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Thermo Scientific Orion AQUAfast Powder and Tablet Reagent
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1. cccscccceeees 54 AC4P46 Nitrite as Nitrogen N Low Range Diazotization Azo Method Powder Test Procedure 55 ACD004 Nitrogen Total Low Range Persulfate Digestion Method Digestion Tube Test Procedure 56 ACDO07 Nitrogen Total High Range Persulfate Digestion Method Digestion Tube Test Procedure 58 AC2048 Ozone Indigo Blue Tablet Test Procedure cccccccccccsssssssseceeececessesesaeseeeeecesseseaaeseseeseessessaaeess 60 AC2001 pH Phenol Red Method Tablet Test Procedure cccccssssssccececessessnneseeeeeceeseseaaeseeeesenssessaaeees 62 AC3001 pH Phenol Red Method Liquid Test Procedure cccsessssccececessessnseceeeeecessesssaeseeeeseessessaaeess 63 AC2095 Phosphate Ortho Low Range Phosphomolybdic Acid Ascorbic acid Method Tablet Test Proce QU cenie a E EA E acdeZe cach lcctesaledhas aa EE AE E ENEA E arc 64 AC2096 Phosphate Ortho High Range Vanadomolybdate Method Tablet Test Procedure 65 AC4P95 Phosphate Ortho Ascorbic Acid Method Powder Test Procedure ccccecssssececeeeeessessnaeees 66 ACDO095 Phosphate as Phosphorous P Total Persulfate Digestion Ascorbic Acid Method Digestion Tube Test Procedure ausriorore ai aAA teadh ns has oh aaa tagead deaths daghed ESFE RS 67 ACDO95AH Phosphate as Phosphorous P Acid Hydrolyzable Acid Digestion Ascorbic Acid Method Digestion Tube Test ProC Cure ccccssssscccecessssessnaesececscesseeneaeeeeecesesseseaeeesecsses
2. Thermo Scientific Orion AQUAfast Powder and Tablet Reagent Chemistry User Guide for use with AquaMate 7000 Vis and AquaMate 8000 UV Vis Spectrophotometers 2012 Thermo Fisher Scientific Inc All rights reserved All trademarks are the property of Thermo Fisher Scientific Inc and Its subsidiaries Table of Contents Chapter TOVErNIEW eeereee eee ere a rae ee rere re pee ear er cence er eccrine er rence eet reer fe eee per er ore ey pene S 1 Table 1 Orion AQUAfast Power and Tablet Reagent Chemistries ccccccsssssssscececessesssssaeeeeeesseeses 2 Chapter 2 Reagent Chemistry Instructions cccssccccccscsssessnececececsesecneaeeeeecesseseeaeaeeeescssseeaaeaeeeesesssesaaees 4 Recommendations for Avoiding Measurement Errors csccccccccecssssssceeececesseseaeaeeeeecesseseaeeeeeessessnssnaees 4 Loading and Running a Water Analysis Method on the Spectrophotometel cccseessssceeeeeeessessaeees 5 Loading a Test Method from the USB Stick to the AquaMate InstrUMent cccccccecesssssseeeeeeseessees 5 Running a Test Method from the USB Stick c cccccccssssssssececececessesseaeeeceesceeseeeaececeescessesaeaeeeeseseeseees 8 Running a Test Method from the AquaMate Instrument LiDrary ccccccceseesssseceeecessessssaeeeeeeesessees 8 Running a Test Method from the AquaMate SmartStart M Nu ccccccccccssssssssssecececesessesseaeeeeeesseesees 8 Using the One Point Adjustment Calibration Featu
3. 10 ml of this pre treated solution is used for the following analysis Perform as described by the selected test method m Water which has been treated with organic compounds like corrosion inhibitors must be oxidized where necessary to break down the iron Therefore add 1 ml concentrated sulfuric acid and 1 ml concentrated nitric acid to 100 ml water sample and boil to approximately half volume After cooling down proceed as described above Page 45 AC2078 Iron Low Range III Soluble TPTZ Method Tablet Test Procedure 0 01 1 mg L Fe 1 2 8 9 Load and run the AC207824 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Iron LR Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial Wait for a reaction period of 5 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L iron Notes This method determines the total
4. Close the sample chamber door 9 Press the Measure Sample function key to display the result in pH units Notes For photometric determination of pH values only use Phenol Red Tablets in black printed foil pack and marked with Meter Water samples with low values of alkalinity m below 35 mg L CaCO may give wrong pH readings pH values below 6 5 and above 8 4 can produce results inside the measuring range A plausibility test pH meter is recommended The accuracy of the colorimetric determination of pH values depends on various boundary conditions buffer capacity of the sample salt contents etc Salt error Correction of test results average values for samples with salt contents of Indicator Salt Content Phenol Red 1 molar 2 molar 3 molar 0 21 0 26 0 29 The values of Parson and Douglas 1926 are based on the use of Clark and Lubs buffers 1 Mol NaCl 58 4 g l 5 8 Page 62 AC3001 pH Phenol Red Method Liquid Test Procedure 6 5 8 4 pH 1 Load and run the AC3001 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add six drops of Phenol Re
5. Press the Measure Sample function key to display the result in mg L ammonia as N Notes Strong alkaline or acidic water samples must be adjusted to approximately pH 7 before analysis use 1 mol l hydrochloric acid or 1 mol l sodium hydroxide If chlorine is known to be present add one drop of 0 1 mol l sodium thiosulfate for each 0 3 mg L Cl in a one liter water sample Iron interferes with the test The interferences will be eliminated as follows Determine the amount of total iron present in the water sample To produce the blank add an iron standard solution with the same iron concentration to the vial point 1 instead of deionized water Page 17 ACR012 Ammonia as Nitrogen N LR Salicylate Method Reaction Tube Test Procedure 0 02 2 5 mg L N 1 8 9 Load and run the ACRO12 method Open one white capped 16mm reaction vial and add 2 ml of deionized water this is the blank Open a second white capped 16mm reaction vial and add 2 ml of sample this is the sample Add the contents of one Ammonia Salicylate F5 Powder Pack straight from the foil to each vial Close the vials tightly with the caps and swirl or invert several times to mix the contents Wipe the exteriors of the vials Wait for a reaction period of 20 minutes Place the blank vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door Remove
6. this is the sample Close the vials tightly with the caps and shake the vials for at least 30 seconds to mix the contents The reagent many not dissolve completely Heat the digestion vials for 30 minutes in the preheated reactor at a temperature of 100 C CAUTION The vials will be hot Remove the digestion vials from the reactor and allow them to cool to room temperature Open the cooled digestion vials and add one TN Reagent A Power Pack straight from the foil to each vial Use a funnel to add the reagent Close the vials tightly with the caps and shake the vials for at least 15 seconds to mix the contents Wait for a reaction period of 3 minutes Open the digestion vials and add one TN Reagent B Power Pack straight from the foil to each vial Use a funnel to add the reagent Close the vials tightly with the caps and shake the vials for at least 15 seconds to mix the contents The reagent will not completely dissolve Wait for a reaction period of 2 minutes Open two TN Acid LR HR Reagent C Vials and add 2 ml of the digested treated blank to the first vial this is the blank Add 2 ml of the digested treated sample to the second vial this is the sample Close the vials tightly with the caps and gently invert the vials at least 10 times to mix the contents 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 Return the vial to
7. 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Citrat Powder Pack straight from the foil to the vial 7 Close the vial tightly with the cap and swirl or invert several times to mix the contents 8 Add one Sodium Periodate Powder Pack straight from the foil to the vial 9 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 10 Wait for a reaction period of 2 minutes 11 Place the vial into the holder in the sample chamber Close the sample chamber door 12 Press the Measure Sample function key to display the result in mg L manganese Notes e This test is applicable for the determination of soluble manganese in water and wastewater e Highly buffered water samples or extreme pH values may exceed the buffering capacity of the reagents and requires sample pre treatment If samples were acidified for storing adjust the pH between 4 and 5 with 5 mol l 5 N Sodium hydroxide before test Do not exceed pH 5 as manganese may precipitate e Interferences Interfering Substance Interference Level Calcium Greater than 700 mg L Chloride Greater than 70 000 mg L Iron Greater than 5 mg L Magnesium Greater than 100 000 mg L Page 51 AC4P42 Molybdate Molybdenum Mercaptoacetic Acid Method Powder Test Procedure 0 5 66 mg L
8. Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Silica No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 7 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved 8 Wait for a reaction period of 5 minutes 9 Add one Silica PR Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 10 Add one Silica No 2 Tablet straight from the foil to the same vial Crush the tablet with a clean stir rod 11 Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved Wipe the exterior of the vial 12 Wait for a reaction period of 1 minute 13 Place the vial into the holder in the sample chamber Close the sample chamber door 14 Press the Measure Sample function key to display the result in mg L silica Notes The tablets must be added in the correct sequence Phosphate ions do not interfere under the given reaction conditions If phosphate is known to be absent the addition of the Silica PR Tablet may be omitted Page 73 AC4P60 Silica High Range Silicomolybdate Method Powder Test Procedure 1 90 mg L SiO 1 Load and run the AC4P60 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Temperature of the sample should be 15 C to 25 C Close the vial t
9. Stored Tests function key Water Analysis 11 04am 240ct12 BLANK Test Name AC4P 71 Saved Measurement Mode Absorbance Wavelength 510nnm ipt Adjust On Adjust Factor 1 233 Reverse Color off Sample Positioner Manual 3 IDH O OFF 1 Statistics off Auto Save Data off More parameters Press t or to select item to change Calculate Save Stored un pt Adjust Test Tests Test 7 Press the A W keys to highlight Load test from USB drive and press the Enter key Water Analysis 11 05am 240ct12 BLANK Load internal test Measurement Load _ test from USB drivel Wavelength ipt Adjust Press Tf or to select Adjust Facto Press ENTER Reverse Colo Press ESC to exit Sample Posit IDH O OFF 1 Statistics off Auto Save Data off More parameters Press f or to select item to change 8 Press the A W keys to highlight the test method to be loaded and press the Load Test function key Utility Files Directory 11 05am 240ct12 AC4P12 WA 26Juni2Z AC4P 1 WA 240ct12 AC4P 2Z WA 27Jun12 ICODLOO WA 240ct12 More tests Press T or to select test Delete Load Test Test 9 Press the Save Test function key Water Analysis 11 06am 240ct12 BLANK Test Name CODLOO Saved Measurement Mode Absorbance Wavelength 420nnm ipt Adjust orf Reverse Color off Sample P
10. Wipe the exterior of the vial Wait for a reaction period of 2 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L ortho phosphate Notes Ortho phosphate ions react with the reagent to form an intense blue color Phosphate in organic and condensed inorganic forms meta pyro and polyphosphates must be converted to ortho phosphate ions before analysis Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms Organically combined phosphates are converted to ortho phosphate ions by heating with acid and persulfate The amount of organically combined phosphates can be calculated mg L phosphate organic mg L phosphate total mg L phosphate acid hydrolysable Application for water wastewater and seawater Highly buffered samples or samples with extreme pH values should be adjusted between pH 2 and pH 10 before analysis with 1 mol l Hydrochloric acid or 1 mol l sodium hydroxide Phosphate ortho Phosphorus reactive Interferences Large amounts of turbidity may cause inconsistent results Interference Interference Level Interference Interference Level Aluminum greater than 200 mg L Nickel greater than 300 mg L Arsenate at any level Silica Silicium dioxide greater than 50 mg L Chromium greater than 100 mg L Silicate greater than
11. adjusted between pH 6 and pH 7 before the reagent is added use 0 5 mol l sulfuric acid or 1 mol l sodium hydroxide Exceeding the measuring range Concentrations above 10 mg L chlorine using tablets can lead to results showing 0 mg L In this event the water sample must be diluted with water free of chlorine 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated Page 25 Turbidity can lead to errors The use of the DPD No 1 Tablet in samples with high calcium ion contents and or high conductivity can lead to turbidity of the sample and therefore incorrect measurements In this event the reagent DPD No 1 High Calcium Tablet should be used as an alternative Even if turbidity does occur after the DPD No 3 Tablet has been added it can be prevented by using the DPD No 1 High Calcium Tablet It is not possible to give exact values because the development of turbidity depends on the nature of the sample Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine Page 26 AC3072 Chlorine Total High Range KI Acid Method Tablet Test Procedure 5 200 mg L Cl 1 2 9 Load and run the AC3072 method Fill a clean AQUAfast 16 mm round vial Cat No AC2V16 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press th
12. be mixed with the reagent and the measurement repeated Oxidizing agents such as chlorine or ozone interfere as they react in the same way as bromine Page 19 AC2017 Chloride Silver Nitrate Turbidity Method Tablet Test Procedure 0 5 1 2 9 25 mg L Cl Load and run the AC2017 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Chloride T1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Add one Chloride T2 Tablet straight from the foil to the same vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl gently until the tablet is dissolved Wipe the exterior of the vial Wait for a reaction period of 2 minutes 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L chloride Notes Ensure that all particles of the tablet are dissolved chloride causes an extremely fine distributed turbidity with a milky appearance Heavy shaking leads to bigger sized particles which can cause false readings High concentr
13. digestion with acid refer to the Iron Digestion Method section Very strong alkaline or acidic samples must be adjusted to a pH value between 3 and 5 before analysis Accuracy is not affected by undissolved powder Water samples containing visible rust should be allowed to react for at least five minutes Page 47 AC4P79 Iron Total TPTZ Method Powder Test Procedure 0 02 1 8 mg L Fe 1 9 Load and run the AC4P79 method Use two clean AQUAfast 24mm round vials Cat No AC2V24 Pour 10 ml of deionized water into the first vial this is the blank vial Pour 10 ml of sample into the second vial this is the sample vial Add the contents of one Iron TPTZ F10 Powder Pack straight from the foil to each vial Close the vials tightly with the caps and swirl or invert several times to mix the contents Wipe the exteriors of the vials Wait for a reaction period of 3 minutes Place the blank vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door Remove the blank vial from the holder 10 Place the sample vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L iron Notes For determination of total Iron digestion is required TPTZ reagent recovers most insoluble iron oxides without digestion Rinse all glassware w
14. dissolved iron as Fe and Fe The Iron Il LR Tablet is used for differentiation as described in the Iron Digestion Method section instead of the Iron LR Tablet For the determination of total dissolved and undissolved iron digestion is required An example is described in the Iron Digestion Method section Page 46 AC4P78 Iron II amp III Soluble 1 10 Phenanthroline Method Powder Test Procedure 0 02 3 mg L Fe 1 2 8 9 Load and run the AC4P78 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Ferro F10 Powder Pack straight from the foil to the vial Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial Wait for a reaction period of 3 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L iron Notes The reagent reacts with all soluble iron and most insoluble forms of iron in the water sample Iron oxide requires prior digestion use mild vigorous or Digesdahl digestion For an example of
15. errors Conversion mg L NO mg L N x 3 29 Page 54 AC4P46 Nitrite as Nitrogen N Low Range Diazotization Azo Method Powder Test Procedure 0 01 0 3 mg LN 1 Load and run the AC4P46 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Nitri 3 Powder Pack straight from the foil to the vial 7 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 8 Wait for a reaction period of 20 minutes 9 Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L Nitrite as N Notes e Interferences o Strong oxidizing and reducing substances interfere o Cupric and ferrous ions cause low results o Antimonous auric bismuth chloroplatinate ferric lead mercurous metavanadate and silver ions interfere by causing precipitation o In samples with very high concentrations of Nitrate gt 100 mg L N a small amount of Nitrite will be found Such high levels of Nitrate appear to undergo a slight amount of reduction to Nitri
16. ortho phosphate ions react Phosphate in organic and condensed inorganic forms meta pyro and polyphosphates must be converted to ortho phosphate ions before analysis Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms Organically combined phosphates are converted to ortho phosphate ions by heating with acid and persulfate The amount of organically combined phosphates can be calculated mg L phosphate organic mg L phosphate total mg L phosphate acid hydrolysable The ortho phosphate ions react with the Vanadate molybdate reagent under acid conditions to form a yellow colored product Phosphate ortho Phosphorus reactive Page 65 AC4P95 Phosphate Ortho Ascorbic Acid Method Powder Test Procedure 0 06 2 5 mg L PO 1 2 8 9 Load and run the AC4P95 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Phosphate Rgt F10 Powder Pack straight from the foil to the vial Close the vial tightly with the cap and swirl or invert several times for 10 15 seconds to mix the contents The powder will not dissolve completely
17. remaining in the vial Add one DPD No 1 Tablet and one DPD No 3 Tablet straight from the foil to the vial Crush the tablets with a clean stir rod Add sample to the 10 ml mark on the vial Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 10 Wait for a reaction period of 2 minutes 11 Place the vial into the holder in the sample chamber Close the sample chamber door 12 Press the Measure Sample function key to display the result in mg L total chlorine Notes Vial cleaning As many household cleaners i e dishwasher detergent contain reducing substances the subsequent determination of chlorine may show lower results To avoid any measurement errors only use glassware free of chlorine demand Preparation Put all applicable glassware into sodium hypochlorite solution 0 1 g l for one hour and then rinse all glassware thoroughly with deionized water For individual testing of free and total chlorine the use of different sets of glassware is recommended EN ISO 7393 2 5 3 Preparing the sample When preparing the sample the escape of chlorine gases i e by pipetting or shaking must be avoided The analysis must take place immediately after taking the sample The DPD color development is carried out at a pH value of 6 2 to 6 5 The reagents therefore contain a buffer for the pH adjustment Strong alkaline or acidic water samples must be
18. sulfuric acid or 1 mol l sodium hydroxide Exceeding the measuring range Concentrations above 10 mg L chlorine using tablets can lead to results showing 0 mg L In this event the water sample must be diluted with water free of chlorine 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated Turbidity can lead to errors The use of the DPD No 1 Tablet in samples with high calcium ion contents and or high conductivity can lead to turbidity of the sample and therefore incorrect measurements In this event the reagent DPD No 1 High Calcium Tablet should be used as an alternative Even if turbidity does occur after the DPD No 3 Tablet has been added it can be prevented by using the DPD No 1 High Calcium Tablet It is not possible to give exact values because the development of turbidity depends on the nature of the sample Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine Page 22 AC2071 Chlorine Free DPD Method Tablet Test Procedure 0 01 6 mg L Cl 1 2 Load and run the AC207124 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sa
19. the blank vial from the holder 10 Place the sample vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L ammonia as N Notes Strong alkaline or acidic water samples must be adjusted to approximately pH 7 before analysis use 1 mol l hydrochloric acid or 1 mol l sodium hydroxide If chlorine is known to be present add one drop of 0 1 mol l sodium thiosulfate for each 0 3 mg L Cl in a one liter water sample Iron interferes with the test The interferences will be eliminated as follows Determine the amount of total iron present in the water sample To produce the blank add an iron standard solution with the same iron concentration to the vial point 1 instead of deionized water Page 18 AC2035 Bromine DPD Method Tablet Test Procedure 0 05 13 mg L Br 1 2 Load and run the AC203524 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Empty the vial leaving a few drops of sample remaining in the vial Add one DPD No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod
20. the reagent is added must be removed by filtration 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L hydrazine Notes If the water sample is cloudy you must filter it before performing the blank measurement The temperature of the water sample should not exceed 21 C Using the Hydrazine spoon 1 g is equivalent to one level spoon Qualitative folded filter papers for medium precipitates are recommended In order to check whether the reagent has aged if it has been stored for a lengthy period perform the test as described above using tap water If the result is above the detection limit of 0 05 mg L you should only use the reagent with reservations as there may be a major deviation in results Page 44 Iron Digestion Method lron Determination soluble and insoluble soluble Iron Iron Filtration Digestion Fe 7 Fe Fe Fe 2 Fe IRON LR IRON II LR methods tablet tablet 220 222 223 l result A minus result B Fe Digestion procedure for the determination of total soluble and insoluble iron 1 Add 1 ml of concentrated sulfuric acid to 100 ml water sample Heat and boil for 10 minutes or until all particles are dissolved After cooling down the sample is set to a pH value of 3 to 6 by using ammonia solution Refill with deionized water to the previous volume of 100 ml and mix well
21. the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Empty the vial leaving a few drops of sample remaining in the vial Add one DPD No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Add sample to the 10 ml mark on the vial Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Sample function key to display the result in mg L chlorine dioxide Chlorine Dioxide Measurement in Presence of Chlorine 1 2 10 11 Load and run the AC209924 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Empty the vial leaving a few drops of sample remaining in the vial Add one DPD No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Fill a second clean AQUAfast 24mm round vial with 10 ml of sample Add one Glycine Tablet straight from the foil to the vial Crush the t
22. to display the result in mg L zinc Notes Reverse color methods use a reagent that when prepared with samples deceases in color as the concentration of the species being measured in the samples increases Reverse color methods require the use of both a blank and a reagent blank The blank is a clear solution deionized water with zero absorbance The reagent blank is a mixture of the reagent and sample with no EDTA reagent and provides a zero concentration point with the darkest color highest absorbance The color of samples prepared with the EDTA reagent will decrease as the concentration increases for this method Measuring the reagent blank needs to be done with each sample analysis The tablets must be added in the correct sequence In the case of high levels of residual chlorine perform the analysis with a dechlorinated water sample To dechlorinate add one Dechlor Tablet to the water sample in step 2 Crush and mix to dissolve the tablet Then add the Copper Zinc LR Tablet step 3 and continue with the test procedure as described above Page 78 Thermo Fisher Scientific Water Analysis Instruments Chelmsford MA USA Quality Management System 4 Registered to ISO 9001 Certified System thermoscientific com water 2012 Thermo Fisher Scientific Inc All rights reserved All trademarks are the property of Thermo Fisher Scientific Inc amp its subsidiaries Water Analysis Instruments North America Netherlan
23. to save the test 13 Press the Run Test function key to begin using the test method Refer to the specific reagent chemistry section for detailed instructions Water Analysis 11 09am 240ct12 BLANK Test Name CODLOO Saved Measurement Mode Absorbance Wave length 420nnm ipt Adjust orf Reverse Color orf Sample Positioner Manual 3 ID O OFF 1 Statistics off Auto Save Data On Data File Name coD More parameters Press T or to select item to change Test Tests Test Page 7 Running a Test Method from the USB Stick 1 Make sure the test method to be run is in the Thermo folder on the USB stick and the USB stick is connected to the USB port on the front of the AquaMate spectrophotometer From the initial measurement screen press the Test key to access the test types Press the A V keys to highlight Water Analysis and press the Enter key Press the Stored Tests function key Press the A F keys to highlight Load test from USB drive and press the Enter key Press the A W keys to highlight the appropriate test method and press the Load Test function key Press the Run Test function key Running a Test Method from the AquaMate Instrument Library 1 From the initial measurement screen press the Test key to access the test types Press the A V keys to highlight Water Analysis and press the Enter key Press the Stored Tes
24. vial 8 Place the vial into the holder in the sample chamber Close the sample chamber door 9 Press the Measure Sample function key to display the result in mg L free chlorine Notes Vial cleaning As many household cleaners i e dishwasher detergent contain reducing substances the subsequent determination of chlorine may show lower results To avoid any measurement errors only use glassware free of chlorine demand Preparation Put all applicable glassware into sodium hypochlorite solution 0 1 g l for one hour and then rinse all glassware thoroughly with deionized water For individual testing of free and total chlorine the use of different sets of glassware is recommended EN ISO 7393 2 5 3 Preparing the sample When preparing the sample the escape of chlorine gases i e by pipetting or shaking must be avoided The analysis must take place immediately after taking the sample The DPD color development is carried out at a pH value of 6 2 to 6 5 The reagents therefore contain a buffer for the pH adjustment Strong alkaline or acidic water samples must be adjusted between pH 6 and pH 7 before the reagent is added use 0 5 mol l sulfuric acid or 1 mol l sodium hydroxide Exceeding the measuring range Concentrations above 2 mg L chlorine using powder packs can lead to results showing 0 mg L In this event the water sample must be diluted with water free of chlorine 10 ml of the diluted sample should be mixed with the reage
25. 10 mg L Copper greater than 10 mg L Sulfide at any level Iron greater than 100 mg L Zinc greater than 80 mg L Page 66 ACD095 Phosphate as Phosphorous P Total Persulfate Digestion Ascorbic Acid Method Digestion Tube Test Procedure 0 02 1 1 mg L P 1 Open one white capped 16mm PO4 P Acid Reagent Digestion Tube and add 5 ml of sample 2 Add one Potassium Persulfate F10 Power Pack straight from the foil to the vial Use a funnel to add the reagent 3 Close the vial tightly with the cap and invert the vial several times to mix the contents 4 Heat the vial for 30 minutes in the preheated reactor at a temperature of 100 C 5 CAUTION The vials will be hot Remove the vial from the reactor and allow it to cool to room temperature 6 Open the cooled digestion vial and add 2 ml of 1 54 N Sodium Hydroxide Solution to the vial 7 Close the vial tightly with the cap and gently invert the vial several times to mix the contents Wipe the exterior of the vial 8 Load and run the ACDO95 method 9 Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Blank function key to measure the blank 11 Open the sample chamber door Remove the vial from the holder 12 Add one Phosphate Rgt F10 Power Pack straight from the foil to the vial Use a funnel to add the reagent 13 Close the vial tightly with the cap and swirl the vial for 10 15 seconds to mix the
26. 5 Copper Zincon Method Tablet Copper AC4P29 AC4P29 Copper Free Bicinchoninate Method Powder Cyanuric Acid AC2098 AC2098 Cyanuric Acid Melamine Method Tablet Fluoride AC2009 AC2009 Fluoride SPADNS Kit Method Liquid Hard Total Low R Metallphthalei Hardness Ac30327 ac3o327TL total Low Range eee Tablet Method Hardness AC3032T AC3032TH Hardness Total High Range Metallphthalein Tablet Method Page 2 Hydrazine AC2030 AC2030 Hydrazine Dimethylamino benzaldehyde Method Powder Iron AC2078 AC207824 Iron Low Range IIl Soluble TPTZ Method Tablet lron AC4P78 AC4P78 Iron Il amp Ill Soluble 1 10 Phenanthroline Method Powder Iron AC4P79 AC4P79 Iron Total TPTZ Method Powder Manganese AC2055 AC2055 Manganese Formaldoxime Method Tablet Powd Manganese AC4P54 AC4P54 Manganese Low Range PAN Method eon M nganese ACAPSS ACAPSS Manganese High Range Periodate Oxidation Powder Method Molybdate ACAPA2 ACAPA2 Molybdate Molybdenum Mercaptoacetic Acid aan Molybdenum Method f gt Reaction Nitrate ACR007 ACR007 Nitrate as Nitrogen N Chromotropic Acid Method Tube Nitrite AC2046 AC2046 Nitrite as Nitrogen N Diazotization Azo Method Tablet Nire ACAPAG ACAPAG Nitrite as Nitrogen N Low Range Diazotization Powder Azo Method Nitrogen ACDOO4 ACDOO4 Nitrogen Total Low Range Persulfate Digestion Digestion
27. Add sample to the 10 ml mark on the vial Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L bromine Notes Vial cleaning As many household cleaners i e dishwasher detergent contain reducing substances the subsequent determination of bromine may show lower results To avoid any measurement errors only use glassware free of chlorine demand Preparation Put all applicable glassware into sodium hypochlorite solution 0 1 g l for one hour and then rinse all glassware thoroughly with deionized water Preparing the sample When preparing the sample the escape of bromine gases i e by pipetting or shaking must be avoided The analysis must take place immediately after taking the sample The DPD color development is carried out at a pH value of 6 2 to 6 5 The reagent tablet therefore contains a buffer for the pH adjustment Strong alkaline or acidic water samples must be adjusted between pH 6 and pH 7 before the reagent is added use 0 5 mol I sulfuric acid or 1 mol l sodium hydroxide Exceeding the measuring range Concentrations above 22 mg L bromine can lead to results showing 0 mg L In this event the water sample must be diluted with water free of bromine 10 ml of the diluted sample should
28. L Arsenate at any level Chromium greater than 100 mg L Copper greater than 10 mg L Iron greater than 100 mg L Nickel greater than 300 mg L Silica Silicium dioxide greater than 50 mg L Silicate greater than 10 mg L Sulfide at any level Zinc greater than 80 mg L Page 68 ACD095AH Phosphate as Phosphorous P Acid Hydrolyzable Acid Digestion Ascorbic Acid Method Digestion Tube Test Procedure 0 02 1 6 mg L P 1 Open one white capped 16mm PO4 P Acid Reagent Digestion Tube and add 5 ml of sample 2 Close the vial tightly with the cap and gently invert the vial several times to mix the contents 3 Heat the vial for 30 minutes in the preheated reactor at a temperature of 100 C 4 CAUTION The vials will be hot Remove the vial from the reactor and allow it to cool to room temperature 5 Open the cooled digestion vial and add 2 ml of 1 00 N Sodium Hydroxide Solution to the vial 6 Close the vial tightly with the cap and gently invert the vial several times to mix the contents Wipe the exterior of the vial 7 Load and run the ACDO95AH method 8 Place the vial into the holder in the sample chamber Close the sample chamber door 9 Press the Measure Blank function key to measure the blank 10 Open the sample chamber door Remove the vial from the holder 11 Add one Phosphate Rgt F10 Power Pack straight from the foil to the vial Use a funnel to add the reagent 12 Close the vial ti
29. MoO 0 3 40 mg L Mo 1 Load and run the AC4P42 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Molybdenum HR 1 F10 Powder Pack straight from the foil to the vial 7 Close the vial tightly with the cap and swirl or invert several times to mix the contents 8 Add one Molybdenum HR 2 F10 Powder Pack straight from the foil to the same vial 9 Close the vial tightly with the cap and swirl or invert several times to mix the contents 10 Add one Molybdenum HR 3 F10 Powder Pack straight from the foil to the same vial 11 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 12 Wait for a reaction period of 5 minutes 13 Place the vial into the holder in the sample chamber Close the sample chamber door 14 Press the Measure Sample function key to display the result in mg L Molybdate Molybdenum Notes Filter turbid water samples using filter paper and funnel before analysis Highly buffered water samples or extreme pH values should be adjusted to a pH of nearly 7 with 1 mol l nitric acid or 1 mol l sodium hydroxide Conce
30. O N Nitrite Greater than 12 mg L NO N Phosphate Greater than 100 mg L PO P Sulfate Greater than 300 mg L SO Sulfide Intensifies the color Glycine Less common interferences such as hydrazine and glycine will cause intensified Hydrazine colors in the prepared sample Turbidity and color will give erroneous high Color Turbidity values Samples with severe interferences require distillation Page 16 ACR011 Ammonia as Nitrogen N HR Salicylate Method Reaction Tube Test Procedure 1 50 mg L N 1 Load and run the ACRO11 method 2 Open one white capped 16mm reaction vial and add 0 1 ml of deionized water this is the blank 3 Open a second white capped 16mm reaction vial and add 0 1 ml of sample this is the sample 4 Add the contents of one Ammonia Salicylate F5 Powder Pack straight from the foil to each vial 5 Add the contents of one Ammonia Cyanurate F5 Powder Pack straight from the foil to each vial 6 Close the vials tightly with the caps and swirl or invert several times to mix the contents Wipe the exteriors of the vials 7 Wait for a reaction period of 20 minutes 8 Place the blank vial into the holder in the sample chamber Close the sample chamber door 9 Press the Measure Blank function key to measure the blank 10 Open the sample chamber door Remove the blank vial from the holder 11 Place the sample vial into the holder in the sample chamber Close the sample chamber door 12
31. PO the interference is approximately 11 Sulfide Interferes at all levels Occasionally water samples contain forms of silica which reacts very slowly with molybdate The nature of these forms is not known Page 74 e Apre treatment with sodium hydrogen carbonate and then with sulfuric acid will make these forms reactive to molybdate pre treatment is given in Standard Methods for the Examination of Water and Wastewater under Silica Digestion with Sodium Bicarbonate Page 75 AC4P82 Sulfate Barium Sulfate Turbidity Method Powder Test Procedure 5 100 mg L SO 1 2 8 9 Load and run the AC4P82 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Sulpha 4 F10 Powder Pack straight from the foil to the vial Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial Wait for a reaction period of 5 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L sulfate Notes If sulfate ion
32. Place the blank vial into the holder in the sample chamber Close the sample chamber door 8 Press the Measure Blank function key to measure the blank 9 Open the sample chamber door Remove the blank vial from the holder 10 Place the sample vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L COD Notes e Run samples and blanks with the same batch of vials The blank is stable when stored in the dark and can be used for further measurements with vials of the same batch e Do not place the hot vials in the sample chamber Cool the vials to room temperature for final measurements e Suspended solids in the vial lead to incorrect measurements For this reason it is important to place the vials carefully in the sample chamber The precipitate at the bottom of the sample should be not suspended e Clean the outside of the vials with a towel Finger prints or other marks must be removed e Samples can be measured when the chloride content does not exceed 1000 mg L e In exceptional cases compounds contained in the water cannot be oxidized adequately so results may be lower than reference methods e For samples under 100 mg L COD it is recommended to repeat the test using the reaction tube test for COD LR Page 34 CODHPO COD High Range Dichromate Reactor Digestion Method Digestion Tube Test Procedure 0 15000 mg L O 1 Open
33. Total Method Tube Nitrogen ACDOO7 ACDOO7 Nitrogen Total High Range Persulfate Digestion Digestion Total Method Tube Ozone AC2048 AC204824 Ozone Indigo Blue Method Tablet pH AC2001 AC2001 pH Phenol Red Method Tablet pH AC3001 AC3001 pH Phenol Red Method Liquid Phosphate Low Range Phosphomolybdic Phosphate AC2095 AC2095 Acid Ascorbic Acid Method Tablet Phosphate AC2096 AC2096 Phosphate High Range Vanadomolybdate Method Tablet Phosphate AC4P95 AC4P95 Phosphate Ortho Ascorbic Acid Method Powder Phosphate as Phosphorous P Total Persulfate Digestion Penne ARDS ReneS Digestion Ascorbic Acid Method Tube Phosphate as Phosphorous P Acid Hydrolyzable Digestion pulesP Hate BCDRLE OM ACDOASIAR Acid Digestion Ascorbic Acid Method Tube Reacti Phosphate ACRO95 ACRO95 Phosphate Ortho Ascorbic Acid Method Sig en Silica AC2060 AC2060 Silica Silicomolybdate Method Tablet Silica Sili lybdate Method with Phosphat Silica Ac2061 AC2061 aes ere emer meee liT objet Removal Silica AC4P60 AC4P60 Silica High Range Silicomolybdate Method Powder Sulfate AC4P82 AC4P82 Sulfate Barium Sulfate Turbidity Method Powder Sulfide AC2016 AC2016 Sulfide Methylene Blue Method Tablet Zinc AC2065 AC2065 Zinc Zincon Method Tablet Page 3 Chapter 2 Reagent Chemistry Instructions The measurement ranges specified in the following test procedures are provided by the chemistry manufacturer and are based on standard solutions me
34. able 15 To save the adjustment correction factor to the test method press the Save Test function key and overwrite the existing test method or save as a new test method 16 Press the Run Test function key When running a test with an adjustment correction factor in use the display will show 1pt Adj next to the test name the Reverse Color Feature Reverse color methods use a reagent that when prepared with samples deceases in color as the concentration of the species being measured in the samples increases Reverse color methods require the use of both a blank and a reagent blank The blank is a clear solution deionized water with zero absorbance The reagent blank is a mixture of the reagent and deionized water or initial reagent and sam colo ple as in the zinc by zincon method and provides a zero concentration point with the darkest r highest absorbance The color of samples prepared with the reagent will decrease as the concentration increases The following provides an overview how to perform a reverse color method 1 9 10 11 12 Load and run the method The Reverse Color parameter should be set to On for the method Fill a vial with deionized water Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and r
35. ablets with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Transfer the contents of the second vial into the first vial Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Page 30 12 Press the Measure Sample function key to display the result in mg L chlorine dioxide Notes Vial cleaning As many household cleaners i e dishwasher detergent contain reducing substances the subsequent determination of chlorine dioxide may show lower results To avoid any measurement errors only use glassware free of chlorine demand Preparation Put all applicable glassware into sodium hypochlorite solution 0 1 g l for one hour and then rinse all glassware thoroughly with deionized water Preparing the sample When preparing the sample the escape of chlorine dioxide gases i e by pipetting or shaking must be avoided The analysis must take place immediately after taking the sample The DPD color development is carried out at a pH value of 6 2 to 6 5 The reagent tablet therefore contains a buffer for the pH adjustment Strong alkaline or acidic water samples must be adjusted between pH 6 and pH 7 before the tablet is added use 0 5 mol l sulfuric acid or 1 mol l sodium hydroxide Exceeding the measurin
36. al will be filled up to the top 7 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 8 Place the vial into the holder in the sample chamber Close the sample chamber door 9 Press the Measure Rgnt Blank function key to measure the reagent blank 10 Open the sample chamber door and remove the vial from the sample chamber 11 Empty the vial rinse the vial and cap several times and fill the vial with exactly 10 ml of sample 12 Add exactly 2 ml SPADNS Solution to the vial CAUTION The vial will be filled up to the top 13 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 14 Place the vial into the holder in the sample chamber Close the sample chamber door 15 Press the Measure Sample function key to display the result in mg L fluoride Notes Reverse color methods use a reagent that when prepared with samples deceases in color as the concentration of the species being measured in the samples increases Reverse color methods require the use of both a blank and a reagent blank The blank is a clear solution deionized water with zero absorbance The reagent blank is a mixture of the reagent and deionized water and provides a zero concentration point with the darkest color highest absorbance The color of samples prepared with the reagent will decrease as the concentration increases for this m
37. assware thoroughly with deionized water For individual testing of free and total chlorine the use of different sets of glassware is recommended EN ISO 7393 2 5 3 Preparing the sample When preparing the sample the escape of chlorine gases i e by pipetting or shaking must be avoided The analysis must take place immediately after taking the sample The DPD color development is carried out at a pH value of 6 2 to 6 5 The reagents therefore contain a buffer for the pH adjustment Strong alkaline or acidic water samples must be adjusted between pH 6 and pH 7 before the reagent is added use 0 5 mol l sulfuric acid or 1 mol l sodium hydroxide Exceeding the measuring range Concentrations above 2 mg L chlorine using powder packs can lead to results showing 0 mg L In this event the water sample must be diluted with water free of chlorine 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine Page 29 AC2099 Chlorine Dioxide DPD Method Tablet Test Procedure 0 05 11 mg L Clo Chlorine Dioxide Measurement in Absence of Chlorine 1 2 10 11 Load and run the AC209924 method Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close
38. asured under ideal conditions These ranges may vary due to the type of sample being measured since various interferences can have a major influence on the accuracy of the method Due to the fact that each sample is different the only way to check the tolerance precision is the Standard Additions Method According to this method first the original sample is tested Then further samples 2 to 4 are taken and small amounts of a standard solution are added and further results are obtained The amounts added range from approximately half up to double the amount present in the sample itself These supplementary results make it possible to estimate the actual concentration of the original sample by comparison Test methods and ranges are subject to change without notice For a list of the most up to date test methods visit www thermoscientific com water Recommendations for Avoiding Measurement Errors Thoroughly clean vials caps and stir rods after each analysis in order to prevent carry over errors Even minute reagent residues lead to incorrect measurements Ensure that the outer walls of the vials are dry and clean before performing the analysis Fingerprints or water droplets on the light entry surfaces of the vials lead to incorrect measurements Blank and measurement procedures should be performed using the same vial whenever possible since different vials can possess slightly different tolerances Always take all readi
39. ations of electrolytes and organic compounds have different effects on the precipitation reaction lons which also form deposits with silver nitrate in acidic media such as bromides iodides and thiocyanates interfere with the analysis Highly alkaline water should if necessary be neutralized using nitric acid before analysis Page 20 AC2070 Chlorine Free amp Total DPD Method Tablet Test Procedure 0 01 6 mg L Cl 1 Load and run the AC207024 method 2 Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Empty the vial leaving a few drops of sample remaining in the vial 7 Add one DPD No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 8 Add sample to the 10 ml mark on the vial 9 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L free chlorine 12 Open the sample chamber door and remove the vial from the sample chambe
40. blet Alkalinity AC3002P AC3002P Alkalinity P Acid Indicator Method Tablet Aluminum AC2027 AC2027 Aluminum Eriochrome Cyanine R Method Tablet Aluminum AC4P27 AC4P27 Aluminum Eriochrome Cyanine R Method a Amani AC2012 AC2012 Ammonia as Nitrogen N Indophenole Phenate Tablet Method Ammonia AC4P12 AC4P12 Ammonia as Nitrogen N Salicylate Method Powder Ammoni ACRO11 ACRO11 Ammonia as Nitrogen N High Range Salicylate Reaction Method Tube Ammonis ACRO12 ACRO12 Ammonia as Nitrogen N Low Range Salicylate Reaction Method Tube Bromine AC2035 AC203524 Bromine DPD Method Tablet Chloride AC2017 AC2017 Chloride Silver Nitrate Turbidity Method Tablet Chlorine AC2070 AC207024 Chlorine Free amp Total DPD Method Tablet Chlorine AC2071 AC207124 Chlorine Free DPD Method Tablet Chlorine AC2072 AC207224 Chlorine Total DPD Method Tablet Chlorine AC3072 AC3072 Chlorine Total High Range KI Acid Method Tablet Chlorine AC4P71 AC4P71 Chlorine Free DPD Method Powder Chlorine AC4P72 AC4P72 Chlorine Total DPD Method Powder pons Ac2099 AC209924 Chlorine Dioxide DPD Method Tablet Dioxide coD CODLOO CODLOO COD Low Range Dichromate Reactor Digestion Digestion Method Tube COD CODHOO CODHOO COD Mid Range Dichromate Reactor Digestion Digestion Method Tube COD CODHPO CODHPO COD High Range Dichromate Reactor Digestion Digestion Method Tube Copper AC2029 AC202924 Copper Free amp Total Biquinoline Method Tablet Copper AC2065 AC206
41. chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Phosphate No 1 LR 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Add one Phosphate No 2 LR Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved Wipe the exterior of the vial Wait for a reaction period of 10 minutes 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L ortho phosphate Notes Only ortho phosphate ions react The tablets must be added in the correct sequence The test sample should have a pH value between 6 and 7 Interferences Higher concentrations of Cu Ni Cr III V V and W VI interfere due to their color Silicates do not interfere masked by citric acid in the tablets Ortho phosphate ions react with the reagent to form an intense blue color Phosphate in organic and condensed inorganic forms meta pyro and polyphosphates must be converted to ortho phosphate ions before analysis Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms Organically combined phosphates are converted to o
42. contents The reagent will not completely dissolve Wipe the exterior of the vial 14 Wait for a reaction period of 2 minutes 15 Place the vial into the holder in the sample chamber Close the sample chamber door 16 Press the Measure Sample function key to display the result in mg L total phosphate Notes Appropriate safety precautions and good lab technique should be used during the whole procedure Ortho phosphate ions react with the reagent to form an intense blue color Phosphate in organic and condensed inorganic forms meta pyro and polyphosphates must be converted to ortho phosphate ions before analysis Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms Organically combined phosphates are converted to ortho phosphate ions by heating with acid and persulfate The amount of organically combined phosphates can be calculated mg L phosphate organic mg L phosphate total mg L phosphate acid hydrolysable Page 67 Application for water wastewater and seawater Highly buffered samples or samples with extreme pH values should be adjusted between pH 2 and pH 10 before analysis with 1 mol l Hydrochloric acid or 1 mol l sodium hydroxide Phosphate ortho Phosphorus reactive Interferences Large amounts of turbidity may cause inconsistent results Interfering Substance Interference Level Aluminum greater than 200 mg
43. d Solution to the vial Add drops of the same size by holding the bottle vertically and squeezing slowly 7 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 8 Place the vial into the holder in the sample chamber Close the sample chamber door 9 Press the Measure Sample function key to display the result in pH units Notes When testing chlorinated water the residual chlorine contents can influence the color reaction of the liquid reagent This can be avoided without interfering with the pH measurement by adding a small crystal of sodium thiosulfate Na S20 e 5 H20 to the sample before adding the Phenol Red solution Phenol Red tablets already contain thiosulfate Due to differing drop sizes results can show a discrepancy in accuracy by comparison with tablets This can be minimized by using a pipette 0 18 ml Phenol Red solution is equivalent to 6 drops After use replace the bottle cap securely Store the Phenol Red solution in a cool dry place ideally at between 6 C and 10 C Page 63 AC2095 Phosphate Ortho Low Range Phosphomolybdic Acid Ascorbic acid Method Tablet Test Procedure 0 05 4 mg L PO 1 2 9 Load and run the AC2095 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample
44. d of 5 minutes 9 Add one EDTA Tablet straight from the foil to the same vial Crush the tablet with a clean stir rod 10 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 11 Place the vial into the holder in the sample chamber Close the sample chamber door 12 Press the Measure Sample function key to display the result in mg L copper Notes The tablets must be added in the correct sequence If the sample is zinc free it is not necessary to add the EDTA Tablet Page 37 AC4P29 Copper Free Bicinchoninate Method Powder Test Procedure 0 05 5 mg L Cu 1 2 8 9 Load and run the AC4P29 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Cu 1 F10 Powder Pack straight from the foil to the vial Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial Wait for a reaction period of 2 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the resul
45. de and the Thermo Scientific Orion AquaMate Master Methods List document Information for methods in the Merck and CHEMetrics folders can be found in the Thermo Scientific Orion AquaMate Master Methods List document and on the manufacturer s website Recommendation A copy of the methods on the USB memory stick should be saved to a computer or other data source in case the USB memory stick is accidentally deleted or otherwise corrupted Loading a Test Method from the USB Stick to the AquaMate Instrument 1 Access the USB memory stick using a computer Copy the desired test method s from the Orion Merck and or CHEMetrics folders to the Thermo folder Remove the USB memory stick from the computer and insert it into the USB port on the front of the AquaMate spectrophotometer When the AquaMate spectrophotometer is first powered on it will display the initial measurement screen Press the Test key to access the test types Absorbance 10 59am 240ct12 0 001A 450nnm Measure Set Change Blank nm Mode Page 5 5 Press the A W keys to highlight Water Analysis and press the Enter key Test Types 11 00am 240ct12 Advanced A T C Standard Curve Absorbance Ratio Absorbance Difference Kinetics Scanning 3 Point Net Multiwavelength Performance Verification Press t or to select Smart Stored Basic Start Tests ATC 6 Press the
46. different temperature can lead to higher or lower results Page 77 AC2065 Zinc Zincon Method Tablet Test Procedure 0 02 1 mg L Zn 1 Load and run the AC202924 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of deionized water Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Empty and dry the vial and then fill the vial with 10 ml of sample 6 Add one Copper Zinc LR Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 7 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 8 Wait for a reaction period of 5 minutes 9 Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Rgnt Blank function key to measure the reagent blank 11 Open the sample chamber door and remove the vial from the sample chamber 12 Add one EDTA Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 13 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 14 Place the vial into the holder in the sample chamber Close the sample chamber door 15 Press the Measure Sample function key
47. ds India Japan Toll Free 1 800 225 1480 Tel 31 033 2463887 Tel 91 22 4157 8800 Tel 81 045 453 9175 Tel 1 978 232 6000 info water uk thermo com wai asia thermofisher com wai asia thermofisher com info water thermo com China Singapore Australia Tel 86 21 68654588 Tel 65 6778 6876 Tel 613 9757 4300 wai asia thermofisher com wai asia thermofisher com in Australia 1300 735 295 InfoWaterAU thermofisher com UG_268888 001 E_1012_RevA Thermo SCIENTIFIC Part of Thermo Fisher Scientific
48. e by pipetting or shaking must be avoided The analysis must take place immediately after taking the sample Strong alkaline or acidic water samples must be adjusted between pH 6 and pH 7 before the tablet is added use 0 5 mol l sulfuric acid or 1 mol l sodium hydroxide The malonic acid in the tablet prevents chlorine from interfering with the process Bromine or bromide oxidized by the ozone interferes with the analysis 1 mol HOBr is equivalent to 0 4 mol ozone H O and organic peroxides react extremely slowly and the interference is therefore negligible Fe III does not interfere Mn II is oxidized by ozone and interferes with the analysis Page 61 AC2001 pH Phenol Red Method Tablet Test Procedure 6 5 8 4 pH 1 Load and run the AC2001 method 2 Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Phenol Red Meter Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 7 Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved Wipe the exterior of the vial 8 Place the vial into the holder in the sample chamber
49. e Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Chlorine HR KI Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Add one Acidifying GP Tablet straight from the foil to the same vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L chlorine Notes Oxidizing agents interfere as they react in the same way as chlorine Page 27 AC4P71 Chlorine Free DPD Method Powder Test Procedure 0 02 2 mg L Cl 1 Load and run the AC4P71 method 2 Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Chlorine Free DPD F10 Powder Pack straight from the foil to the vial 7 Close the vial tightly with the cap and swirl or invert several times to mix the contents approximately 20 seconds Wipe the exterior of the
50. e sample chamber Close the sample chamber door 12 Press the Measure Blank function key to measure the blank 13 Open the sample chamber door Remove the blank vial from the holder 14 Place the sample vial into the holder in the sample chamber Close the sample chamber door 15 Press the Measure Sample function key to display the result in mg L aluminum Notes e Before use clean the vials and the measuring beaker with hydrochloric acid approximately 20 Rinse them thoroughly with deionized water e To get accurate results the sample temperature must be between 20 C and 25 C e A low test result may be given in the presence of fluorides and polyphosphates The effect of this is generally insignificant unless the water has fluoride added artificially Page 14 AC2012 Ammonia as Nitrogen N Indophenole Phenate Method Tablet Test Procedure 0 02 1 mg L N 1 Load and run the AC2012 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Ammonia No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 7 Add one Ammonia No 2 Tablet straight from the f
51. ean stir rod 7 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved see notes below Wipe the exterior of the vial 8 Place the vial into the holder in the sample chamber Close the sample chamber door 9 Press the Measure Sample function key to display the result in mg L cyanuric acid Notes If cyanuric acid is present a cloudy solution will occur Small single particles are not necessarily caused by cyanuric acid Dissolve the tablet completely swirl the vial for approximately 1 minute Undissolved particles of the tablet can cause results that are too high Exceeding the measurement range samples with concentration above 90mg L must be diluted with water free of cyanuric acid 10 ml of the diluted sample should be tested as described above and the displayed results calculated using the dilution factor Page 39 AC2009 Fluoride SPADNS Kit Method Liquid Test Procedure 0 05 2 mg L F 1 Load and run the AC2009 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with exactly 10 ml of deionized water Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add exactly 2 ml SPADNS Solution to the vial CAUTION The vi
52. ed solids in the vial lead to incorrect measurements For this reason it is important to place the vials carefully in the sample chamber The precipitate at the bottom of the sample should be not suspended e Clean the outside of the vials with a towel Finger prints or other marks must be removed e Samples can be measured when the chloride content does not exceed 1000 mg L e In exceptional cases compounds contained in the water cannot be oxidized adequately so results may be lower than reference methods e For samples under 1000 mg L COD it is recommended to repeat the test using the reaction tube test for COD MR or for samples under 100 mg L COD it is recommended to repeat the test using the reaction tube test for COD LR Page 35 AC2029 Copper Free amp Total Biquinoline Method Tablet Test Procedure 0 05 5 mg L Cu 1 2 10 11 12 13 14 Load and run the AC202924 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Copper No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several tim
53. emove the vial from the sample chamber Add the reagent s to the vial Close the vial tightly with the cap and mix the contents Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Rgnt Blank function key to measure the reagent blank Open the sample chamber door and remove the vial from the sample chamber Empty and rinse the vial and then fill the vial with sample Add the reagent s to the vial Close the vial tightly with the cap and mix the contents Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Sample function key to display the results Page 10 AC2002 Alkalinity M Alkalinity to pH 4 3 Acid Indicator Method Tablet Test Procedure 5 200 mg L CaCO 1 Load and run the AC2002 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Alka M Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 7 Close the vial tightly with the cap and swirl or invert several times until the tablet is dis
54. es until the tablet is dissolved Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Sample function key to display the result in mg L free copper Open the sample chamber door and remove the vial from the sample chamber Add one Copper No 2 Tablet straight from the foil to the same vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Sample function key to display the result in mg L total copper Page 36 AC2065 Copper Zincon Method Tablet Test Procedure 0 02 1 mg L Cu 1 Load and run the AC2065 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Copper Zinc LR Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 7 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved 8 Wait for a reaction perio
55. esaaaeseseceseeseaaeaeseesesseesegs 69 ACRO95 Phosphate Ortho Ascorbic Acid Method Reaction Tube Test Procedure c cccccccessesssteees 71 AC2060 Silica Silicomolybdate Method Tablet Test Procedure cccccesssssscecececessessaeeeeeeseessessaaeeeeees 72 AC2061 Silica Silicomolybdate Method with Phosphate Removal Tablet Test Procedure 0 73 AC4P60 Silica High Range Silicomolybdate Method Powder Test Procedure cccceceestsseeeeeeeeeeeees 74 AC4P82 Sulfate Barium Sulfate Turbidity Method Powder Test Procedure cccsccessseesseeeesseeeseees 76 AC2016 Sulfide Methylene Blue Method Tablet Test Procedure ccccccsssscecececessessnaeeeeeesesssessaaeees 77 AC2065 Zinc Zincon Method Tablet Test ProCc Cure c ccccccscssssssscscscscsescsceaeeeseaeseeeeeeeaeaeeeaeeeeeaeanees 78 Chapter 1 Overview Thermo Scientific Orion AquaMate 8000 UV Vis and AquaMate 7000 Vis spectrophotometers include a USB memory stick that contains over 260 preprogrammed methods for use with Orion AQUAfast Merck and CHEMetrics reagent chemistries Preprogrammed methods provide values for the test parameters required to run specific reagent chemistries on the instrument including wavelength cell path length concentration factors curves and measurement unit All preprogrammed methods are stored on the USB memory stick so operators can select and load only the methods needed for their applications Up to 90 methods ca
56. ethod The same batch of SPADNS reagent solution must be used for testing reagent blank and sample measurement and one point calibration procedures The one point calibration process needs to be performed for each new batch of SPADNS reagent solution see Standard Methods 20 ed 1998 APHA AWWA WEF 4500 F D 4 a During testing blank reagent blank and sample measurement and one point calibration procedures the same vial should be used as different vials may exhibit minor tolerances The calibration solution and water samples should have the same temperature 1 C Page 40 As the test result is highly dependent on exact sample and reagent volumes the sample and reagent volumes should always be measured using a 10 ml or 2 ml volumetric pipette class A The accuracy of the test methods decreases above a level of 1 2 mg L fluoride Although the results are sufficiently accurate for most applications even more exact results can be achieved by 1 1 dilution of the sample prior to use and subsequent multiplication of the result by 2 SPADNS reagent solution contains arsenite Chlorine concentrations up to 5 mg L do not interfere Seawater and wastewater samples must be distilled Page 41 AC3032T Hardness Total Low Range Metallphthalein Method Tablet Test Procedure 2 50 mg L CaCO 1 2 8 9 Load and run the AC3032TL method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 m
57. g L NO mg L N x 4 43 Page 53 AC2046 Nitrite as Nitrogen N Diazotization Azo Method Tablet Test Procedure 0 01 0 5 mg L N 1 2 8 9 Load and run the AC2046 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Nitrite LR Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved Wipe the exterior of the vial Wait for a reaction period of 10 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L nitrite as N Notes The following ions can produce interferences since under the reaction conditions they cause precipitation antimony III iron Ill lead mercury I silver chloroplatinate metavanadate and bismuth Copper II ions may cause lower test results as they accelerate the decomposition of the diazonium salt It is unlikely in practice that these interfering ions will occur in such high concentrations that they cause significant reading
58. g range Concentrations above 19 mg L chlorine dioxide can lead to results showing 0 mg L In this event the water sample must be diluted with water free of chlorine dioxide 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated Oxidizing agents such as chlorine or ozone interfere as they react in the same way as chlorine dioxide Page 31 CODLOO COD Low Range Dichromate Reactor Digestion Method Digestion Tube Test Procedure 0 150 mg L O 1 Open one white capped 16mm COD reaction vial and add 2 ml of deionized water this is the reagent blank 2 Open a second white capped 16mm reaction vial and add 2 ml of sample this is the sample 3 Close the vials tightly with the caps and gently invert the vials several times to mix the contents CAUTION The vials will become hot during mixing 4 Heat the vials for 120 minutes in the preheated reactor at a temperature of 150 C 5 CAUTION The vials will be hot Remove the vials from the reactor and allow them to cool to 60 C or less Gently invert the vials several times to mix the contents while still warm Then allow the vials to cool to ambient temperature before measuring Wipe the exteriors of the vials 6 Load and run the CODLOO method 7 Filla clean AQUAfast 16mm round vial Cat No AC2V16 with deionized water this is the blank Close the vial tightly with the cap Wipe the exterior of the vial 8 Place the blank vial in
59. ghtly with the cap and swirl the vial for 10 15 seconds to mix the contents The reagent will not completely dissolve Wipe the exterior of the vial 13 Wait for a reaction period of 2 minutes 14 Place the vial into the holder in the sample chamber Close the sample chamber door 15 Press the Measure Sample function key to display the result in mg L acid hydrolysable phosphate Notes Appropriate safety precautions and good lab technique should be used during the whole procedure Ortho phosphate ions react with the reagent to form an intense blue color Phosphate in organic and condensed inorganic forms meta pyro and polyphosphates must be converted to ortho phosphate ions before analysis Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms Organically combined phosphates are converted to ortho phosphate ions by heating with acid and persulfate The amount of organically combined phosphates can be calculated mg L phosphate organic mg L phosphate total mg L phosphate acid hydrolysable Application for water wastewater and seawater Page 69 Highly buffered samples or samples with extreme pH values should be adjusted between pH 2 and pH 10 before analysis with 1 mol l Hydrochloric acid or 1 mol l sodium hydroxide Phosphate ortho Phosphorus reactive Interferences Large amounts of turbidity may cause inconsistent results Interfering S
60. ightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Silica HR Molybdate F10 Powder Pack straight from the foil to the vial 7 Close the vial tightly with the cap and swirl or invert several times to mix the contents 8 Add one Silica HR Acid Rgt F10 Powder Pack straight from the foil to the same vial If silica or phosphate is present a yellow color will develop 9 Close the vial tightly with the cap and swirl or invert several times to mix the contents 10 Wait for a reaction period of 10 minutes 11 Add one Silica Citric Acid F10 Powder Pack straight from the foil to the same vial In this step any yellow color due to phosphate is removed 12 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 13 Wait for a reaction period of 2 minutes 14 Place the vial into the holder in the sample chamber Close the sample chamber door 15 Press the Measure Sample function key to display the result in mg L silica Notes Interferences Substance Interference Iron Large amounts interfere Phosphate Does not interfere at concentrations less than 50 mg L PO At 60 mg L PO the interference is approximately 2 At 75 mg L
61. ith 1 1 hydrochloric acid solution first and then rinse with deionized water to remove iron deposits that can cause slightly high results Strong alkaline or acidic water samples must be adjusted between pH 3 and pH 8 before the reagent is added use 0 5 mol l sulfuric acid or 1 mol l sodium hydroxide Interferences When interferences occur color development is inhibited or a precipitate is formed The values below refer to a standard with an iron concentration of 0 5 mg L The following substances do not interfere when present up to the levels given Substance No Interference To Substance No Interference To Cadmium 4 0 mg L Manganese 50 mg L Chromium 0 25 mg L Mercury 0 4 mg L Chromium 1 2 mg L Molybdenum 4 0 mg L Cobalt 0 05 mg L Nickel 1 0 mg L Copper 0 6 mg L Nitrite lon 0 8 mg L Cyanide 2 8 mg L Page 48 AC2055 Manganese Formaldoxime Method Tablet Test Procedure 0 2 4 mg L Mn 1 2 9 Load and run the AC2055 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Manganese LR 1 Tablet straight from the foil to the vial Crush the
62. l of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Hardcheck P Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial Wait for a reaction period of 5 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L total hardness Notes Strong alkaline or acidic water samples must be adjusted between pH 4 and pH 10 before the tablet is added use 1 mol l hydrochloric acid or 1 mol l sodium hydroxide Page 42 AC3032T Hardness Total High Range Metallphthalein Method Tablet Test Procedure 20 500 mg L CaCO 1 2 8 9 Load and run the AC3032TH method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 1 ml of sample and 9 ml of deionized water Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and rem
63. ment must be repeated for checking the effectiveness of the digestion e Application for water wastewater and seawater e Interferences Interfering substances that resulted in a concentration change of 10 Bromide more than 60 mg L and Chloride more than 1000 mg L produce positive interferences Page 59 AC2048 Ozone Indigo Blue Tablet Test Procedure 0 05 0 5 mg L O 1 Load and run the AC204824 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of deionized water Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Rinse a clean beaker with deionized water Add one Ozone Tablet straight from the foil to the beaker Crush the tablet with a clean stir rod Add exactly 20 ml of deionized water to the beaker Carefully mix the solution using the stir rod until all particles are fully dissolved 7 Empty and dry the vial and add the solution from the beaker to the 10 ml mark on the vial 8 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 9 Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Rgnt Blank function key to measure the
64. mes for samples and blank should always be metered by using 2 ml volumetric pipettes class A e One blank is sufficient for each set of samples After taking the blank measurement it is possible to measure several samples e Itis very important to remove the vials from the reactor after exactly 30 minutes e Large quantities of nitrogen free organic compounds which are included in some water samples may reduce the effectiveness of the digestion by reacting with the persulfate reagent Samples which are well known to contents large quantities of organic compounds must be diluted and digestion and measurement must be repeated for checking the effectiveness of the digestion e Application for water wastewater and seawater e Interferences Interfering substances that resulted in a concentration change of 10 Bromide more than 60 mg L and Chloride more than 1000 mg L produce positive interferences Page 57 ACD007 Nitrogen Total High Range Persulfate Digestion Method Digestion Tube Test Procedure 5 150 mg L N 1 Open two TN Hydroxide HR Digestion Vials and add one TN Persulfate Reagent Power Pack 10 11 12 13 14 15 16 17 18 straight from the foil to each vial Use a funnel to add the reagent Wipe off any persulfate reagent that may get on the lid or the tube threads Add 0 5 ml of deionized water to the first digestion vial this is the blank Add 0 5 ml of sample to the second digestion vial
65. mple chamber Empty the vial leaving a few drops of sample remaining in the vial Add one DPD No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Add sample to the 10 ml mark on the vial Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L free chlorine Notes Vial cleaning As many household cleaners i e dishwasher detergent contain reducing substances the subsequent determination of chlorine may show lower results To avoid any measurement errors only use glassware free of chlorine demand Preparation Put all applicable glassware into sodium hypochlorite solution 0 1 g l for one hour and then rinse all glassware thoroughly with deionized water For individual testing of free and total chlorine the use of different sets of glassware is recommended EN ISO 7393 2 5 3 Preparing the sample When preparing the sample the escape of chlorine gases i e by pipetting or shaking must be avoided The analysis must take place immediately after taking the sample The DPD color development is carried out at a pH value of 6 2 to 6 5 The reagents therefore contain a buffer for the pH adjustment Strong alkaline or acidic water samples must be adjusted between
66. n be stored on the AquaMate spectrophotometer and stored methods can be added or removed as needed AquaMate spectrophotometers allow a one point adjustment on any preprogrammed method using a known standard to correct for variations in batch to batch reagent chemistries Operators can also modify preprogrammed methods or create their own custom methods so additional parameters and test methods can be added at any time The following instructions are for using Orion AQUAfast reagent chemistries with the AquaMate spectrophotometer Preprogrammed methods use a specific vial size path length in the formula and the vial size specified in these instructions must be used for accurate analysis The majority of AQUAfast reagent methods use a 24mm round vial Cat No AC2V24 Other vial sizes are noted in the individual reagent chemistry instructions Use the information in the following table to identify method names on the USB memory stick and the test parameters associated with each method This information is also included in the Thermo Scientific AquaMate Master Methods List available on the user guide CD or on our website at www thermoscientific com water Page 1 Table 1 Orion AQUAfast Power and Tablet Reagent Chemistries Reagent Method A Reagent Parameter Part Name Description Type Alkalinity AC2002 AC2002 Alkalinity M Acid Indicator Method Ta
67. ndensed inorganic forms meta pyro and polyphosphates must be converted to ortho phosphate ions before analysis Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms Organically combined phosphates are converted to ortho phosphate ions by heating with acid and persulfate The amount of organically combined phosphates can be calculated mg L phosphate organic mg L phosphate total mg L phosphate acid hydrolysable Application for water wastewater and seawater Highly buffered samples or samples with extreme pH values should be adjusted between pH 2 and pH 10 before analysis with 1 mol l Hydrochloric acid or 1 mol l sodium hydroxide Phosphate ortho Phosphorus reactive Interferences Large amounts of turbidity may cause inconsistent results Interference Interference Level Interference Interference Level Aluminum greater than 200 mg L Nickel greater than 300 mg L Arsenate at any level Silica Silicium dioxide greater than 50 mg L Chromium greater than 100 mg L Silicate greater than 10 mg L Copper greater than 10 mg L Sulfide at any level Iron greater than 100 mg L Zinc greater than 80 mg L Page 71 AC2060 Silica Silicomolybdate Method Tablet Test Procedure 0 05 4 mg L SiO 1 Load and run the AC2060 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial
68. ngs with capped vials Bubbles on the inside walls of the vial can lead to incorrect measurements To prevent this cap the vial and remove the bubbles by swirling the vial before performing the test Always add the reagent to the sample straight from the foil The reagent should never touch fingers or hands Major temperature differentials between the instrument and environment can lead to incorrect measurements i e due to the formation of condensate in the area of the lens or on the vial Specified tolerances at T 20 C For the best results use a pipette to measure and add samples to vials or beakers Page 4 Loading and Running a Water Analysis Method on the Spectrophotometer The USB memory stick included with the AquaMate spectrophotometers contains over 260 preprogrammed methods for use with Orion AQUAfast Merck and CHEMetrics reagent chemistries Methods can be accessed directly from the USB memory stick when connected to the AquaMate spectrophotometer or up to 90 methods can be stored on the instrument for quick and easy access The USB memory stick contains four folders Thermo Orion Merck and CHEMetrics The Thermo folder is empty and all methods to be loaded on the AquaMate spectrophotometer need to be copied to the Thermo folder The Orion Merck and CHEMetrics folders contain preprogrammed methods specific to that manufacturer Information for methods in the Orion folder can be found in this user gui
69. nt and the measurement repeated Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine Page 28 AC4P72 Chlorine Total DPD Method Powder Test Procedure 0 02 2 mg L Cl 1 2 8 9 Load and run the AC4P72 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Chlorine Total DPD F10 Powder Pack straight from the foil to the vial Close the vial tightly with the cap and swirl or invert several times to mix the contents approximately 20 seconds Wipe the exterior of the vial Wait for a reaction period of 3 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L total chlorine Notes Vial cleaning As many household cleaners i e dishwasher detergent contain reducing substances the subsequent determination of chlorine may show lower results To avoid any measurement errors only use glassware free of chlorine demand Preparation Put all applicable glassware into sodium hypochlorite solution 0 1 g l for one hour and then rinse all gl
70. ntrations above 10 mg L Cu causes too high test values if the reaction time of 5 minutes is increased So it is very important to perform the test procedure as described Substances which may interfere when present in concentrations at Aluminum 50 mg L Chromium 1000 mg L Iron 50 mg L Nickel 50 mg L Nitrite All Levels Page 52 ACR007 Nitrate as Nitrogen N Chromotropic Acid Method Reaction Tube Test Procedure 1 30 mg L N 1 Load and run the ACR007 method 2 Open one white capped 16mm reaction vial Reagent A and add 1 ml of deionized water this is the blank 3 Open a second white capped 16mm reaction vial Reagent A and add 1 ml of sample this is the sample 4 Add the contents of one Nitrate Chromotropic Powder Pack straight from the foil to each vial 5 Close the vials tightly with the caps and invert gently about 10 times to mix the contents Some solids may not dissolve Wipe the exteriors of the vials 6 Wait for a reaction period of 5 minutes 7 Place the blank vial into the holder in the sample chamber Close the sample chamber door 8 Press the Measure Blank function key to measure the blank 9 Open the sample chamber door Remove the blank vial from the holder 10 Place the sample vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L nitrate as N Notes Conversion m
71. o room temperature for final measurements Suspended solids in the vial lead to incorrect measurements For this reason it is important to place the vials carefully in the sample chamber The precipitate at the bottom of the sample should be not suspended Clean the outside of the vials with a towel Finger prints or other marks must be removed Samples can be measured when the chloride content does not exceed 1000 mg L In exceptional cases compounds contained in the water cannot be oxidized adequately so results may be lower than reference methods Page 33 CODHOO0 COD Mid Range Dichromate Reactor Digestion Method Digestion Tube Test Procedure 0 1500 mg L O 1 Open one white capped 16mm COD reaction vial and add 2 ml of deionized water this is the blank 2 Open a second white capped 16mm COD reaction vial and add 2 ml of sample this is the sample 3 Close the vial tightly with the cap and gently invert the vials several times to mix the contents CAUTION The vials will become hot during mixing 4 Heat the vials for 120 minutes in the preheated reactor at a temperature of 150 C 5 CAUTION The vials will be hot Remove the vials from the reactor and allow them to cool to 60 C or less Gently invert the vials several times to mix the contents while still warm Then allow the vials to cool to ambient temperature before measuring Wipe the exteriors of the vials 6 Load and run the CODHOO method 7
72. od Tablet Test Procedure sssssessrerrrrrrrerrrrrerererrrrrerrrrrererrrrrereree 23 AC2072 Chlorine Total DPD Method Tablet Test Procedure ssssssessrenerrrerrrrrrrrrrrrrerererrrerererrrererere 25 AC3072 Chlorine Total High Range KI Acid Method Tablet Test ProceCure ccccsscccsssceeseeessees 27 AC4P71 Chlorine Free DPD Method Powder Test Procedure esssessrrserrrererrrrrrrerrrrrerererrrrrerrrererere 28 AC4P72 Chlorine Total DPD Method Powder Test Procedure ssesssesererrrerrrrrrrerrrrrererrrrrererrrrrereree 29 AC2099 Chlorine Dioxide DPD Method Tablet Test Procedure ssssssserrrerrrrrrrerererererererrrerrrrrrrrrrres 30 CODLOO COD Low Range Dichromate Reactor Digestion Method Digestion Tube Test Procedure 32 CODHOO COD Mid Range Dichromate Reactor Digestion Method Digestion Tube Test Procedure 34 CODHPO COD High Range Dichromate Reactor Digestion Method Digestion Tube Test Procedure 35 AC2029 Copper Free amp Total Biquinoline Method Tablet Test Procedure ccceseessssceeeeeeessessaeees 36 AC2065 Copper Zincon Method Tablet Test Procedure ccccsessscceceecessesenseceeeeecesseseaaeseeeeseessessaaees 37 AC4P29 Copper Free Bicinchoninate Method Powder Test Procedure ccccccccccccssssssssceceeseessessaeees 38 AC2098 Cyanuric Acid Melamine Method Tablet Test ProC Cure ssssscccccecsssessseeceeeceesssessaeeeeess 39 AC2009 Fluo
73. of one Ammonia Salicylate F10 Powder Pack straight from the foil to each vial Close the vials tightly with the caps and swirl or invert several times to mix the contents 6 Wait for a reaction period of 3 minutes 7 Add the contents of one Ammonia Cyanurate F10 Powder Pack straight from the foil to each vial Close the vials tightly with the caps and swirl or invert several times to mix the contents Wipe the exteriors of the vials 8 Wait for a reaction period of 15 minutes 9 Place the blank vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Blank function key to measure the blank 11 Open the sample chamber door Remove the blank vial from the holder 12 Place the sample vial into the holder in the sample chamber Close the sample chamber door 13 Press the Measure Sample function key to display the result in mg L ammonia as N Notes e Extremely basic or acidic water samples should be adjusted with 0 5 mol l 1 N sulfuric acid solution or 1 mol l 1 N sodium hydroxide solution to pH 7 e Interferences Interference Interference Levels and Treatments Calcium Greater than 1000 mg L CaCO Iron Interferes at all levels To correct determine the concentration of iron in the sample by performing a total iron test Add the same iron concentration to the deionized water step 3 Iron will be blanked out successfully Magnesium Greater than 6000 mg L CaCO Nitrate Greater than 100 mg L N
74. oil to the same sample in the vial Crush the tablet with a clean stir rod 8 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 9 Wait for a reaction period of 10 minutes 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L ammonia as N Notes The tablets must be added in the correct sequence The Ammonia No 1 Tablet will only dissolve completely after the Ammonia No 2 Tablet has been added The temperature of the sample is important for full color development At a temperature below 20 C the reaction period is 15 minutes Sea water samples Ammonia conditioning reagent is required when testing sea water or brackish water samples to prevent precipitation of salts Fill the test tube with the sample to the 10 ml mark and add one level spoonful of Conditioning Powder Mix to dissolve and then continue as described in the test instructions Page 15 AC4P12 Ammonia as Nitrogen N Salicylate Method Powder Test Procedure 0 01 0 8 mg L N 1 Load and run the AC4P12 method 2 Use two clean AQUAfast 24mm round vials Cat No AC2V24 3 Pour 10 ml of deionized water into the first vial this is the blank vial 4 Pour 10 ml of sample into the second vial this is the sample vial 5 Add the contents
75. onds to mix the contents The reagent will not completely dissolve 12 Wait for a reaction period of 2 minutes 13 Open two TN Acid LR HR Reagent C Vials and add 2 ml of the digested treated blank to the first vial this is the blank 14 Add 2 ml of the digested treated sample to the second vial this is the sample 15 Close the vials tightly with the caps and gently invert the vials at least 10 times to mix the contents 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 Return the vial to the upright position Wait for all the solution to flow to the bottom of the vial This process is one inversion 10 inversions equal about 30 seconds Wipe the exteriors of the vials CAUTION The vials will become warm during mixing 16 Wait for a reaction period of 5 minutes 17 Load and run the ACD004 method 18 Place the blank vial into the holder in the sample chamber Close the sample chamber door Page 56 19 Press the Measure Blank function key to measure the blank 20 Open the sample chamber door Remove the blank vial from the holder 21 Place the sample vial into the holder in the sample chamber Close the sample chamber door 22 Press the Measure Sample function key to display the result in mg L nitrogen Notes e Appropriate safety precautions and a good lab technique should be used during the whole procedure e Volu
76. one white capped 16mm COD reaction vial and add 0 2 ml of deionized water this is the blank 2 Open a second white capped 16mm COD reaction vial and add 0 2 ml of sample this is the sample 3 Close the vial tightly with the cap and gently invert the vials several times to mix the contents CAUTION The vials will become hot during mixing 4 Heat the vials for 120 minutes in the preheated reactor at a temperature of 150 C 5 CAUTION The vials will be hot Remove the vials from the reactor and allow them to cool to 60 C or less Gently invert the vials several times to mix the contents while still warm Then allow the vials to cool to ambient temperature before measuring Wipe the exteriors of the vials 6 Load and run the CODHPO method 7 Place the blank vial into the holder in the sample chamber Close the sample chamber door 8 Press the Measure Blank function key to measure the blank 9 Open the sample chamber door Remove the blank vial from the holder 10 Place the sample vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L COD Notes e Run samples and blanks with the same batch of vials The blank is stable when stored in the dark and can be used for further measurements with vials of the same batch e Do not place the hot vials in the sample chamber Cool the vials to room temperature for final measurements e Suspend
77. ositioner Manual 3 ID O OFF 1 Statistics off Auto Save Data On Data File Name coD More parameters Press t or to select item to change ave Stored un Test Tests Test Page 6 10 Press the A V keys to highlight Save as an internal test and press the Enter key Water Analysis 11 07am 240ct12 BLANK Save as an internal test Measure Save test to the USB drive Wavelen Save test to internal and ipt Adj IReverse Press f or to select Sample Press ENTER ID 0 Press ESC to exit Statist Auto Save Data On Data File Name coD More parameters Press f or to select item to change 11 Press the Accept Name function key Create Test Name 11 07am 240ct12 QBCDEFGH I JELMNOPQRS TUVWXYZ0123456789 labcdefghijkIlmnopqrstuywxyz _ pO Test Name CODLOO Press t or to select character Press Accept Name to save the test Delete i Delete Accept Name Character Character Name 12 Press the A V keys to highlight Include as a SmartStart test or Do not include as a SmartStart test and press the Enter key Create Test Name 11 08am 240ct12 AliMinclude as a SmartStart test Do not include as a SmartStart test la Press f or to select Press ENTER Press ESC to exit Press fT or to select character Press mis Name
78. ove the vial from the sample chamber Add one Hardcheck P Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial Wait for a reaction period of 5 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L total hardness Notes Strong alkaline or acidic water samples must be adjusted between pH 4 and pH 10 before the tablet is added use 1 mol l hydrochloric acid or 1 mol l sodium hydroxide Page 43 AC2030 Hydrazine Dimethylamino benzaldehyde Method Powder Test Procedure 0 05 0 5 mg L N gt H 1 2 8 9 Load and run the AC2030 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one gram 1 g Hydrazine Powder to the vial Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial Wait for a reaction period of 10 minutes The slight turbidity that occurs when
79. pH 6 and pH 7 before the reagent is added use 0 5 mol l sulfuric acid or 1 mol l sodium hydroxide Exceeding the measuring range Concentrations above 10 mg L chlorine using tablets can lead to results showing 0 mg L In this event the water sample must be diluted with water free of chlorine 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated Turbidity can lead to errors The use of the DPD No 1 Tablet in samples with high calcium ion contents and or high conductivity can lead to turbidity of the sample and therefore incorrect Page 23 measurements In this event the reagent DPD No 1 High Calcium Tablet should be used as an alternative It is not possible to give exact values because the development of turbidity depends on the nature of the sample Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine Page 24 AC2072 Chlorine Total DPD Method Tablet Test Procedure 0 01 6 mg L Cl 1 2 Load and run the AC207224 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Empty the vial leaving a few drops of sample
80. r 13 Add one DPD No 3 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 14 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 15 Wait for a reaction period of 2 minutes 16 Place the vial into the holder in the sample chamber Close the sample chamber door 17 Press the Measure Sample function key to display the result in mg L total chlorine Notes Vial cleaning As many household cleaners i e dishwasher detergent contain reducing substances the subsequent determination of chlorine may show lower results To avoid any measurement errors only use glassware free of chlorine demand Preparation Put all applicable glassware into sodium hypochlorite solution 0 1 g l for one hour and then rinse all glassware thoroughly with deionized water For individual testing of free and total chlorine the use of different sets of glassware is recommended EN ISO 7393 2 5 3 Preparing the sample When preparing the sample the escape of chlorine gases i e by pipetting or shaking must be avoided The analysis must take place immediately after taking the sample Page 21 The DPD color development is carried out at a pH value of 6 2 to 6 5 The reagents therefore contain a buffer for the pH adjustment Strong alkaline or acidic water samples must be adjusted between pH 6 and pH 7 before the reagent is added use 0 5 mol l
81. r with hydrochloric acid approximately 20 Rinse them thoroughly with deionized water To get accurate results the sample temperature must be between 20 C and 25 C A low test result may be given in the presence of fluorides and polyphosphates The effect of this is generally insignificant unless the water has fluoride added artificially Page 13 AC4P27 Aluminum Eriochrome Cyanine R Method Powder amp Liquid Test Procedure 0 01 0 25 mg L Al 1 Load and run the AC4P27 method 2 Use two clean AQUAfast 24mm round vials Cat No AC2V24 and mark one as the blank 3 Pour 20 ml of sample into a 100 ml beaker 4 Add the contents of one Aluminum ECR F20 Powder Pack straight from the foil to the sample in the beaker Dissolve the powder using a clean stirring rod 5 Wait for a reaction period of 30 seconds 6 Add the contents of one Hexamine F20 Powder Pack straight from the foil to the same sample in the beaker Dissolve the powder using a clean stirring rod 7 Add 1 drop of Aluminum ECR Masking Reagent in the vial marked as blank Add 10 ml of the prepared sample to the same vial this is the blank vial 8 Add the remaining 10 ml of the prepared sample to the second vial this is the sample vial 9 Close the vials tightly with the caps and swirl or invert several times to mix the contents Wipe the exteriors of the vials 10 Wait for a reaction period of 5 minutes 11 Place the blank vial into the holder in th
82. re c cccccccccsssssssecececessessseseeeescsssesenaeeeeeeseesesseaaeess 9 Using the Reverse Color Feature lt cncsacecccesccc das ceesten ved cbe cen e aeaea in stetbea ceded dou stcndeavedsaadeastecdeatelededonsecdec 10 AC2002 Alkalinity M Alkalinity to pH 4 3 Acid Indicator Method Tablet Test Procedure 06 11 AC3002P Alkalinity P Alkalinity to pH 8 2 Acid Indicator Method Tablet Test Procedure 12 AC2027 Aluminum Eriochrome Cyanine R Method Tablet Test Procedure cccecsessececeeeeessesseaeees 13 AC4P27 Aluminum Eriochrome Cyanine R Method Powder amp Liquid Test Procedure c0cseseees 14 AC2012 Ammonia as Nitrogen N Indophenole Phenate Method Tablet Test Procedure 0 15 AC4P12 Ammonia as Nitrogen N Salicylate Method Powder Test Procedure ccccsscccceesseeceesees 16 ACRO11 Ammonia as Nitrogen N HR Salicylate Method Reaction Tube Test Procedure 00 17 ACRO12 Ammonia as Nitrogen N LR Salicylate Method Reaction Tube Test Procedur 00 18 AC2035 Bromine DPD Method Tablet Test Procedure sssssrsrrerererrrrrerrrerrrrrrrerererererererrrrrerrrerrreres 19 AC2017 Chloride Silver Nitrate Turbidity Method Tablet Test Proce Cure cccccccssccesseesseeecsseeeseees 20 AC2070 Chlorine Free amp Total DPD Method Tablet Test Procedure cccceecssssesseeseetscsteeeeeeeeeeeeees 21 AC2071 Chlorine Free DPD Meth
83. reagent blank 11 Open the sample chamber door and remove the vial from the sample chamber 12 Rinse a clean beaker with the sample to be measured Add one Ozone Tablet straight from the foil to the beaker Crush the tablet with a clean stir rod Add exactly 20 ml of sample to the beaker Carefully mix the solution using the stir rod until all particles are fully dissolved 13 Empty the vial rinse the vial and cap several times and add the solution from the beaker to the 10 ml mark on the vial 14 Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial 15 Place the vial into the holder in the sample chamber Close the sample chamber door 16 Press the Measure Sample function key to display the result in mg L ozone Notes Reverse color methods use a reagent that when prepared with samples deceases in color as the concentration of the species being measured in the samples increases Reverse color methods require the use of both a blank and a reagent blank The blank is a clear solution deionized water with zero absorbance The reagent blank is a mixture of the reagent and deionized water and provides a zero concentration point with the darkest color highest absorbance The color of samples prepared with the reagent will decrease as the concentration increases for this method Page 60 Preparing the sample When preparing the sample the escape of ozone gases i
84. ride SPADNS Kit Method Liquid Test ProC Cure c cccccccscssssscecececsssessseceeeessessestsaeeeeess 40 AC3032T Hardness Total Low Range Metallphthalein Method Tablet Test Procedure 0c006 42 AC3032T Hardness Total High Range Metallphthalein Method Tablet Test Procedure 006 43 AC2030 Hydrazine Dimethylamino benzaldehyde Method Powder Test Procedure cccceseeserteees 44 Iron Digestion Method svcr sicche ck edevSendateevel haves a a a bevva eae eeeels Pov a avon eae 45 AC2078 Iron Low Range Ill Soluble TPTZ Method Tablet Test Procedure cccsessessseceeeeessessnaeees 46 AC4P78 Iron II amp III Soluble 1 10 Phenanthroline Method Powder Test Procedure nacesce 47 AC4P79 Iron Total TPTZ Method Powder Test Procedure sssseserererererrrererrrererererrrrrererrrererrrerrreree 48 AC2055 Manganese Formaldoxime Method Tablet Test Procedure cccssscccccecsssessnteceeeesesssessaeees 49 AC4P54 Manganese Low Range PAN Method Powder amp Liquid Test Procedure cccccccccscesssssseees 50 AC4P55 Manganese High Range Periodate Oxidation Method Powder Test Procedure 0 006 51 AC4P42 Molybdate Molybdenum Mercaptoacetic Acid Method Powder Test Procedure 52 ACROO7 Nitrate as Nitrogen N Chromotropic Acid Method Reaction Tube Test Procedure 53 AC2046 Nitrite as Nitrogen N Diazotization Azo Method Tablet Test Procedure
85. rtho phosphate ions by heating with acid and persulfate The amount of organically combined phosphates can be calculated mg L phosphate organic mg L phosphate total mg L phosphate acid hydrolyzable Phosphate ortho Phosphorus reactive Page 64 AC2096 Phosphate Ortho High Range Vanadomolybdate Method Tablet Test Procedure 1 80 mg L PO 1 2 9 Load and run the AC2096 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Phosphate HR P1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Add one Phosphate HR P2 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved Wipe the exterior of the vial Wait for a reaction period of 10 minutes 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L ortho phosphate Notes For samples under 5 mg L PO it is recommended to analyze the sample using the AC2095 method Only
86. s are present a cloudy solution will appear Page 76 AC2016 Sulfide Methylene Blue Method Tablet Test Procedure 0 04 0 5 mg LS 1 2 9 Load and run the AC2016 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Sulfide No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Add one Sulfide No 2 Tablet straight from the foil to the same vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved Wipe the exterior of the vial Wait for a reaction period of 10 minutes 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L sulfide Notes The tablets must be added in the correct sequence Chlorine and other oxidizing agents which react with DPD do not interfere with the test To avoid loss of sulfide collect the sample carefully with a minimum of aeration It is essential to test the sample immediately after collection The sample temperature should be 20 C A
87. solved Wipe the exterior of the vial 8 Place the vial into the holder in the sample chamber Close the sample chamber door 9 Press the Measure Sample function key to display the result in mg L total alkalinity Notes The terms total alkalinity alkalinity m m value and alkalinity to pH 4 3 are identical For accurate results exactly 10 ml of water sample must be taken for the test Page 11 AC3002P Alkalinity P Alkalinity to pH 8 2 Acid Indicator Method Tablet Test Procedure 5 500 mg L CaCO 1 Load and run the AC3002P method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Alka P Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 7 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 8 Place the vial into the holder in the sample chamber Close the sample chamber door 9 Press the Measure Sample function key to display the result in mg L total alkalinity Notes The terms alkalinity p p value and alkalinity to pH 8 2 are identical For accurate test results exactl
88. t in mg L free copper Notes For determination of total copper digestion is required Extremely acid water samples pH 2 or less must be adjusted between pH 4 and pH 6 before the reagent is added with 8 mol l potassium hydroxide solution KOH Accuracy is not affected by undissolved powder Interferences Cyanide Cyanide prevents full color development Add 0 2 ml formaldehyde to 10 ml water CN sample and wait for a reaction time of 4 minutes cyanide is masked After this perform test as described Multiply the result by 1 02 to correct the sample dilution by formaldehyde Silver If turbidity remains and turns black silver interference is likely Add 10 drops of Ag saturated potassium chloride solution to 75 ml of water sample Filtrate through a fine filter Use 10 ml of the filtered water sample to perform test Page 38 AC2098 Cyanuric Acid Melamine Method Tablet Test Procedure 5 90 mg L CyA 1 Load and run the AC2098 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Cyanuric Acid Tablet straight from the foil to the vial Crush the tablet with a cl
89. tablet with a clean stir rod Add one Manganese LR 2 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved Wipe the exterior of the vial Wait for a reaction period of 5 minutes 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L manganese Page 49 AC4P54 Manganese Low Range PAN Method Powder amp Liquid Test Procedure 0 01 0 7 mg L Mn 1 Load and run the AC4P54 method 2 Use two clean AQUAfast 24mm round vials Cat No AC2V24 3 Pour 10 ml of deionized water into the first vial this is the blank vial 4 Pour 10 ml of sample into the second vial this is the sample vial 5 Add the contents of one Ascorbic Acid Powder Pack straight from the foil to each vial Close the vials tightly with the caps and swirl or invert several times to mix the contents 6 Add 15 drops of Alkaline Cyanide Reagent Solution to each vial Add drops of the same size by holding the bottle vertically and squeezing slowly Close the vials tightly with the caps and swirl or invert several times to mix the contents 7 Add 21 drops of PAN Indicator Solution to each vial Add drops of the same size by holding the bottle vertically and squeezing slowly Close the vials tightly with the caps and swirl or in
90. te either spontaneously or during the reaction time of the test Page 55 ACD004 Nitrogen Total Low Range Persulfate Digestion Method Digestion Tube Test Procedure 0 5 25 mg L N 1 Open two TN Hydroxide LR Digestion Vials and add one TN Persulfate Reagent Power Pack straight from the foil to each vial Use a funnel to add the reagent Wipe off any persulfate reagent that may get on the lid or the tube threads 2 Add 2 ml of deionized water to the first digestion vial this is the blank 3 Add 2 ml of sample to the second digestion vial this is the sample 4 Close the vials tightly with the caps and shake the vials for at least 30 seconds to mix the contents The reagent many not dissolve completely 5 Heat the digestion vials for 30 minutes in the preheated reactor at a temperature of 100 C 6 CAUTION The vials will be hot Remove the digestion vials from the reactor and allow them to cool to room temperature 7 Open the cooled digestion vials and add one TN Reagent A Power Pack straight from the foil to each vial Use a funnel to add the reagent 8 Close the vials tightly with the caps and shake the vials for at least 15 seconds to mix the contents 9 Wait for a reaction period of 3 minutes 10 Open the digestion vials and add one TN Reagent B Power Pack straight from the foil to each vial Use a funnel to add the reagent 11 Close the vials tightly with the caps and shake the vials for at least 15 sec
91. the upright position Wait for all the solution to flow to the bottom of the vial This process is one inversion 10 inversions equal about 30 seconds Wipe the exteriors of the vials CAUTION The vials will become warm during mixing Wait for a reaction period of 5 minutes Load and run the ACD007 method Place the blank vial into the holder in the sample chamber Close the sample chamber door Page 58 19 Press the Measure Blank function key to measure the blank 20 Open the sample chamber door Remove the blank vial from the holder 21 Place the sample vial into the holder in the sample chamber Close the sample chamber door 22 Press the Measure Sample function key to display the result in mg L nitrogen Notes e Appropriate safety precautions and a good lab technique should be used during the whole procedure e Volumes for samples and blank should always be metered by using 2 ml volumetric pipettes class A e One blank is sufficient for each set of samples After taking the blank measurement it is possible to measure several samples e Itis very important to remove the vials from the reactor after exactly 30 minutes e Large quantities of nitrogen free organic compounds which are included in some water samples may reduce the effectiveness of the digestion by reacting with the persulfate reagent Samples which are well known to contents large quantities of organic compounds must be diluted and digestion and measure
92. tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the Measure Blank function key to measure the blank 5 Open the sample chamber door and remove the vial from the sample chamber 6 Add one Silica No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 7 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved 8 Wait for a reaction period of 5 minutes 9 Add one Silica No 2 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod 10 Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved Wipe the exterior of the vial 11 Wait for a reaction period of 1 minute 12 Place the vial into the holder in the sample chamber Close the sample chamber door 13 Press the Measure Sample function key to display the result in mg L silica Notes The tablets must be added in the correct sequence Page 72 AC2061 Silica Silicomolybdate Method with Phosphate Removal Tablet Test Procedure 0 05 4 mg L SiO 1 Load and run the AC2061 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door 4 Press the
93. to the holder in the sample chamber Close the sample chamber door 9 Press the Measure Blank function key to measure the blank 10 Open the sample chamber door Remove the blank vial from the holder 11 Place the reagent blank vial into the holder in the sample chamber Close the sample chamber door 12 Press the Measure Rgnt Blank function key to measure the reagent blank 13 Open the sample chamber door Remove the reagent blank vial from the holder 14 Place the sample vial into the holder in the sample chamber Close the sample chamber door 15 Press the Measure Sample function key to display the result in mg L COD Notes e Reverse color methods use a reagent that when prepared with samples deceases in color as the concentration of the species being measured in the samples increases Reverse color methods require the use of both a blank and a reagent blank The blank is a clear solution deionized water with zero absorbance The reagent blank is a mixture of the reagent and deionized water and provides a zero concentration point with the darkest color highest absorbance The color of samples prepared with the reagent will decrease as the concentration increases for this method e Run samples and blanks with the same batch of vials The blank is stable when stored in the dark and can be used for further measurements with vials of the same batch Page 32 Do not place the hot vials in the sample chamber Cool the vials t
94. tration within the method range and near the expected sample concentration Refer to the specific reagent chemistry section for detailed instructions Press the Calculate 1pt Adjust function key Use the numeric keypad to enter the concentration of the standard and press the Enter key Wipe the exterior of the blank vial and place the blank vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key Open the sample chamber door and remove the vial from the sample chamber For reverse color methods only a Wipe the exterior of the reagent blank vial and place the reagent blank vial into the holder in the sample chamber Close the sample chamber door b Press the Measure Rgnt Blank function key c Open the sample chamber door and remove the vial from the sample chamber Wipe the exterior of the standard vial and place the standard vial into the holder in the sample chamber Close the sample chamber door Press the Measure Standard function key Open the sample chamber door and remove the vial from the sample chamber Page 9 Using 13 The display will show the standard concentration that was entered in step 5 the measured concentration without a correction and the calculated adjustment correction factor 14 Press the Accept function key if the calculated adjustment correction factor is acceptable Typically a correction factor of 0 7 to 1 3 within 30 is accept
95. ts function key Press the A V keys to highlight Load internal test and press the Enter key Press the A W keys to highlight the appropriate test method and press the Load Test function key Press the Run Test function key Running a Test Method from the AquaMate SmartStart Menu 1 From the initial measurement screen press the Test key to access the test types Press the SmartStart function key Press the A V keys to highlight the appropriate test method and press the Load Test function key Press the Run Test function key Page 8 Using the One Point Adjustment Calibration Feature Use the one point adjustment feature prior to running a preprogrammed test method to ensure accurate measurements This procedure is recommended each time a new batch of reagents are used to account for variations in batch to batch reagent composition and other factors that affect the accuracy of a method with a fixed calibration curve When the one point adjustment feature is off no adjustment is applied when running the test and test results are calculated exactly according to the preprogrammed equation 10 11 12 Load the test method in the Water Analysis test menu If the 1pt Adjust parameter is set to Off press the A W keys to highlight 1pt Adjust and press the Enter key to set the parameter to On Prepare a blank reagent blank reverse color methods only and calibration standard with a known concen
96. ubstance Interference Level Aluminum greater than 200 mg L Arsenate at any level Chromium greater than 100 mg L Copper greater than 10 mg L Iron greater than 100 mg L Nickel greater than 300 mg L Silica Silicium dioxide greater than 50 mg L Silicate greater than 10 mg L Sulfide at any level Zinc greater than 80 mg L Page 70 ACRO95 Phosphate Ortho Ascorbic Acid Method Reaction Tube Test Procedure 0 06 5 mg L PO 1 2 8 9 Load and run the ACRO95 method Open one white capped 16mm PO4 P Dilution Tube and add 5 ml of sample Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door Remove the vial from the holder Add one Phosphate Rgt F10 Power Pack straight from the foil to the vial Use a funnel to add the reagent Close the vial tightly with the cap and swirl the vial for 10 15 seconds to mix the contents The reagent will not completely dissolve Wipe the exterior of the vial Wait for a reaction period of 2 minutes Place the vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Sample function key to display the result in mg L ortho phosphate Notes Ortho phosphate ions react with the reagent to form an intense blue color Phosphate in organic and co
97. vert several times to mix the contents Wipe the exteriors of the vials 8 Wait for a reaction period of 2 minutes 9 Place the blank vial into the holder in the sample chamber Close the sample chamber door 10 Press the Measure Blank function key to measure the blank 11 Open the sample chamber door Remove the blank vial from the holder 12 Place the sample vial into the holder in the sample chamber Close the sample chamber door 13 Press the Measure Sample function key to display the result in mg L manganese Notes Rinse all glassware with 1 1 nitric acid solution first and then rinse with deionized water Water samples that contain more than 300 mg L CaCO hardness after adding the Ascorbic Acid Powder Pack add additionally 10 drops of Rochelle Salt Solution After addition of the Alkaline Cyanide Reagent Solution a cloudy or turbid solution may form in some water samples The turbidity should disappear after the PAN Indicator Solution is added Water samples containing more than 5 mg L iron should be allowed to react for at least 10 minutes Page 50 AC4P55 Manganese High Range Periodate Oxidation Method Powder Test Procedure 0 1 18 mg L Mn 1 Load and run the AC4P55 method 2 Filla clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial 3 Place the vial into the holder in the sample chamber Close the sample chamber door
98. y 10 ml of water sample must be taken for the test This method was developed from a volumetric procedure for the determination of alkalinity p Due to undefined conditions the deviations from the standardized method may be greater Page 12 AC2027 Aluminum Eriochrome Cyanine R Method Tablet Test Procedure 0 01 0 3 mg LAl 1 2 9 Load and run the AC2027 method Fill a clean AQUAfast 24mm round vial Cat No AC2V24 with 10 ml of sample Close the vial tightly with the cap Wipe the exterior of the vial Place the vial into the holder in the sample chamber Close the sample chamber door Press the Measure Blank function key to measure the blank Open the sample chamber door and remove the vial from the sample chamber Add one Aluminum No 1 Tablet straight from the foil to the vial Crush the tablet with a clean stir rod and mix well to dissolve the tablet completely Add one Aluminum No 2 Tablet straight from the foil to the same vial Crush the tablet with a clean stir rod and mix well to dissolve the tablet completely Close the vial tightly with the cap and swirl or invert several times to mix the contents Wipe the exterior of the vial Wait for a reaction period of 5 minutes 10 Place the vial into the holder in the sample chamber Close the sample chamber door 11 Press the Measure Sample function key to display the result in mg L aluminum Notes Before use clean the vials and the measuring beake
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