cylinder immediately after use to remove all cadmium particles A deposit of unoxidized metal will remain after the Nitrate MR Reagent Pillow 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 47 D Procedures 1 C MAC Mode Nitrate MR 1 Fill a sample cell with 10 mL of sample the prepared sample 2 Add the contents of one Nitrate MR Reagent Pillow to the cylinder Stopper Shake the sample cell vigorously for 1 minutes A 5 minute reaction period will begin An amber color will develop if nitrate is present 3 Fill another sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 54 HACH DR 890 54 DR 2010 2500 353 DR 4000 2520 Nitrate MR Cadmium Reduction Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 6 Within 2 minutes after the timer beeps Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell i Press Enter Results will appear in mg L NOs N 48 Cra Required Reagents Interferences Sampling Stora
38. ample e and mix x thoroughly Continue with step of the cyanide procedure O Adjust a 25 mL portion of the alkaline sample to pH 7 9 with 2 5 N HCI Standard Solution E Count the number of drops of acid added 0 Add 4 drops of KI Solution and 4 drops of Starch Indicator Solution to the sample Swirl to mix The sample should be colorless Reducin d Add Bromine Water drop wise until a blue color appears Swirl the sample thoroughly after Agen each addition Count the number of drops 0 Take another 25 mL sample and add the total number of drops of HCI Acid Standard Solution counted in step O Add the total number of drops of Bromine Water counted in step c to the sample and mix E thoroughly Continue with Sien of the cyanide procedure Turbidity Large amounts of turbidity will cause high readings Use filter paper and a funnel to filter highly _ turbid water samples The test results should then be recorded as soluble cyanide Cyanide 21 Tips Techniques Sampling Storage 8 Preservation Acid Distillation Cyanide Cyanide Use a water bath to maintain the optimum temperature for the reaction in this test 25 C Samples at less than 23 C require longer reaction times and samples at greater than 25 C yield low results longer reaction times and samples at greater than 25 C yield low results water in place of the sample Subtract the reagent blank value from the final results or perform a rea
39. ampling Storage amp Preservation Chlorine Free 5 Chlorine Free E Procedures DPD Method 5 Add the contents of one DPD Free Chlorine Reagent Pillow to the sample cell the prepared sample Swirl the sample cell for 20 seconds to mix 1 Fill a sample cell with 10 mL of sample the blank 6 Within 1 minute of adding the reagent wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Ch 2 After choosing C MAC mode in the program choose Prog 9 1 C MAC Model HACH DR 890 9 DR 2010 amp 2500 80 DR 4000 1450 e 3 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 4 Fill a second sample cell with 10 mL of sample Chlorine Free 6 Chlorine Total e Chlorine Total 0 02 2 00 mg L Cle DPD Method mac Required DPD Total Chlorine Reagent Pillow Cat NO 11310 00 Reagents EE ias A O O t No effect at less than 1 000 mg L as CaCO OOO yg aaa Chloramines organic e Hardness After adjusting sample pH to 6 7 add 3 drops KI 30g L to a 25mL sample Mix and wait 1 minute Add 3 drops sodium arsenite 5g L and mix Analyze 10mL of the treated sample Substract the result from this test from the original analysis to obtain the correct bromine concentration Interferences Mi Mear Cro When read within 1 minutes after
40. ank value from the final results of perform a reagent blank adjust Chromium Hexavalent 11 D Procedures 1 Fill a sample cell with 10 mL of sample the prepared sample 2 Add the contents of one Chromium 3 Reagent Pillow to the sample cell Cap and invert gently to mix A 5 minute reaction period will begin A purple color will form if hexavlent chromium is present 3 Fill a second sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 13 C MAC Mode HacH DR 890 13 DR 2010 2500 90 DR 4000 1560 Chromium Hexavalent Chromium Hexavalent 1 5 Diphenylcarbohydrazide Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 6 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Cr 12 Chromium Total e Chromium Total 0 01 0 60 mg L Cr Alkaline Hypobromite Oxidation Pied Smac Acid Reagent Pillow Required Chromium 3 Reagent Pillow l Cat NO 11520 00 Reagents Chromium 1 Reagent Pillow Chromium 2 Reagent Pillow Extreme sample pH or may exceed the buffering capacity of the reagents and require highly buffered samples sample pretreatment May inhibit complete oxidation of trivalent chromium Interferences Organic material f i 5 WEN If high levels of organic materia
41. ar in mg L NH3 N 2 Add the contents of Ammonia Reagent 1 Pillow to each vial a Cap vials and shake to dissolve Add the contents of Ammonia Reagent 2 Pillow to each vial Cap vials and shake to dissolve A 20 minute reaction period will begin A green color will develop if ammonia is present 4 After choosing C MAC mode in the program choose Prog 66 1 C MAC Model HACH DR 890 66 DR 2010 2500 342 DR 4000 2460 Nitrogen Ammonia LR 58 Nitrogen Ammonia HR e Nitrogen Ammonia HR 0 4 50 0 mg L NHa N Salicylate Method l mac Required Reagents Interferences Sampling Storage amp Preservation Tips amp Techniques Ammonia Nitrogen HR Vial Salicylate Method Ammonia Reagent Pillow 1 Cat NO 10333 00 Ammonia Reagent Pillow 2 Calcium 50 000 mg L as CaCO3 Iron Blank with ammonia free water of the same iron concentration Magnesium 300 000 mg L as CaCO3 Nitrite 600 mg L as NO2 N Nitrate 5 000 mg L as NOs N Orthophosphate 0 5 000 mg L as PO P pH Use 1N NaOH solution for acidic samples and 1N HCI solution for basic samples Sulfate 6 000 mg L as SO Sulfide 0 Add the contents of one Sulfide Inhibitor Reagent Pillow Swin to mix Filter Other Hydrazine glycine turbidity color Distillate Collect samples in clean plastic or glass bottles Best results are obtained with immediate analysis If chlorine is known to be present add one drop of 0 1N Sodium
42. ccuracy analyze a minimum of three replicates and average the results Oxygen Demand Chemical CODcr UHR 73 D Procedures 1 Hold one vial at a 45 degree angle Add 0 2 mL of sample to vial the prepared sample Hold one vial at a 45 degree angle Add 0 2 mL of deionized water to vial the blank 2 Cap the vials tightly Rinse them with deionized water and wipe with a clean paper towel Hold the vials by the cap over a sink Invert gently several times to mix The samples vials will becoming very hot during mixing 3 Place the vials in the COD reactor preheated to 150 C Heat for 2 hours Tum the reactor off Wait about 20 minutes for the vials to cool to 120 C or less 4 Invert each vials several times while still warm Place the vials into a rack and cool to room temperature Oxygen Demand Chemical CODcr UHR Chemical Oxygen Demand CODc UHR Reactor Digestion Method 5 After choosing C MAC mode in the program choose Prog 17 1 C MAC Model HACH DR 890 17 DR 2010 2500 435 DR 4000 2720 6 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks 7 Place the blank into the cell holder Place the cover on the vial Press Zero 8 Place prepared sample into the cell holder Place the cover on the vial Press Enter Results will appear in mg L COD Multiply the result by 10 76 Phosphorus Reactive
43. d sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 9 1 C MAC Model HacH DR 890 9 DR 2010 2500 80 DR 4000 1450 Chlorine Total 8 Chlorine Dioxide C Chlorine Dioxide 0 04 5 00 mg L CIO DPD Method Smac Required DPD Free Chlorine Reagent Pillow i Cat NO 11430 00 Reagents Glycine Reagent Acidity Greater than 150 mg L CaCOz C t Greater than 2 mg L Alkalinity Greater than 250 mg L CaCO3 Copper Greater than 10 mg L Metals _ Nickel Greater than 50 mg L Cl 0 6mg L l Other metals may also interfere Chlorine Greater than 6 mg L add more glycine Bromine At all levels Chloramines organic At all levels When read within 1 minutes after reagent Interferences Flocculating agents E Greater than Al SO4 3 500 mg L Monochloramine addition 3mg L monochloramine causes Cl 0 6mg L Greater than FeCl 200 mg L less than a 0 1 mg L increase in the reading E EE SE CaCO3 lodine At all levels Peroxides l At all levels Hardness Ozone Greater than 1 5mg L pe a er PER Neutralize to pH 6 7 ar Do At all levels l Ma Mn highly buffered samples Sampling Avoid plastic containers Pretreat glass sample containers to remove any chlorine demand by soaking in a dilute bleach solution Storage Bleach 1mL per liter for at least 1hour Rinse thoroughly with deionized or distilled water If sampling from a tap allow the amp water to f
44. e blank 5 After choosing C MAC mode in the program choose Prog 57 HACH DR 890 57 DR 2010 amp 2500 344 DR 4000 2511 ero i Pe 6 Wipe the blank and place it into the ho cell holder Place the cover on the vial Al Press Zero 7 Within 5 minutes wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appear in mg L NOs N 2 Cap vials and invert 10 times to mix 3 Add the contents of Nitrate Chromotropic Acid Method Reagent Pillow to each vial 4 Cap vials and invert 10 times to mix Some solid matter will not dissolve A 5 minute reaction period will begin Do not invert the vial again A yellow color will develop if Nitrate Nitrogen is present Nitrate HR 44 CA Required Reagents Interferences Sampling Storage Preservation Tips amp Techniques Nitrate LR Nitrate LR Nitrate LR 0 01 0 50 mg L NOz3 N Cadmium Reduction Method l D Nitrate LR Reagent Pillow Cadmium Reduction Method Cat NO 10422 11 Nitrite LR Reagent Pillow Calcium 100 mg L Sue Concentrations Above 100 mg L will cause low results The test may be used at seawater but l a Calibration must be done using standards spiked to the same chloride concentration Ferric iron At all levels At all levels This method measures both the nitrate and nitrite in the sample If nitrite is present NO2 N LR Test Prog 6
45. e buffering capacity of the reagents and require samples or extreme pH sample pretreatment Temperature Less than 18 C Greater than 25 C Fluoride thorium bismuth thiosulfate or thiocyanate Pyrophosphate tetraborate selenate benzoate citrate oxalate Other lactate tartrate salicylate Al Fe Mg Ca Ba t Srt Lit Nat K NH4 Cd Mn7 NO3 NO SOa SO3 Pb Hg Hg Sn Cu Ni Ag U Zn AsO3 Br CO3 ClO4 CN JO SIO4 Above 1000 mg L Collect samples in plastic or glass bottles that have been acid cleaned with 1 1 HCI and rinsed with deionized water Do not use commercial detergents containing phosphate for cleaning glassware used in this test Analyze samples immediately after collection for best results If prompt analysis is impossible samples may be preserved up to 28 days by adjusting the pH to 2 or less with sulfuric acid about 2 mL per liter and storing at 4 C Warm samples to room temperature and neutralize with 5N NaOH before analysis Phosphorus Reactive Orthophosphate HR 79 D Procedures 1 Add 5 mL of sample to one Ammonia Nitrogen HR Vial the prepared sample Add 5 mL of deionized water to another vial the blank 2 Cap and mix A 3 minute reaction period will begin A 7 minute reaction time is for samples at 23 C For samples at 13 C wait 15 minutes For samples at 33 C wait 2 minutes Read the sample within 2 minutes after the timer beeps 3 After c
46. e contents of one PO P LR Reagent Pillow to the vial Cap and shake for 10 15 seconds The powder will not dissolve completely A 2 minute reaction period will begin Read samples between 2 and 8 minutes after adding the reagent 1 After choosing C MAC mode in the program choose Prog 82 HACH DR 890 82 DR 2010 amp 2500 535 DR 4000 3035 6 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks 2 Add 5 mL of sample to a vial Cap and mix 7 Wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appear in mg L P Generally chemical fom of hach spectrophotometer is PO4 3 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks 4 Wipe the blank and place it into the cell holder Place the cover on the vial Press Zero Phosphorus Reactive Orthophosphate LR 78 Phosphorus Reactive Orthophosphate HR Phosphorus Reactive HR H 1 0 100 mg L PO 0 4 30 0 mg L P Gx Molybdovanadate Method Required Reagents Interferences Sampling Storage amp Preservation Phosphorus Vial TP Solution 2 Cat NO 10723 00 Arsenate Only interferes if the sample is heated ao ee Molybdate Above 1000 mg L negative inteference Silica Only interferes if the sample is heated Highly buffered May exceed th
47. e sample cell i Press Enter Results will appear in mg L NOs N 30 Nitrite LR AA Mac Nitrite LR 0 002 0 350 mg L NOe N Diazotization Method Required Nitrite LR Reagent Pillow Cat NO 10512 00 Reagents Aluminous ions Auric ions L a ae Ge Sa S e SES A S S Sg e E Mercurous ions Metavanadate ions Interferences Silver ions Cupric ions Ferrous ions 0 Cause low results E ea on oa Fee a a T i At all levels highly buffered samples Sampling Collect samples in clean plastic or glass bottles Store at 4 C 30 F or lower if the Storage sample is to be analyzed within 24 to 48 hours Warm to room temperature before running amp Preservation the test Do not use acid preservatives Tips For more accurate results determine a reagent blank value for each new lot of reagent amp Follow the procedure using deionized water in place of the sample Subtract the reagent Techniques blank value from the final results of perform a reagent blank adjust Nitrite LR 51 D Procedures 1 Fill a sample cell with 10 mL of sample the prepared sample 2 Add the contents of one Nitrite LR Reagent Pillow Cap and shake to dissolve A pink color will develop if nitrite is present A 20 minutes reaction period will begin 3 Fill another sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 60 C MAC Model HacH DR 890 60 DR 2010 2500
48. ed at 4 C can be stored up to 28 days Some of the chemicals and apparatus used in this procedure may be hazardous to the health and safety of the user if inappropriately handled or accidentally misused Wear appropriate eye protection and clothing for adequate user protection If contact occurs flush the affected area with running water Place a safety shield in front of the COD reactor to prevent injury if splattering occurs The reagent mixture is light sensitive Keep unused vials in the opaque shipping container Refrigerate if possible Spilled reagent will affect test accuracy and is hazardous to skin and other materials Wash spills with running water Run one blank with each set of samples Run all tests the samples and the blank with the same lot of vials For greater accuracy analyze a minimum of three replicates and average the results Oxygen Demand Chemical CODcr LR 71 D Procedures 1 Hold one vial at a 45 degree angle Add 2 mL of sample to vial the prepared sample Hold one vial at a 45 degree angle Add 2 mL of deionized water to vial the blank 2 Cap the vials tightly Rinse them with deionized water and wipe with a clean paper towel Hold the vials by the cap over a sink Invert gently several times to mix The samples vials will becoming very hot during mixing 3 Place the vials in the COD reactor preheated to 150 C Heat for 2 hours Tum the reactor off Wait about 20 minutes for the vial
49. epared sample Add 2 mL of digested treated reagent blank to the second Total Nitrogen Acid Solution Vial the blank 13 Wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appear in mg L N 10 Cap vials and invert 10 times to mix Use slow deliberate inversions for complete recovery The vials will be wam A 5 minute reaction period will begin The yellow color will intensify 11 After choosing C MAC mode in the program choose Prog 58 1 C MAC Modef HACH DR 890 58 DR 2010 2500 350 DR 4000 2558 12 Wipe the blank and place it into the cell holder Place the cover on the vial Press Zero Nitrogen Total TN LR 63 Total Nitrogen TN HR Nitrogen Total TN HR 10 150 mg L N Chromotropic Acid Method l Required Reagents Interferences Sampling Storage amp Preservation Tips amp Techniques Nitrogen Total TN HR Chloride Total Nitrogen Hydroxide Vial Total Nitrogen Persulfate Reagent Pillow Total Nitrogen Acid Solution Vial Cat NO 10213 00 Total Nitrogen Reagent 1 Pillow Total Nitrogen Reagent 2 Pillow Barium gt 10 mg L Magnesium gt 2000 mg L Bromide gt 240 mg L Positive Organic carbon gt 600 mg L Calcium gt 1200 mg L pH gt 13 gt 3000 mg L Positive Phosphorus gt 400 mg L Chromium gt 2 mg L Silica gt 600 mg L Iron gt 8 mg L Silver gt 3 mg L
50. ge 8 Preservation Tips amp Techniques Nitrate HR Nitrate HR Nitrate HR 0 3 30 0 mg L NOz3 N Cadmium Reduction Method l Nitrate HR Reagent Pillow Cadmium Reduction Method Cat NO 10424 11 Calcium 100 mg L Concentrations Above 100 mg L will cause low results The test may be used at seawater but Chloride e E f f a calibration must be done using standards spiked to the same chloride concentration Ferric iron At all levels At all levels This method measures both the nitrate and nitrite in the sample If nitrite is present NO2 N LR Test Prog 60 should be done on the sample Pretreat the nitrate nitrogen sample with the following Nitrite pretreatment Then subtract the amount of nitrite found from the results of the NO2 N LR Test E Add 30 g L Bromine Water dropwise to the sample in step 2 until a yellow color remains Mix after each drop Add one drop of 30 g L Phenol Solution to destroy the color Le E ee require sample pretreatment 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 2mL of sulfuric acid per liter and store at 4 C Before analysis wam the sample to room temperature and adjust the pH to 7 with 5N NaOH solution Do not use mercury compounds as preservatives For more
51. gen Total TN LR 3 0 25 0 mg L N Chromotropic Acid Method Cac Required Reagents Interferences Sampling Storage amp Preservation Tips amp Techniques Nitrogen Total TN LR Total Nitrogen Hydroxide Vial Bromide Chloride Total Nitrogen Persulfate Reagent Pillow Total Nitrogen Acid Solution Vial Total Nitrogen Reagent 1 Pillow Total Nitrogen Reagent 2 Pillow Cat NO 10212 00 Barium gt 2 6 mg L Magnesium gt 500 mg L gt 60 mg L Positive Organic carbon gt 150 mg L Calcium gt 300 mg L ou gt 13 gt 1000 mg L Positive Phosphorus gt 100 mg L Chromium gt 0 5 mg L Silica gt 150 mg L Iron gt 2 mg L Silver gt 0 9 mg L gt 1 5 mg L Lead gt 6 60 L Tin Collect samples in clean plastic or glass bottles Best results are obtained with immediate analysis Adjust sample pH to 2 or less with Concentrated Sulfuric Acid about 2 mL per liter Store at 4 C 39 F or less Preserved samples may be stored up to 28 days Warm the samples to room temperature and neutralize with 5N NaOH solution before analysis This test is technique sensitive Invert the vials as described here to avoid low results Hold the vial in a vertical position with the cap pointing up Turn the vial upside down Wait for all of the solution to flow down to the cap Pause Retum the vial to an upright position Wait for all the solution to flow to the bottom of the vial This process e
52. gent blank adjust The timing of reagent adding is critical You may find it useful to open the necessary reagents before starting this sequence All samples to be analyzed for cyanide should be treated by acid distillation except when experience has shown that there is no difference in results obtained with or without distillation Collect samples in glass or plastic bottles and analyze as quickly as possible The presence of oxidizing agents sulfides and fatty acids can cause the loss of cyanide during sample storage Samples containing these substances must be pretreated as described below before preservation with NaOH If the sample contains sulfide and is not pretreated it must be analyzed within 24 hours Preserve the sample by adding 4 0 mL of 5 0 N NaOH to each liter or quart of sample using a glass serological pipet and pipet filler Store the samples at 4 C 39 F or less Samples preserved in this manner can be stored for 14days Before testing samples should be adjusted to approximately pH 7 with 2 5 N HCI With most compounds a one hour reflux is adequate If thiocyanate is present in the original sample a distillation step is absolutely necessary as thiocyanate causes a positive interference High concentrations of Sulfidethiocyanate can yield a substantial quantity of sulfide in the distillate The rotten egg smell of hydrogen sulfide will accompany the distillate when sulfide is present The sulfide must be removed from the di
53. hoosing C MAC mode in the program choose Prog 86 1 C MAC Model HACH DR 890 86 DR 2010 2500 540 DR 4000 3000 4 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks Phosphorus Reactive Orthophosphate HR Phosphorus Reactive Orthophosphate HR Molybdovanadate Method 5 Wipe the blank and place it into the cell holder Place the cover on the vial Press Zero Ae Wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appear in mg L P Generally Chemical form of hach spectrophotometer is PO 80 Cra Required Reagents Interferences Sampling Storage 8 Preservation Tips Techniques Phosphorus Total TP LR Arsenate Chromium Copper Silicate samples or extreme pH Total Phosphorus TP LR Phosphorus Total LR 0 06 3 50 mg L PO 0 02 1 10 mg L P Acid Persulfate Method TP Vial TP Solution 1 TP Persulfate Reagent Pillow TP LR Reagent Pillow Cat NO 10612 00 Aluminum Greater than 200 mg L Nickel Greater than 300 mg L At all levels Silica Greater than 50 mg L Greater than 100 mg L Turbidity May cause inconsistent results Greater than 10 mg L Zinc Greater than 80mg L Iron Greater than 100 mg L NEE May exceed the buffering capacity of the reagents and require sample pretreatment E SE Sen o S
54. idic sample pH lt 4 Use only glass stoppered cylinders in this procedure Tips Wash glassware with 1 1 HCI and rinse with deionized water before use i Use plastic droppers in this procedure Droppers with rubber bulbs may contaminate the reagent Techniques Adjust the pH of the sample after the total phosphorus digestion to 4 5 with NaOH before analysis When Zinc Reagent pillow is dissolved sample should be orange If the sample is brown or blue either the zinc concentration is too high or an interfering metal is present Dilute the sample and repeat the test Zinc 95 Zinc E Digestion Zincon Method Digestion is required if total zinc is being determined The following is not the USEPA digestion 1 If nitric acid has not been added to the sample previously add 5 mL of Concentrated Nitric Acid to one liter of sample use a glass serological pipet and pipet filler If the sample was acidified at collection add 3 mL of nitric acid to one liter of sample Transfer 100 mL of acidified sample to a 250 mL Erlenmeyer flask Add 5 mL of 1 1 Hydrochloric Acid Heat sample on a Hot Plate for 15 minutes at 95 C 203 F Make sure the sample does not boil Filter cooled sample through a membrane filter and adjust the volume to 100 mL with Deionized Water 6 Adjust the pH to A 5 with DN NaOH Solution before analysis Digestion U Bb q N Zinc 96 D Procedures Zinc 1 Fill a 25 mL graduated cylinder with 2
55. l are present digestion is required i For turbid samples treat the 25 mL blank and the sample the same Turbidity i during steps 1 6 Sampling Collect samples in acid washed glass or plastic containers To preserve samples adjust the pH to 2 Storage or less with nitric acid about 2mL per liter Store preserved samples at room temperature up to six amp Preservation months Adjust the pH to about 4 with 5 0 N NaOH Undissolved powder does not affect accuracy Tips Prepare a boiling water bath For more accurate results determine a reagent blank value for each amp new lot of reagent Follow the procedure using deionized water in place of the sample Subtract Techniques the reagent blank value from the final results of perform a reagent blank adjust Use finger cots to handle hot sample cells Chromium Total 13 Chromium Total E Procedures Alkaline Hypobromite Oxidation Method 5 Add the contents of one Chromium 2 Reagent Pillow to the sample cell Cap and invert gently to mix 1 Fill a sample cell with 25 mL of sample 2 Add the contents of one Chromium 1 6 Add the contents of one Acid Reagent Pillow to the sample cell Cap and invert gently to mix Reagent Pillow to the sample cell Cap and invert gently to mix the prepared sample 7 Add the contents of one Chromium 3 Reagent Pillow to the sample cell A 5 minute reaction period will begin 3 Remove the cap and place the prepared sample into a b
56. l develop if nitrite is present A 20 minutes reaction period will begin 3 Fill an empty vial with 5 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 63 1 C MAC Modell HACH DR 890 63 DR 2010 2500 345 DR 4000 2630 Zero Pagetown Nitrite LR TEST KIT Diazotization Method TEST KIT 5 Wipe the blank and place it into the cell holder Place the cover on the vial Press Zero 6 Wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appear in mg L NO N o4 C mac Required Reagents Interferences Sampling Storage amp Preservation Tips amp Techniques Nitrite HR Nitrite HR 2 150 mg L NO Nitrite HR Ferrous Sulfate Method l Nitrite HR Reagent Pillow Cat NO 10513 00 This test does not measure nitrates nor is it applicable to glycol based samples Dilute glycol based samples and follow the Low Range Nitrite procedure Collect samples in clean plastic or glass bottles The following storage instructions are impossible Store at 4 C 30 F or lower if the sample is to be analyzed within 24 to 48 hours Warm to room temperature before running the test Do not use acid preservatives necessary only when prompt analysis is For more accurate results determine a reagent blank value for each new lot of reagent Follow the procedure using deionized wate
57. lace the cover on the sample cell Press Enter Results will appear in mg L Fe 38 Manganese LR Manganese LR 0 007 0 700 mg L Mn PAN Method amac Cyanide Reagent Ascorbic Acid Powder Pillow Cat NO 12511 00 PAN Indicator Solution 0 1 Required Reagents Aluminum 0 20 mg L 0 Lead 0 5 mg L Cadmium 10 mg L Magnesium 300 mg L as CaCOz Calcium 1000 mg L as CaCO3 Nickel 40 mg L Interferences Cobalt 20 mg L Zinc 15 mg L Copper 50 mg L Iron E GC 3 10 minute reaction period in step 5 Collect samples in clean plastic bottles To preserve samples adjust the sample pH to 2 or less with concentrated Nitric Acid about 2 mL per liter Samples preserved in this manner can be stored up to six months at room temperature Before testing adjust the sample pH to 4 5 with 5N NaOH Sampling Storage amp Preservation Ti Digestion is required for determining total manganese ips amp Techniques Rinse all glassware with 1 1 Nitric Acid Solution Rinse again with deionized water The alkaline cyanide solution contains cyanide Be sure cyanide solutions are stored in a caustic solution with pH gt 11 to prevent release of hydrogen cyanide gas Manganese LR 39 Manganese LR T Procedures PAN Method 5 Add 21 drops of 0 8 mL 0 1 PAN Indicator solution to each cell Cap and mix gently An orange color will develop if manganese is present A 2 minute reaction period will begin 1 Fill
58. le cell Swirl to mix A 2 minute reaction period will begin Any yellow color due to phosphorus is removed in this step Silica Silicomolybdate Method 5 Fill a second sample cell with 10 mL of the original sample the blank 6 After choosing C MAC mode in the program choose Prog 89 HACH DR 890 89 DR 2010 2500 656 DR 4000 3350 7 Within 3 minutes after the timer beeps wipe the blank and place it into the cell holder la Place the cover on the sample cell Press Zero 8 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L SiO2 90 Sulfate Q Sulfate 2 70 mg L SO Sulfate Method Mac ISS Sulfate reagent pillow Cat NO 13010 00 Reagents Calcium 20 000 mg L as CaCO3 Chloride 40 000 mg L as Cl Sampling Storage amp Preservation Tips amp Techniques Sulfate Magnesium 10 000 mg L as CaCO Silica 500 mg L as SIO2 Collect samples in clean plastic or glass bottles Samples may be stored up to 7 days by cooling to 4 C 39 F or lower Warm to room temperature before analysis For best results perform a new calibration for each lot of reagent 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 bla
59. low at least 5minutes to ensure a representative sample Allow several volumes of water to overflow the container Preservation and cap the container so there is no headspace above the sample Analyze samples immediately Do not preserve Tips Many factors including reactant concentrations sunlight pH temperature and salinity influence decomposition of chlorine i amp Techniques dioxide in water 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 of perform a reagent blank adjust If the chlorine dioxide concentration exceeds the upper limit of the test the color may fade or the sample turn yellow Chiorine Dioxide 9 Chlorine Dioxide E Procedures DPD Method 1 After choosing C MAC mode in the 5 Add the contents of one DPD Free program choose Prog 101 Chlorine Reagent Pillow to the sample 1 C MAC Mode HACH DR 890 112 cell the prepared sample Cap the cell DR 2010 2500 76 and swir to mix Wait 30 seconds for DR 4000 1530 undissolved powder to settle 6 Within 1 minute of adding the reagent wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L CIO 2 Fill a sample cell with 10 mL of sample the prepared sample Fill a second sample cell with 10 mL of sample the bla
60. n acid washed glass or plastic bottles No acid addition is necessary if analyzing the enti sample immediately To preserve samples adjust the sample pH to 2 or less with concentrated Nitric Acid eee about 2 mL per liter Samples preserved in this manner can be stored up to six months at room temperature Before testing adjust the sample pH to 3 5 with Ammonium Hydroxide Digestion is required for total iron determination Accuracy is not affected by undissolved powder Tips For more accurate results determine a reagent blank value for each new lot of reagent Follow the i procedure using deionized water in place of the sample Subtract the reagent blank value from Techniques the final results of perform a reagent blank adjust iron Total 37 D Procedures Iron Total 1 Fill a sample cell with 10 mL of sample the prepared sample 2 Add the contents of one Total Iron Reagent Pillow to the sample cell Cap and mix A 3 minute reacition period will begin Allow samples that contain rust to react for at least 5 minutes 3 Fill another sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 33 HACH DR 890 33 DR 2010 2500 265 DR 4000 2165 Iron Total Total Iron Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 6 Wipe the prepared sample and place it into the cell holder P
61. nk Zato No 3 Wipe the blank and place it into the PaneDown cell holder Place the cover on the sample cell Press Zero 4 Add 4 drops of Glycine Reagent to the sample cell Swi to mix Chlorine Dioxide 10 Chromium Hexavalent e Chromium Hexavalent 0 01 0 60 mg L cr 1 5 Diphenylcarbohydrazide Method mac Required Chromium 3 Reagent Pillow Cat NO 11510 00 Reagents Iron May interfere above 1 mg L Mercurous amp i f slightly Mercunc lons 3 Highly buffered samples or extreme sample pH may exceed the buffering capacity Interferences E of the reagents and require sample pretreatment Vanadium May interfere above 1 mg L For turbid samples treat the blank with the contents of one Acid Reagent Powder Pillow Turbidity This will ensure that any turbidity dissolved by the acid in the Chromium 3 Reagent Chromium 3 Reagent will also be dissolved in the blank Sampling Storage Collect samples in a cleaned glass or plastic container Store at 4 C 39 F up to 24 hours amp Preservation Samples must be analyzed within 24 hours At high chromium levels a precipitate will form Tips The final samples are highly acidic Neutralize to pH 6 9 with NaOH Standard Solution and flush down amp the drain for disposal For more accurate results determine a reagent blank value for each new lot of Techniques reagent Follow the procedure using deionized water in place of the sample Subtract the reagent bl
62. nk adjust Filter highly colored or turbid samples using filter paper and a funnel Undissolved powder that has settled does not affect accuracy 91 Sulfate E Procedures Sulfate Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 1 Fill a sample cell with 10 mL of sample the prepared sample 6 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L SO 2 Add the contents of one Sulfate Reagent Pillow to the sample cell Swirl to mix A 5 minute reaction period will begin Do not disturb the cell during this time 7 Clean the sample cells with soap and a brush 3 Fill a second sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 91 HACH DR 890 91 DR 2010 2500 680 DR 4000 3450 Sulfate 92 Sulfide e Sulfide 0 005 0 700 mg L Si Methylene Blue Method l Mac Required Reagents Interferences Sampling Storage amp Preservation Tips amp Techniques Sulfate Sulfide Solution 1 J 13410 Sulfide Solution 2 carang PARTAA Strong reducing Sulfite thiosulfate hydrosulfite etc by reducing the blue color substances or its development ia E SE EES Se SC Sulfide high levels and sample dilution Some sulfide loss may occur when the sample is diluted
63. nto a rack from the reactor Cool the vials to room temperature 8 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks Phosphorus Total TP LR 82 Total Phosphorus TP LR T Procedures Acid Persulfate Method 9 Wipe the blank and place it into the cell holder Place the cover on the vial Press Zero 10 Add the contents of one TP LR Reagent Pillow to the vial Cap and shake for 10 15 seconds The powder will not dissolve completely A 2 minute reaction period will begin Read samples between 2 and 8 minutes after adding the reagent 11 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks 12 Wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appear in mg L P Generally Chemical form of hach spectrophotometer is PO Phosphorus Total TP LR 83 Total Phosphorus TP HR Phosphorus Total HR Molybdovanadate SC 1 0 100 mg L PO 0 4 30 0 mg L P Method TP Vial Required TP Solution 1 Geer Reagents TP Persulfate Reagent Pillow ES EES TP Solution 2 Arsenate Only interferes if the sample is heated Iron ferrous Above 100 mg L Molybdate Above 1000 mg L negative inteference Silica Only interferes if the sample is heated Interferences Sampling Storage amp Preservation Phosphorus Total
64. ogen Total TN HR 67 Chemical Oxygen Demand CODc ULR Reactor Digestion Method Oxygen Demand Chemical CODcr ie ULR 2 40 mg L COD Required COD ULR Vial Cat NO 10111 00 Reagents Chloride is the primary interference when determining COD concentration Samples with higher chloride concentrations should be diluted If sample dilution will cause the COD concentration to be too low for accurate determination add 0 5 g of mercuric sulfate to each COD vial before the sample is added Maximum CI Suggested CT of When 0 5g HgSO added Interference mg L diluted samples mg L Maximum CI mg L ULR 2000 1000 NA LR HR 2000 1000 LR 8000 HR 4000 UHR 20 000 10 000 40 000 Sampling Collect samples in glass bottles Use plastic bottles only if they are known to be free of organic contamination Storage Test biologically active samples as soon as possible Homogenize samples containing solids to assure amp representative samples Samples treated with sulfuric acid to a pH of less than 2 about 2 mL per liter Preservation and refrigerated at 4 C can be stored up to 28 days Some of the chemicals and apparatus used in this procedure may be hazardous to the health and safety of the user if inappropriately handled or accidentally misused Wear appropriate eye protection and clothing for adequate user protection If contact occurs flush the affected area with running water Tips Place a safety shield in front of the COD
65. oiling water bath A 5 minute reaction period will begin 4 When the timer beeps remove the prepared sample Using running water cool the cell to 25 C Be sure the caps are on tightly 8 Fill a second sample cell with 25 mL of sample the blank Chromium Total 14 D Procedures 1 C MAC Mode Chromium Total 9 After choosing C MAC mode in the program choose Prog 15 HACH DR 890 15 DR 2010 2500 100 DR 4000 1580 10 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 11 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L Cr Chromium Total Alkaline Hypobromite Oxidation Method 15 Copper e Copper 0 04 5 00 mg L Cu Bicinchoninate Method ma Required Copper Reagent Pillow Cat NO 11710 00 Reagents Acidity If the sample is extremely acidic pH 2 or less a precipitate may form Add __ 8N_KOH Standard Solution drop wise while swirling to dissolve the turbidity Follow the powder pillow procedure above but substitute a copper reagent Aluminum AT powder A for Copper Reagent Pillow Results obtained will include total _ dissolved copper free and complexed Requires a 25 mL sample cell Before adding the Copper reagent powder add 0 2 mL of formaldehyde Cyanide CN to the 10 mL sample Wait 4 minutes before taking the reading Multiply
66. quals one inversion 61 Total Nitrogen TN LR E Procedures Chromotropic Acid Method 1 Add the contents of Total Nitrogen Persulfate Reagent Pillow to each Total Nitrogen Hydroxide Vial Wipe off any reagent that may get on the lid or the vial threads 5 Remove the caps from the digested vials and add the contents of one Total Nitrogen Reagent 1 Pillow to each vials 2 Add 2 mL of sample to one Ammonia Nitrogen LR Vial the prepared sample Add 2 mL of deionized water to another vial the blank 6 Cap the vials and shake for 15 seconds A 3 minute reaction period will begin 3 Cap vials and shake to dissolve vigorously for at least 30 seconds to mix The reagent may not dissolve completely after shaking This will not affect accuracy 7 Add the contents of one Total Nitrogen Reagent 2 Pillow to each vials 8 Cap the vials and shake for 15 seconds A 2 minute reaction period will begin The reagent may not dissolve completely after shaking This will not affect accuracy The solution will begin to tum light yellow 4 Place the vials in the reactor preheated to 105 C Heat for exactly 30 minutes Place the hot vials into a rack from the reactor Cool the vials to room temperature Nitrogen Total TN LR 62 Total Nitrogen TN LR E Procedures Chromotropic Acid Method 9 Remove the caps from two vials and add 2 mL of digested treated sample to one Total Nitrogen Acid Solution Vial the pr
67. r in place of the sample Subtract the reagent blank value from the final results of perform a reagent blank adjust 29 D Procedures 1 Fill a vial with 10 mL of sample the prepared sample 2 Add the contents of one Nitrite HR Reagent Pillow Cap and shake to dissolve A 10 minutes reaction period will begin Do not disturb it during the reaction period 3 Fill another sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 59 1 C MAC Mode HACH DR 890 59 DR 2010 amp 2500 373 DR 4000 2600 Nitrite HR Nitrite HR Ferrous Sulfate Method 5 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 6 After the timer beeps gently invert the prepared sample twice Avoid excessive mixing or low results may occur 7 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L NOz 36 Nitrogen Ammonia LR e Nitrogen Ammonia LR 0 02 2 50 mg L NHs N Salicylate Method mac Ammonia Nitrogen LR Vial Salicylate Method Required Ammonia Reagent Pillow 1 Cat NO 10332 00 Reagents Ammonia Reagent Pillow 2 Calcium 2500 mg L as CaCO3 Iron Blank with ammonia free water of the same iron concentration Magnesium 15000 mg L as CaCO Nitrite 20 mg L as NO N Interferences Nitrate 250 mg L as NO3 N O
68. reactor to prevent injury if splattering occurs Techniques The reagent mixture is light sensitive Keep unused vials in the opaque shipping container Refrigerate if possible Spilled reagent will affect test accuracy and is hazardous to skin and other materials Wash spills with running water Run one blank with each set of samples Run all tests the samples and the blank with the same lot of vials For greater accuracy analyze a minimum of three replicates and average the results Oxygen Demand Chemical CODc ULR 69 D Procedures 1 Hold one vial at a 45 degree angle Add 2 mL of sample to vial the prepared sample Hold one vial at a 45 degree angle Add 2 mL of deionized water to vial the blank 2 Cap the vials tightly Rinse them with deionized water and wipe with a clean paper towel Hold the vials by the cap over a sink Invert gently several times to mix The samples vials will becoming very hot during mixing 3 Place the vials in the COD reactor preheated to 150 C Heat for 2 hours Tum the reactor off Wait about 20 minutes for the vials to cool to 120 C or less 4 Invert each vials several times while still warm Place the vials into a rack and cool to room temperature Oxygen Demand Chemical CODc ULR Chemical Oxygen Demand CODc ULR Reactor Digestion Method 5 After choosing C MAC mode in the program choose Prog 12 HACH DR 2010 amp 2500 431 DR 4000 2700
69. rthophosphate 250 mg L as PO P pH Use 1N NaOH solution for acidic samples and 1N HCI solution for basic samples Sulfate 200 mg L as SO Sulfide Add the contents of one Sulfide Inhibitor Reagent Pillow Swin to mix Filter Other Hydrazine glycine turbidity color Distillate Get Collect samples in clean plastic or glass bottles Best results are obtained with immediate analysis S S If chlorine is known to be present add one drop of 0 IN Sodium thiosulfate for each 0 3mg L Cl Gs in a 1L sample Preserve the sample by reducing the pH to 2 or less with at least 2 mL of HCI GE Store at 4 C 39 F or less Preserved samples may be stored up to 28 days Before analysis warm samples to room temperature and neutralize to pH 7 with 5N NaOH solution Tips The ammonia salicylate reagent contains sodium nitroferricyanide Be sure cyanide solutions are Techniques stored in a caustic solution with pH gt 11 to prevent release of hydrogen cyanide gas Nitrogen Ammonia LR GYA Nitrogen Ammonia LR E Procedures Salicylate Method 1 Add 2 mL of sample to one Ammonia Zoe E TE TT EE RE apela Wipe the blank an ace it into the Nitrogen LR Vial the prepared sample i N ider Pi e E H tal cell holder Place the cover on the vial Add 2 mL of deionized water to another S j f Press Zero vial the blank 6 Wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appe
70. s to cool to 120 C or less 4 Invert each vials several times while still warm Place the vials into a rack and cool to room temperature Oxygen Demand Chemical CODc LR Chemical Oxygen Demand CODcr LR Reactor Digestion Method 5 After choosing C MAC mode in the program choose Prog 16 1 C MAC Model HACH DR 890 16 DR 2010 2500 430 DR 4000 2710 6 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks 7 Place the blank into the cell holder Place the cover on the vial Press Zero 8 Place prepared sample into the cell holder Place the cover on the vial Press Enter Results will appear in mg L COD 72 Chemical Oxygen Demand CODcr HR Cra Oxygen Demand Chemical CODcr HR 100 Reactor Digestion Method 1500 mg L COD Required Reagents Interference Sampling Storage amp Preservation Tips amp Techniques COD HR Vial Cat NO 10113 00 Chloride is the primary interference when determining COD concentration Samples with higher chloride concentrations should be diluted If sample dilution will cause the COD concentration to be too low for accurate determination add 0 5 g Ont mercuric sulfate to each COD Vial before the sample is added Maximum cr Suggested cr of When 0 59 HgSO4 added mg L diluted samples mg L Maximum CT mg L ULR 2000 1000 NA LR HR E 2000 1000 LR 8000 HR 20
71. sphorus Total TP HR Total Phosphorus TP HR Molybdovanadate Method 5 Add 2 mL of TP Solution 1 to each vials 6 Cap and invert to mix 7 Add 0 5 mL of TP Solution 2 to each vials 8 Cap and invert to mix A 7 minute reaction period will begin Read samples between 7 and 9 minutes after adding the TP Solution 2 86 D Procedures 9 After choosing C MAC mode in the program choose Prog 87 1 C MAC Model HACH DR 890 87 DR 2010 2500 541 DR 4000 3040 10 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks ZarolNo 11 Wipe the blank and place it into the Pagetown cell holder CC Place the cover on the vial sc Press Zero 12 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L P Generally Chemical form of hach spectrophotometer is PO Phosphorus Total TP HR Total Phosphorus TP HR Molybdovanadate Method 87 Silica Q Silica 1 0 75 0 mg L SiO2 Silicomolybdate Method Mac Required Reagents Interferences Sampling Storage amp Preservation Tips amp Techniques Acid Reagent Pillow for Silica Citric Acid Pillow Cat NO 12710 00 Molybdate Reagent Pillow Color Turbidity Eliminated by zeroing the instrument with the original sample Iron High levels of Fe and Fe interfere gt 60 mg
72. stillate prior to testing If cyanide is not present the amount of thiocyanate can be determined The sample is not distilled and the final reading is multiplied by 2 2 The result is mg L SCN The distillate can be tested and treated for sulfide after the last step of the distillation procedure by using the following lead acetate treatment procedure O Place a drop of the distillate already diluted to 250 mL on a disc of Hydrogen Sulfide Test Paper that has been wetted with pH 4 0 Buffer Solution O If the test paper darkens add 2 5 N HCI Standard Solution drop wise to the distillate until a neutral pH is obtained Add a 1 g measuring spoon of lead acetate to the distillate and mix Repeat step 1 O If the test paper continues to tum dark keep adding lead acetate until the distillate tests negative for sulfide Filter the black lead sulfide precipitate through filter paper and a funnel Neutralize the liquid filtrate to pH 7 and immediately analyze for cyanide Acid Distillation Procedure O Fill a 100 mL sample below 0 05 mg CN at 500 mL distillation flask and dilute to 250 mL with deionized water Adding 2 3 drops phenolphthalein ethylalcohol solution 0 5 W V as indicator Neutralize with phosphoric acid or 2 NaOH solution and set up cyanide distillatilling apparatus Adding ammonium sulfamate solution 10 W V 1mL phosphoric acid 10 mL and EDTA solution for cyanide test 10 mL Waiting for several minute Heat the flask Distillating
73. thiosulfate for each 0 3mg L Cl in a 1L sample Preserve the sample by reducing the pH to 2 or less with at least 2 mL of HCI Store at 4 C 39 F or less Preserved samples may be stored up to 28 days Before analysis warm samples to room temperature and neutralize to pH 7 with 5N NaOH solution The ammonia salicylate reagent contains sodium nitroferricyanide Be sure cyanide solutions are stored in a caustic solution with pH gt 11 to prevent release of hydrogen cyanide gas 09 Nitrogen Ammonia HR Nitrogen Ammonia HR E Procedures Salicylate Method 1 Add 0 1 mL of sample to one Ammonia O D Wipe the blank and place it into the Pagetown cell holder Place the cover on the vial Press Zero Nitrogen HR Vial the prepared sample Add 0 1mL of deionized water to another vial the blank 6 Wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appear in mg L NH3 N 2 Add the contents of Ammonia Reagent 1 Pillow to each vial a Cap vials and shake to dissolve Add the contents of Ammonia Reagent 2 Pillow to each vial Cap vials and shake to dissolve A 20 minute reaction period will begin A green color will develop if ammonia is present 4 After choosing C MAC mode in the program choose Prog 67 1 C MAC Model HACH DR 890 67 DR 2010 2500 343 DR 4000 2465 Nitrogen Ammonia HR 60 Total Nitrogen TN LR Nitro
74. to mix the prepared sample A 2 minute reaction period will begin 3 Fill a second sample cell with 10 mL of sample the blank 4 After choosing C MAC mode in the program choose Prog 20 1 C0 MAC Mode HACH DR 890 20 DR 2010 2500 135 DR 4000 1700 Copper 18 Copper Copper 0 002 0 210 mg L Cu Porphyrin Method Smac Copper Masking Reagent Pillow Porphyrin 1 Reagent Pillow Cat NO 11720 00 Porphyrin 2 Reagent Pillow Required Reagents Copper Interferences Sampling Storage amp Preservation Tips amp Techniques Aluminum AT Cadmium Cd Calcium Ca Chloride CF Chromium CT Cobalt Co Fluoride E 10 mg L 1500 mg L 90 000 mg L 110 mg L 100 mg L 30 000 mg L 60 mg L dl eee A d ae i Se Molybdenum Nickel Ni2 Potassium K Sodium Na Zinc Zn 140 mg L 3 mg L a 1 60 mg L 60 000 mg L 90 000 mg L 9 mg L Lead Pb 3 mg L Iron Fei 6 mg L Chelating agents Unless digestion is performed Extreme sample pH or may exceed the buffering capacity of the highly buffered samples reagents and require sample pretreatment Magnasium 10 000 mg L Collect samples in acid washed glass or plastic containers To preserve samples adjust the pH to 2 or less with nitric acid about 5mL per liter Store preserved samples at room temperature up to six months at room temperature Before testing adj
75. ust the pH of the preserved sample to between 2 6 If the sample is too acidic adjust the pH with 5 0 N NaOH solution Digestion is required for determining total copper Wash all glassware with detergent Rinse with tap water Rinse again with 1 1 Nitric Acid Solution Rinse a third time with 1 1 Nitric Acid Solution Rinse a third time with copper free deionized water 19 Copper E Procedures Porphyrin Method 5 After choosing C MAC mode in the program choose Prog 22 1 C MAC Model HACH DR 890 22 DR 2010 amp 2500 145 DR 4000 1720 1 Fill two round sample cells with 10 mL of sample 2 Add the contents of one Copper Masking Reagent Pillow to the sample cell Cap and invert gently to mix the blank The second sample cell is the prepared sample 6 Wipe the blank and place it into the cell holder Place the cover on the sample cell i Press Zero 7 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell 1 PH Press Enter Results will appear in mg L Cu 3 Add the contents of one Porphyrin 1 Reagent Pillow to each sample cell Cap and invert gently to mix 4 Add the contents of one Porphyrin 2 Reagent Pillow to each sample cell Cap and invert gently to mix If copper is present the sample will turn blue mometarily then return to yellow A 3 minute reaction period will begin Copper 20 Cyanide e Cyanide 0 001 0 240 mg L C
76. ve completely after shaking This will not affect accuracy 7 Add the contents of one Total Nitrogen Reagent 2 Pillow to each vials 8 Cap the vials and shake for 15 seconds A 2 minute reaction period will begin The reagent may not dissolve completely after shaking This will not affect accuracy The solution will begin to tum light yellow 4 Place the vials in the reactor preheated to 105 C Heat for exactly 30 minutes Place the hot vials into a rack from the reactor Cool the vials to room temperature Nitrogen Total TN HR 66 Total Nitrogen TN HR E Procedures Chromotropic Acid Method 9 Remove the caps from two vials and add 2 mL of digested treated sample to one Total Nitrogen Acid Solution Vial the prepared sample Add 2 mL of digested treated reagent blank to the second Total Nitrogen Acid Solution Vial the blank 13 Wipe the prepared sample and place it into the cell holder Place the cover on the vial Press Enter Results will appear in mg L N 10 Cap vials and invert 10 times to mix Use slow deliberate inversions for complete recovery The vials will be wam A 5 minute reaction period will begin The yellow color will intensify 11 After choosing C MAC mode in the program choose Prog 69 1 C MAC Model HACH DR 890 69 DR 2010 2500 395 DR 4000 2559 12 Wipe the blank and place it into the cell holder Place the cover on the vial Press Zero Nitr
77. y Rinse them with deionized water and wipe with a clean paper towel Hold the vials by the cap over a sink Invert gently several times to mix The samples vials will becoming very hot during mixing 3 Place the vials in the COD reactor preheated to 150 C Heat for 2 hours Tum the reactor off Wait about 20 minutes for the vials to cool to 120 C or less 4 Invert each vials several times while still warm Place the vials into a rack and cool to room temperature Oxygen Demand Chemical CODc HR Chemical Oxygen Demand CODcr HR Reactor Digestion Method 5 After choosing C MAC mode in the program choose Prog 17 1 C MAC Model HACH DR 890 17 DR 2010 2500 435 DR 4000 2720 6 Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks 7 Place the blank into the cell holder Place the cover on the vial Press Zero 8 Place prepared sample into the cell holder Place the cover on the vial Press Enter Results will appear in mg L COD 74 Chemical Oxygen Demand CODcr UHR LA Oxygen Demand Chemical CODcr UHR 1000 15000 mg L COD Reactor Digestion Method Required Reagents Interference Sampling Storage 8 Preservation Tips amp Techniques COD HR Vial Cat NO 10113 00 Chloride is the primary interference when determining COD concentration Samples with higher chloride concentrations should
78. yze a standard solution several times and adjust the shaking time to obtain the correct result Use this time for analyzing samples 45 D Procedures 1 Fill a 25 ml graduated mixing cylinder with 15 mL of sample 2 Add the contents of one Nitrate LR Reagent Pillow to the cylinder Stopper Shake the cylinder vigorously for 3 minutes A 2 minute reaction period will begin 3 When the timer beeps carefully pour 10 mL of the sample into sample cell Do not transfer any cadmium particles to the sample cell 4 Add the contents of Nitrite LR Reagent Pillow to each cell Cap and mix gently the prepared sample A pink color develop if nitrate is present A 15 minute reaction period will begin Nitrate LR Nitrate LR Cadmium Reduction Method 5 Fill a second sample cell with 10 mL of original sample the blank 6 After choosing C MAC mode in the program choose Prog 55 HACH DR 890 55 DR 2010 amp 2500 351 DR 4000 2515 7 Wipe the blank and place it into the cell holder Place the cover on the sample cell Press Zero 8 Wipe the prepared sample and place it into the cell holder Place the cover on the sample cell Press Enter Results will appear in mg L NOz N 46 Cra Required Reagents Interferences Sampling Storage 8 Preservation Tips amp Techniques Nitrate MR Nitrate MR Nitrate MR 0 1 5 0 mg L NO3 N Cadmium Reduction Method l

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